#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2011585.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_2011585 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2000 _journal_volume 56 _journal_page_first 1361 _journal_page_last 1363 _publ_section_title ; Disappearance of intramolecular stacking due to one atom movement or increment of a "propylene linker" in pyrazolo[3,4-d]pyrimidine-based flexible models ; loop_ _publ_author_name 'Maulik, Prakas R.' 'Avasthi, Kamlakar' 'Sarkhel, Sanjay' 'Chandra, Tilak' 'Rawat, Diwan S.' 'Logsdon, Brad' 'Jacobson, Robert A.' _chemical_name_common Pyrazolo[3,4-d]pyrimidine _chemical_formula_sum 'C18 H22 N8 O2 S2' _chemical_formula_weight 446.56 _chemical_melting_point 150 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.736(7) _cell_length_b 8.308(2) _cell_length_c 17.467(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.12(2) _cell_angle_gamma 90.00 _cell_volume 4169.8(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.423 _diffrn_ambient_temperature 293(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 .08564(6) .62969(18) -.28542(10) .0591(4) Uani d . 1 . . N N2 .09756(6) .7441(2) -.32902(11) .0705(4) Uani d . 1 . . N C3 .09214(8) .8831(3) -.29923(14) .0688(5) Uani d . 1 . . C H3 .0979 .9821 -.3177 .083 Uiso calc R 1 . . H C3A .07636(6) .8636(2) -.23533(12) .0568(4) Uani d . 1 . . C C4 .06206(6) .9544(2) -.18356(12) .0549(4) Uani d . 1 . . C O4 .06165(5) 1.11449(15) -.19000(10) .0693(4) Uani d . 1 . . O CO4 .04383(8) 1.2044(3) -.13974(15) .0752(6) Uani d . 1 . . C HO4A .0432 1.3168 -.1528 .113 Uiso calc R 1 . . H HO4B .0635 1.1877 -.0809 .113 Uiso calc R 1 . . H HO4C .0129 1.1686 -.1520 .113 Uiso calc R 1 . . H N5 .04876(5) .88416(17) -.12953(10) .0551(4) Uani d . 1 . . N C6 .04910(6) .7220(2) -.12731(11) .0542(4) Uani d . 1 . . C S6 .03384(2) .62550(6) -.05308(4) .0699(2) Uani d . 1 . . S CS6 .01876(9) .7890(3) -.00360(16) .0864(7) Uani d . 1 . . C HS6A .0093 .7481 .0381 .130 Uiso calc R 1 . . H HS6B -.0064 .8488 -.0454 .130 Uiso calc R 1 . . H HS6C .0452 .8582 .0232 .130 Uiso calc R 1 . . H N7 .05989(5) .62061(18) -.17441(10) .0574(4) Uani d . 1 . . N C7A .07327(6) .6979(2) -.22805(11) .0540(4) Uani d . 1 . . C N1' .21661(5) .19233(19) -.16005(9) .0570(4) Uani d . 1 . . N N2' .22763(6) .0909(2) -.21125(10) .0673(4) Uani d . 1 . . N C3' .22196(7) -.0549(3) -.18828(12) .0678(5) Uani d . 1 . . C H3' .2271 -.1484 -.2124 .081 Uiso calc R 1 . . H C3'A .20724(6) -.0533(2) -.12306(11) .0581(4) Uani d . 1 . . C C4' .19595(7) -.1701(2) -.07508(12) .0619(5) Uani d . 1 . . C O4' .19753(6) -.31573(18) -.07920(11) .0862(5) Uani d . 1 . . O N5' .18098(5) -.09753(18) -.01662(9) .0574(4) Uani d . 1 . . N C5' .17019(9) -.2054(3) .03898(15) .0774(6) Uani d . 1 . . C H5'1 .1785 -.3136 .0318 .116 Uiso calc R 1 . . H H5'2 .1375 -.2002 .0248 .116 Uiso calc R 1 . . H H5'3 .1875 -.1729 .0967 .116 Uiso calc R 1 . . H C6' .17761(6) .0666(2) -.01024(10) .0511(4) Uani d . 1 . . C S6' .154665(17) .13194(6) .06014(3) .06088(19) Uani d . 1 . . S CS6' .15532(8) .3456(3) .04607(14) .0684(5) Uani d . 1 . . C HS6D .1412 .3981 .0784 .103 Uiso calc R 1 . . H HS6E .1382 .3714 -.0127 .103 Uiso calc R 1 . . H HS6F .1869 .3818 .0650 .103 Uiso calc R 1 . . H N7' .18896(5) .17353(18) -.05219(9) .0532(3) Uani d . 1 . . N C7'A .20397(6) .1076(2) -.10772(10) .0519(4) Uani d . 1 . . C C8 .08687(7) .4594(2) -.30225(13) .0657(5) Uani d . 1 . . C H8A .0862 .4455 -.3579 .079 Uiso calc R 1 . . H H8B .0594 .4080 -.3023 .079 Uiso calc R 1 . . H C9 .12961(7) .3788(2) -.23766(12) .0611(5) Uani d . 1 . . C H9A .1258 .2631 -.2446 .073 Uiso calc R 1 . . H H9B .1323 .4052 -.1817 .073 Uiso calc R 1 . . H C10 .17456(6) .4267(2) -.24342(11) .0597(4) Uani d . 1 . . C H10A .1744 .3835 -.2951 .072 Uiso calc R 1 . . H H10B .1761 .5431 -.2459 .072 Uiso calc R 1 . . H C11 .21670(6) .3659(2) -.16919(12) .0587(4) Uani d . 1 . . C H11A .2444 .3975 -.1758 .070 Uiso calc R 1 . . H H11B .2181 .4160 -.1180 .070 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 .0683(9) .0549(9) .0614(9) .0026(7) .0346(7) -.0009(7) N2 .0866(11) .0689(11) .0694(10) .0038(8) .0460(9) .0066(8) C3 .0837(13) .0626(12) .0735(12) .0059(9) .0464(11) .0100(9) C3A .0581(9) .0518(10) .0639(10) .0047(7) .0292(8) .0068(8) C4 .0541(9) .0475(10) .0645(10) .0018(7) .0264(8) .0032(7) O4 .0872(9) .0456(7) .0887(10) .0050(6) .0504(8) .0072(6) CO4 .0965(15) .0497(11) .0857(14) .0093(10) .0446(12) -.0030(10) N5 .0574(8) .0496(8) .0620(9) .0017(6) .0289(7) .0017(6) C6 .0540(9) .0504(10) .0604(10) -.0001(7) .0265(8) .0011(7) S6 .0917(4) .0570(3) .0802(4) .0014(2) .0549(3) .0063(2) CS6 .1172(18) .0799(15) .0858(14) .0203(13) .0658(14) .0088(12) N7 .0645(9) .0490(8) .0650(9) -.0012(6) .0335(7) -.0003(6) C7A .0532(9) .0521(10) .0590(9) .0022(7) .0260(7) .0010(7) N1' .0695(9) .0587(9) .0528(8) .0089(7) .0356(7) -.0018(7) N2' .0825(10) .0721(11) .0604(9) .0118(8) .0429(8) -.0074(8) C3' .0805(12) .0679(13) .0613(10) .0129(10) .0362(9) -.0135(9) C3'A .0671(10) .0550(10) .0530(9) .0097(8) .0262(8) -.0061(8) C4' .0729(11) .0510(11) .0586(10) .0082(8) .0247(9) -.0055(8) O4' .1227(12) .0478(8) .0925(11) .0073(8) .0500(10) -.0075(7) N5' .0693(9) .0488(8) .0548(8) .0050(6) .0271(7) .0030(6) C5' .1006(15) .0556(12) .0846(14) .0015(10) .0477(12) .0127(10) C6' .0571(9) .0493(9) .0467(8) .0044(7) .0217(7) -.0008(7) S6' .0752(3) .0635(3) .0556(3) .0044(2) .0389(2) .00198(19) CS6' .0860(13) .0624(11) .0710(12) .0039(9) .0471(10) -.0100(9) N7' .0690(8) .0486(8) .0491(7) .0064(6) .0318(6) -.0008(6) C7'A .0585(9) .0534(10) .0465(8) .0089(7) .0249(7) -.0019(7) C8 .0713(11) .0605(11) .0701(11) -.0038(9) .0347(9) -.0120(9) C9 .0747(11) .0497(10) .0686(11) .0003(8) .0399(9) .0018(8) C10 .0731(11) .0551(10) .0593(10) .0006(8) .0360(9) .0023(8) C11 .0676(10) .0594(11) .0589(10) -.0026(8) .0364(9) -.0026(8) 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 C7A . 1.347(2) ? N1 N2 . 1.368(2) ? N1 C8 . 1.449(2) ? N2 C3 . 1.307(3) ? C3 C3A . 1.413(3) ? C3A C7A . 1.390(3) ? C3A C4 . 1.393(3) ? C4 N5 . 1.322(2) ? C4 O4 . 1.334(2) ? O4 CO4 . 1.439(2) ? N5 C6 . 1.348(2) ? C6 N7 . 1.320(2) ? C6 S6 . 1.7582(18) ? S6 CS6 . 1.781(2) ? N7 C7A . 1.345(2) ? N1' C7'A . 1.343(2) ? N1' N2' . 1.378(2) ? N1' C11 . 1.451(2) ? N2' C3' . 1.313(3) ? C3' C3'A . 1.403(3) ? C3'A C7'A . 1.375(3) ? C3'A C4' . 1.424(3) ? C4' O4' . 1.214(3) ? C4' N5' . 1.430(2) ? N5' C6' . 1.376(2) ? N5' C5' . 1.465(3) ? C6' N7' . 1.296(2) ? C6' S6' . 1.7597(17) ? S6' CS6' . 1.794(2) ? N7' C7'A . 1.364(2) ? C8 C9 . 1.504(3) ? C9 C10 . 1.525(2) ? C10 C11 . 1.501(3) ?