#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2005217.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2005217 loop_ _publ_author_name 'Das, A. K.' 'Dutta, M.' 'Mazumdar, S. K.' 'Mazumdar, B.' 'Mukhopadhyay, A.' 'Talapatra, S. K.' _publ_section_title ; 9-Benzyl-7-[(E)-2-butenyl]-2,3-dihydro-6-hydroxy-1,3-dimethylpyrimido[2,1-f]purine-4,8(1H,9H)-dione ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2076 _journal_page_last 2078 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac 'C21 H23 N5 O3' _chemical_formula_sum 'C21 H23 N5 O3' _chemical_formula_weight 393.4 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90. _cell_angle_beta 92.100(10) _cell_angle_gamma 90. _cell_formula_units_Z 8 _cell_length_a 15.7540(10) _cell_length_b 19.2900(10) _cell_length_c 13.2050(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296 _cell_measurement_theta_max 61 _cell_measurement_theta_min 58 _cell_volume 4010.2(4) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'PARST (Nardelli, 1983)' _computing_structure_refinement 'SHELX76 (Sheldrick, 1976)' _computing_structure_solution 'MULTAN78 (Main et al., 1978)' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6585 _diffrn_reflns_theta_max 60 _diffrn_standards_decay_% +-0.5 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.734 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.24 _refine_diff_density_min -0.21 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.98 _refine_ls_number_parameters 681 _refine_ls_number_reflns 4425 _refine_ls_R_factor_obs 0.056 _refine_ls_shift/esd_max 0.29 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/\s^2^(F)' _refine_ls_wR_factor_obs 0.062 _reflns_number_observed 4425 _reflns_number_total 5950 _reflns_observed_criterion F>4\s(F) _[local]_cod_data_source_file bm1044.cif _[local]_cod_data_source_block bm1044a _cod_database_code 2005217 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2+y,1/2-z 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 .075(2) .077(2) .086(3) .0132(19) .0048(19) -.008(2) C2 .111(3) .072(3) .070(3) .004(3) .017(3) -.007(2) N3 .101(3) .065(2) .069(2) -.005(2) -.0076(19) .0022(18) C4 .093(3) .061(3) .059(2) .000(3) -.005(2) .007(2) C5 .076(3) .060(2) .057(2) .007(2) .007(2) .002(2) N5 .070(2) .060(2) .0645(19) .0049(17) .0050(17) .0028(16) C6 .073(3) .065(3) .086(3) .002(2) .004(2) .012(2) C7 .090(3) .064(3) .101(3) .007(2) .018(3) -.001(3) C8 .102(4) .062(3) .080(3) -.005(3) .013(3) -.004(2) N9 .079(2) .066(2) .072(2) -.0057(19) .0066(18) -.0041(18) C9 .063(3) .059(2) .061(2) -.005(2) .0054(19) -.002(2) N10 .067(2) .077(2) .066(2) -.0024(18) .0055(17) -.0007(18) C10 .066(3) .069(3) .060(2) .002(2) .007(2) .006(2) C11 .116(4) .115(4) .145(5) .037(4) .010(4) -.018(4) C12 .210(5) .067(3) .089(3) .005(4) -.036(4) -.019(3) O13 .079(2) .087(2) .115(2) -.0051(17) -.0299(18) -.0045(18) O14 .0714(19) .095(2) .122(3) .0109(17) -.0147(18) -.0019(19) C15 .120(4) .091(4) .151(5) .031(3) -.007(4) -.011(4) C16 .145(5) .180(7) .122(5) .041(5) .018(5) -.071(5) C17 .146(5) .187(8) .148(6) .043(6) .043(6) -.017(6) C18 .177(7) .201(8) .168(7) -.053(6) -.025(6) -.036(6) O19 .134(3) .071(2) .107(2) -.0035(18) .013(2) -.0244(19) C20 .096(3) .066(3) .076(3) -.025(2) .008(2) -.004(2) C21 .086(3) .073(3) .083(3) -.021(3) -.003(3) -.003(3) C22 .140(4) .074(3) .086(4) -.018(3) .013(3) -.007(3) C23 .164(5) .098(4) .077(4) -.017(4) .011(4) -.007(3) C24 .170(5) .131(6) .095(4) -.017(5) -.026(5) .016(4) C25 .136(5) .140(5) .119(5) -.002(4) -.020(4) .013(5) C26 .103(4) .104(4) .096(4) -.021(3) -.006(3) .003(3) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv N1 .8263(3) -.0410(2) .1389(4) .0790(10) C2 .7829(4) -.0734(3) .0521(4) .084(2) N3 .6912(3) -.0746(2) .0618(3) .0790(10) C4 .6495(4) -.0194(3) .0981(4) .071(2) C5 .7038(3) .0297(3) .1479(4) .0640(10) N5 .6844(3) .0887(2) .2050(3) .0650(10) C6 .6091(4) .1256(3) .2138(5) .074(2) C7 .6103(4) .1841(3) .2705(5) .084(2) C8 .6892(4) .2077(3) .3205(5) .081(2) N9 .7614(3) .1657(2) .3097(3) .0720(10) C9 .7582(3) .1069(3) .2530(4) .0610(10) N10 .8233(3) .0650(2) .2369(3) .0700(10) C10 .7872(3) .0169(3) .1723(4) .065(2) C11 .9175(5) -.0507(4) .1502(6) .125(3) C12 .6435(5) -.1252(3) -.0002(5) .123(2) O13 .5706(3) -.0152(2) .0920(3) .0950(10) O14 .5405(2) .1001(2) .1652(3) .0960(10) C15 .5297(5) .2245(4) .2828(7) .121(3) C16 .4858(7) .2003(5) .3749(8) .149(3) C17 .4099(7) .1675(6) .3853(8) .160(4) C18 .3531(6) .1604(5) .2972(8) .183(4) O19 .6958(3) .2607(2) .3714(3) .1040(10) C20 .8435(4) .1868(3) .3575(4) .079(2) C21 .8613(4) .1569(3) .4622(5) .081(2) C22 .8154(5) .1780(3) .5440(6) .100(2) C23 .8347(6) .1521(4) .6395(6) .113(3) C24 .8990(7) .1075(5) .6557(7) .133(3) C25 .9461(6) .0841(5) .5737(7) .132(3) C26 .9244(5) .1103(4) .4776(6) .101(2) N1' .8730(3) -.2973(3) .5414(4) .095(2) C2' .8879(4) -.3634(4) .5898(5) .104(2) N3' .8133(4) -.3951(3) .6259(4) .094(2) C4' .7366(4) -.3867(3) .5813(4) .076(2) C5' .7319(3) -.3327(3) .5097(4) .0690(10) N5' .6619(3) -.3043(2) .4546(3) .0630(10) C6' .5770(4) -.3239(3) .4432(4) .079(2) C7' .5235(3) -.2857(3) .3835(4) .084(2) C8' .5557(4) -.2264(3) .3324(4) .089(2) N9' .6402(3) -.2083(2) .3486(3) .0730(10) C9' .6925(3) -.2470(3) .4094(4) .063(2) N10' .7743(3) -.2346(2) .4306(3) .0730(10) C10' .7966(3) -.2888(3) .4934(4) .0690(10) C11' .9471(4) -.2557(3) .5172(5) .113(2) C12' .8296(5) -.4503(4) .6999(6) .150(3) O13' .6752(3) -.4236(2) .6034(3) .1010(10) O14' .5563(2) -.3824(2) .4924(3) .1040(10) C15' .4281(5) -.3009(4) .3807(6) .125(3) C16' .3939(6) -.3224(5) .2814(6) .174(4) C17' .3919(6) -.3894(5) .2472(7) .198(5) C18' .3596(7) -.4120(5) .1459(8) .204(5) O19' .5104(3) -.1897(2) .2758(3) .125(2) C20' .6734(4) -.1469(3) .2981(4) .086(2) C21' .6654(4) -.0808(3) .3610(4) .077(2) C22' .7346(5) -.0572(3) .4210(5) .104(2) C23' .7256(7) .0025(4) .4768(6) .130(3) C24' .6535(8) .0380(4) .4761(6) .131(3) C25' .5858(6) .0148(4) .4172(7) .124(3) C26' .5926(5) -.0453(4) .3600(5) .100(2) H21 .7981(4) -.0446(3) -.0150(4) .062(3) H22 .8054(4) -.1260(3) .0453(4) .062(3) H111 .9346(4) -.1001(3) .1184(5) .074(4) H112 .9364(4) -.0495(3) .2296(5) .074(4) H113 .9494(4) -.0097(3) .1110(5) .074(4) H121 .6860(5) -.1656(3) -.0236(5) .118(5) H122 .6157(5) -.0998(3) -.0664(6) .118(5) H123 .5939(5) -.1476(3) .0436(5) .118(5) H151 .4883(5) .2170(4) .2167(7) .069(4) H162 .5448(5) .2789(4) .2907(7) .069(4) H161 .5216(7) .2082(5) .4453(8) .072(5) H171 .3917(7) .1482(6) .4582(8) .111(5) H181 .2959(6) .1345(5) .3193(8) .268(7) H182 .3835(6) .1301(5) .2401(8) .268(7) H183 .3371(6) .2110(5) .2669(8) .268(7) H201 .8933(4) .1698(3) .3091(5) .062(3) H202 .8445(4) .2426(3) .3630(5) .062(3) H221 .7645(5) .2150(3) .5332(6) .072(4) H23 .7978(6) .1687(4) .7025(6) .072(5) H24 .9136(7) .0879(6) .7310(7) .091(5) H25 .9983(6) .0484(5) .5856(7) .072(5) H26 .9593(5) .0921(4) .4139(6) .063(4) H21' .9330(4) -.3567(4) .6526(5) .072(4) H22' .9143(4) -.3977(4) .5345(5) .072(4) H111' 1.0006(5) -.2715(4) .5651(6) .085(3) H112' .9338(5) -.2015(4) .5299(6) .085(3) H113' .9617(5) -.2634(4) .4387(6) .085(3) H121' .7706(5) -.4718(4) .7246(6) .098(6) H122' .8655(5) -.4299(4) .7644(6) .098(6) H123' .8660(5) -.4904(4) .6643(6) .098(6) H151' .3952(5) -.2546(4) .4030(6) .109(4) H152' .4164(5) -.3419(4) .4342(6) .109(4) H161' .3684(6) -.2826(5) .2314(6) .099(6) H171' .4159(6) -.4290(5) .2984(7) .077(8) H181' .3657(7) -.4676(5) .1396(8) .241(8) H182' .3959(7) -.3873(5) .0883(8) .241(8) H183' .2936(7) -.3977(5) .1359(8) .241(8) H201' .7398(4) -.1556(3) .2848(4) .053(3) H202' .6391(4) -.1397(3) .2266(4) .053(3) H221' .7940(5) -.0851(3) .4224(5) .053(4) H23' .7784(7) .0203(4) .5244(6) .069(6) H24' .6480(8) .0849(4) .5201(6) .098(6) H25' .5268(6) .0435(4) .4144(7) .075(6) H26' .5384(5) -.0641(4) .3156(5) .048(4) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C10 N1 C11 122.2(5) no C2 N1 C11 117.4(5) no C2 N1 C10 113.8(5) no N1 C2 N3 112.2(4) no C2 N3 C12 116.9(5) no C2 N3 C4 121.1(5) no C4 N3 C12 118.6(5) no N3 C4 O13 121.8(6) no N3 C4 C5 113.5(5) no C5 C4 O13 124.7(5) no C4 C5 C10 123.2(5) no C4 C5 N5 130.5(5) no N5 C5 C10 104.3(5) no C5 N5 C9 105.2(4) no C5 N5 C6 131.4(4) no C6 N5 C9 123.4(5) no N5 C6 O14 116.8(5) no N5 C6 C7 118.5(6) no C7 C6 O14 124.7(6) no C6 C7 C15 119.8(6) no C6 C7 C8 120.3(6) no C8 C7 C15 119.9(6) no C7 C8 O19 124.2(6) no C7 C8 N9 116.9(5) no N9 C8 O19 118.9(5) no C8 N9 C20 119.8(4) no C8 N9 C9 121.5(5) no C9 N9 C20 118.7(4) no N5 C9 N9 119.3(4) no N9 C9 N10 125.6(5) no N5 C9 N10 115.0(5) no C9 N10 C10 101.9(4) no C5 C10 N10 113.5(5) no N1 C10 N10 125.2(5) no N1 C10 C5 121.1(5) no C7 C15 C16 110.1(7) no C15 C16 C17 131.3(10) yes C16 C17 C18 118.8(10) yes N9 C20 C21 114.5(5) no C20 C21 C26 120.1(6) no C20 C21 C22 121.1(6) no C22 C21 C26 118.8(7) no C21 C22 C23 120.2(7) no C22 C23 C24 121.2(8) no C23 C24 C25 120.0(9) no C24 C25 C26 117.6(8) no C21 C26 C25 122.2(7) no C10' N1' C11' 122.4(5) no C2' N1' C11' 117.7(5) no C2' N1' C10' 116.3(5) no N1' C2' N3' 113.9(6) no C2' N3' C12' 114.2(6) no C2' N3' C4' 123.1(6) no C4' N3' C12' 121.2(6) no N3' C4' O13' 121.7(5) no N3' C4' C5' 114.3(6) no C5' C4' O13' 124.0(5) no C4' C5' C10' 123.4(5) no C4' C5' N5' 131.0(5) no N5' C5' C10' 104.8(5) no C5' N5' C9' 105.1(4) no C5' N5' C6' 132.9(4) no C6' N5' C9' 122.0(5) no N5' C6' O14' 115.1(5) no N5' C6' C7' 119.4(5) no C7' C6' O14' 125.5(6) no C6' C7' C15' 120.0(6) no C6' C7' C8' 119.1(5) no C8' C7' C15' 120.5(5) no C7' C8' O19' 122.4(5) no C7' C8' N9' 119.0(5) no N9' C8' O19' 118.6(5) no C8' N9' C20' 119.4(5) no C8' N9' C9' 120.9(5) no C9' N9' C20' 119.7(4) no N5' C9' N9' 119.6(5) no N9' C9' N10' 126.1(5) no N5' C9' N10' 114.3(5) no C9' N10' C10' 102.4(5) no C5' C10' N10' 113.4(4) no N1' C10' N10' 125.5(5) no N1' C10' C5' 121.0(5) no C7' C15' C16' 114.0(6) no C15' C16' C17' 124.6(8) yes C16' C17' C18' 125.4(9) yes N9' C20' C21' 112.9(5) no C20' C21' C26' 120.7(6) no C20' C21' C22' 120.0(5) no C22' C21' C26' 119.3(6) no C21' C22' C23' 118.8(7) no C22' C23' C24' 122.2(8) no C23' C24' C25' 119.0(8) no C24' C25' C26' 120.4(8) no C21' C26' C25' 120.4(7) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N1 C2 1.454(7) no N1 C10 1.357(7) no N1 C11 1.451(9) no C2 N3 1.455(9) no N3 C4 1.348(7) no N3 C12 1.464(9) no C4 C5 1.421(8) no C4 O13 1.245(8) yes C5 N5 1.405(7) no C5 C10 1.364(7) no N5 C6 1.392(8) no N5 C9 1.350(7) no C6 C7 1.354(9) no C6 O14 1.331(7) yes C7 C8 1.459(9) no C7 C15 1.504(10) no C8 N9 1.408(8) no C8 O19 1.226(7) no N9 C9 1.359(7) no N9 C20 1.476(8) no C9 N10 1.329(7) no N10 C10 1.370(7) no C15 C16 1.496(14) no C16 C17 1.364(16) yes C17 C18 1.448(15) no C20 C21 1.515(8) no C21 C22 1.383(10) no C21 C26 1.350(10) no C22 C23 1.380(11) no C23 C24 1.340(14) no C24 C25 1.409(14) no C25 C26 1.397(12) no N1' C2' 1.442(9) no N1' C10' 1.350(7) no N1' C11' 1.462(8) no C2' N3' 1.423(9) no N3' C4' 1.335(9) no N3' C12' 1.462(10) no C4' C5' 1.407(8) no C4' O13' 1.244(8) yes C5' N5' 1.410(7) no C5' C10' 1.349(7) no N5' C6' 1.393(8) no N5' C9' 1.353(7) no C6' C7' 1.351(8) no C6' O14' 1.348(7) yes C7' C8' 1.431(8) no C7' C15' 1.530(9) no C8' N9' 1.385(8) no C8' O19' 1.237(7) no N9' C9' 1.354(7) no N9' C20' 1.465(7) no C9' N10' 1.330(7) no N10' C10' 1.372(7) no C15' C16' 1.459(11) no C16' C17' 1.369(14) yes C17' C18' 1.479(14) no C20' C21' 1.530(8) no C21' C22' 1.400(9) no C21' C26' 1.335(10) no C22' C23' 1.377(10) no C23' C24' 1.326(15) no C24' C25' 1.372(14) no C25' C26' 1.390(11) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag C6 C7 C15 C16 91.5(8) yes C8 C7 C15 C16 -87.9(8) yes C8 N9 C20 C21 93.2(6) yes C9 N9 C20 C21 -89.1(6) yes C7 C15 C16 C17 -114.3(12) yes C15 C16 C17 C18 -9.0(18) yes N9 C20 C21 C22 -69.4(8) yes N9 C20 C21 C26 112.5(7) yes C6' C7' C15' C16' -117.7(7) yes C8' C7' C15' C16' 69.4(8) yes C8' N9' C20' C21' 90.4(6) yes C9' N9' C20' C21' -90.4(6) yes C7' C15' C16' C17' 87.6(10) yes C15' C16' C17' C18' -178.3(9) yes N9' C20' C21' C22' 96.8(7) yes N9' C20' C21' C26' -82.8(7) yes