#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200173.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_2200173 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first o151 _journal_page_last o153 _publ_section_title ; 4-(4-Bromophenyl)-3,7,7-trimethyl-4,7,8,9-tetrahydro-2H-pyrazolo[3,4-b]- quinolin-5(6H)-one ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' 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 H20 Br N3 O' _chemical_formula_sum 'C19 H20 Br N3 O' _chemical_formula_weight 386.29 _chemical_melting_point 587 _symmetry_cell_setting monoclinic 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 8.6673(2) _cell_length_b 14.6092(3) _cell_length_c 14.4783(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.2870(10) _cell_angle_gamma 90.00 _cell_volume 1750.46(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(10) _exptl_crystal_density_diffrn 1.466 _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 Br1 -.09022(4) 1.01949(2) .84992(2) .04207(15) Uani d . 1 . . Br N1 .0258(3) .50866(14) .62544(15) .0199(5) Uani d . 1 . . N N2 .0657(3) .49693(14) .72350(15) .0195(5) Uani d . 1 . . N C3 .1663(3) .56229(17) .77329(17) .0169(5) Uani d . 1 . . C C31 .2301(3) .55976(19) .88096(18) .0239(6) Uani d . 1 . . C C3A .1942(3) .62174(17) .70591(18) .0174(5) Uani d . 1 . . C C4 .2828(3) .71108(16) .71244(17) .0162(5) Uani d . 1 . . C C41 .1923(3) .78752(16) .74617(17) .0173(5) Uani d . 1 . . C C42 .0503(3) .82395(18) .68373(18) .0236(6) Uani d . 1 . . C C43 -.0344(4) .89235(19) .7149(2) .0282(6) Uani d . 1 . . C C44 .0238(3) .92447(18) .8085(2) .0270(6) Uani d . 1 . . C C45 .1620(3) .88979(19) .8717(2) .0265(6) Uani d . 1 . . C C46 .2455(3) .82105(18) .84023(18) .0219(6) Uani d . 1 . . C C4A .3055(3) .73065(16) .61405(17) .0152(5) Uani d . 1 . . C C5 .4245(3) .79835(16) .61028(18) .0164(5) Uani d . 1 . . C O51 .5056(2) .83908(12) .68440(12) .0204(4) Uani d . 1 . . O C6 .4554(3) .81778(18) .51496(17) .0199(5) Uani d . 1 . . C C71 .3517(3) .81299(19) .33254(18) .0243(6) Uani d . 1 . . C C72 .1785(3) .87697(18) .42704(18) .0217(6) Uani d . 1 . . C C7 .3065(3) .80477(17) .42642(17) .0175(5) Uani d . 1 . . C C8 .2430(3) .70802(17) .43343(17) .0177(5) Uani d . 1 . . C C8A .2205(3) .68698(16) .53010(17) .0159(5) Uani d . 1 . . C N9 .1125(2) .61950(14) .52916(15) .0195(5) Uani d . 1 . . N C9A .1066(3) .58405(16) .61735(17) .0169(5) Uani d . 1 . . C H2 .0295 .4515 .7512 .023 Uiso calc R 1 . . H H31A .1566 .5241 .9070 .036 Uiso calc R 1 . . H H31B .2383 .6223 .9064 .036 Uiso calc R 1 . . H H31C .3372 .5312 .9002 .036 Uiso calc R 1 . . H H4 .3918 .7043 .7608 .019 Uiso calc R 1 . . H H42 .0112 .8018 .6193 .028 Uiso calc R 1 . . H H43 -.1312 .9166 .6722 .034 Uiso calc R 1 . . H H45 .2002 .9123 .9361 .032 Uiso calc R 1 . . H H46 .3409 .7965 .8839 .026 Uiso calc R 1 . . H H6A .5426 .7768 .5084 .024 Uiso calc R 1 . . H H6B .4941 .8816 .5155 .024 Uiso calc R 1 . . H H71A .4421 .7718 .3350 .037 Uiso calc R 1 . . H H71B .3835 .8762 .3247 .037 Uiso calc R 1 . . H H71C .2585 .7963 .2777 .037 Uiso calc R 1 . . H H72A .0872 .8711 .3681 .033 Uiso calc R 1 . . H H72B .2258 .9382 .4296 .033 Uiso calc R 1 . . H H72C .1408 .8678 .4838 .033 Uiso calc R 1 . . H H8A .1382 .7004 .3827 .021 Uiso calc R 1 . . H H8B .3197 .6632 .4204 .021 Uiso calc R 1 . . H H9 .0478 .5987 .4742 .023 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 Br1 .0643(3) .0205(2) .0551(2) .01212(14) .03881(18) .00133(14) N1 .0265(12) .0141(11) .0202(11) -.0007(9) .0088(9) .0009(9) N2 .0274(12) .0137(10) .0197(11) -.0013(8) .0105(9) .0038(9) C3 .0200(13) .0133(13) .0193(12) .0041(10) .0088(10) .0016(10) C31 .0314(15) .0206(14) .0204(13) .0005(11) .0090(11) .0028(11) C3A .0173(13) .0126(12) .0220(13) .0020(9) .0054(10) .0002(10) C4 .0198(13) .0135(12) .0150(12) .0009(10) .0045(9) .0001(10) C41 .0236(13) .0105(12) .0206(12) -.0037(10) .0108(10) .0005(10) C42 .0332(15) .0187(14) .0198(13) .0031(11) .0092(11) .0020(11) C43 .0359(16) .0198(15) .0319(15) .0080(12) .0146(12) .0086(12) C44 .0377(16) .0153(14) .0360(16) .0002(11) .0234(12) .0015(12) C45 .0343(16) .0232(15) .0283(15) -.0089(12) .0191(12) -.0089(12) C46 .0232(14) .0220(14) .0219(13) -.0051(11) .0087(10) -.0040(11) C4A .0197(12) .0093(12) .0174(12) .0023(9) .0068(9) .0002(9) C5 .0156(12) .0113(12) .0221(13) .0058(9) .0051(10) .0018(10) O51 .0209(9) .0179(9) .0213(9) -.0021(7) .0046(7) -.0051(8) C6 .0194(13) .0188(13) .0224(13) -.0034(10) .0075(10) -.0010(10) C71 .0303(14) .0233(15) .0226(14) -.0020(11) .0125(11) .0012(11) C72 .0261(14) .0160(13) .0233(14) .0030(10) .0078(10) -.0003(11) C7 .0207(13) .0131(12) .0199(13) -.0014(10) .0075(10) .0016(10) C8 .0234(13) .0126(13) .0181(12) -.0003(10) .0078(10) -.0005(10) C8A .0167(12) .0115(12) .0200(13) .0020(9) .0060(9) .0029(10) N9 .0231(11) .0159(11) .0168(10) -.0050(9) .0020(8) -.0002(9) C9A .0214(13) .0118(13) .0191(12) .0023(10) .0081(10) .0035(10) 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 Br1 C44 . 1.901(3) yes N1 C9A . 1.329(3) yes N1 N2 . 1.368(3) yes N2 C3 . 1.348(3) yes N2 H2 . .8800 no C3 C3A . 1.380(4) no C3 C31 . 1.492(3) no C31 H31A . .9800 no C31 H31B . .9800 no C31 H31C . .9800 no C3A C9A . 1.395(3) no C3A C4 . 1.503(3) no C4 C4A . 1.522(3) no C4 C41 . 1.526(3) no C4 H4 . 1.0000 no C41 C46 . 1.391(4) no C41 C42 . 1.398(4) no C42 C43 . 1.392(4) no C42 H42 . .9500 no C43 C44 . 1.381(4) no C43 H43 . .9500 no C44 C45 . 1.370(4) no C45 C46 . 1.391(4) no C45 H45 . .9500 no C46 H46 . .9500 no C4A C8A . 1.377(3) no C4A C5 . 1.442(3) no C5 O51 . 1.246(3) no C5 C6 . 1.509(4) no C6 C7 . 1.537(3) no C6 H6A . .9900 no C6 H6B . .9900 no C71 C7 . 1.527(3) no C71 H71A . .9800 no C71 H71B . .9800 no C71 H71C . .9800 no C72 C7 . 1.533(3) no C72 H72A . .9800 no C72 H72B . .9800 no C72 H72C . .9800 no C7 C8 . 1.531(3) no C8 C8A . 1.501(3) no C8 H8A . .9900 no C8 H8B . .9900 no C8A N9 . 1.357(3) yes N9 C9A . 1.393(3) yes N9 H9 . .8800 no _cod_database_code 2200173