############################################################################## # # # 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_I _database_code_depnum_ccdc_archive 'CCDC 1509626' _audit_creation_method 'SHELXL-2014/7' _journal_date_recd_electronic 2016-08-31 _journal_date_accepted 2016-10-13 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2016 _journal_volume 72 _journal_issue 11 _journal_page_first 1587 _journal_page_last 1589 _journal_paper_category GO _journal_paper_doi 10.1107/S2056989016016273 _journal_coeditor_code HB7614 _publ_contact_author_name 'Hidehiro Uekusa' _publ_contact_author_address ; Department of Chemistry and Materials Science, Tokyo Institute of Technology, Ookayama 2-12-1, Meguro-ku, Tokyo 152-8551, Japan ; _publ_contact_author_email 'uekusa@cms.titech.ac.jp' _publ_contact_author_fax '+81-3-5734-3529' _publ_contact_author_phone '+81-3-5734-3529' _publ_section_title ; Crystal structure of olivetolic acid: a natural product from Cetrelia sanguinea (Schaer.) ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Ismed, Friardi' . ; The Laboratory of Natural Resource of Sumatra (LBS) and Faculty of Pharmacy, Andalas University, 26163 Padang, Indonesia ; 'Farhan, Aulia' . ; The Laboratory of Natural Resource of Sumatra (LBS) and Faculty of Pharmacy, Andalas University, 26163 Padang, Indonesia ; 'Bakhtiar, Amri' . ; The Laboratory of Natural Resource of Sumatra (LBS) and Faculty of Pharmacy, Andalas University, 26163 Padang, Indonesia ; 'Zaini, Erizal' . ; The Laboratory of Natural Resource of Sumatra (LBS) and Faculty of Pharmacy, Andalas University, 26163 Padang, Indonesia ; 'Nugraha, Yuda Prasetya' . ; Department of Chemistry and Materials Science, Tokyo Institute of Technology, Ookayama 2-12-1, Meguro-ku, Tokyo 152-8551, Japan ; 'Dwichandra Putra, Okky' . ; Department of Chemistry and Materials Science, Tokyo Institute of Technology, Ookayama 2-12-1, Meguro-ku, Tokyo 152-8551, Japan ; 'Uekusa, Hidehiro' . ; Department of Chemistry and Materials Science, Tokyo Institute of Technology, Ookayama 2-12-1, Meguro-ku, Tokyo 152-8551, Japan ; _publ_section_synopsis ; The packing in olivetolic acid is similar to that in resorcinolic acid. ; _chemical_name_systematic ; 2,4-Dihydroxy-6-pentylbenzoic acid ; _chemical_name_common 'olivetolic acid' _chemical_formula_moiety 'C12 H16 O4' _chemical_formula_sum 'C12 H16 O4' _chemical_formula_iupac 'C12 H16 O4' _chemical_formula_weight 224.25 _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 monoclinic _space_group_name_H-M_alt 'P 21/n' _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 14.2527(8) _cell_length_b 4.7524(3) _cell_length_c 17.6489(11) _cell_angle_alpha 90 _cell_angle_beta 103.538(4) _cell_angle_gamma 90 _cell_volume 1162.22(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12628 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 68.2 _cell_measurement_temperature 173(2) _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.121 _exptl_crystal_size_mid 0.101 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (ABSCOR; Higashi, 1995) ; _shelx_estimated_absorpt_T_min 0.910 _shelx_estimated_absorpt_T_max 0.925 _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.924 _diffrn_ambient_temperature 173(2) _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54186 _diffrn_measurement_device_type 'RIGAKU R-AXIS RAPID II' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 10.0 _diffrn_reflns_number 12627 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_theta_min 3.600 _diffrn_reflns_theta_max 68.231 _diffrn_reflns_theta_full 67.686 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _refine_special_details ? _reflns_number_total 2087 _reflns_number_gt 1762 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_gt 0.1293 _refine_ls_wR_factor_ref 0.1359 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_number_reflns 2087 _refine_ls_number_parameters 158 _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^)+(0.0808P)^2^+0.1676P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary none _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.294 _refine_diff_density_min -0.183 _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' 0.0181 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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; PROCESS-AUTO (Rigaku, 1998) ; _computing_cell_refinement ; PROCESS-AUTO (Rigaku, 1998) ; _computing_data_reduction ; PROCESS-AUTO (Rigaku, 1998) ; _computing_structure_solution ; SHELXS2014 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_molecular_graphics ? _computing_publication_material ; SHELXL2014 (Sheldrick, 2015) ; 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 O O1 0.38939(8) 0.5564(2) 0.16723(7) 0.0419(3) Uani d 1 . . C C1 0.32068(11) 0.2528(3) 0.06446(9) 0.0333(4) Uani d 1 . . H H1 0.3726 0.2983 0.0413 0.040 Uiso calc 1 . . H H1A 0.3901(15) 0.588(4) 0.2194(14) 0.060(6) Uiso d 1 . . O O2 0.09864(8) 0.0870(2) 0.17140(6) 0.0348(3) Uani d 1 . . H H2 0.0574(18) -0.059(5) 0.1389(14) 0.079(7) Uiso d 1 . . C C2 0.31656(11) 0.3787(3) 0.13488(9) 0.0321(4) Uani d 1 . . C C3 0.24081(11) 0.3235(3) 0.16913(9) 0.0317(4) Uani d 1 . . H H3 0.2370 0.4140 0.2163 0.038 Uiso calc 1 . . O O3 0.03156(7) -0.2603(2) 0.06590(6) 0.0345(3) Uani d 1 . . C C4 0.17037(10) 0.1334(3) 0.13338(8) 0.0286(4) Uani d 1 . . O O4 0.10317(8) -0.3497(2) -0.03022(6) 0.0378(3) Uani d 1 . . H H4 0.0556(18) -0.491(6) -0.0410(14) 0.080(7) Uiso d 1 . . C C5 0.17377(10) -0.0040(3) 0.06311(8) 0.0275(3) Uani d 1 . . C C6 0.25149(10) 0.0639(3) 0.02743(8) 0.0287(4) Uani d 1 . . C C7 0.25914(11) -0.0625(3) -0.04994(9) 0.0336(4) Uani d 1 . . H H7A 0.1981 -0.0241 -0.0887 0.040 Uiso calc 1 . . H H7B 0.2648 -0.2692 -0.0435 0.040 Uiso calc 1 . . C C8 0.34233(11) 0.0400(3) -0.08352(9) 0.0368(4) Uani d 1 . . H H8A 0.3396 0.2476 -0.0879 0.044 Uiso calc 1 . . H H8B 0.4042 -0.0109 -0.0474 0.044 Uiso calc 1 . . C C9 0.33918(12) -0.0863(3) -0.16340(9) 0.0374(4) Uani d 1 . . H H9A 0.3426 -0.2939 -0.1587 0.045 Uiso calc 1 . . H H9B 0.2768 -0.0377 -0.1992 0.045 Uiso calc 1 . . C C10 0.42080(13) 0.0161(4) -0.19841(10) 0.0454(5) Uani d 1 . . H H10A 0.4185 0.2240 -0.2015 0.054 Uiso calc 1 . . H H10B 0.4831 -0.0373 -0.1632 0.054 Uiso calc 1 . . C C11 0.41710(14) -0.1014(4) -0.27894(11) 0.0516(5) Uani d 1 . . H H11A 0.4215 -0.3071 -0.2762 0.077 Uiso calc 1 . . H H11B 0.4713 -0.0265 -0.2982 0.077 Uiso calc 1 . . H H11C 0.3562 -0.0466 -0.3145 0.077 Uiso calc 1 . . C C12 0.09866(10) -0.2112(3) 0.03296(8) 0.0283(3) Uani 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 O1 0.0439(6) 0.0464(7) 0.0368(7) -0.0190(5) 0.0123(5) -0.0070(5) C1 0.0333(8) 0.0361(8) 0.0328(8) -0.0048(6) 0.0128(6) 0.0029(6) O2 0.0348(6) 0.0417(6) 0.0319(6) -0.0064(5) 0.0160(5) -0.0050(5) C2 0.0332(7) 0.0317(7) 0.0307(8) -0.0051(6) 0.0061(6) 0.0033(6) C3 0.0372(8) 0.0312(8) 0.0270(8) -0.0014(6) 0.0081(7) -0.0017(6) O3 0.0350(6) 0.0378(6) 0.0342(6) -0.0084(4) 0.0151(5) -0.0036(5) C4 0.0300(7) 0.0292(7) 0.0278(8) 0.0010(6) 0.0094(6) 0.0048(6) O4 0.0409(6) 0.0421(6) 0.0350(6) -0.0140(5) 0.0182(5) -0.0108(5) C5 0.0297(7) 0.0273(7) 0.0267(8) -0.0001(6) 0.0089(6) 0.0041(6) C6 0.0309(7) 0.0285(7) 0.0271(8) -0.0006(6) 0.0076(6) 0.0054(6) C7 0.0363(8) 0.0352(8) 0.0327(9) -0.0053(6) 0.0148(7) 0.0004(6) C8 0.0381(8) 0.0414(9) 0.0348(9) -0.0073(7) 0.0161(7) -0.0018(7) C9 0.0399(8) 0.0406(9) 0.0362(9) -0.0048(7) 0.0179(7) -0.0009(7) C10 0.0467(9) 0.0509(10) 0.0457(10) -0.0076(8) 0.0253(8) -0.0038(8) C11 0.0581(11) 0.0594(11) 0.0462(11) -0.0007(9) 0.0299(9) 0.0023(9) C12 0.0310(7) 0.0279(7) 0.0271(7) -0.0004(6) 0.0090(6) 0.0034(6) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C2 . 1.3563(18) ? O1 H1A . 0.93(2) ? C1 C6 . 1.380(2) ? C1 C2 . 1.393(2) ? C1 H1 . 0.9500 ? O2 C4 . 1.3657(16) ? O2 H2 . 1.00(3) ? C2 C3 . 1.380(2) ? C3 C4 . 1.388(2) ? C3 H3 . 0.9500 ? O3 C12 . 1.2520(16) ? C4 C5 . 1.412(2) ? O4 C12 . 1.3094(17) ? O4 H4 . 0.94(3) ? C5 C6 . 1.4333(19) ? C5 C12 . 1.460(2) ? C6 C7 . 1.519(2) ? C7 C8 . 1.5243(19) ? C7 H7A . 0.9900 ? C7 H7B . 0.9900 ? C8 C9 . 1.523(2) ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? C9 C10 . 1.519(2) ? C9 H9A . 0.9900 ? C9 H9B . 0.9900 ? C10 C11 . 1.516(2) ? C10 H10A . 0.9900 ? C10 H10B . 0.9900 ? C11 H11A . 0.9800 ? C11 H11B . 0.9800 ? C11 H11C . 0.9800 ? 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 C2 O1 H1A . . 110.4(13) ? C6 C1 C2 . . 121.82(13) ? C6 C1 H1 . . 119.1 ? C2 C1 H1 . . 119.1 ? C4 O2 H2 . . 103.8(14) ? O1 C2 C3 . . 122.28(14) ? O1 C2 C1 . . 117.06(13) ? C3 C2 C1 . . 120.66(14) ? C2 C3 C4 . . 118.78(14) ? C2 C3 H3 . . 120.6 ? C4 C3 H3 . . 120.6 ? O2 C4 C3 . . 115.27(13) ? O2 C4 C5 . . 122.70(13) ? C3 C4 C5 . . 122.02(13) ? C12 O4 H4 . . 110.8(15) ? C4 C5 C6 . . 118.06(13) ? C4 C5 C12 . . 117.30(12) ? C6 C5 C12 . . 124.61(13) ? C1 C6 C5 . . 118.60(13) ? C1 C6 C7 . . 119.31(13) ? C5 C6 C7 . . 122.09(13) ? C6 C7 C8 . . 116.69(13) ? C6 C7 H7A . . 108.1 ? C8 C7 H7A . . 108.1 ? C6 C7 H7B . . 108.1 ? C8 C7 H7B . . 108.1 ? H7A C7 H7B . . 107.3 ? C9 C8 C7 . . 112.14(13) ? C9 C8 H8A . . 109.2 ? C7 C8 H8A . . 109.2 ? C9 C8 H8B . . 109.2 ? C7 C8 H8B . . 109.2 ? H8A C8 H8B . . 107.9 ? C10 C9 C8 . . 113.00(13) ? C10 C9 H9A . . 109.0 ? C8 C9 H9A . . 109.0 ? C10 C9 H9B . . 109.0 ? C8 C9 H9B . . 109.0 ? H9A C9 H9B . . 107.8 ? C11 C10 C9 . . 113.66(15) ? C11 C10 H10A . . 108.8 ? C9 C10 H10A . . 108.8 ? C11 C10 H10B . . 108.8 ? C9 C10 H10B . . 108.8 ? H10A C10 H10B . . 107.7 ? C10 C11 H11A . . 109.5 ? C10 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C10 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? O3 C12 O4 . . 119.78(13) ? O3 C12 C5 . . 122.09(13) ? O4 C12 C5 . . 118.12(12) ? 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 C6 C1 C2 O1 . . . . 178.54(13) ? C6 C1 C2 C3 . . . . -1.8(2) ? O1 C2 C3 C4 . . . . -178.34(14) ? C1 C2 C3 C4 . . . . 2.0(2) ? C2 C3 C4 O2 . . . . 179.08(12) ? C2 C3 C4 C5 . . . . -0.2(2) ? O2 C4 C5 C6 . . . . 178.97(12) ? C3 C4 C5 C6 . . . . -1.8(2) ? O2 C4 C5 C12 . . . . -2.5(2) ? C3 C4 C5 C12 . . . . 176.76(13) ? C2 C1 C6 C5 . . . . -0.3(2) ? C2 C1 C6 C7 . . . . 179.01(13) ? C4 C5 C6 C1 . . . . 2.0(2) ? C12 C5 C6 C1 . . . . -176.44(13) ? C4 C5 C6 C7 . . . . -177.26(12) ? C12 C5 C6 C7 . . . . 4.3(2) ? C1 C6 C7 C8 . . . . -2.5(2) ? C5 C6 C7 C8 . . . . 176.74(13) ? C6 C7 C8 C9 . . . . -176.33(13) ? C7 C8 C9 C10 . . . . 179.26(14) ? C8 C9 C10 C11 . . . . -178.38(15) ? C4 C5 C12 O3 . . . . 2.4(2) ? C6 C5 C12 O3 . . . . -179.11(13) ? C4 C5 C12 O4 . . . . -176.99(12) ? C6 C5 C12 O4 . . . . 1.5(2) ? 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 O1 H1A O2 2 0.93(2) 1.90(2) 2.8168(16) 169.6(19) O2 H2 O3 . 1.00(3) 1.58(3) 2.5043(14) 152(2) O4 H4 O3 3_545 0.94(3) 1.70(3) 2.6368(15) 177(2) _shelx_hkl_file ; 0 0 2 604.66 22.90 0 0 2 582.95 21.44 0 0 2 587.67 20.41 0 0 -2 595.94 22.00 0 0 -2 618.94 21.57 0 0 -2 592.23 21.80 0 0 -2 588.60 21.60 0 0 -2 613.58 22.42 0 0 3 -0.01 0.37 0 0 3 0.07 0.39 0 0 3 -0.10 0.05 0 0 -3 0.39 0.17 0 0 -3 0.03 0.05 0 0 -3 0.03 0.03 0 0 -3 -0.00 0.21 0 0 -3 0.00 0.20 0 0 4 81.65 5.08 0 0 4 98.66 2.51 0 0 4 78.81 4.82 0 0 -4 83.55 3.53 0 0 -4 94.44 2.31 0 0 -4 84.67 3.70 0 0 -4 83.10 1.96 0 0 -4 80.75 3.21 0 0 5 -0.17 0.36 0 0 5 -0.01 0.03 0 0 5 0.02 0.34 0 0 -5 -0.03 0.22 0 0 -5 -0.01 0.20 0 0 -5 0.02 0.03 0 0 -5 0.00 0.18 0 0 6 679.79 29.46 0 0 6 700.72 30.22 0 0 -6 750.09 31.40 0 0 -6 757.71 31.88 0 0 -6 742.62 30.97 0 0 7 0.06 0.51 0 0 7 -0.05 0.50 0 0 -7 0.08 0.32 0 0 -7 0.05 0.26 0 0 -7 0.08 0.30 0 0 8 2499.32 142.60 0 0 8 2488.35 142.21 0 0 -8 2514.15 142.33 0 0 -8 2499.81 141.78 0 0 -8 2445.80 139.44 0 0 9 0.01 0.27 0 0 9 0.07 0.46 0 0 9 0.09 0.47 0 0 9 0.04 0.29 0 0 -9 -0.03 0.25 0 0 10 945.70 44.92 0 0 10 872.32 41.21 0 0 10 882.30 42.20 0 0 10 883.44 41.49 0 0 -10 906.20 41.89 0 0 11 -0.08 0.36 0 0 11 0.02 0.62 0 0 11 0.03 0.35 0 0 11 -0.39 0.35 0 0 -11 -0.04 0.20 0 0 12 0.64 0.53 0 0 12 0.61 0.52 0 0 -12 0.67 0.29 0 0 13 0.17 0.47 0 0 13 0.13 0.46 0 0 -13 0.26 0.39 0 0 14 3.58 0.91 0 0 14 3.29 0.91 0 0 -14 3.28 0.87 0 0 15 -0.10 0.82 0 0 15 -0.07 0.84 0 0 -15 0.31 0.29 0 0 16 10.02 1.27 0 0 16 10.82 1.34 0 0 -16 7.67 1.16 0 0 17 0.31 0.59 0 0 17 0.00 0.56 0 0 -17 0.00 0.19 0 0 18 0.01 1.15 0 0 18 2.17 1.18 0 0 -18 2.79 0.41 0 0 19 0.01 0.38 0 0 19 -0.05 0.39 0 1 0 0.21 0.44 0 1 0 0.01 0.23 0 -1 0 0.08 0.24 0 1 0 0.14 0.42 0 -1 0 0.11 0.42 0 1 0 0.05 0.23 0 -1 0 0.02 0.42 0 1 0 -0.01 0.16 0 -1 0 0.16 0.43 0 1 1 1315.82 61.27 0 1 1 1212.45 57.60 0 -1 1 1331.55 62.82 0 1 1 1358.31 67.24 0 -1 1 1409.00 66.05 0 1 1 1333.19 66.45 0 -1 1 1340.53 67.40 0 -1 1 1388.06 69.15 0 -1 -1 1316.31 65.22 0 1 -1 1352.83 63.57 0 -1 -1 1289.25 63.68 0 1 -1 1356.51 64.95 0 -1 -1 1414.92 66.55 0 1 -1 1397.99 64.74 0 -1 -1 1347.47 63.17 0 1 -1 1325.62 63.61 0 1 -1 1310.29 61.05 0 1 2 699.04 29.37 0 -1 2 712.28 30.57 0 1 2 696.63 27.71 0 -1 2 653.24 26.00 0 1 2 681.89 28.77 0 -1 2 693.95 29.67 0 1 2 674.23 27.91 0 -1 2 705.07 28.90 0 -1 -2 673.07 29.71 0 1 -2 719.87 32.94 0 -1 -2 697.03 25.72 0 1 -2 698.10 27.79 0 1 -2 732.70 30.22 0 1 -2 717.93 30.76 0 -1 -2 706.45 28.83 0 1 -2 699.42 28.64 0 -1 -2 683.38 27.19 0 -1 -2 708.41 31.51 0 1 3 20.60 1.39 0 -1 3 21.72 0.72 0 1 3 21.74 0.73 0 1 3 21.21 1.38 0 -1 3 21.16 1.68 0 1 3 22.01 0.99 0 -1 3 23.65 1.69 0 -1 3 22.76 0.99 0 -1 -3 21.64 0.72 0 1 -3 22.69 1.68 0 1 -3 24.41 1.34 0 1 -3 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1.95 0 2 -3 54.29 2.88 0 2 -3 54.97 2.95 0 -2 -3 54.38 2.55 0 -2 -3 51.05 1.72 0 2 -3 52.57 2.26 0 2 4 17.39 2.24 0 -2 4 17.94 2.57 0 2 4 19.08 1.09 0 2 4 17.76 1.06 0 -2 4 18.30 2.64 0 2 4 18.16 1.49 0 -2 4 17.01 0.94 0 -2 4 16.92 0.68 0 -2 -4 17.58 1.28 0 -2 -4 18.17 1.33 0 2 -4 17.25 1.72 0 2 -4 18.10 0.79 0 2 -4 17.60 1.07 0 2 -4 17.69 1.68 0 -2 -4 16.97 0.69 0 2 -4 16.79 1.07 0 -2 -4 17.37 0.96 0 2 5 146.62 5.86 0 2 5 152.32 4.94 0 -2 5 139.09 5.93 0 2 5 143.74 5.79 0 -2 5 149.02 5.74 0 2 5 149.22 5.45 0 -2 5 142.58 4.87 0 -2 5 139.03 7.47 0 -2 -5 143.34 6.48 0 2 -5 148.95 6.44 0 -2 -5 146.81 5.16 0 -2 -5 143.95 4.93 0 -2 -5 142.88 6.30 0 2 -5 147.23 5.52 0 2 -5 139.24 4.59 0 2 -5 142.97 6.26 0 2 -5 137.16 5.31 0 2 -5 149.70 5.46 0 2 6 123.36 5.02 0 2 6 115.24 4.76 0 -2 6 123.22 5.32 0 -2 6 120.46 4.61 0 -2 6 125.07 5.21 0 -2 6 117.70 3.78 0 -2 6 122.88 6.73 0 -2 6 122.91 6.54 0 2 6 120.42 4.90 0 2 -6 122.62 4.41 0 2 -6 123.66 5.03 0 2 -6 101.40 3.26 0 -2 -6 128.01 4.81 0 -2 -6 126.27 4.71 0 -2 -6 121.51 4.58 0 2 -6 125.74 4.83 0 -2 -6 121.15 3.88 0 -2 7 32.22 2.15 0 -2 7 32.27 2.02 0 2 7 30.49 1.82 0 -2 7 32.13 2.12 0 -2 7 32.74 1.27 0 -2 7 33.12 2.29 0 2 7 32.17 1.77 0 2 7 29.70 1.83 0 2 -7 32.02 1.78 0 -2 -7 34.40 2.40 0 2 -7 29.89 1.36 0 -2 -7 31.45 1.22 0 -2 -7 34.68 2.55 0 2 -7 32.03 1.73 0 -2 8 20.78 1.72 0 -2 8 17.94 1.03 0 -2 8 19.72 1.70 0 2 8 19.04 0.94 0 -2 8 19.91 1.80 0 2 8 18.64 2.11 0 2 8 18.12 2.05 0 -2 8 20.71 2.85 0 2 -8 20.09 1.48 0 2 -8 19.51 1.28 0 2 -8 19.40 1.38 0 -2 -8 17.79 1.03 0 -2 -8 20.24 1.35 0 -2 -8 20.11 1.25 0 -2 9 7.91 0.67 0 -2 9 9.67 1.38 0 2 9 9.67 1.06 0 2 9 10.36 1.05 0 -2 9 8.51 1.48 0 -2 -9 8.09 0.68 0 2 -9 8.29 0.60 0 2 -9 8.21 1.16 0 -2 -9 9.07 0.87 0 -2 -9 9.17 0.95 0 2 10 27.73 1.85 0 2 10 28.25 1.80 0 -2 10 28.35 3.67 0 -2 10 29.64 3.42 0 2 -10 28.86 2.09 0 2 11 70.91 3.47 0 -2 11 71.55 3.86 0 2 11 69.02 3.29 0 -2 11 71.47 3.77 0 2 -11 65.28 3.69 0 2 12 16.51 2.28 0 -2 12 17.60 1.86 0 2 12 16.50 1.58 0 -2 12 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3 0.69 0.44 17 0 -7 0.81 0.46 17 0 -7 0.48 0.30 -17 0 7 0.28 0.30 17 0 -6 0.01 0.30 17 0 -6 -0.06 0.21 -17 0 6 -0.02 0.21 17 0 -5 0.23 0.33 17 0 -5 -0.18 0.43 -17 0 5 0.08 0.43 17 0 -4 0.15 0.26 17 0 -4 -0.10 0.26 -17 0 4 0.12 0.41 17 0 -3 0.14 0.16 17 0 -3 0.13 0.31 -17 0 3 0.16 0.31 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 43872 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL F01070 - EXOR New: P21/n CELL 1.54186 14.2527 4.7524 17.6489 90.000 103.538 90.000 ZERR 4 0.0008 0.0003 0.0011 0.000 0.004 0.000 LATT 1 SYMM 0.50000 - X , 0.50000 + Y , 0.50000 - Z SFAC C H O UNIT 48 64 16 SIZE 0.121 0.101 0.100 TEMP -100 CONF HTAB BOND $H ACTA LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! L.S. 5 FMAP 2 PLAN -20 ACTA EQIV $1 -x, -y-1, -z EQIV $2 -x+1/2, y+1/2, -z+1/2 HTAB O1 O2_$2 HTAB O2 O3 HTAB O4 O3_$1 OMIT 8 1 9 CONF REM RESI 0 WGHT 0.080800 0.167600 FVAR 0.56030 O1 3 0.389393 0.556395 0.167228 11.00000 0.04388 0.04644 = 0.03682 -0.00700 0.01229 -0.01903 C1 1 0.320684 0.252847 0.064462 11.00000 0.03334 0.03610 = 0.03281 0.00294 0.01276 -0.00485 AFIX 43 H1 2 0.372569 0.298336 0.041287 11.00000 -1.20000 AFIX 0 H1A 2 0.390133 0.588332 0.219422 11.00000 0.05970 O2 3 0.098637 0.086957 0.171396 11.00000 0.03482 0.04172 = 0.03187 -0.00501 0.01598 -0.00637 H2 2 0.057357 -0.059445 0.138909 11.00000 0.07885 C2 1 0.316558 0.378668 0.134879 11.00000 0.03324 0.03168 = 0.03073 0.00328 0.00614 -0.00507 C3 1 0.240814 0.323487 0.169129 11.00000 0.03724 0.03122 = 0.02700 -0.00171 0.00811 -0.00136 AFIX 43 H3 2 0.236974 0.413986 0.216304 11.00000 -1.20000 AFIX 0 O3 3 0.031562 -0.260345 0.065899 11.00000 0.03499 0.03780 = 0.03416 -0.00356 0.01507 -0.00838 C4 1 0.170368 0.133364 0.133380 11.00000 0.03003 0.02924 = 0.02775 0.00476 0.00940 0.00099 O4 3 0.103175 -0.349685 -0.030220 11.00000 0.04095 0.04208 = 0.03502 -0.01083 0.01821 -0.01398 H4 2 0.055632 -0.491054 -0.041026 11.00000 0.07994 C5 1 0.173772 -0.004033 0.063108 11.00000 0.02965 0.02734 = 0.02673 0.00412 0.00886 -0.00006 C6 1 0.251490 0.063946 0.027430 11.00000 0.03094 0.02849 = 0.02710 0.00545 0.00755 -0.00063 C7 1 0.259140 -0.062518 -0.049942 11.00000 0.03625 0.03522 = 0.03271 0.00042 0.01483 -0.00526 AFIX 23 H7A 2 0.198050 -0.024064 -0.088672 11.00000 -1.20000 H7B 2 0.264845 -0.269220 -0.043527 11.00000 -1.20000 AFIX 0 C8 1 0.342333 0.039983 -0.083521 11.00000 0.03807 0.04136 = 0.03481 -0.00176 0.01612 -0.00729 AFIX 23 H8A 2 0.339566 0.247649 -0.087902 11.00000 -1.20000 H8B 2 0.404234 -0.010930 -0.047393 11.00000 -1.20000 AFIX 0 C9 1 0.339181 -0.086319 -0.163399 11.00000 0.03989 0.04062 = 0.03621 -0.00087 0.01794 -0.00482 AFIX 23 H9A 2 0.342617 -0.293856 -0.158724 11.00000 -1.20000 H9B 2 0.276768 -0.037671 -0.199151 11.00000 -1.20000 AFIX 0 C10 1 0.420800 0.016057 -0.198412 11.00000 0.04674 0.05088 = 0.04573 -0.00376 0.02531 -0.00756 AFIX 23 H10A 2 0.418452 0.224030 -0.201492 11.00000 -1.20000 H10B 2 0.483105 -0.037282 -0.163238 11.00000 -1.20000 AFIX 0 C11 1 0.417099 -0.101403 -0.278941 11.00000 0.05809 0.05936 = 0.04624 0.00227 0.02985 -0.00071 AFIX 137 H11A 2 0.421469 -0.307100 -0.276214 11.00000 -1.50000 H11B 2 0.471257 -0.026466 -0.298166 11.00000 -1.50000 H11C 2 0.356179 -0.046559 -0.314488 11.00000 -1.50000 AFIX 0 C12 1 0.098661 -0.211173 0.032962 11.00000 0.03099 0.02789 = 0.02712 0.00336 0.00902 -0.00037 HKLF 4 REM F01070 - EXOR New: P21/n REM R1 = 0.0446 for 1762 Fo > 4sig(Fo) and 0.0497 for all 2087 data REM 158 parameters refined using 0 restraints END WGHT 0.0808 0.1676 REM Instructions for potential hydrogen bonds HTAB O1 O2_$2 HTAB O2 O3 HTAB O4 O3_$1 REM Highest difference peak 0.294, deepest hole -0.183, 1-sigma level 0.051 Q1 1 0.1767 0.0477 0.0757 11.00000 0.05 0.29 Q2 1 0.2163 -0.0305 0.0572 11.00000 0.05 0.28 Q3 1 0.2998 -0.0220 -0.0596 11.00000 0.05 0.24 Q4 1 0.3399 -0.0385 -0.1246 11.00000 0.05 0.21 Q5 1 0.2580 -0.0349 -0.0047 11.00000 0.05 0.19 Q6 1 0.2662 0.3810 0.1460 11.00000 0.05 0.19 Q7 1 0.3815 -0.0362 -0.1831 11.00000 0.05 0.18 Q8 1 0.0972 -0.2649 0.0778 11.00000 0.05 0.18 Q9 1 0.2244 0.1844 0.1552 11.00000 0.05 0.17 Q10 1 0.1813 0.1706 0.2013 11.00000 0.05 0.16 Q11 1 0.0618 -0.4075 0.0787 11.00000 0.05 0.16 Q12 1 0.1566 -0.3192 -0.0364 11.00000 0.05 0.16 Q13 1 0.3940 0.2474 -0.0582 11.00000 0.05 0.16 Q14 1 0.0992 -0.2625 -0.0400 11.00000 0.05 0.15 Q15 1 0.1063 -0.3375 0.0136 11.00000 0.05 0.15 Q16 1 0.1045 -0.3140 -0.0751 11.00000 0.05 0.15 Q17 1 0.4752 0.1454 -0.1743 11.00000 0.05 0.14 Q18 1 0.2417 -0.2318 -0.0631 11.00000 0.05 0.14 Q19 1 0.1375 -0.0854 0.1962 11.00000 0.05 0.14 Q20 1 0.4231 0.1481 -0.0454 11.00000 0.05 0.13 ; _shelx_res_checksum 39073