#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2200175.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_2200175 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first o157 _journal_page_last o159 _publ_section_title ; 3,7,7-Trimethyl-4-phenyl-4,7,8,9-tetrahydro-2H-pyrazolo[3,4-b]quinolin-5- (6H)-one ; loop_ _publ_author_name 'Cannon, Debbie' 'Quesada, Antonio' 'Quiroga, Jairo' "Mej\'ia, Diana" 'Insuasty, Braulio' 'Abonia, Rodrigo' 'Cobo, Justo' 'Nogueras, Manuel' "S\'anchez, Adolfo" 'Low, John Nicolson' _chemical_formula_moiety 'C19 H21 N3 O' _chemical_formula_sum 'C19 H21 N3 O' _chemical_formula_weight 307.39 _chemical_melting_point 502 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_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 10.0870(5) _cell_length_b 14.1978(5) _cell_length_c 11.1928(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.0340(14) _cell_angle_gamma 90.00 _cell_volume 1594.08(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(10) _exptl_crystal_density_diffrn 1.281 _diffrn_ambient_temperature 150.0(10) 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 .03979(17) .48816(12) .66069(15) .0288(4) Uani d . 1 . . N N2 .08492(17) .49441(12) .77984(15) .0301(4) Uani d . 1 . . N C3 .1736(2) .42667(14) .81730(18) .0272(5) Uani d . 1 . . C C3A .18685(19) .37042(14) .71874(17) .0248(5) Uani d . 1 . . C C31 .2363(2) .42237(16) .94324(18) .0372(6) Uani d . 1 . . C C4 .26485(19) .28267(13) .69798(17) .0253(5) Uani d . 1 . . C C41 .1994(2) .19599(14) .74721(17) .0253(5) Uani d . 1 . . C C42 .0970(2) .14951(14) .6799(2) .0309(5) Uani d . 1 . . C C43 .0345(2) .07262(15) .7259(2) .0365(6) Uani d . 1 . . C C44 .0739(2) .04152(16) .8410(2) .0405(6) Uani d . 1 . . C C45 .1757(2) .08656(15) .9089(2) .0388(6) Uani d . 1 . . C C46 .2388(2) .16331(14) .86258(19) .0319(5) Uani d . 1 . . C C4A .27697(19) .27521(14) .56348(18) .0248(5) Uani d . 1 . . C C5 .37729(19) .21344(14) .52547(18) .0249(5) Uani d . 1 . . C O51 .45326(13) .16825(10) .59917(12) .0309(4) Uani d . 1 . . O C6 .39161(19) .20477(15) .39318(18) .0294(5) Uani d . 1 . . C C7 .2616(2) .21729(14) .31167(17) .0264(5) Uani d . 1 . . C C71 .2881(2) .22044(16) .17987(18) .0353(6) Uani d . 1 . . C C72 .1679(2) .13499(15) .3284(2) .0352(6) Uani d . 1 . . C C8A .19262(19) .32104(13) .47854(18) .0245(5) Uani d . 1 . . C C8 .1995(2) .31012(14) .34582(17) .0291(5) Uani d . 1 . . C N9 .09775(16) .38222(12) .50788(14) .0286(4) Uani d . 1 . . N C9A .10411(19) .41232(14) .62706(18) .0260(5) Uani d . 1 . . C H2 .0587 .5384 .8276 .036 Uiso calc R 1 . . H H31A .2159 .4802 .9854 .056 Uiso calc PR .50 . . H H31B .3330 .4160 .9437 .056 Uiso calc PR .50 . . H H31C .2012 .3680 .9838 .056 Uiso calc PR .50 . . H H31D .2842 .3626 .9565 .056 Uiso calc PR .50 . . H H31E .1671 .4268 .9982 .056 Uiso calc PR .50 . . H H31F .2989 .4748 .9581 .056 Uiso calc PR .50 . . H H4 .3564 .2895 .7410 .030 Uiso calc R 1 . . H H42 .0689 .1706 .6008 .037 Uiso calc R 1 . . H H43 -.0355 .0413 .6781 .044 Uiso calc R 1 . . H H44 .0306 -.0108 .8730 .049 Uiso calc R 1 . . H H45 .2034 .0652 .9880 .047 Uiso calc R 1 . . H H46 .3096 .1938 .9103 .038 Uiso calc R 1 . . H H6A .4289 .1419 .3779 .035 Uiso calc R 1 . . H H6B .4563 .2526 .3713 .035 Uiso calc R 1 . . H H71A .3314 .1618 .1590 .053 Uiso calc R 1 . . H H71B .3464 .2739 .1670 .053 Uiso calc R 1 . . H H71C .2035 .2276 .1291 .053 Uiso calc R 1 . . H H72A .2097 .0761 .3060 .053 Uiso calc R 1 . . H H72B .0840 .1443 .2772 .053 Uiso calc R 1 . . H H72C .1500 .1317 .4127 .053 Uiso calc R 1 . . H H8A .2522 .3628 .3173 .035 Uiso calc R 1 . . H H8B .1082 .3146 .3040 .035 Uiso calc R 1 . . H H9 .0345 .4022 .4537 .034 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 .0358(10) .0259(10) .0242(10) .0021(8) .0004(8) -.0023(8) N2 .0394(11) .0260(10) .0252(10) -.0006(8) .0045(8) -.0040(8) C3 .0309(11) .0244(11) .0259(12) -.0041(10) .0009(9) .0015(9) C3A .0258(11) .0243(11) .0239(11) -.0021(9) .0011(9) .0013(9) C31 .0477(14) .0353(13) .0277(13) -.0035(11) -.0004(11) -.0030(10) C4 .0257(11) .0263(11) .0229(11) -.0002(9) -.0019(9) .0014(9) C41 .0290(11) .0239(11) .0240(12) .0061(9) .0067(9) -.0003(9) C42 .0332(12) .0329(13) .0265(12) -.0004(10) .0033(10) .0005(10) C43 .0416(13) .0312(13) .0372(14) -.0090(11) .0067(11) -.0029(11) C44 .0548(16) .0268(12) .0421(15) -.0016(11) .0151(13) .0025(11) C45 .0560(15) .0317(13) .0297(13) .0076(12) .0092(12) .0060(11) C46 .0386(13) .0291(12) .0278(12) .0026(10) .0028(10) .0014(10) C4A .0250(11) .0250(11) .0244(11) -.0014(9) .0024(9) .0010(9) C5 .0226(10) .0236(11) .0283(12) -.0036(9) .0008(9) .0020(9) O51 .0306(8) .0309(9) .0304(9) .0041(7) -.0001(7) .0058(7) C6 .0270(11) .0337(12) .0280(12) .0025(10) .0045(9) .0015(10) C7 .0287(11) .0270(11) .0232(12) .0009(9) .0009(9) -.0014(9) C71 .0364(12) .0415(14) .0275(12) .0024(11) .0013(10) -.0027(10) C72 .0366(13) .0312(13) .0373(14) -.0014(10) .0009(10) -.0030(10) C8A .0257(11) .0203(11) .0272(12) -.0006(9) .0018(9) -.0013(9) C8 .0336(12) .0293(12) .0240(12) .0018(10) .0008(9) .0021(9) N9 .0295(10) .0314(10) .0233(10) .0057(8) -.0048(8) -.0036(8) C9A .0285(11) .0225(11) .0267(12) -.0023(9) .0023(9) -.0021(9) 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 C9A . 1.332(2) yes N1 N2 . 1.366(2) yes N2 C3 . 1.350(3) yes N2 H2 . .8800 no C3 C3A . 1.380(3) no C3 C31 . 1.484(3) no C3A C9A . 1.387(3) no C3A C4 . 1.505(3) no C31 H31A . .9800 no C31 H31B . .9800 no C31 H31C . .9800 no C31 H31D . .9800 no C31 H31E . .9800 no C31 H31F . .9800 no C4 C41 . 1.526(3) no C4 C4A . 1.527(3) no C4 H4 . 1.0000 no C41 C42 . 1.381(3) no C41 C46 . 1.390(3) no C42 C43 . 1.386(3) no C42 H42 . .9500 no C43 C44 . 1.381(3) no C43 H43 . .9500 no C44 C45 . 1.370(3) no C44 H44 . .9500 no C45 C46 . 1.389(3) no C45 H45 . .9500 no C46 H46 . .9500 no C4A C8A . 1.371(3) no C4A C5 . 1.437(3) no C5 O51 . 1.244(2) no C5 C6 . 1.508(3) no C6 C7 . 1.527(3) no C6 H6A . .9900 no C6 H6B . .9900 no C7 C8 . 1.525(3) no C7 C72 . 1.526(3) no C7 C71 . 1.527(3) no C71 H71A . .9800 no C71 H71B . .9800 no C71 H71C . .9800 no C72 H72A . .9800 no C72 H72B . .9800 no C72 H72C . .9800 no C8A N9 . 1.358(2) yes C8A C8 . 1.502(3) no C8 H8A . .9900 no C8 H8B . .9900 no N9 C9A . 1.396(2) yes N9 H9 . .8800 no