#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200163.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2200163 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first o328 _journal_page_last o329 _publ_section_title ; Ethyl 4-(2,3,5,6-tetrahydro-3,3-dimethyl-5,6-dioxo-1,2-cycloheptapyrazol-2-yl)- benzoate ; loop_ _publ_author_name 'Kubo, Kanji' 'Mori, Akira' _chemical_formula_moiety 'C19 H18 N2 O4' _chemical_formula_sum 'C19 H18 N2 O4' _chemical_formula_iupac 'C19 H18 N2 O4' _chemical_formula_weight 338.35 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 19.028(3) _cell_length_b 19.166(3) _cell_length_c 9.4466(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3445.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _exptl_crystal_density_diffrn 1.305 _diffrn_ambient_temperature 296(2) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol N1 .88831(14) .14229(13) .0112(3) .0469(7) Uani d . 1 . . N N2 .86161(13) .08041(12) .0463(3) .0435(7) Uani d . 1 . . N O1 .75989(15) .38435(12) .2298(3) .0966(10) Uani d . 1 . . O O2 .72097(12) .28665(12) .4086(3) .0699(8) Uani d . 1 . . O O3 1.01239(14) -.15229(13) -.3384(3) .0802(9) Uani d . 1 . . O O4 .94270(12) -.21630(13) -.1981(3) .0688(8) Uani d . 1 . . O C1 .7870(2) .32710(17) .2157(4) .0602(11) Uani d . 1 . . C C2 .75567(18) .26834(17) .3058(4) .0526(9) Uani d . 1 . . C C3 .76344(17) .19528(16) .2746(4) .0517(9) Uani d . 1 . . C H3 .7350 .1657 .3275 .062 Uiso calc R 1 . . H C4 .80545(16) .16337(15) .1810(3) .0411(8) Uani d . 1 . . C C5 .85689(16) .19151(15) .0873(3) .0426(8) Uani d . 1 . . C C6 .87661(17) .26265(15) .0660(4) .0534(9) Uani d . 1 . . C H6 .9144 .2702 .0056 .064 Uiso calc R 1 . . H C7 .8474(2) .31988(16) .1223(4) .0598(10) Uani d . 1 . . C H7 .8691 .3616 .0977 .072 Uiso calc R 1 . . H C8 .80673(16) .08491(14) .1579(3) .0417(8) Uani d . 1 . . C C9 .73500(16) .05919(15) .1045(4) .0533(9) Uani d . 1 . . C H9A .7367 .0096 .0904 .080 Uiso calc R 1 . . H H9B .7240 .0818 .0166 .080 Uiso calc R 1 . . H H9C .6995 .0701 .1733 .080 Uiso calc R 1 . . H C10 .83016(18) .04850(15) .2944(3) .0556(10) Uani d . 1 . . C H10A .8311 -.0010 .2795 .083 Uiso calc R 1 . . H H10B .7977 .0593 .3691 .083 Uiso calc R 1 . . H H10C .8763 .0644 .3200 .083 Uiso calc R 1 . . H C11 .88638(16) .02091(15) -.0251(3) .0401(8) Uani d . 1 . . C C12 .86496(17) -.04586(15) .0119(3) .0470(9) Uani d . 1 . . C H12 .8323 -.0520 .0841 .056 Uiso calc R 1 . . H C13 .89192(17) -.10316(16) -.0580(3) .0472(8) Uani d . 1 . . C H13 .8776 -.1476 -.0312 .057 Uiso calc R 1 . . H C14 .93974(16) -.09575(17) -.1668(4) .0483(8) Uani d . 1 . . C C15 .95942(17) -.02876(18) -.2044(4) .0576(10) Uani d . 1 . . C H15 .9912 -.0227 -.2781 .069 Uiso calc R 1 . . H C16 .93345(16) .02937(17) -.1359(4) .0532(9) Uani d . 1 . . C H16 .9474 .0738 -.1638 .064 Uiso calc R 1 . . H C17 .96954(19) -.1561(2) -.2448(4) .0588(10) Uani d . 1 . . C C18 .9630(2) -.27980(19) -.2713(4) .0785(13) Uani d . 1 . . C H18A 1.0137 -.2814 -.2820 .094 Uiso calc R 1 . . H H18B .9420 -.2808 -.3648 .094 Uiso calc R 1 . . H C19 .93878(19) -.34069(18) -.1878(4) .0796(13) Uani d . 1 . . C H19A .9520 -.3829 -.2355 .119 Uiso calc R 1 . . H H19B .8886 -.3390 -.1782 .119 Uiso calc R 1 . . H H19C .9601 -.3396 -.0957 .119 Uiso calc R 1 . . H 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 N1 .0529(18) .0388(15) .0489(17) -.0065(14) .0043(15) .0014(14) N2 .0482(16) .0353(15) .0472(18) -.0002(13) .0113(14) .0002(14) O1 .109(2) .0492(16) .131(3) .0277(15) -.001(2) .0067(17) O2 .0709(17) .0655(16) .0734(18) .0176(13) -.0015(15) -.0229(15) O3 .0790(19) .0847(19) .077(2) .0077(15) .0273(17) -.0220(16) O4 .0736(17) .0551(16) .0776(19) .0036(13) .0131(15) -.0263(15) C1 .072(3) .038(2) .070(3) .0117(19) -.020(2) -.005(2) C2 .050(2) .051(2) .057(2) .0113(16) -.014(2) -.015(2) C3 .051(2) .047(2) .058(2) -.0047(17) .006(2) -.0025(18) C4 .0421(18) .0397(18) .042(2) .0014(16) -.0009(17) .0016(17) C5 .042(2) .0393(19) .046(2) -.0035(16) -.0019(18) .0035(17) C6 .061(2) .043(2) .057(2) -.0079(17) -.0037(19) .0033(18) C7 .074(3) .040(2) .066(3) -.007(2) -.012(2) .0039(19) C8 .0471(19) .0381(18) .040(2) .0010(16) .0089(17) .0014(16) C9 .050(2) .0447(19) .065(2) -.0102(16) .0072(19) -.0059(18) C10 .073(2) .049(2) .046(2) -.0006(18) .0039(19) .0044(18) C11 .041(2) .0419(19) .037(2) .0050(16) .0009(16) -.0014(16) C12 .050(2) .047(2) .044(2) .0015(17) .0059(17) .0010(17) C13 .054(2) .0411(19) .046(2) .0034(16) -.0055(19) -.0017(17) C14 .046(2) .052(2) .047(2) .0071(17) .0009(19) -.0089(19) C15 .052(2) .066(2) .055(2) -.0014(18) .014(2) -.008(2) C16 .056(2) .049(2) .054(2) -.0008(18) .013(2) -.0028(18) C17 .050(2) .066(3) .061(3) .003(2) -.003(2) -.020(2) C18 .086(3) .064(3) .085(3) .012(2) -.003(3) -.043(3) C19 .070(3) .058(2) .110(4) .009(2) .009(3) -.026(3) 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 N1 C5 . 1.328(3) yes N1 N2 . 1.332(3) yes N2 C8 . 1.486(4) yes N2 C11 . 1.406(3) yes O1 C1 . 1.220(4) yes O2 C2 . 1.225(4) yes O3 C17 . 1.205(4) ? O4 C17 . 1.337(4) ? O4 C18 . 1.452(3) ? C1 C2 . 1.533(5) yes C1 C7 . 1.455(5) yes C2 C3 . 1.439(4) yes C3 C4 . 1.340(4) yes C3 H3 . .9300 ? C4 C5 . 1.426(4) yes C4 C8 . 1.520(4) yes C5 C6 . 1.428(4) yes C6 C7 . 1.339(4) yes C6 H6 . .9300 ? C7 H7 . .9300 ? C8 C9 . 1.536(4) yes C8 C10 . 1.533(4) yes C9 H9A . .9600 ? C9 H9B . .9600 ? C9 H9C . .9600 ? C10 H10A . .9600 ? C10 H10B . .9600 ? C10 H10C . .9600 ? C11 C16 . 1.387(4) ? C11 C12 . 1.388(4) ? C12 C13 . 1.380(4) ? C12 H12 . .9300 ? C13 C14 . 1.380(4) ? C13 H13 . .9300 ? C14 C15 . 1.384(4) ? C14 C17 . 1.484(5) ? C15 C16 . 1.380(4) ? C15 H15 . .9300 ? C16 H16 . .9300 ? C18 C19 . 1.482(5) ? C18 H18A . .9700 ? C18 H18B . .9700 ? C19 H19A . .9600 ? C19 H19B . .9600 ? C19 H19C . .9600 ? _cod_database_code 2200163