#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006641.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_2006641 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 1667 _journal_page_last 1669 _publ_section_title ; N-3-Allylation of 2-(N,N-Dimethylaminomethyleneamino)-6-formylpteridin-4-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 'Helliwell, Madeleine' 'Dinsmore, Andrew' 'Garner, C. David' 'Joule, John A.' _chemical_formula_sum 'C13 H14 N6 O2' _chemical_formula_weight 286.30 _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 11.056(4) _cell_length_b 8.340(2) _cell_length_c 15.5461(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.829(13) _cell_angle_gamma 90.00 _cell_volume 1385.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296 _exptl_crystal_density_diffrn 1.372 _diffrn_ambient_temperature 296.2 _refine_ls_R_factor_obs .0500 _refine_ls_wR_factor_obs .1276 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol O4 .3976(2) .2512(2) .28824(10) .0670(5) Uani d . 1 . O O61 .0633(2) .6595(3) .46793(14) .0819(6) Uani d . 1 . O N1 .5402(2) .2230(2) .55662(11) .0504(5) Uani d . 1 . N N3 .5450(2) .1595(2) .40822(11) .0483(5) Uani d . 1 . N N5 .2827(2) .4230(2) .39944(12) .0526(5) Uani d . 1 . N N8 .3809(2) .3775(3) .58304(12) .0607(6) Uani d . 1 . N N21 .6990(2) .0648(2) .52440(12) .0518(5) Uani d . 1 . N N23 .8456(2) -.0516(2) .63782(12) .0532(5) Uani d . 1 . N C2 .5933(2) .1517(3) .50012(14) .0471(5) Uani d . 1 . C C4 .4394(2) .2484(3) .36852(14) .0500(5) Uani d . 1 . C C4a .3836(2) .3321(3) .43168(14) .0457(5) Uani d . 1 . C C6 .2322(2) .4915(3) .4592(2) .0521(6) Uani d . 1 . C C7 .2811(2) .4654(3) .5496(2) .0592(6) Uani d . 1 . C C8a .4362(2) .3097(3) .52331(14) .0471(5) Uani d . 1 . C C22 .7427(2) .0298(3) .60947(15) .0502(6) Uani d . 1 . C C24 .8893(3) -.1072(4) .7293(2) .0690(8) Uani d . 1 . C C25 .9202(3) -.0980(6) .5775(3) .0820(10) Uani d . 1 . C C31 .6040(3) .0689(3) .3480(2) .0574(6) Uani d . 1 . C C32 .7091(3) .1584(4) .3266(2) .0812(9) Uani d . 1 . C C33 .7161(5) .2072(6) .2524(3) .1147(14) Uani d . 1 . C C61 .1225(3) .5950(3) .4238(2) .0666(7) Uani d . 1 . C H7 .241(3) .520(4) .5888(19) .082(9) Uiso d . 1 . H H22 .701(2) .057(3) .6549(15) .047(6) Uiso d . 1 . H H24A .835(3) -.061(4) .7630(19) .081(9) Uiso d . 1 . H H24B .889(3) -.228(4) .731(2) .091(10) Uiso d . 1 . H H24C .971(3) -.064(4) .750(2) .088(10) Uiso d . 1 . H H25A .968(4) -.197(5) .599(2) .115(13) Uiso d . 1 . H H25B .987(4) -.023(6) .586(3) .134(16) Uiso d . 1 . H H25C .881(4) -.093(5) .525(3) .119(15) Uiso d . 1 . H H31A .541(2) .040(3) .2964(18) .067(8) Uiso d . 1 . H H31B .638(2) -.029(4) .3786(18) .071(8) Uiso d . 1 . H H32 .786(4) .193(5) .377(3) .142(15) Uiso d . 1 . H H33A .795(3) .261(4) .245(2) .092 Uiso d . 1 . H H33B .643(3) .194(4) .203(2) .092 Uiso d . 1 . H H61 .099(3) .598(4) .357(2) .084(9) Uiso d . 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 O4 .0815(12) .0802(12) .0376(9) .0098(10) .0122(8) -.0025(8) O61 .0784(13) .0837(14) .0899(14) .0184(11) .0327(11) -.0023(11) N1 .0496(10) .0627(12) .0391(10) -.0032(9) .0120(8) -.0047(9) N3 .0540(11) .0536(11) .0396(10) -.0045(9) .0165(8) -.0024(8) N5 .0585(12) .0546(12) .0455(10) -.0028(9) .0150(9) .0010(9) N8 .0631(12) .0783(14) .0416(11) .0069(11) .0150(9) -.0078(10) N21 .0491(11) .0607(12) .0471(11) -.0032(9) .0151(8) .0009(9) N23 .0482(11) .0647(13) .0468(10) -.0001(9) .0122(8) -.0023(9) C2 .0478(12) .0525(13) .0421(11) -.0101(11) .0136(9) -.0017(10) C4 .0566(13) .0543(13) .0401(12) -.0059(11) .0143(10) .0006(10) C4a .0498(12) .0470(12) .0416(11) -.0085(10) .0140(9) -.0022(10) C6 .0555(13) .0514(13) .0518(13) -.0051(11) .0182(11) -.0015(11) C7 .0623(15) .067(2) .0500(14) .0033(13) .0184(12) -.0073(12) C8a .0497(12) .0517(13) .0407(11) -.0099(10) .0131(10) -.0046(10) C22 .0493(13) .0573(14) .0457(13) -.0066(11) .0153(10) -.0059(11) C24 .072(2) .080(2) .0497(15) .010(2) .0058(13) -.0024(14) C25 .064(2) .117(3) .073(2) .021(2) .030(2) .011(2) C31 .070(2) .060(2) .0466(14) .0048(13) .0224(13) -.0041(12) C32 .093(2) .081(2) .086(2) -.001(2) .054(2) -.006(2) C33 .129(4) .138(4) .096(3) -.032(3) .065(3) -.005(3) C61 .066(2) .071(2) .063(2) .0069(14) .0172(13) .0014(14) 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 O4 C4 . 1.215(2) no O61 C61 . 1.192(3) no N1 C2 . 1.317(3) no N1 C8a . 1.344(3) no N3 C4 . 1.387(3) no N3 C2 . 1.393(3) no N3 C31 . 1.479(3) no N5 C6 . 1.329(3) no N5 C4a . 1.335(3) no N8 C7 . 1.316(3) no N8 C8a . 1.359(3) no N21 C22 . 1.319(3) no N21 C2 . 1.344(3) no N23 C22 . 1.302(3) no N23 C25 . 1.451(4) no N23 C24 . 1.456(3) no C4 C4a . 1.464(3) no C4a C8a . 1.407(3) no C6 C7 . 1.388(3) no C6 C61 . 1.475(4) no C7 H7 . .96(3) no C22 H22 . .97(2) no C24 H24A . .97(3) no C24 H24B . 1.00(3) no C24 H24C . .95(3) no C25 H25A . .99(4) no C25 H25B . .95(4) no C25 H25C . .82(4) no C31 C32 . 1.488(4) no C31 H31A . .95(3) no C31 H31B . .98(3) no C32 C33 . 1.243(5) no C32 H32 . 1.04(4) no C33 H33A . 1.01(3) no C33 H33B . .97(3) no C61 H61 . 1.00(3) no _cod_database_code 2006641