############################################################################## # # # 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_1 _audit_creation_method ; Olex2 1.2 (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _journal_data_validation_number ? _journal_date_recd_electronic 2018-10-31 _journal_date_accepted 2018-11-16 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2018 _journal_volume 74 _journal_issue 12 _journal_page_first 1872 _journal_page_last 1877 _journal_paper_category GO _journal_paper_doi 10.1107/S2056989018016316 _journal_coeditor_code LH5885 _publ_contact_author_name ; R. Sausa R. Sausa ; _publ_contact_author_address 'ARL' _publ_contact_author_email rosario.c.sausa.civ@mail.mil _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; Synthesis and crystal structures of 5,5'-(propane-2,2-diyl)bis(2-hydroxybenzaldehyde) and 5,5'-(propane-2,2-diyl)bis(2-hydroxyisophthalaldehyde) ; _publ_section_title_footnote . loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Sausa, Rosario C.' . ; US Army Research Laboratory, RDRL-WML-B, Aberdeen Proving Ground, MD 21005 USA ; 'Lastovickova, Dominika N.' ; Oak Ridge Institute for Science and Education (ORISE) Postdoctoral Research Fellow. ; ; US Army Research Laboratory, RDRL-WML-G, Aberdeen Proving Ground, MD 21005 USA ; 'La Scala, John J.' . ; US Army Research Laboratory, RDRL-WML-G, Aberdeen Proving Ground, MD 21005 USA ; _publ_section_synopsis ; The molecule of (1) presents a >C(CH~3~)~2~ group that bridges two nearly planar salicylaldehyde groups, each comprising a planar phenyl ring bonded with a hydroxyl and an aldehyde group. Similarly, molecule (2) presents the same bridging group, but it connects two nearly planar appendants, each comprising a phenyl ring bonded with a hydroxyl and two aldehyde groups. Compound (2) exhibits a strong visible luminescence when excited with ultraviolet radiation. ; _chemical_name_systematic ; 5,5'-(Propane-2,2-diyl)bis(2-hydroxybenzaldehyde) ; _chemical_name_common ? _chemical_formula_moiety 'C17 H16 O4' _chemical_formula_sum 'C17 H16 O4' _chemical_formula_iupac 'C17 H16 O4' _chemical_formula_weight 284.30 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.6108(6) _cell_length_b 12.0803(6) _cell_length_c 7.0946(4) _cell_angle_alpha 90 _cell_angle_beta 90.396(4) _cell_angle_gamma 90 _cell_volume 1423.59(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2453 _cell_measurement_theta_min 2.0830 _cell_measurement_theta_max 25.1790 _cell_measurement_temperature 298.00(10) _exptl_crystal_description irregular _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Bourhis et al., 2015) ; _exptl_absorpt_correction_T_min 0.86079 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 298.00(10) _diffrn_source ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_device_type 'Rigaku Oxford Diffraction SuperNova, Dualflex, EosS2' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.0945 _diffrn_reflns_number 6271 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_unetI/netI 0.0224 _diffrn_reflns_theta_min 2.085 _diffrn_reflns_theta_max 25.339 _diffrn_reflns_theta_full 25.339 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 6 _refine_special_details ? _reflns_number_total 2589 _reflns_number_gt 2036 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_gt 0.1155 _refine_ls_wR_factor_ref 0.1222 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_number_reflns 2589 _refine_ls_number_parameters 195 _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^)+(0.0347P)^2^+0.7348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.210 _refine_diff_density_min -0.198 _refine_ls_extinction_method ; SHELXL-2016/4 (Sheldrick 2016) ; _refine_ls_extinction_coef 0.0035(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 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 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' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; CrysAlisPro (Rigaku OD, 2015) ; _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2015) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2015) ; _computing_structure_solution ; ShelXT (Sheldrick, 2015a) ; _computing_structure_refinement ; ShelXL (Sheldrick, 2015b) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; 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 0.60832(9) 0.41639(19) 0.2405(3) 0.0801(6) Uani d 1 . . O O2 0.52036(10) 0.26273(16) 0.0724(3) 0.0736(5) Uani d 1 . . H H2 0.562402 0.293270 0.104187 0.110 Uiso calc 1 . . O O3 0.01645(12) 0.31117(19) 0.6564(4) 0.1054(9) Uani d 1 . . H H3 -0.028389 0.315525 0.607948 0.158 Uiso calc 1 . . O O4 -0.08657(10) 0.34768(16) 0.3823(4) 0.0932(7) Uani d 1 . . C C1 0.24872(11) 0.53761(17) 0.2163(3) 0.0461(5) Uani d 1 . . C C2 0.26777(14) 0.6426(2) 0.3303(4) 0.0721(8) Uani d 1 . . H H2A 0.218770 0.681998 0.354821 0.108 Uiso calc 1 . . H H2B 0.303523 0.688954 0.259696 0.108 Uiso calc 1 . . H H2C 0.292921 0.622372 0.447559 0.108 Uiso calc 1 . . C C3 0.21711(14) 0.5742(2) 0.0216(4) 0.0662(7) Uani d 1 . . H H3A 0.199791 0.510478 -0.048481 0.099 Uiso calc 1 . . H H3B 0.259284 0.611212 -0.045502 0.099 Uiso calc 1 . . H H3C 0.172540 0.623899 0.037436 0.099 Uiso calc 1 . . C C4 0.32352(11) 0.46576(17) 0.1856(3) 0.0411(5) Uani d 1 . . C C5 0.31596(13) 0.36340(18) 0.0949(3) 0.0482(5) Uani d 1 . . H H5 0.264923 0.339291 0.059134 0.058 Uiso calc 1 . . C C6 0.38080(13) 0.29743(19) 0.0566(3) 0.0524(6) Uani d 1 . . H H6 0.373339 0.230404 -0.005545 0.063 Uiso calc 1 . . C C7 0.45731(12) 0.33011(19) 0.1102(3) 0.0486(5) Uani d 1 . . C C8 0.46721(11) 0.43126(19) 0.2017(3) 0.0448(5) Uani d 1 . . C C9 0.40007(11) 0.49711(18) 0.2366(3) 0.0430(5) Uani d 1 . . H H9 0.407386 0.564808 0.296766 0.052 Uiso calc 1 . . C C10 0.54638(13) 0.4685(2) 0.2607(3) 0.0600(7) Uani d 1 . . H H10 0.550084 0.537495 0.318412 0.072 Uiso calc 1 . . C C11 0.18592(11) 0.47158(16) 0.3248(3) 0.0420(5) Uani d 1 . . C C12 0.20564(13) 0.4232(2) 0.4976(3) 0.0569(6) Uani d 1 . . H H12 0.258393 0.428440 0.541446 0.068 Uiso calc 1 . . C C13 0.15019(15) 0.3682(2) 0.6053(4) 0.0699(8) Uani d 1 . . H H13 0.165623 0.336218 0.719130 0.084 Uiso calc 1 . . C C14 0.07106(14) 0.36060(19) 0.5433(4) 0.0651(7) Uani d 1 . . C C15 0.04964(12) 0.40537(18) 0.3714(4) 0.0519(6) Uani d 1 . . C C16 0.10733(12) 0.45953(18) 0.2658(3) 0.0469(5) Uani d 1 . . H H16 0.092278 0.489091 0.149790 0.056 Uiso calc 1 . . C C17 -0.03227(14) 0.3944(2) 0.3020(5) 0.0717(8) Uani d 1 . . H H17 -0.044107 0.426019 0.185508 0.086 Uiso calc 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 0.0374(9) 0.1197(17) 0.0831(13) 0.0130(10) 0.0031(8) 0.0127(12) O2 0.0616(10) 0.0765(13) 0.0828(13) 0.0281(9) 0.0117(10) -0.0046(10) O3 0.0797(13) 0.0857(15) 0.152(2) 0.0139(12) 0.0501(14) 0.0595(15) O4 0.0470(10) 0.0713(13) 0.162(2) -0.0120(9) 0.0304(12) -0.0243(13) C1 0.0356(10) 0.0403(11) 0.0624(14) 0.0016(9) 0.0024(9) 0.0008(10) C2 0.0487(13) 0.0455(14) 0.122(2) 0.0000(11) 0.0113(14) -0.0231(15) C3 0.0496(13) 0.0670(17) 0.0819(18) 0.0083(12) 0.0080(12) 0.0270(14) C4 0.0368(10) 0.0402(11) 0.0463(12) -0.0006(9) 0.0021(8) 0.0001(9) C5 0.0441(11) 0.0461(13) 0.0543(13) -0.0033(10) -0.0030(10) -0.0045(10) C6 0.0619(14) 0.0427(12) 0.0527(13) 0.0055(11) 0.0038(11) -0.0083(11) C7 0.0479(12) 0.0526(14) 0.0456(12) 0.0123(10) 0.0096(9) 0.0050(11) C8 0.0372(10) 0.0559(13) 0.0413(12) 0.0023(9) 0.0039(8) 0.0064(10) C9 0.0412(11) 0.0419(11) 0.0459(12) -0.0021(9) 0.0021(9) -0.0013(9) C10 0.0406(12) 0.0845(18) 0.0551(14) -0.0010(12) 0.0014(10) 0.0087(13) C11 0.0357(10) 0.0377(11) 0.0526(13) 0.0041(8) 0.0020(9) -0.0049(10) C12 0.0436(12) 0.0644(15) 0.0625(15) 0.0130(11) -0.0022(11) 0.0059(12) C13 0.0669(16) 0.0731(18) 0.0698(17) 0.0226(13) 0.0113(13) 0.0274(14) C14 0.0550(14) 0.0443(14) 0.096(2) 0.0109(11) 0.0266(14) 0.0164(14) C15 0.0404(11) 0.0390(12) 0.0762(17) 0.0021(9) 0.0084(11) -0.0042(12) C16 0.0408(11) 0.0457(12) 0.0543(13) 0.0015(9) 0.0011(9) -0.0026(10) C17 0.0424(13) 0.0641(17) 0.109(2) -0.0049(12) 0.0080(14) -0.0208(16) _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 C10 . 1.216(3) ? O2 H2 . 0.8200 ? O2 C7 . 1.355(2) ? O3 H3 . 0.8200 ? O3 C14 . 1.354(3) ? O4 C17 . 1.210(3) ? C1 C2 . 1.536(3) ? C1 C3 . 1.539(3) ? C1 C4 . 1.532(3) ? C1 C11 . 1.526(3) ? C2 H2A . 0.9600 ? C2 H2B . 0.9600 ? C2 H2C . 0.9600 ? C3 H3A . 0.9600 ? C3 H3B . 0.9600 ? C3 H3C . 0.9600 ? C4 C5 . 1.399(3) ? C4 C9 . 1.373(3) ? C5 H5 . 0.9300 ? C5 C6 . 1.368(3) ? C6 H6 . 0.9300 ? C6 C7 . 1.381(3) ? C7 C8 . 1.393(3) ? C8 C9 . 1.393(3) ? C8 C10 . 1.449(3) ? C9 H9 . 0.9300 ? C10 H10 . 0.9300 ? C11 C12 . 1.395(3) ? C11 C16 . 1.376(3) ? C12 H12 . 0.9300 ? C12 C13 . 1.372(3) ? C13 H13 . 0.9300 ? C13 C14 . 1.386(4) ? C14 C15 . 1.379(4) ? C15 C16 . 1.385(3) ? C15 C17 . 1.450(3) ? C16 H16 . 0.9300 ? C17 H17 . 0.9300 ? 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 C7 O2 H2 . . 109.5 ? C14 O3 H3 . . 109.5 ? C2 C1 C3 . . 107.6(2) ? C4 C1 C2 . . 112.22(17) ? C4 C1 C3 . . 107.89(18) ? C11 C1 C2 . . 107.77(18) ? C11 C1 C3 . . 111.89(17) ? C11 C1 C4 . . 109.48(16) ? C1 C2 H2A . . 109.5 ? C1 C2 H2B . . 109.5 ? C1 C2 H2C . . 109.5 ? H2A C2 H2B . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? C1 C3 H3A . . 109.5 ? C1 C3 H3B . . 109.5 ? C1 C3 H3C . . 109.5 ? H3A C3 H3B . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C5 C4 C1 . . 119.71(17) ? C9 C4 C1 . . 123.83(18) ? C9 C4 C5 . . 116.42(18) ? C4 C5 H5 . . 118.7 ? C6 C5 C4 . . 122.5(2) ? C6 C5 H5 . . 118.7 ? C5 C6 H6 . . 119.9 ? C5 C6 C7 . . 120.2(2) ? C7 C6 H6 . . 119.9 ? O2 C7 C6 . . 119.0(2) ? O2 C7 C8 . . 122.0(2) ? C6 C7 C8 . . 118.96(19) ? C7 C8 C9 . . 119.45(19) ? C7 C8 C10 . . 120.7(2) ? C9 C8 C10 . . 119.8(2) ? C4 C9 C8 . . 122.5(2) ? C4 C9 H9 . . 118.8 ? C8 C9 H9 . . 118.8 ? O1 C10 C8 . . 124.9(3) ? O1 C10 H10 . . 117.6 ? C8 C10 H10 . . 117.6 ? C12 C11 C1 . . 120.33(18) ? C16 C11 C1 . . 123.53(19) ? C16 C11 C12 . . 116.1(2) ? C11 C12 H12 . . 118.7 ? C13 C12 C11 . . 122.5(2) ? C13 C12 H12 . . 118.7 ? C12 C13 H13 . . 120.2 ? C12 C13 C14 . . 119.6(2) ? C14 C13 H13 . . 120.2 ? O3 C14 C13 . . 118.6(3) ? O3 C14 C15 . . 121.8(2) ? C15 C14 C13 . . 119.5(2) ? C14 C15 C16 . . 119.2(2) ? C14 C15 C17 . . 120.0(2) ? C16 C15 C17 . . 120.7(2) ? C11 C16 C15 . . 123.0(2) ? C11 C16 H16 . . 118.5 ? C15 C16 H16 . . 118.5 ? O4 C17 C15 . . 125.7(3) ? O4 C17 H17 . . 117.2 ? C15 C17 H17 . . 117.2 ? 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 O2 C7 C8 C9 . . . . 180.0(2) ? O2 C7 C8 C10 . . . . 0.0(3) ? O3 C14 C15 C16 . . . . 176.9(2) ? O3 C14 C15 C17 . . . . -3.8(4) ? C1 C4 C5 C6 . . . . 177.4(2) ? C1 C4 C9 C8 . . . . -178.02(19) ? C1 C11 C12 C13 . . . . 176.4(2) ? C1 C11 C16 C15 . . . . -175.8(2) ? C2 C1 C4 C5 . . . . 175.9(2) ? C2 C1 C4 C9 . . . . -6.4(3) ? C2 C1 C11 C12 . . . . -67.3(2) ? C2 C1 C11 C16 . . . . 109.9(2) ? C3 C1 C4 C5 . . . . -65.7(2) ? C3 C1 C4 C9 . . . . 112.0(2) ? C3 C1 C11 C12 . . . . 174.6(2) ? C3 C1 C11 C16 . . . . -8.2(3) ? C4 C1 C11 C12 . . . . 55.0(3) ? C4 C1 C11 C16 . . . . -127.7(2) ? C4 C5 C6 C7 . . . . 0.9(3) ? C5 C4 C9 C8 . . . . -0.3(3) ? C5 C6 C7 O2 . . . . 179.3(2) ? C5 C6 C7 C8 . . . . -0.5(3) ? C6 C7 C8 C9 . . . . -0.2(3) ? C6 C7 C8 C10 . . . . 179.8(2) ? C7 C8 C9 C4 . . . . 0.6(3) ? C7 C8 C10 O1 . . . . -1.6(4) ? C9 C4 C5 C6 . . . . -0.5(3) ? C9 C8 C10 O1 . . . . 178.4(2) ? C10 C8 C9 C4 . . . . -179.4(2) ? C11 C1 C4 C5 . . . . 56.3(3) ? C11 C1 C4 C9 . . . . -126.0(2) ? C11 C12 C13 C14 . . . . -0.7(4) ? C12 C11 C16 C15 . . . . 1.6(3) ? C12 C13 C14 O3 . . . . -176.5(2) ? C12 C13 C14 C15 . . . . 2.1(4) ? C13 C14 C15 C16 . . . . -1.6(4) ? C13 C14 C15 C17 . . . . 177.7(2) ? C14 C15 C16 C11 . . . . -0.3(3) ? C14 C15 C17 O4 . . . . -0.2(4) ? C16 C11 C12 C13 . . . . -1.1(3) ? C16 C15 C17 O4 . . . . 179.1(2) ? C17 C15 C16 C11 . . . . -179.6(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 O2 H2 O1 . 0.82 1.93 2.642(3) 145 O3 H3 O4 . 0.82 1.90 2.619(4) 145 _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. ; _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _shelx_hkl_file ; 0 0 -1 0.14 0.25 0 0 -2 1725.86 17.08 0 0 2 1738.10 14.71 0 0 3 -0.08 0.19 0 0 -3 -0.08 0.59 0 0 4 123.13 2.34 0 0 -4 129.59 4.05 0 0 -5 0.00 0.72 0 0 -6 46.83 3.10 0 0 -7 6.39 1.52 0 0 -8 5.82 1.55 0 1 0 0.16 0.14 0 1 -1 310.11 3.56 0 -1 -1 302.42 4.14 0 1 2 3011.28 25.93 0 1 -2 3084.48 27.20 0 -1 -2 3064.66 28.04 0 1 3 50.28 1.49 0 -1 -3 50.46 2.38 0 1 -3 53.40 2.15 0 -1 4 204.76 2.86 0 1 4 201.77 3.51 0 -1 -4 200.40 5.38 0 1 -4 207.36 4.97 0 -1 -5 5.19 1.23 0 1 -5 5.38 1.04 0 1 -6 1.97 0.82 0 -1 -6 0.82 0.83 0 1 -7 31.39 2.63 0 -1 -7 30.64 2.76 0 1 -8 5.55 1.43 0 -1 -8 7.69 1.73 0 2 0 3018.68 26.08 0 2 1 2395.55 21.39 0 2 -1 2377.95 19.87 0 -2 -1 2400.55 21.64 0 2 -1 2443.73 20.87 0 2 -2 4846.41 40.60 0 2 2 4784.85 40.91 0 -2 -2 4756.59 42.59 0 -2 -3 16.89 1.48 0 2 -3 18.38 1.20 0 2 3 18.21 1.06 0 -2 -4 933.12 13.64 0 2 -4 904.08 11.81 0 2 4 916.04 10.56 0 -2 -5 3.88 1.25 0 2 -5 4.76 0.98 0 -2 -6 7.58 1.51 0 2 -6 8.35 1.28 0 -2 -7 12.11 1.93 0 2 -7 10.15 1.63 0 -2 -8 4.04 1.43 0 2 -8 4.65 1.26 0 3 0 0.03 0.39 0 3 1 297.75 4.82 0 -3 -1 313.37 4.75 0 3 -1 308.13 4.53 0 3 2 294.57 4.94 0 3 -2 298.52 3.95 0 -3 -2 290.93 5.54 0 3 -2 302.24 4.27 0 3 3 337.36 5.61 0 -3 -3 340.43 6.75 0 3 -3 342.29 5.27 0 -3 -4 50.34 2.94 0 3 4 46.36 2.03 0 3 -4 44.11 2.04 0 3 -5 74.63 3.05 0 -3 -5 75.33 3.88 0 3 -6 3.80 0.97 0 -3 -6 2.31 1.14 0 3 -7 0.58 0.67 0 -3 -7 0.02 1.02 0 -3 -8 0.87 1.14 0 4 0 622.39 8.28 0 -4 0 625.30 6.64 0 4 1 2286.10 22.42 0 -4 -1 2322.91 21.65 0 4 -1 2247.72 21.83 0 -4 -2 443.34 7.34 0 4 -2 441.68 6.15 0 4 -2 433.79 4.75 0 4 2 439.37 6.97 0 -4 -3 1109.10 14.62 0 4 -3 1105.38 11.51 0 4 3 1105.17 13.25 0 -4 -4 226.97 6.34 0 4 4 214.02 4.92 0 4 -4 219.30 4.48 0 4 -5 7.22 0.96 0 4 5 6.80 0.95 0 -4 -5 7.01 1.51 0 -4 -6 5.64 1.53 0 4 -6 4.86 0.95 0 -4 -7 1.85 1.17 0 -4 -8 8.36 1.92 0 5 0 0.95 0.71 0 -5 0 0.37 0.27 0 -5 -1 318.72 5.38 0 5 1 327.73 6.11 0 5 -1 311.94 5.76 0 5 -2 117.77 3.14 0 5 -2 110.41 1.66 0 5 2 118.26 3.62 0 -5 -2 122.79 3.71 0 5 3 2.34 0.76 0 -5 -3 0.88 0.71 0 5 -3 1.91 0.35 0 5 -3 1.84 0.49 0 -5 -4 0.42 0.84 0 5 4 1.17 0.66 0 5 -4 -0.14 0.30 0 5 5 14.55 1.45 0 -5 -5 13.74 1.89 0 -5 -6 2.07 1.31 0 -5 -7 -1.37 1.10 0 -5 -8 3.73 1.64 0 6 0 75.86 2.95 0 -6 0 77.17 2.00 0 -6 -1 230.43 4.59 0 6 1 219.76 5.34 0 6 -1 219.62 5.06 0 6 -2 95.49 3.10 0 -6 -2 93.89 3.32 0 6 2 99.39 3.54 0 6 -3 7.02 0.92 0 6 -3 4.51 0.42 0 6 3 7.44 1.21 0 -6 -3 7.02 1.21 0 -6 -4 58.15 3.32 0 6 4 60.02 2.94 0 6 5 38.82 2.46 0 -6 -5 44.56 3.23 0 -6 -6 11.89 2.02 0 -6 -7 2.30 1.25 0 -7 0 14.87 0.99 0 7 0 17.72 1.71 0 7 1 145.07 4.56 0 7 -1 145.84 4.35 0 -7 -1 145.96 3.79 0 7 2 17.01 1.68 0 -7 -2 21.43 1.71 0 7 -2 21.73 1.65 0 7 3 2.01 0.87 0 -7 -3 3.29 0.90 0 7 -3 2.67 0.73 0 7 4 2.71 0.86 0 -7 -4 2.86 1.10 0 7 5 9.72 1.44 0 -7 -5 7.47 1.61 0 -7 -6 0.96 0.98 0 -7 -7 23.74 2.91 0 -8 0 10.00 0.83 0 8 0 11.22 1.52 0 -8 -1 2.27 0.66 0 8 -1 0.87 0.76 0 8 1 0.95 0.80 0 -8 -2 4.08 0.92 0 8 2 4.15 1.14 0 8 -2 4.36 0.97 0 -8 -3 -0.57 0.72 0 8 3 -0.06 0.76 0 8 -3 0.01 0.57 0 8 4 46.24 2.98 0 -8 -4 52.78 3.44 0 8 5 10.70 1.55 0 -8 -5 7.69 1.56 0 -8 -6 11.80 2.00 0 -8 -7 2.73 1.45 0 9 0 3.13 1.14 0 9 1 0.86 0.97 0 9 -1 0.32 0.80 0 9 2 8.72 1.53 0 -9 -2 10.27 1.31 0 9 -2 9.59 1.28 0 9 -3 20.58 1.76 0 -9 -3 23.68 2.15 0 9 3 20.83 2.12 0 9 -4 51.50 2.61 0 9 4 51.46 3.28 0 -9 -4 47.80 3.28 0 -9 -5 -0.10 0.98 0 9 5 0.72 0.78 0 -9 -6 2.41 1.20 0 10 0 64.57 3.49 0 10 1 8.85 1.51 0 10 -1 10.25 1.49 0 10 2 0.05 0.83 0 10 -2 0.98 0.69 0 10 3 8.35 1.56 0 -10 -3 8.25 1.37 0 10 -3 8.12 1.29 0 10 -4 -0.82 0.71 0 10 4 1.15 1.13 0 -10 -4 0.74 1.00 0 -10 -5 0.07 0.98 0 10 5 1.18 1.10 0 -10 -6 0.22 0.97 0 11 0 -0.04 1.02 0 11 1 1.26 1.01 0 11 -1 0.49 0.94 0 11 2 4.71 1.43 0 11 -2 3.76 1.15 0 11 3 1.22 1.03 0 11 -3 2.33 0.94 0 -11 -4 22.69 2.34 0 11 -4 21.99 2.00 0 11 4 23.00 2.42 0 -11 -5 0.58 0.92 0 11 5 0.33 0.92 0 12 0 7.41 1.43 0 12 -1 13.24 1.84 0 12 1 14.68 2.10 0 12 2 8.39 1.70 0 12 -2 7.90 1.48 0 12 3 2.52 1.17 0 12 -3 2.32 0.97 0 12 4 3.67 1.37 0 13 0 3.61 1.35 0 13 1 0.65 0.96 0 13 -1 -0.07 0.87 0 13 2 36.10 3.23 0 13 -2 34.45 2.91 0 13 3 5.39 1.67 0 13 -3 4.97 1.37 0 14 0 3.08 1.50 0 14 -1 14.27 2.09 0 14 1 11.79 2.07 0 14 -2 31.38 2.84 0 14 2 36.82 3.39 1 0 -8 2.59 1.21 1 0 -7 0.89 1.08 1 0 -6 190.05 5.99 1 0 -5 0.12 0.70 1 0 -4 26.55 2.00 -1 0 4 22.92 0.80 -1 0 3 0.34 0.14 1 0 -3 0.49 0.58 1 0 -2 2193.03 20.60 1 0 -1 0.33 0.24 -1 0 -1 0.43 0.31 -1 0 -2 187.34 3.70 1 0 3 0.27 0.25 -1 0 -3 -0.67 0.71 1 0 4 651.07 7.34 -1 0 -4 636.85 10.22 -1 0 -5 0.59 0.78 -1 0 -6 49.91 3.18 -1 0 -7 2.06 1.14 -1 0 -8 13.16 2.02 1 -1 -8 3.51 1.33 1 1 -8 3.39 1.16 1 -1 -7 33.45 2.90 1 1 -7 39.87 2.99 1 1 -6 1.53 0.88 1 -1 -6 1.41 1.06 1 -1 -5 21.27 1.98 1 1 -5 20.52 1.75 -1 1 4 5.83 0.55 1 1 -4 5.51 0.94 -1 -1 4 4.87 0.32 1 -1 -4 8.56 1.21 -1 1 3 307.95 4.00 1 -1 -3 309.62 6.10 1 1 -3 315.86 5.58 1 1 -2 2983.06 26.42 1 -1 -2 2925.08 27.22 -1 1 2 2959.04 25.02 1 1 -1 115.91 1.76 1 -1 -1 100.12 2.06 -1 -1 0 147.51 1.78 1 1 0 144.71 2.02 -1 1 0 144.45 1.98 -1 1 -1 9999.00 80.38 1 1 1 9934.17 80.55 -1 -1 -1 9888.00 81.34 1 1 2 251.80 3.61 -1 1 -2 263.61 4.29 -1 -1 -2 262.35 4.73 1 1 3 1145.31 11.61 -1 1 -3 1159.34 13.33 -1 -1 -3 1141.85 14.18 1 1 4 126.31 2.85 -1 1 -4 125.42 3.96 -1 -1 -4 120.81 4.13 -1 -1 -5 12.58 1.71 -1 1 -5 9.39 1.43 -1 -1 -6 9.88 1.60 -1 1 -6 10.34 1.44 -1 1 -7 0.98 0.88 -1 -1 -7 -0.15 0.97 -1 -1 -8 2.85 1.21 -1 1 -8 3.07 1.21 1 2 -8 6.24 1.42 1 -2 -8 5.61 1.62 1 2 -7 11.21 1.61 1 -2 -7 9.59 1.86 1 -2 -6 7.83 1.41 1 2 -6 7.65 1.28 1 2 -5 5.70 1.06 1 -2 -5 5.80 1.26 1 -2 -4 316.87 7.11 -1 2 4 316.60 4.93 1 2 -4 318.86 6.12 1 2 -3 138.97 3.30 1 -2 -3 133.12 3.93 -1 2 3 126.56 2.72 -1 2 2 1291.69 12.69 1 2 -2 1320.68 12.62 1 2 -2 1275.77 11.67 1 -2 -2 1263.95 14.05 1 -2 -1 136.05 2.70 1 2 -1 141.83 2.00 1 2 -1 143.57 2.42 -1 2 1 139.60 2.60 -1 -2 0 11.69 0.50 -1 2 0 10.96 0.67 1 2 0 11.54 0.70 -1 2 -1 976.48 9.52 1 2 1 994.27 10.05 -1 -2 -1 961.18 10.18 1 2 2 1733.07 16.59 -1 2 -2 1737.03 16.29 -1 -2 -2 1706.64 17.94 -1 -2 -3 465.50 8.13 -1 2 -3 477.33 7.01 1 2 3 470.15 6.53 -1 2 -4 10.18 1.13 1 2 4 10.17 0.94 -1 -2 -4 16.63 1.79 -1 2 -5 191.45 5.27 1 2 5 205.07 4.36 -1 -2 -5 195.70 6.24 -1 2 -6 12.48 1.49 -1 -2 -6 9.45 1.59 -1 -2 -7 0.62 0.99 -1 2 -7 1.60 0.88 -1 -2 -8 1.48 0.93 -1 2 -8 -0.13 0.81 1 -3 -8 1.54 1.23 1 -3 -7 5.42 1.59 1 3 -7 5.28 1.21 1 -3 -6 11.30 1.76 1 3 -6 11.96 1.50 1 -3 -5 106.78 4.46 1 3 -5 110.37 3.69 1 3 -4 828.85 10.84 -1 3 4 844.63 10.32 1 -3 -4 830.98 12.84 -1 3 3 513.06 7.18 1 3 -3 528.34 6.95 1 -3 -3 508.14 8.56 1 3 -2 423.42 5.40 1 -3 -2 424.71 6.80 -1 3 2 415.09 6.07 1 3 -2 430.40 5.10 -1 3 1 6060.95 51.27 1 3 -1 6023.92 50.85 1 -3 -1 5983.19 51.00 1 3 -1 6045.44 49.01 1 3 0 2.93 0.57 -1 -3 0 3.87 0.39 -1 3 0 4.81 0.61 1 -3 0 4.20 0.32 1 3 1 657.89 8.04 -1 -3 -1 627.16 7.69 -1 3 -1 646.93 7.50 -1 -3 -2 79.08 2.74 -1 3 -2 77.27 1.79 1 3 2 79.44 2.42 1 3 3 92.30 2.78 -1 3 -3 95.05 2.57 -1 -3 -3 95.72 3.48 -1 3 -4 172.37 4.18 -1 -3 -4 179.55 5.50 1 3 4 177.02 4.16 -1 3 -5 85.48 3.26 1 3 5 89.29 3.03 -1 -3 -5 89.10 4.22 -1 -3 -6 1.52 1.09 -1 3 -6 0.90 0.65 -1 3 -7 1.17 0.72 -1 -3 -7 0.29 1.01 -1 -3 -8 0.20 1.12 1 -4 -8 3.02 1.57 1 -4 -7 -0.94 1.01 1 -4 -6 33.12 2.80 1 4 -6 35.39 2.25 1 4 -5 0.81 0.64 1 -4 -5 -0.96 1.17 1 -4 -4 136.75 4.76 1 4 -4 135.70 3.42 -1 4 4 139.89 3.80 -1 4 3 618.74 8.75 1 -4 -3 626.23 10.00 1 4 -3 597.67 7.35 1 4 -3 601.19 7.35 1 -4 -2 221.84 4.82 1 4 -2 214.33 3.04 1 4 -2 211.67 3.96 -1 4 2 218.22 4.52 1 4 -1 1969.07 19.39 -1 -4 1 1972.36 16.66 -1 4 1 2026.51 19.90 1 -4 -1 1963.46 19.04 1 4 -1 1973.45 17.02 1 4 0 2634.45 25.18 1 -4 0 2655.60 22.56 -1 4 0 2665.43 25.05 -1 -4 0 2644.83 23.08 -1 4 -1 446.01 6.42 1 4 1 451.13 6.92 -1 4 -2 35.85 0.97 -1 -4 -2 35.62 1.99 1 4 2 36.01 1.84 -1 4 -2 39.24 1.62 -1 -4 -3 292.34 6.66 -1 4 -3 285.78 4.47 1 4 3 295.91 5.72 -1 -4 -4 78.75 3.75 -1 4 -4 78.11 2.58 1 4 4 78.68 2.94 -1 4 -5 37.87 2.06 -1 -4 -5 34.71 2.83 1 4 5 37.53 2.11 -1 -4 -6 1.92 1.34 -1 4 -6 0.11 0.53 -1 -4 -7 3.71 1.36 -1 -4 -8 -0.70 1.08 1 -5 -8 2.89 1.47 1 -5 -7 0.26 1.15 1 -5 -6 186.56 6.64 1 -5 -5 22.98 2.27 1 5 -5 20.83 1.45 1 -5 -4 18.84 1.92 -1 5 4 20.96 1.62 1 5 -4 18.99 1.18 1 5 -3 150.85 2.83 1 -5 -3 158.02 4.75 -1 5 3 156.35 4.27 1 5 -3 153.06 3.47 1 -5 -2 5.48 1.01 1 5 -2 3.82 0.37 -1 5 2 3.55 0.85 1 5 -2 3.32 0.62 -1 -5 1 165.79 2.30 -1 5 1 169.64 4.20 1 5 -1 175.02 4.10 1 -5 -1 186.01 3.79 1 5 0 23.14 1.52 -1 5 0 25.11 1.60 1 -5 0 20.77 0.85 -1 -5 0 22.29 1.04 1 5 1 800.31 10.77 -1 5 -1 784.71 10.18 -1 -5 -1 790.90 9.93 -1 -5 -2 252.34 5.54 1 5 2 248.97 5.49 -1 5 -2 250.98 4.83 1 5 3 42.79 2.30 -1 -5 -3 42.21 2.54 -1 5 -3 41.92 1.33 1 5 4 4.23 0.89 -1 5 -4 3.31 0.55 -1 -5 -4 2.49 1.02 -1 -5 -5 0.44 0.96 1 5 5 0.62 0.70 -1 -5 -6 -0.46 1.04 -1 -5 -7 0.69 1.05 -1 -5 -8 1.40 1.01 1 -6 -7 1.93 1.37 1 -6 -6 -1.23 1.00 1 -6 -5 14.79 2.15 -1 6 5 14.85 1.61 -1 6 4 14.08 1.51 1 -6 -4 15.54 1.72 1 6 -3 42.32 1.32 1 -6 -3 45.90 2.64 -1 6 3 44.78 2.46 1 6 -3 43.79 2.00 1 -6 -2 53.35 2.49 1 6 -2 46.20 1.18 -1 -6 2 52.00 1.10 -1 6 2 50.22 2.52 1 6 -2 48.01 2.22 -1 6 1 108.99 3.59 -1 -6 1 105.41 1.85 1 6 -1 107.85 3.47 1 -6 -1 116.26 3.08 1 6 0 103.72 3.49 -1 -6 0 102.91 2.36 -1 6 0 104.22 3.42 1 -6 0 102.32 2.11 1 6 1 385.61 7.30 -1 6 -1 376.40 6.83 -1 -6 -1 384.61 6.45 -1 6 -2 33.33 1.82 1 6 2 31.81 2.06 -1 -6 -2 35.33 2.08 -1 -6 -3 11.43 1.47 -1 6 -3 15.87 1.24 1 6 3 13.59 1.45 -1 -6 -4 0.55 0.93 1 6 4 1.89 0.72 -1 -6 -5 7.08 1.58 1 6 5 6.06 1.09 -1 -6 -6 3.57 1.35 -1 -6 -7 1.95 1.27 1 -7 -7 5.28 1.59 1 -7 -6 1.92 1.04 -1 7 5 2.29 0.97 1 -7 -5 -0.25 0.97 -1 7 4 2.87 0.98 1 -7 -4 1.25 0.87 1 7 -4 1.63 0.50 1 7 -3 57.46 2.52 1 -7 -3 62.07 3.10 -1 7 3 63.82 3.10 1 -7 -2 54.27 2.58 1 7 -2 49.12 2.45 -1 7 2 46.13 2.65 -1 -7 1 21.77 0.80 1 7 -1 22.98 1.68 -1 7 1 24.81 1.99 1 -7 -1 23.30 1.43 -1 7 0 61.28 2.86 1 7 0 53.60 2.74 1 -7 0 56.55 1.61 -1 -7 0 60.63 1.99 -1 7 -1 44.55 2.35 -1 -7 -1 44.62 2.10 1 7 1 44.30 2.59 -1 7 -2 1.91 0.73 -1 -7 -2 2.21 0.80 1 7 2 1.25 0.92 -1 -7 -3 20.81 1.92 1 7 3 20.98 1.92 -1 7 -3 18.84 1.45 -1 -7 -4 -0.10 0.94 1 7 4 -0.44 0.96 1 7 5 13.39 1.65 -1 -7 -5 18.11 2.16 -1 -7 -6 4.56 1.52 -1 -7 -7 -0.30 1.33 1 -8 -7 2.74 1.63 1 -8 -6 3.06 1.27 1 -8 -5 5.59 1.44 -1 8 5 10.55 1.59 -1 8 4 1.26 0.97 1 8 -4 0.60 0.54 1 -8 -4 0.97 0.90 1 -8 -3 2.12 0.89 1 8 -3 1.47 0.66 -1 8 3 2.22 0.98 -1 8 2 1.32 0.83 1 -8 -2 0.59 0.61 1 8 -2 1.31 0.76 1 8 -1 62.50 2.98 1 -8 -1 67.66 2.47 -1 8 1 67.01 3.21 1 8 0 3.68 1.01 -1 8 0 3.66 1.03 -1 -8 0 4.22 0.63 -1 -8 -1 31.42 1.87 1 8 1 27.24 2.22 -1 8 -1 32.29 2.16 1 8 2 -0.20 0.78 -1 -8 -2 0.30 0.61 -1 8 -2 0.11 0.60 1 8 3 1.33 0.84 -1 8 -3 2.64 0.72 -1 -8 -3 3.59 1.06 -1 -8 -4 9.92 1.68 1 8 4 9.00 1.44 1 8 5 -1.01 1.00 -1 -8 -5 1.23 1.11 -1 -8 -6 6.97 1.74 -1 -8 -7 6.88 2.26 1 -9 -6 10.04 1.94 -1 9 5 8.25 1.46 1 -9 -5 7.08 1.48 1 -9 -4 11.63 1.69 -1 9 4 13.34 1.76 1 9 -4 15.88 1.53 -1 9 3 2.38 1.02 1 9 -3 1.92 0.79 1 -9 -3 -0.36 0.79 1 -9 -2 -0.05 0.68 1 9 -2 0.42 0.73 -1 9 2 0.32 0.72 -1 9 1 16.31 1.80 1 9 -1 13.31 1.57 -1 9 0 16.49 1.77 1 9 0 17.91 1.83 -1 9 -1 3.97 1.00 1 9 1 5.75 1.25 -1 -9 -1 6.12 0.93 -1 -9 -2 11.99 1.43 -1 9 -2 13.30 1.52 1 9 2 13.63 1.74 -1 -9 -3 8.73 1.44 -1 9 -3 10.68 1.36 1 9 3 8.18 1.49 -1 -9 -4 5.30 1.48 1 9 4 2.87 1.14 1 9 5 -0.42 0.92 -1 -9 -5 0.40 0.99 -1 -9 -6 1.12 1.20 1 -10 -6 7.74 1.80 -1 10 5 9.37 1.67 1 -10 -5 8.38 1.60 1 -10 -4 33.25 2.69 1 10 -4 32.58 2.28 -1 10 4 38.96 2.97 1 -10 -3 71.23 3.55 1 10 -3 65.89 3.32 -1 10 3 67.86 3.75 -1 10 2 11.85 1.72 1 10 -2 13.80 1.68 -1 10 1 0.83 0.98 1 10 -1 -0.74 0.97 1 10 0 -0.34 0.93 -1 10 0 -0.59 1.04 -1 10 -1 33.23 2.52 1 10 1 33.93 2.70 1 10 2 0.63 0.93 -1 10 -2 1.24 0.83 1 10 3 -0.16 0.88 -1 10 -3 1.22 0.83 -1 -10 -3 0.85 0.74 1 10 4 21.55 2.39 -1 -10 -4 20.79 2.33 -1 -10 -5 2.05 1.12 1 10 5 0.68 0.90 -1 -10 -6 4.30 1.54 1 -11 -5 0.10 1.02 -1 11 5 2.23 1.22 -1 11 4 3.29 1.25 1 11 -3 36.66 2.63 -1 11 3 46.36 3.35 1 11 -2 12.07 1.64 -1 11 2 15.52 2.03 1 11 -1 13.45 1.75 -1 11 1 10.00 1.65 -1 11 0 36.07 2.77 1 11 0 33.03 2.72 1 11 1 33.90 2.83 -1 11 -1 37.84 2.80 -1 11 -2 1.65 0.94 1 11 2 -0.25 0.92 -1 11 -3 1.11 0.78 1 11 3 -0.61 0.96 -1 -11 -4 -0.27 0.98 1 11 4 -0.30 0.90 1 11 5 5.83 1.39 -1 -11 -5 4.69 1.44 -1 12 4 0.20 0.93 -1 12 3 17.76 2.27 1 12 -3 15.56 1.86 1 12 -2 2.00 1.13 -1 12 2 0.88 1.23 -1 12 1 4.69 1.37 1 12 -1 2.02 1.10 1 12 0 6.42 1.42 -1 12 0 8.00 1.58 -1 12 -1 1.75 0.98 1 12 1 3.90 1.24 1 12 2 26.69 2.66 -1 12 -2 24.53 2.33 1 12 3 37.95 3.16 -1 12 -3 39.62 2.87 1 12 4 3.13 1.33 -1 13 3 -2.27 1.35 1 13 -3 0.62 0.89 1 13 -2 2.50 1.24 -1 13 2 0.92 1.07 -1 13 1 14.78 2.13 1 13 -1 12.31 1.96 1 13 0 0.31 1.14 -1 13 0 0.41 0.94 1 13 1 4.70 1.50 -1 13 -1 6.99 1.50 -1 13 -2 37.51 3.03 1 13 2 34.61 3.20 1 13 3 4.91 1.52 -1 13 -3 9.44 1.65 -1 14 2 24.99 2.82 1 14 -2 30.60 2.91 -1 14 1 11.87 2.05 1 14 -1 9.95 1.88 -1 14 0 4.97 1.53 1 14 0 5.14 1.53 1 14 1 -0.42 1.19 -1 14 -1 -0.35 0.99 1 14 2 15.57 2.40 -1 14 -2 12.60 1.92 2 0 -8 6.06 1.36 2 0 -7 3.91 1.31 2 0 -6 173.41 5.74 2 0 -5 0.10 0.76 2 0 -4 1.89 0.85 2 0 -3 0.66 0.68 2 0 -2 882.18 10.05 2 0 -1 -0.33 0.29 2 0 0 1502.00 13.09 -2 0 0 1493.13 12.88 -2 0 -1 0.00 0.31 -2 0 -2 368.50 5.60 -2 0 -3 0.59 0.64 -2 0 -4 314.89 6.83 2 0 4 318.59 4.72 2 0 5 0.11 0.33 -2 0 -5 0.15 0.72 -2 0 -6 16.42 1.95 -2 0 -7 -0.64 0.93 -2 0 -8 0.79 1.01 2 1 -8 4.22 1.30 2 -1 -8 4.62 1.47 2 1 -7 1.78 0.93 2 -1 -7 -0.52 0.94 2 -1 -6 3.09 1.04 2 1 -6 7.04 1.33 2 -1 -5 5.14 1.12 2 1 -5 4.24 0.96 -2 1 4 0.32 0.19 2 1 -4 0.69 0.54 2 -1 -4 0.77 0.68 -2 1 3 258.99 3.29 2 1 -3 281.03 5.19 2 -1 -3 266.53 5.43 2 -1 -2 721.67 9.08 -2 1 2 750.87 7.19 2 1 -2 781.04 8.73 -2 1 1 408.09 4.36 2 -1 -1 404.27 5.10 2 1 -1 421.00 4.24 2 1 -1 424.66 4.80 -2 -1 0 2.42 0.28 2 -1 0 2.24 0.25 2 1 0 2.82 0.30 2 1 0 2.78 0.34 2 1 1 78.22 1.66 -2 1 -1 83.83 1.74 -2 -1 -1 77.06 1.95 -2 -1 -2 22.60 1.39 2 1 2 21.36 0.96 -2 1 -2 23.99 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1.45 -19 -2 -1 5.53 1.38 19 2 2 3.73 1.33 -19 2 -2 6.04 1.44 -19 -2 -2 4.02 1.32 19 3 -2 13.77 2.25 19 -3 -2 15.09 2.16 -19 3 2 12.02 1.78 -19 -3 2 15.10 2.11 19 -3 -1 4.28 1.31 19 3 -1 2.70 1.42 19 3 -1 5.09 1.27 -19 3 1 4.99 1.18 -19 -3 1 3.68 1.27 19 3 0 -0.01 0.95 19 -3 0 2.06 1.31 -19 3 0 -0.08 0.78 19 3 1 2.51 1.09 -19 3 -1 2.44 1.16 -19 -3 -1 3.05 1.29 19 4 -1 0.32 0.74 -19 4 1 -0.27 0.83 -19 -4 1 0.98 1.17 19 4 -1 -0.96 1.36 19 -4 -1 0.12 0.99 19 4 0 6.87 1.51 19 -4 0 6.53 1.69 -19 4 0 5.03 1.43 -19 -4 0 7.63 1.65 19 4 1 3.11 1.26 -19 4 -1 5.81 1.41 -19 -4 -1 5.07 1.57 20 0 0 6.71 1.40 -20 0 0 7.79 1.53 0 0 0 0.00 0.00 TITL APG D3 C3 1 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 16.610837 12.080278 7.094619 90.0000 90.3958 90.0000 ZERR 6.00 0.000641 0.000625 0.000420 0.0000 0.0043 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 66.00 60.00 6.00 6.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 7452 _shelx_res_file ; TITL apgd3c31_a.res in P2(1)/c apgd3c31.res created by SHELXL-2016/4 at 14:59:33 on 13-Aug-2018 REM Old TITL APG D3 C15 1 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.214, Rweak 0.292, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C17 N O3 CELL 0.71073 16.6108 12.0803 7.0946 90 90.396 90 ZERR 4 0.0006 0.0006 0.0004 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 68 64 16 L.S. 4 PLAN 6 TEMP 24.85 HTAB O3 O4 HTAB O2 O1 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 REM REM REM WGHT 0.034700 0.734800 EXTI 0.003451 FVAR 0.69910 O1 3 0.608317 0.416391 0.240475 11.00000 0.03741 0.11973 = 0.08311 0.01267 0.00307 0.01303 O2 3 0.520365 0.262733 0.072381 11.00000 0.06162 0.07649 = 0.08285 -0.00463 0.01166 0.02812 AFIX 147 H2 2 0.562402 0.293270 0.104187 11.00000 -1.50000 AFIX 0 O3 3 0.016454 0.311169 0.656435 11.00000 0.07970 0.08566 = 0.15152 0.05948 0.05012 0.01386 AFIX 147 H3 2 -0.028389 0.315525 0.607948 11.00000 -1.50000 AFIX 0 O4 3 -0.086568 0.347676 0.382294 11.00000 0.04697 0.07129 = 0.16175 -0.02430 0.03044 -0.01200 C1 1 0.248721 0.537610 0.216327 11.00000 0.03556 0.04035 = 0.06240 0.00082 0.00239 0.00157 C2 1 0.267768 0.642568 0.330278 11.00000 0.04871 0.04548 = 0.12226 -0.02308 0.01132 0.00002 AFIX 137 H2A 2 0.218770 0.681998 0.354821 11.00000 -1.50000 H2B 2 0.303523 0.688954 0.259696 11.00000 -1.50000 H2C 2 0.292921 0.622372 0.447559 11.00000 -1.50000 AFIX 0 C3 1 0.217110 0.574247 0.021625 11.00000 0.04963 0.06702 = 0.08195 0.02696 0.00798 0.00826 AFIX 137 H3A 2 0.199791 0.510478 -0.048481 11.00000 -1.50000 H3B 2 0.259284 0.611212 -0.045502 11.00000 -1.50000 H3C 2 0.172540 0.623899 0.037436 11.00000 -1.50000 AFIX 0 C4 1 0.323521 0.465759 0.185633 11.00000 0.03680 0.04024 = 0.04629 0.00014 0.00210 -0.00062 C5 1 0.315964 0.363403 0.094856 11.00000 0.04406 0.04606 = 0.05432 -0.00447 -0.00304 -0.00329 AFIX 43 H5 2 0.264923 0.339291 0.059134 11.00000 -1.20000 AFIX 0 C6 1 0.380803 0.297433 0.056637 11.00000 0.06191 0.04270 = 0.05272 -0.00826 0.00377 0.00552 AFIX 43 H6 2 0.373339 0.230404 -0.005545 11.00000 -1.20000 AFIX 0 C7 1 0.457314 0.330108 0.110150 11.00000 0.04790 0.05257 = 0.04557 0.00499 0.00957 0.01226 C8 1 0.467210 0.431265 0.201689 11.00000 0.03722 0.05592 = 0.04130 0.00636 0.00387 0.00229 C9 1 0.400069 0.497106 0.236642 11.00000 0.04117 0.04194 = 0.04587 -0.00128 0.00213 -0.00212 AFIX 43 H9 2 0.407386 0.564808 0.296766 11.00000 -1.20000 AFIX 0 C10 1 0.546379 0.468536 0.260725 11.00000 0.04060 0.08447 = 0.05506 0.00875 0.00144 -0.00102 AFIX 43 H10 2 0.550084 0.537495 0.318412 11.00000 -1.20000 AFIX 0 C11 1 0.185916 0.471584 0.324833 11.00000 0.03575 0.03767 = 0.05264 -0.00493 0.00201 0.00411 C12 1 0.205643 0.423216 0.497560 11.00000 0.04364 0.06442 = 0.06254 0.00590 -0.00223 0.01303 AFIX 43 H12 2 0.258393 0.428440 0.541446 11.00000 -1.20000 AFIX 0 C13 1 0.150194 0.368207 0.605251 11.00000 0.06692 0.07315 = 0.06979 0.02745 0.01129 0.02259 AFIX 43 H13 2 0.165623 0.336218 0.719130 11.00000 -1.20000 AFIX 0 C14 1 0.071057 0.360595 0.543318 11.00000 0.05497 0.04428 = 0.09636 0.01640 0.02663 0.01086 C15 1 0.049638 0.405373 0.371381 11.00000 0.04043 0.03900 = 0.07623 -0.00419 0.00844 0.00207 C16 1 0.107329 0.459528 0.265825 11.00000 0.04079 0.04573 = 0.05428 -0.00262 0.00109 0.00152 AFIX 43 H16 2 0.092278 0.489091 0.149790 11.00000 -1.20000 AFIX 0 C17 1 -0.032270 0.394393 0.301955 11.00000 0.04238 0.06406 = 0.10873 -0.02084 0.00798 -0.00492 AFIX 43 H17 2 -0.044107 0.426019 0.185508 11.00000 -1.20000 AFIX 0 HKLF 4 REM apgd3c31_a.res in P2(1)/c REM R1 = 0.0507 for 2036 Fo > 4sig(Fo) and 0.0651 for all 2589 data REM 195 parameters refined using 0 restraints END WGHT 0.0349 0.7335 REM Highest difference peak 0.210, deepest hole -0.198, 1-sigma level 0.032 Q1 1 -0.0546 0.3132 0.5124 11.00000 0.05 0.21 Q2 1 0.4671 0.4022 0.1096 11.00000 0.05 0.16 Q3 1 0.2850 0.5051 0.1994 11.00000 0.05 0.14 Q4 1 0.1022 0.3947 0.6078 11.00000 0.05 0.14 Q5 1 0.4960 0.4547 0.2078 11.00000 0.05 0.13 Q6 1 0.4637 0.3737 0.2224 11.00000 0.05 0.13 ; _shelx_res_checksum 90680 data_2 _audit_creation_method ; Olex2 1.2 (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _chemical_name_systematic ; 5,5'-(propane-2,2-diyl)bis(2-hydroxyisophthalaldehyde) ; _chemical_name_common ? _chemical_formula_moiety 'C19 H16 O6' _chemical_formula_sum 'C19 H16 O6' _chemical_formula_iupac 'C19 H16 O6' _chemical_formula_weight 340.32 _chemical_melting_point ? _space_group_crystal_system monoclinic _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 13.4327(4) _cell_length_b 7.9920(3) _cell_length_c 15.2062(5) _cell_angle_alpha 90 _cell_angle_beta 90.348(3) _cell_angle_gamma 90 _cell_volume 1632.42(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4266 _cell_measurement_theta_min 2.0120 _cell_measurement_theta_max 25.9990 _cell_measurement_temperature 297.5(5) _exptl_crystal_description Irregular _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlisPro; Bourhis et al., 2015) ; _exptl_absorpt_correction_T_min 0.81035 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 297.5(5) _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Oxford Diffraction SuperNova, Dualflex, EosS2' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0945 _diffrn_reflns_number 13629 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_unetI/netI 0.0241 _diffrn_reflns_theta_min 2.017 _diffrn_reflns_theta_max 26.370 _diffrn_reflns_theta_full 26.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_radiation_probe x-ray _refine_special_details ? _reflns_number_total 3331 _reflns_number_gt 2586 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_gt 0.1546 _refine_ls_wR_factor_ref 0.1669 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_number_reflns 3331 _refine_ls_number_parameters 249 _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^)+(0.0850P)^2^+0.5400P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.253 _refine_diff_density_min -0.273 _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 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' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; CrysAlisPro (Rigaku OD, 2015) ; _computing_cell_refinement ; CrysAlisPro (Rigaku OD, 2015) ; _computing_data_reduction ; CrysAlisPro (Rigaku OD, 2015) ; _computing_structure_solution ; ShelXT (Sheldrick, 2015a) ; _computing_structure_refinement ; ShelXL (Sheldrick, 2015b) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; Mercury (Macrae et al., 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 0.56797(16) 0.2277(3) 0.75859(13) 0.0451(5) Uani d 1 . . C C2 0.5020(3) 0.0866(3) 0.79457(17) 0.0744(8) Uani d 1 . . H H2A 0.433239 0.115432 0.786234 0.112 Uiso calc 1 . . H H2B 0.515438 0.071710 0.856159 0.112 Uiso calc 1 . . H H2C 0.516230 -0.015436 0.763805 0.112 Uiso calc 1 . . C C3 0.67756(19) 0.1817(3) 0.77738(16) 0.0650(7) Uani d 1 . . H H3A 0.719548 0.274519 0.762469 0.098 Uiso calc 1 . . H H3B 0.695707 0.086163 0.742724 0.098 Uiso calc 1 . . H H3C 0.685618 0.155720 0.838652 0.098 Uiso calc 1 . . C C4 0.55349(14) 0.2495(2) 0.65879(12) 0.0398(4) Uani d 1 . . C C5 0.62192(14) 0.3416(3) 0.61068(13) 0.0425(5) Uani d 1 . . H H5 0.674345 0.392670 0.640554 0.051 Uiso calc 1 . . C C6 0.61570(15) 0.3610(3) 0.51995(13) 0.0442(5) Uani d 1 . . C C7 0.53582(16) 0.2880(3) 0.47460(13) 0.0477(5) Uani d 1 . . C C8 0.46395(15) 0.2017(3) 0.52114(14) 0.0470(5) Uani d 1 . . C C9 0.47444(15) 0.1818(3) 0.61219(14) 0.0458(5) Uani d 1 . . H H9 0.426579 0.120883 0.642407 0.055 Uiso calc 1 . . C C10 0.69131(19) 0.4569(3) 0.47277(17) 0.0598(6) Uani d 1 . . H H10 0.683(2) 0.462(3) 0.4070(19) 0.073(8) Uiso d 1 . . C C11 0.37722(19) 0.1293(4) 0.4765(2) 0.0669(7) Uani d 1 . . H H11 0.324(2) 0.068(3) 0.5214(17) 0.065(7) Uiso d 1 . . C C12 0.53648(14) 0.3898(3) 0.80494(12) 0.0400(5) Uani d 1 . . C C13 0.44519(15) 0.4626(3) 0.78465(13) 0.0449(5) Uani d 1 . . H H13 0.407023 0.415913 0.739712 0.054 Uiso calc 1 . . C C14 0.40839(15) 0.6016(3) 0.82828(13) 0.0460(5) Uani d 1 . . C C15 0.46436(15) 0.6737(3) 0.89671(13) 0.0421(5) Uani d 1 . . C C16 0.55783(14) 0.6066(3) 0.91700(13) 0.0426(5) Uani d 1 . . C C17 0.59223(14) 0.4663(3) 0.87119(12) 0.0422(5) Uani d 1 . . H H17 0.654434 0.422634 0.885479 0.051 Uiso calc 1 . . C C18 0.31154(19) 0.6673(4) 0.80118(17) 0.0662(7) Uani d 1 . . H H18 0.277(2) 0.595(4) 0.755(2) 0.087(9) Uiso d 1 . . C C19 0.61762(17) 0.6814(3) 0.98792(16) 0.0571(6) Uani d 1 . . H H19 0.5921(19) 0.790(3) 1.0142(17) 0.067(7) Uiso d 1 . . O O1 0.36389(14) 0.1404(3) 0.39694(14) 0.0851(7) Uani d 1 . . O O2 0.53075(14) 0.3050(3) 0.38619(10) 0.0706(5) Uani d 1 . . H H2 0.479652 0.260776 0.367754 0.106 Uiso calc 1 . . O O3 0.75935(14) 0.5285(3) 0.50684(12) 0.0779(6) Uani d 1 . . O O4 0.27133(14) 0.7886(3) 0.83289(13) 0.0869(7) Uani d 1 . . O O5 0.43151(13) 0.8023(2) 0.94557(11) 0.0565(4) Uani d 1 . . H H5A 0.366(3) 0.834(4) 0.932(2) 0.096(10) Uiso d 1 . . O O6 0.69410(13) 0.6221(3) 1.01611(13) 0.0749(6) 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 C1 0.0571(12) 0.0433(12) 0.0349(10) 0.0031(9) -0.0028(8) 0.0021(9) C2 0.119(2) 0.0514(15) 0.0532(14) -0.0140(15) 0.0114(14) 0.0062(12) C3 0.0797(16) 0.0667(16) 0.0484(13) 0.0329(13) -0.0166(12) -0.0045(11) C4 0.0436(10) 0.0397(11) 0.0362(10) 0.0046(8) -0.0029(8) -0.0034(8) C5 0.0428(10) 0.0440(11) 0.0405(11) -0.0006(9) -0.0066(8) -0.0020(9) C6 0.0460(10) 0.0449(12) 0.0417(11) 0.0012(9) -0.0013(8) 0.0007(9) C7 0.0560(12) 0.0477(12) 0.0392(11) 0.0097(10) -0.0085(9) -0.0048(9) C8 0.0427(10) 0.0479(12) 0.0503(12) 0.0050(9) -0.0095(9) -0.0094(10) C9 0.0422(10) 0.0467(12) 0.0486(12) -0.0006(9) 0.0004(9) -0.0036(9) C10 0.0656(14) 0.0639(16) 0.0498(13) -0.0071(12) -0.0004(11) 0.0063(12) C11 0.0536(13) 0.0721(17) 0.0746(18) 0.0058(12) -0.0217(13) -0.0220(14) C12 0.0458(10) 0.0433(11) 0.0309(9) 0.0013(8) 0.0006(8) 0.0046(8) C13 0.0458(10) 0.0547(13) 0.0343(10) 0.0009(9) -0.0045(8) -0.0014(9) C14 0.0433(10) 0.0585(13) 0.0362(10) 0.0051(9) -0.0001(8) 0.0039(9) C15 0.0458(10) 0.0432(11) 0.0374(10) -0.0001(9) 0.0060(8) 0.0037(8) C16 0.0427(10) 0.0480(12) 0.0373(10) -0.0043(9) 0.0007(8) 0.0004(9) C17 0.0395(9) 0.0497(12) 0.0373(10) 0.0015(9) -0.0003(8) 0.0034(9) C18 0.0561(13) 0.0870(19) 0.0555(14) 0.0234(13) -0.0084(11) -0.0153(14) C19 0.0472(12) 0.0662(16) 0.0578(14) -0.0025(11) -0.0040(10) -0.0106(12) O1 0.0752(12) 0.1010(15) 0.0786(13) 0.0110(11) -0.0387(10) -0.0277(11) O2 0.0875(13) 0.0870(14) 0.0371(8) 0.0030(10) -0.0139(8) -0.0001(8) O3 0.0766(12) 0.0875(14) 0.0697(12) -0.0279(11) -0.0005(9) 0.0071(10) O4 0.0695(11) 0.1126(16) 0.0784(13) 0.0418(11) -0.0131(10) -0.0226(12) O5 0.0581(9) 0.0565(10) 0.0550(9) 0.0090(8) 0.0009(7) -0.0105(8) O6 0.0604(10) 0.0890(14) 0.0753(12) 0.0004(9) -0.0174(9) -0.0135(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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 . 1.537(3) ? C1 C3 . 1.542(3) ? C2 H2A . 0.9600 ? C2 H2B . 0.9600 ? C2 H2C . 0.9600 ? C3 H3A . 0.9600 ? C3 H3B . 0.9600 ? C3 H3C . 0.9600 ? C4 C1 . 1.539(3) ? C4 C5 . 1.389(3) ? C4 C9 . 1.383(3) ? C5 H5 . 0.9300 ? C5 C6 . 1.390(3) ? C6 C7 . 1.399(3) ? C6 C10 . 1.464(3) ? C7 C8 . 1.384(3) ? C8 C9 . 1.400(3) ? C8 C11 . 1.464(3) ? C9 H9 . 0.9300 ? C10 H10 . 1.01(3) ? C11 H11 . 1.10(3) ? C12 C1 . 1.536(3) ? C12 C17 . 1.393(3) ? C13 C12 . 1.390(3) ? C13 H13 . 0.9300 ? C13 C14 . 1.386(3) ? C14 C18 . 1.460(3) ? C15 C14 . 1.404(3) ? C16 C15 . 1.398(3) ? C16 C19 . 1.468(3) ? C17 C16 . 1.400(3) ? C17 H17 . 0.9300 ? C18 H18 . 1.02(3) ? C19 H19 . 1.02(3) ? O1 C11 . 1.225(3) ? O2 C7 . 1.353(3) ? O2 H2 . 0.8200 ? O3 C10 . 1.194(3) ? O4 C18 . 1.211(3) ? O5 C15 . 1.344(3) ? O5 H5A . 0.94(3) ? O6 C19 . 1.208(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 C2 C1 C3 . . 108.1(2) ? C2 C1 C4 . . 111.37(18) ? C4 C1 C3 . . 108.94(17) ? C12 C1 C2 . . 107.15(18) ? C12 C1 C3 . . 112.43(17) ? C12 C1 C4 . . 108.90(16) ? C1 C2 H2A . . 109.5 ? C1 C2 H2B . . 109.5 ? C1 C2 H2C . . 109.5 ? H2A C2 H2B . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? C1 C3 H3A . . 109.5 ? C1 C3 H3B . . 109.5 ? C1 C3 H3C . . 109.5 ? H3B C3 H3A . . 109.5 ? H3B C3 H3C . . 109.5 ? H3C C3 H3A . . 109.5 ? C5 C4 C1 . . 119.94(17) ? C9 C4 C1 . . 123.58(18) ? C9 C4 C5 . . 116.48(18) ? C4 C5 H5 . . 118.5 ? C4 C5 C6 . . 123.06(18) ? C6 C5 H5 . . 118.5 ? C5 C6 C7 . . 118.93(19) ? C5 C6 C10 . . 120.46(19) ? C7 C6 C10 . . 120.6(2) ? C8 C7 C6 . . 119.40(18) ? O2 C7 C6 . . 118.8(2) ? O2 C7 C8 . . 121.82(19) ? C7 C8 C9 . . 119.73(18) ? C7 C8 C11 . . 121.0(2) ? C9 C8 C11 . . 119.3(2) ? C4 C9 C8 . . 122.31(19) ? C4 C9 H9 . . 118.8 ? C8 C9 H9 . . 118.8 ? C6 C10 H10 . . 115.5(16) ? O3 C10 C6 . . 124.8(2) ? O3 C10 H10 . . 119.8(16) ? C8 C11 H11 . . 113.7(13) ? O1 C11 C8 . . 122.7(3) ? O1 C11 H11 . . 123.6(13) ? C13 C12 C1 . . 119.75(17) ? C13 C12 C17 . . 116.53(19) ? C17 C12 C1 . . 123.62(17) ? C12 C13 H13 . . 118.5 ? C14 C13 C12 . . 123.06(18) ? C14 C13 H13 . . 118.5 ? C13 C14 C15 . . 119.53(18) ? C13 C14 C18 . . 118.2(2) ? C15 C14 C18 . . 122.3(2) ? C16 C15 C14 . . 118.81(19) ? O5 C15 C14 . . 123.20(19) ? O5 C15 C16 . . 117.97(19) ? C15 C16 C17 . . 119.76(18) ? C15 C16 C19 . . 119.5(2) ? C17 C16 C19 . . 120.73(19) ? C12 C17 C16 . . 122.25(18) ? C12 C17 H17 . . 118.9 ? C16 C17 H17 . . 118.9 ? C14 C18 H18 . . 113.3(17) ? O4 C18 C14 . . 125.1(2) ? O4 C18 H18 . . 121.4(17) ? C16 C19 H19 . . 116.9(14) ? O6 C19 C16 . . 124.2(2) ? O6 C19 H19 . . 119.0(15) ? C7 O2 H2 . . 109.5 ? C15 O5 H5A . . 113(2) ? 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 C1 C4 C5 C6 . . . . 177.43(18) ? C1 C4 C9 C8 . . . . -179.08(19) ? C1 C12 C17 C16 . . . . -174.81(18) ? C4 C5 C6 C7 . . . . 1.5(3) ? C4 C5 C6 C10 . . . . -178.8(2) ? C5 C4 C1 C2 . . . . -164.9(2) ? C5 C4 C1 C3 . . . . -45.8(3) ? C5 C4 C1 C12 . . . . 77.2(2) ? C5 C4 C9 C8 . . . . 1.0(3) ? C5 C6 C7 C8 . . . . 1.5(3) ? C5 C6 C7 O2 . . . . -179.06(19) ? C5 C6 C10 O3 . . . . -2.9(4) ? C6 C7 C8 C9 . . . . -3.0(3) ? C6 C7 C8 C11 . . . . 177.5(2) ? C7 C6 C10 O3 . . . . 176.9(2) ? C7 C8 C9 C4 . . . . 1.8(3) ? C7 C8 C11 O1 . . . . 0.3(4) ? C9 C4 C1 C2 . . . . 15.2(3) ? C9 C4 C1 C3 . . . . 134.4(2) ? C9 C4 C1 C12 . . . . -102.7(2) ? C9 C4 C5 C6 . . . . -2.7(3) ? C9 C8 C11 O1 . . . . -179.2(2) ? C10 C6 C7 C8 . . . . -178.3(2) ? C10 C6 C7 O2 . . . . 1.2(3) ? C11 C8 C9 C4 . . . . -178.8(2) ? C12 C13 C14 C15 . . . . -0.4(3) ? C12 C13 C14 C18 . . . . 179.9(2) ? C12 C17 C16 C15 . . . . 0.2(3) ? C12 C17 C16 C19 . . . . 178.5(2) ? C13 C12 C1 C2 . . . . -71.0(2) ? C13 C12 C1 C3 . . . . 170.37(19) ? C13 C12 C1 C4 . . . . 49.6(2) ? C13 C12 C17 C16 . . . . 1.6(3) ? C13 C14 C18 O4 . . . . -179.1(3) ? C14 C13 C12 C1 . . . . 175.04(19) ? C14 C13 C12 C17 . . . . -1.5(3) ? C15 C14 C18 O4 . . . . 1.2(4) ? C15 C16 C19 O6 . . . . 172.1(2) ? C16 C15 C14 C13 . . . . 2.2(3) ? C16 C15 C14 C18 . . . . -178.1(2) ? C17 C12 C1 C2 . . . . 105.3(2) ? C17 C12 C1 C3 . . . . -13.3(3) ? C17 C12 C1 C4 . . . . -134.15(19) ? C17 C16 C15 C14 . . . . -2.2(3) ? C17 C16 C15 O5 . . . . 176.20(18) ? C17 C16 C19 O6 . . . . -6.2(4) ? C19 C16 C15 C14 . . . . 179.5(2) ? C19 C16 C15 O5 . . . . -2.1(3) ? O2 C7 C8 C9 . . . . 177.5(2) ? O2 C7 C8 C11 . . . . -1.9(3) ? O5 C15 C14 C13 . . . . -176.02(19) ? O5 C15 C14 C18 . . . . 3.6(3) ? 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 H2 O1 . 0.82 1.88 2.605(3) 146 O5 H5A O4 . 0.94(4) 2.00(4) 2.745(3) 135(3) O5 H5A O3 4_576 0.94(4) 2.14(4) 2.841(2) 131(3) _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. ; _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _shelx_hkl_file ; 0 0 -2 2251.81 22.37 0 0 2 2248.98 22.36 0 0 3 0.01 0.23 0 0 -3 0.23 0.26 0 0 4 859.79 11.95 0 0 -4 840.00 11.99 0 0 5 1.58 0.62 0 0 -5 2.68 0.66 0 0 6 929.70 14.42 0 0 -6 906.89 14.53 0 0 7 5.02 1.22 0 0 -7 3.83 1.14 0 0 8 1269.76 19.99 0 0 -8 1278.53 20.04 0 0 -9 1.64 0.95 0 0 9 0.42 0.75 0 0 -10 915.78 17.88 0 0 10 875.71 17.31 0 0 -11 1.67 1.03 0 0 11 0.82 0.97 0 0 12 14.66 2.27 0 0 -12 15.90 2.48 0 0 13 2.89 1.37 0 0 -13 2.18 1.30 0 0 14 75.62 5.49 0 0 -14 78.64 5.91 0 0 15 2.38 1.26 0 0 -15 2.13 1.38 0 0 -16 12.08 2.61 0 0 16 17.08 2.91 0 0 -17 -0.46 1.47 0 0 17 -0.86 1.10 0 0 -18 4.01 1.65 0 0 18 5.07 1.91 0 0 19 0.85 1.32 0 0 -19 2.35 1.89 0 1 0 0.22 0.22 0 1 0 0.02 0.10 0 -1 1 313.50 5.27 0 1 -1 326.10 5.38 0 1 -1 319.76 5.07 0 1 -1 322.51 4.49 0 -1 -2 1424.29 14.35 0 -1 2 1383.21 16.46 0 1 -2 1385.81 15.53 0 1 2 1430.39 14.80 0 -1 -3 1159.26 13.32 0 1 -3 1164.34 14.46 0 -1 3 1120.02 14.93 0 1 3 1183.95 13.44 0 -1 -4 54.86 2.31 0 -1 4 55.06 2.73 0 1 4 52.49 2.23 0 1 -4 52.20 2.54 0 1 -5 143.97 4.81 0 -1 -5 151.39 4.47 0 -1 5 147.79 5.01 0 1 5 155.73 4.42 0 1 -6 43.53 2.80 0 1 6 46.92 2.63 0 -1 -6 42.39 2.53 0 -1 6 47.00 2.90 0 -1 7 36.12 2.79 0 1 7 31.47 2.36 0 1 -7 40.38 2.92 0 -1 -7 37.63 2.63 0 -1 -8 433.39 10.21 0 1 -8 458.40 11.03 0 -1 8 429.65 10.66 0 1 8 440.62 9.99 0 1 9 5.91 1.12 0 -1 9 7.04 1.60 0 -1 -9 9.45 1.52 0 1 -9 7.84 1.49 0 1 -10 503.22 13.11 0 -1 -10 505.06 12.44 0 -1 10 507.96 12.79 0 1 10 503.68 12.11 0 -1 -11 36.22 3.39 0 -1 11 34.49 3.45 0 1 11 34.76 3.14 0 1 -11 42.26 3.80 0 1 12 0.44 0.91 0 1 -12 -0.50 0.77 0 -1 -12 0.93 0.95 0 -1 12 -0.29 0.71 0 -1 13 3.11 0.90 0 1 -13 2.84 1.34 0 -1 -13 2.84 1.20 0 1 13 2.31 1.19 0 -1 14 10.83 2.27 0 1 14 8.12 1.85 0 1 -14 7.29 1.90 0 -1 -14 7.63 2.04 0 1 15 1.13 1.01 0 1 -15 5.64 1.73 0 -1 -15 1.53 1.28 0 -1 15 3.58 1.65 0 1 16 3.09 1.31 0 1 -16 1.55 1.02 0 -1 16 1.87 1.32 0 -1 -16 2.80 1.43 0 1 17 0.05 1.08 0 -1 17 -1.44 1.58 0 -1 -17 0.55 1.06 0 1 -17 0.00 1.30 0 -1 18 5.26 2.09 0 1 -18 9.21 2.76 0 -1 -18 0.74 1.09 0 1 18 4.93 1.87 0 2 0 4301.46 41.85 0 2 0 4354.88 43.76 0 -2 0 4306.85 42.63 0 2 0 4349.77 45.28 0 2 -1 460.49 8.52 0 2 -1 486.07 6.43 0 2 1 472.86 9.38 0 2 1 474.01 6.82 0 2 -1 476.66 7.84 0 2 1 473.15 8.30 0 -2 1 473.48 8.20 0 2 2 47.07 2.71 0 2 -2 47.98 2.39 0 2 -2 50.69 2.00 0 2 -2 42.98 2.44 0 2 2 48.93 1.69 0 2 2 46.87 2.39 0 -2 2 46.48 2.47 0 2 3 210.16 6.02 0 -2 3 212.45 5.87 0 2 -3 212.41 5.01 0 -2 -3 210.82 3.72 0 2 3 200.25 3.90 0 2 -4 249.24 6.10 0 -2 -4 245.61 4.85 0 -2 4 251.30 6.83 0 2 4 241.11 4.67 0 2 5 9.29 1.09 0 -2 -5 8.64 0.96 0 2 -5 7.35 1.11 0 -2 5 9.74 1.42 0 -2 6 27.98 2.47 0 2 6 26.90 1.97 0 2 -6 28.14 2.33 0 -2 -6 26.90 1.95 0 2 7 90.83 3.97 0 -2 -7 95.44 4.03 0 -2 7 84.57 4.53 0 2 -7 99.82 4.70 0 -2 8 35.03 3.03 0 2 -8 37.28 3.03 0 -2 -8 35.18 2.61 0 2 8 30.09 2.44 0 2 -9 33.40 3.09 0 -2 9 32.94 3.16 0 2 9 29.13 2.58 0 -2 -9 37.93 2.95 0 2 10 43.66 3.35 0 -2 10 43.46 3.70 0 2 -10 48.18 3.94 0 -2 -10 43.71 3.40 0 -2 11 0.17 0.77 0 2 -11 0.05 0.94 0 2 11 0.90 0.70 0 -2 -11 -0.13 0.72 0 -2 -12 8.00 1.58 0 2 -12 6.68 1.69 0 -2 12 9.36 2.03 0 2 12 4.04 1.20 0 -2 -13 9.74 1.91 0 2 -13 10.68 2.28 0 2 13 13.58 2.26 0 -2 13 11.78 2.41 0 -2 -14 101.04 6.54 0 2 -14 103.01 7.09 0 -2 14 115.16 7.28 0 2 14 100.13 6.26 0 2 -15 1.25 1.09 0 2 15 2.09 1.34 0 -2 15 3.05 1.56 0 -2 -15 1.63 1.00 0 -2 16 2.46 1.34 0 -2 -16 0.44 0.96 0 2 -16 4.73 1.88 0 2 16 3.91 1.56 0 2 17 5.24 1.86 0 -2 17 5.58 2.07 0 -2 -17 4.36 1.74 0 2 -17 5.21 2.18 0 2 -18 12.38 3.13 0 -2 18 14.45 3.09 0 2 18 11.69 2.70 0 -2 -18 11.74 2.84 0 -3 0 0.42 0.37 0 3 0 0.31 0.33 0 3 0 -0.13 0.45 0 3 0 -0.44 0.58 0 3 0 0.23 0.15 0 -3 1 405.90 8.49 0 3 1 418.89 10.41 0 3 -1 422.61 8.21 0 3 1 406.90 7.25 0 3 1 413.08 8.94 0 3 -1 410.35 9.18 0 3 -1 429.76 10.53 0 3 -1 416.61 6.38 0 -3 2 633.87 11.61 0 3 2 628.17 9.18 0 3 -2 620.13 12.14 0 3 -2 636.18 11.20 0 3 2 651.06 11.68 0 3 -2 657.32 9.44 0 3 2 660.42 13.41 0 3 3 590.47 8.64 0 -3 3 588.89 11.65 0 -3 -3 597.41 6.88 0 3 -3 607.79 9.85 0 3 -3 586.67 12.06 0 3 3 611.45 11.31 0 3 3 596.81 13.00 0 3 -4 97.61 3.84 0 -3 4 93.28 4.44 0 3 4 92.16 2.93 0 -3 -4 93.05 2.53 0 3 -4 91.15 4.59 0 3 4 91.47 4.80 0 -3 -5 120.90 3.44 0 3 -5 118.30 4.62 0 3 5 125.12 5.80 0 -3 5 113.02 5.17 0 3 5 116.57 3.49 0 3 -5 111.27 5.21 0 3 6 250.32 5.75 0 3 6 258.74 8.74 0 -3 -6 253.36 5.94 0 3 -6 257.23 7.53 0 -3 6 262.66 8.33 0 3 -7 129.84 5.59 0 -3 -7 131.95 4.55 0 -3 7 134.53 6.07 0 3 7 123.63 4.11 0 -3 -8 93.08 4.15 0 3 8 86.36 4.28 0 -3 8 98.68 5.43 0 3 -8 89.60 4.97 0 -3 9 63.33 4.59 0 -3 -9 59.38 3.56 0 3 -9 61.45 4.33 0 3 9 61.18 3.83 0 -3 -10 27.66 2.61 0 3 -10 25.53 2.99 0 -3 10 24.62 2.98 0 3 10 24.14 2.55 0 3 -11 316.20 11.16 0 -3 -11 300.53 9.55 0 -3 11 320.50 11.13 0 3 11 293.80 9.60 0 3 -12 14.18 2.57 0 3 12 14.47 2.34 0 -3 12 15.78 2.68 0 -3 -12 15.90 2.37 0 3 -13 0.01 1.14 0 -3 13 0.10 1.12 0 -3 -13 -1.10 0.96 0 3 -14 8.23 2.00 0 3 14 8.56 1.85 0 -3 14 6.45 1.80 0 -3 -14 6.83 1.75 0 -3 15 -0.68 1.03 0 3 15 -0.18 0.70 0 -3 -15 -0.03 1.01 0 3 -15 0.94 0.93 0 3 16 23.08 3.39 0 3 -16 29.40 4.36 0 -3 16 21.63 3.42 0 3 -17 17.90 3.66 0 -3 17 13.06 2.84 0 3 -18 15.50 3.57 0 -3 18 17.26 3.48 0 4 0 330.61 7.35 0 4 0 299.32 4.66 0 -4 0 322.67 7.92 0 4 0 335.37 10.34 0 4 0 323.57 8.89 0 -4 -1 177.29 5.55 0 4 1 179.82 6.42 0 -4 1 171.59 5.89 0 4 -1 178.29 6.60 0 4 1 182.73 7.53 0 4 -1 177.79 3.95 0 4 1 189.54 5.12 0 4 -1 173.85 5.51 0 4 -1 191.73 7.76 0 4 -2 66.56 2.68 0 4 -2 68.80 3.61 0 4 2 63.61 3.80 0 4 2 64.30 2.75 0 -4 2 69.84 3.78 0 4 2 64.91 4.50 0 4 -2 63.18 3.94 0 4 3 43.31 3.88 0 -4 3 35.18 2.86 0 4 -3 42.32 2.39 0 4 3 42.20 3.01 0 4 3 41.19 2.08 0 4 -3 38.14 3.14 0 4 4 33.84 3.42 0 4 -4 32.02 3.01 0 4 4 31.90 1.78 0 4 -4 31.88 2.31 0 -4 4 31.87 2.81 0 4 5 1.03 0.77 0 4 -5 1.71 0.88 0 4 -5 0.68 0.46 0 -4 5 0.73 0.56 0 4 5 0.75 0.33 0 -4 -5 0.63 0.27 0 -4 6 7.68 1.63 0 4 6 7.01 0.90 0 -4 -6 6.77 0.86 0 4 -6 5.25 1.14 0 4 -6 7.20 1.64 0 4 6 8.60 1.80 0 4 -7 241.17 9.09 0 -4 7 259.02 9.09 0 4 7 247.88 9.95 0 -4 -7 274.48 6.50 0 4 -7 250.79 8.26 0 4 8 52.02 4.60 0 4 -8 53.25 3.96 0 -4 -8 56.30 3.13 0 4 -9 36.81 3.52 0 -4 9 31.56 3.37 0 4 9 32.68 3.80 0 4 -10 266.88 10.00 0 -4 10 269.08 10.28 0 4 10 282.10 11.59 0 4 -11 158.47 8.06 0 -4 11 182.17 8.71 0 -4 12 1.12 1.04 0 4 -12 2.48 1.30 0 4 -13 0.04 1.06 0 -4 13 1.98 1.22 0 -4 14 6.04 1.78 0 4 -14 8.33 2.15 0 4 -15 2.16 1.32 0 -4 15 4.11 1.68 0 -4 16 0.67 1.37 0 4 -16 1.82 1.17 0 -4 17 -0.26 1.06 0 4 -17 -0.96 1.93 0 5 0 0.17 0.46 0 5 0 0.47 0.74 0 -5 0 1.10 0.64 0 5 0 -0.74 1.07 0 5 1 346.79 10.07 0 5 -1 349.76 10.47 0 5 -1 329.06 6.03 0 5 1 345.87 11.88 0 -5 -1 352.44 8.83 0 5 1 345.22 7.89 0 -5 1 345.12 9.24 0 5 -1 356.07 8.85 0 -5 2 99.27 4.98 0 5 -2 100.74 3.51 0 5 2 107.11 6.47 0 5 2 102.84 5.32 0 -5 -2 105.31 4.58 0 5 -2 110.12 5.77 0 5 2 100.85 3.84 0 5 3 2.30 0.59 0 5 -3 2.01 0.90 0 5 3 1.89 0.94 0 -5 3 1.96 0.86 0 5 -3 2.09 0.55 0 5 3 2.23 0.98 0 -5 4 30.67 2.94 0 5 -4 38.03 3.58 0 5 -4 34.37 2.48 0 5 4 35.79 3.80 0 5 4 30.96 3.03 0 5 5 18.16 2.77 0 -5 5 19.60 2.51 0 5 -5 17.52 2.53 0 5 -5 16.71 1.91 0 5 -6 6.68 1.75 0 -5 6 6.82 1.55 0 5 -6 6.83 1.30 0 5 6 6.42 2.07 0 5 -7 7.71 1.86 0 -5 7 8.54 1.74 0 5 7 8.07 2.14 0 5 -7 10.13 1.86 0 5 -8 28.03 3.40 0 -5 8 25.68 3.19 0 5 8 22.57 3.43 0 5 -8 23.75 2.80 0 5 9 37.05 4.57 0 5 -9 49.08 4.20 0 -5 9 39.30 3.95 0 5 -9 41.46 4.34 0 5 10 105.53 7.62 0 5 -10 101.86 6.33 0 5 -10 99.53 6.94 0 -5 10 113.24 6.88 0 5 11 5.05 2.33 0 -5 11 8.55 2.04 0 5 -11 6.32 1.82 0 5 -11 6.69 2.05 0 5 -12 26.95 3.84 0 5 -12 26.42 3.91 0 5 12 33.63 4.63 0 -5 12 28.75 3.75 0 5 13 3.82 1.76 0 5 -13 6.52 2.26 0 -5 13 5.73 1.66 0 -5 14 -0.36 1.13 0 5 14 -0.94 1.45 0 5 -14 3.07 1.64 0 5 -15 9.06 2.74 0 -5 15 10.19 2.54 0 5 15 10.12 2.96 0 -5 16 -0.30 1.04 0 5 -16 0.32 1.36 0 6 0 80.13 5.15 0 6 0 77.73 6.12 0 6 -1 4.27 1.21 0 6 1 5.45 2.00 0 6 1 3.69 1.25 0 -6 1 2.96 0.81 0 6 2 142.34 6.83 0 6 -2 162.17 7.83 0 6 2 166.54 8.99 0 -6 2 168.29 6.94 0 -6 3 26.11 2.80 0 6 3 31.19 3.25 0 6 -3 24.44 3.00 0 6 3 27.55 3.70 0 -6 4 9.82 1.76 0 6 4 10.18 2.36 0 6 4 13.12 2.13 0 6 -4 7.30 1.97 0 -6 5 109.67 6.09 0 6 -5 109.85 6.68 0 6 5 103.10 7.43 0 6 6 27.00 3.94 0 6 -6 26.98 2.62 0 -6 6 18.84 2.66 0 6 -6 22.50 3.20 0 6 -7 3.53 1.49 0 -6 7 4.79 1.57 0 6 -7 3.02 1.01 0 6 7 1.20 1.13 0 6 -8 76.34 6.02 0 6 -8 86.47 5.35 0 -6 8 87.66 5.96 0 6 8 83.21 7.07 0 6 -9 104.61 7.25 0 6 -9 104.80 6.22 0 -6 9 101.91 6.64 0 6 9 107.01 8.28 0 -6 10 68.34 5.54 0 6 -10 61.55 5.02 0 6 10 72.38 6.91 0 6 -10 55.73 5.49 0 6 -11 183.75 10.17 0 -6 11 182.98 9.47 0 6 11 193.53 11.61 0 6 -11 195.51 9.39 0 6 12 35.95 5.47 0 6 -12 28.20 3.81 0 6 -12 24.98 3.91 0 -6 12 33.85 4.16 0 -6 13 111.16 7.76 0 6 -13 102.07 7.43 0 6 13 117.81 9.50 0 6 -14 4.19 1.64 0 6 14 8.39 3.00 0 -6 14 4.98 1.81 0 6 -15 7.62 2.49 0 -6 15 9.22 2.69 0 6 15 5.85 2.35 0 7 0 13.25 3.11 0 7 0 4.40 1.68 0 7 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1.57 15 1 5 1.59 1.48 -15 -1 -6 4.43 2.35 -15 1 -6 2.48 2.22 -15 1 -6 0.63 1.58 15 -1 6 3.14 1.90 15 -1 6 3.80 2.20 15 1 6 -1.17 1.73 -15 -1 -7 12.37 3.31 -15 1 -7 20.45 4.22 -15 1 -7 8.13 2.43 15 -1 7 11.59 3.44 15 -1 7 12.27 3.09 15 1 7 11.40 3.11 -15 -1 -8 2.28 1.77 -15 1 -8 -0.43 1.19 -15 1 -8 0.44 1.23 15 -1 8 1.32 1.79 15 1 8 0.41 1.64 15 -2 -7 3.13 2.28 15 2 -7 3.66 1.66 -15 -2 7 1.57 1.63 -15 2 7 1.18 1.28 -15 -2 7 3.23 1.91 -15 2 7 3.75 2.17 15 -2 -6 0.88 1.35 15 2 -6 1.49 1.83 -15 -2 6 0.62 1.07 -15 2 6 -1.75 2.05 -15 -2 6 1.80 1.99 -15 2 6 -0.38 1.71 15 -2 -5 -0.94 1.58 15 2 -5 1.09 1.50 -15 -2 5 0.27 1.32 -15 2 5 0.43 1.68 -15 -2 5 3.02 2.08 -15 2 5 1.21 1.57 15 -2 -4 1.43 1.59 15 2 -4 0.69 1.22 -15 -2 4 6.21 2.45 -15 2 4 1.27 1.54 -15 -2 4 0.57 2.19 -15 2 4 0.17 1.27 15 -2 -3 23.34 4.18 15 2 -3 19.77 3.90 -15 -2 3 21.32 3.94 -15 2 3 19.40 4.02 -15 -2 3 17.93 4.19 -15 2 3 24.68 4.62 15 -2 -2 15.18 3.32 15 2 -2 11.49 3.17 -15 -2 2 7.35 2.59 -15 2 2 17.76 3.94 -15 -2 2 13.37 3.67 -15 2 2 17.18 4.00 -15 2 1 46.07 6.22 15 -2 -1 50.36 5.94 -15 -2 1 48.44 5.87 15 2 -1 41.52 5.58 -15 2 1 44.22 6.05 -15 -2 1 50.35 6.68 -15 2 0 -1.60 1.79 15 -2 0 1.04 1.49 15 2 0 3.00 1.83 -15 -2 0 1.59 1.74 -15 2 0 0.41 1.24 -15 -2 0 -1.02 1.19 -15 -2 -1 2.46 1.79 -15 2 -1 0.58 1.73 15 -2 1 0.36 1.31 15 2 1 0.39 1.35 -15 2 -1 2.61 1.91 -15 -2 -2 7.96 2.81 -15 2 -2 3.14 2.08 15 -2 2 7.45 3.03 15 -2 2 5.12 2.08 15 2 2 4.11 2.42 -15 2 -2 3.24 1.86 -15 2 -3 4.56 2.21 -15 -2 -3 7.28 2.84 -15 2 -3 5.10 2.25 15 -2 3 8.19 3.01 15 -2 3 5.59 2.18 15 2 3 9.36 3.02 -15 2 -4 0.59 1.41 -15 -2 -4 0.67 1.79 -15 2 -4 1.41 1.83 15 -2 4 -0.87 1.76 15 -2 4 1.49 1.04 15 2 4 0.39 1.15 -15 -2 -5 5.01 2.41 -15 2 -5 6.47 2.76 -15 2 -5 5.99 2.46 15 -2 5 2.59 2.79 15 -2 5 2.86 1.54 15 2 5 3.07 1.80 -15 -2 -6 5.13 1.99 -15 2 -6 3.63 2.34 -15 2 -6 0.43 1.57 15 -2 6 3.34 1.97 15 -2 6 8.48 2.61 15 2 6 5.80 2.51 -15 -2 -7 5.48 2.86 -15 2 -7 6.72 2.53 -15 2 -7 3.57 1.92 15 -2 7 3.68 2.21 15 2 7 0.62 1.26 15 -3 -6 5.09 2.45 15 3 -6 2.30 1.81 -15 -3 6 0.68 1.11 -15 3 6 0.63 1.43 -15 -3 6 1.28 1.63 -15 3 6 1.42 1.59 15 -3 -5 -0.14 1.32 15 3 -5 1.36 1.36 -15 -3 5 -0.72 1.47 -15 3 5 0.49 1.71 -15 -3 5 1.69 1.95 -15 3 5 -0.41 1.62 15 -3 -4 2.88 2.10 15 3 -4 2.56 1.44 -15 -3 4 3.00 1.61 -15 3 4 3.35 2.08 -15 -3 4 5.00 2.66 -15 3 4 6.91 2.88 15 -3 -3 -0.18 1.67 15 3 -3 2.53 2.02 -15 -3 3 2.74 1.66 -15 3 3 2.69 1.99 -15 -3 3 3.65 2.67 -15 3 3 1.12 1.85 -15 3 2 2.90 2.07 15 -3 -2 3.12 1.73 15 3 -2 2.70 1.90 -15 3 2 3.55 2.07 -15 -3 2 2.34 1.74 -15 3 1 6.01 2.63 15 -3 -1 6.02 2.25 15 3 -1 1.86 1.47 -15 3 1 3.53 2.12 -15 -3 1 4.45 2.57 -15 3 0 3.44 2.22 15 -3 0 4.56 2.06 15 3 0 1.08 1.46 -15 3 0 2.88 2.01 -15 -3 0 5.03 2.41 -15 3 -1 13.86 3.55 15 -3 1 15.33 3.47 15 3 1 11.09 3.10 -15 3 -1 14.95 3.61 -15 -3 -1 16.98 3.88 -15 3 -2 0.81 1.67 -15 -3 -2 -0.63 1.56 -15 3 -2 2.43 1.79 15 -3 2 0.66 1.91 15 -3 2 1.60 1.76 15 3 2 1.09 1.69 -15 -3 -3 -1.00 1.28 -15 3 -3 0.61 1.47 -15 3 -3 0.83 1.43 15 -3 3 -0.61 1.78 15 -3 3 -0.70 1.39 -15 -3 -4 1.41 1.80 -15 3 -4 1.59 1.88 -15 3 -4 3.30 2.26 15 -3 4 2.14 2.64 15 -3 4 2.98 1.84 15 3 4 1.90 1.85 -15 -3 -5 1.95 1.24 -15 3 -5 3.27 1.87 -15 3 -5 1.52 1.88 15 -3 5 1.97 2.19 15 3 5 2.02 1.59 -15 -3 -6 5.44 2.33 -15 3 -6 3.57 1.93 -15 3 -6 2.16 2.06 -15 3 -6 2.54 2.46 15 -3 6 4.90 2.32 15 3 6 5.58 2.61 -15 4 3 2.30 1.94 15 -4 -3 3.27 1.69 15 4 -3 4.71 2.76 -15 4 3 -0.86 1.23 -15 4 2 1.84 2.08 15 -4 -2 3.27 1.97 15 4 -2 1.16 1.81 -15 4 2 4.09 2.31 -15 -4 2 0.38 1.54 -15 4 1 7.91 2.97 15 -4 -1 9.60 2.94 15 4 -1 5.45 2.50 -15 -4 1 8.57 3.06 -15 4 1 6.01 2.65 -15 4 0 6.59 2.70 15 -4 0 8.61 2.64 15 4 0 7.26 2.76 -15 -4 0 10.19 3.13 -15 4 0 11.12 3.44 -15 -4 -1 1.01 1.59 -15 4 -1 1.74 2.02 -15 4 -1 4.62 2.30 15 -4 1 4.88 2.65 15 -4 1 3.06 1.75 15 4 1 4.01 2.39 -15 -4 -2 0.39 1.51 -15 4 -2 -0.04 1.36 -15 4 -2 4.84 2.03 15 -4 2 6.04 2.70 15 -4 2 4.16 1.77 15 4 2 2.13 1.87 -15 4 -3 2.77 1.98 -15 -4 -3 2.43 2.11 -15 4 -3 -1.15 1.07 -15 4 -3 -0.29 1.83 15 -4 3 2.85 1.93 15 -4 3 1.00 1.08 15 4 3 2.35 1.72 16 0 -5 0.27 1.15 -16 0 5 0.88 1.72 -16 0 5 -0.20 1.52 16 0 -4 54.53 6.55 -16 0 4 63.20 7.21 -16 0 4 43.33 6.38 16 0 -3 4.21 2.36 -16 0 3 4.54 2.44 -16 0 3 4.25 2.30 16 0 -2 -0.93 1.86 -16 0 2 -0.37 1.55 -16 0 2 0.99 1.63 16 0 -1 -0.43 1.37 -16 0 1 1.03 1.01 -16 0 1 -0.57 1.62 -16 0 0 7.07 2.83 16 0 0 5.33 2.40 -16 0 0 5.58 1.99 -16 0 -1 -1.84 1.27 16 0 1 -0.20 1.12 -16 0 -1 0.24 1.32 -16 0 -2 8.80 3.26 16 0 2 2.98 2.57 16 0 2 11.24 2.94 -16 0 -2 7.54 2.71 -16 0 -3 -0.02 1.52 16 0 3 -0.45 1.56 -16 0 -3 -0.11 1.54 -16 0 -4 10.13 3.06 -16 0 -4 9.99 3.09 16 0 4 13.61 3.48 -16 0 -5 -0.78 1.31 -16 0 -5 0.77 1.82 16 0 5 2.46 1.99 16 1 -5 3.56 1.58 -16 -1 5 -0.12 1.38 -16 1 5 -0.72 1.43 -16 -1 5 -1.04 1.32 -16 1 5 -1.30 1.61 16 -1 -4 2.82 1.89 16 1 -4 3.67 1.96 -16 -1 4 4.76 2.47 -16 1 4 3.37 2.07 -16 -1 4 2.50 2.24 16 -1 -3 6.28 2.33 16 1 -3 2.55 1.43 -16 -1 3 8.07 3.00 -16 1 3 8.65 2.99 -16 -1 3 11.33 3.99 -16 1 3 7.15 2.90 16 -1 -2 0.98 1.46 16 1 -2 1.80 1.56 -16 -1 2 0.94 1.84 -16 1 2 0.10 1.26 -16 -1 2 1.45 2.15 -16 1 2 1.69 2.11 16 -1 -1 -0.20 1.60 16 1 -1 1.94 1.60 -16 -1 1 3.57 2.12 -16 1 1 0.33 2.03 -16 -1 1 5.00 2.81 -16 1 1 3.93 2.36 -16 1 0 7.54 2.87 16 -1 0 6.01 2.76 16 1 0 5.59 2.53 -16 -1 0 7.98 2.86 -16 1 0 6.00 2.50 -16 -1 0 10.89 3.34 -16 -1 -1 2.06 2.13 -16 1 -1 5.56 2.55 16 -1 1 0.10 1.36 16 1 1 3.00 2.09 -16 -1 -1 3.16 1.55 -16 1 -1 5.21 2.37 -16 -1 -2 3.05 1.94 -16 1 -2 6.48 2.58 16 -1 2 2.43 2.12 16 -1 2 1.22 1.26 16 1 2 8.37 2.96 -16 -1 -2 5.58 2.18 -16 1 -2 6.55 2.63 -16 -1 -3 5.75 2.45 -16 1 -3 2.24 1.63 16 -1 3 0.82 1.64 16 -1 3 1.04 1.40 16 1 3 2.05 1.76 -16 1 -3 2.18 2.03 -16 1 -4 7.21 2.57 -16 -1 -4 5.80 2.80 -16 1 -4 13.90 3.81 16 -1 4 4.94 2.74 16 -1 4 8.44 2.87 16 1 4 6.17 2.46 -16 1 -5 0.41 1.71 -16 -1 -5 -0.93 1.40 -16 1 -5 -0.54 1.52 16 -1 5 1.78 1.69 16 -1 5 0.69 1.65 16 1 5 2.47 1.20 16 -2 -4 -0.65 1.35 16 2 -4 1.45 1.51 -16 -2 4 0.64 1.24 -16 2 4 5.20 3.06 -16 -2 4 -1.53 1.49 -16 2 4 1.72 2.08 16 -2 -3 21.96 4.23 16 2 -3 20.49 4.18 -16 -2 3 23.50 4.37 -16 2 3 19.92 4.12 -16 -2 3 25.05 5.08 -16 2 3 20.09 4.50 16 -2 -2 23.12 4.29 16 2 -2 17.40 3.87 -16 -2 2 14.25 3.44 -16 2 2 16.60 4.21 -16 -2 2 18.00 4.41 -16 2 2 12.92 3.70 -16 2 1 6.55 2.82 16 -2 -1 3.95 2.25 16 2 -1 8.61 3.01 -16 -2 1 2.42 2.11 -16 2 1 5.38 2.44 -16 -2 1 3.71 2.57 -16 2 0 2.51 1.99 16 -2 0 -0.19 1.18 16 2 0 0.66 1.00 -16 2 0 0.14 1.23 -16 -2 0 -1.34 1.58 -16 -2 -1 1.09 1.59 -16 2 -1 1.48 1.63 16 -2 1 -1.06 1.62 16 2 1 -0.78 1.15 -16 2 -1 0.96 1.61 -16 -2 -2 0.01 1.11 -16 2 -2 3.81 2.01 16 -2 2 2.22 2.03 16 2 2 -0.43 1.09 -16 2 -2 2.67 1.99 -16 2 -3 4.27 2.15 -16 -2 -3 11.39 3.66 -16 2 -3 8.72 3.15 16 -2 3 4.00 2.03 16 -2 3 5.74 2.24 16 2 3 5.49 2.26 -16 2 -4 5.99 2.33 -16 -2 -4 14.04 3.78 -16 2 -4 3.20 2.06 16 -2 4 3.00 2.04 16 -2 4 8.95 2.61 16 2 4 13.81 3.78 -16 3 0 1.30 1.63 16 -3 0 2.35 1.74 16 3 0 2.77 2.13 -16 3 0 2.81 1.94 -16 -3 0 1.82 1.60 0 0 0 0.00 0.00 TITL APG-D-C2-1 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 13.432706 7.992018 15.206175 90.0000 90.3484 90.0000 ZERR 7.00 0.000358 0.000282 0.000489 0.0000 0.0027 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 77.00 70.00 7.00 7.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 66258 _shelx_res_file ; TITL apg-d-c2-1_a.res in P2(1)/n apg-d-c2-1.res created by SHELXL-2016/4 at 16:23:57 on 07-Jun-2018 REM Old TITL apg-d-c2-1_a.res in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.176, Rweak 0.016, Alpha 0.030, Orientation as input REM Formula found by SHELXT: C19 N O5 CELL 0.71073 13.4327 7.992 15.2062 90 90.348 90 ZERR 4 0.0004 0.0003 0.0005 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O UNIT 76 64 24 EQIV $1 -0.5+X,1.5-Y,0.5+Z L.S. 4 0 0 PLAN 4 HTAB O6 O1 HTAB O6 O3 HTAB O5 O2 BOND $H list 4 MORE -1 CONF fmap 2 53 acta 52 WGHT 0.085000 0.540000 FVAR 0.64469 O1 3 0.759354 0.528481 0.506840 11.00000 0.07662 0.08749 = 0.06970 0.00705 -0.00047 -0.02785 O2 3 0.363890 0.140419 0.396939 11.00000 0.07524 0.10102 = 0.07861 -0.02768 -0.03866 0.01098 O3 3 0.271328 0.788569 0.832888 11.00000 0.06953 0.11255 = 0.07841 -0.02256 -0.01313 0.04178 O4 3 0.694105 0.622118 1.016114 11.00000 0.06035 0.08895 = 0.07527 -0.01347 -0.01736 0.00044 O5 3 0.530747 0.305031 0.386189 11.00000 0.08753 0.08698 = 0.03713 -0.00006 -0.01386 0.00304 AFIX 147 H5 2 0.479652 0.260776 0.367754 11.00000 -1.50000 AFIX 0 O6 3 0.431505 0.802346 0.945572 11.00000 0.05810 0.05646 = 0.05501 -0.01051 0.00086 0.00903 H6 2 0.365910 0.833907 0.931863 11.00000 0.09633 C0AA 1 0.445188 0.462629 0.784650 11.00000 0.04580 0.05466 = 0.03426 -0.00137 -0.00455 0.00089 AFIX 43 H0AA 2 0.407023 0.415913 0.739712 11.00000 -1.20000 AFIX 0 C1 1 0.553488 0.249493 0.658788 11.00000 0.04356 0.03970 = 0.03616 -0.00343 -0.00288 0.00461 C2 1 0.621925 0.341606 0.610675 11.00000 0.04276 0.04402 = 0.04054 -0.00204 -0.00662 -0.00063 AFIX 43 H2 2 0.674345 0.392670 0.640554 11.00000 -1.20000 AFIX 0 C3 1 0.615696 0.361003 0.519945 11.00000 0.04598 0.04492 = 0.04171 0.00070 -0.00128 0.00122 C4 1 0.535824 0.287960 0.474602 11.00000 0.05599 0.04769 = 0.03918 -0.00478 -0.00853 0.00968 C5 1 0.463951 0.201691 0.521140 11.00000 0.04269 0.04793 = 0.05027 -0.00935 -0.00953 0.00503 C6 1 0.474439 0.181778 0.612189 11.00000 0.04225 0.04674 = 0.04856 -0.00359 0.00043 -0.00064 AFIX 43 H6A 2 0.426579 0.120883 0.642407 11.00000 -1.20000 AFIX 0 C7 1 0.691314 0.456872 0.472775 11.00000 0.06561 0.06386 = 0.04980 0.00629 -0.00036 -0.00709 H7 2 0.682539 0.461801 0.407007 11.00000 0.07320 C8 1 0.377222 0.129343 0.476467 11.00000 0.05365 0.07207 = 0.07461 -0.02195 -0.02169 0.00582 H8 2 0.324450 0.067829 0.521362 11.00000 0.06476 C9 1 0.536485 0.389846 0.804941 11.00000 0.04584 0.04335 = 0.03094 0.00456 0.00063 0.00132 C10 1 0.592229 0.466280 0.871187 11.00000 0.03952 0.04975 = 0.03731 0.00336 -0.00026 0.00146 AFIX 43 H10 2 0.654434 0.422634 0.885479 11.00000 -1.20000 AFIX 0 C11 1 0.557832 0.606562 0.917003 11.00000 0.04267 0.04796 = 0.03731 0.00038 0.00066 -0.00432 C12 1 0.464360 0.673746 0.896712 11.00000 0.04584 0.04318 = 0.03735 0.00373 0.00598 -0.00007 C13 1 0.408390 0.601599 0.828281 11.00000 0.04326 0.05854 = 0.03620 0.00386 -0.00015 0.00510 C14 1 0.617622 0.681374 0.987919 11.00000 0.04722 0.06616 = 0.05782 -0.01063 -0.00398 -0.00248 H14 2 0.592053 0.790376 1.014189 11.00000 0.06683 C15 1 0.311535 0.667347 0.801179 11.00000 0.05614 0.08703 = 0.05547 -0.01527 -0.00836 0.02343 H15 2 0.276580 0.595194 0.755304 11.00000 0.08669 C16 1 0.567970 0.227735 0.758588 11.00000 0.05715 0.04333 = 0.03490 0.00211 -0.00284 0.00305 C17 1 0.677555 0.181688 0.777382 11.00000 0.07974 0.06668 = 0.04839 -0.00446 -0.01656 0.03294 AFIX 137 H17A 2 0.695707 0.086163 0.742724 11.00000 -1.50000 H17B 2 0.685618 0.155720 0.838652 11.00000 -1.50000 H17C 2 0.719548 0.274519 0.762469 11.00000 -1.50000 AFIX 0 C18 1 0.502033 0.086619 0.794573 11.00000 0.11868 0.05136 = 0.05318 0.00617 0.01144 -0.01399 AFIX 137 H18A 2 0.433239 0.115432 0.786234 11.00000 -1.50000 H18B 2 0.515438 0.071710 0.856159 11.00000 -1.50000 H18C 2 0.516230 -0.015436 0.763805 11.00000 -1.50000 AFIX 0 HKLF 4 END WGHT 0.0844 0.5550 REM Highest difference peak 0.253, deepest hole -0.273, 1-sigma level 0.044 Q1 1 0.5602 0.2369 0.7064 11.00000 0.05 0.25 Q2 1 0.4290 0.2247 0.3777 11.00000 0.05 0.23 Q3 1 0.3764 0.6308 0.8142 11.00000 0.05 0.18 Q4 1 0.5248 0.6622 0.8989 11.00000 0.05 0.18 ; _shelx_res_checksum 156