#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/56/2005691.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_2005691 loop_ _publ_author_name 'Zhu, Y.' 'Jia, Z.-J.' 'Shi, J.-G.' 'Wang, H.-Q.' _publ_section_title ; A Pyridine-2,6(1H,3H)-dione Alkaloid ; _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 2791 _journal_page_last 2793 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac 'C10 H13 N O5' _chemical_formula_sum 'C10 H13 N O5' _chemical_formula_weight 227.22 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90. _cell_angle_beta 113.82(1) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 8.5879(7) _cell_length_b 17.4610(8) _cell_length_c 7.893(1) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 39 _cell_measurement_theta_min 20 _cell_volume 1082.76(19) _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 0.040 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 1886 _diffrn_reflns_theta_max 62 _diffrn_standards_decay_% insignificant _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.961 _exptl_absorpt_correction_T_max 0.994 _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_type 'empirical via \y scans (North, Phillips & Mathews, 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.25 _refine_diff_density_min -0.24 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 0.801 _refine_ls_number_parameters 145 _refine_ls_number_reflns 1690 _refine_ls_R_factor_obs 0.054 _refine_ls_shift/esd_max 0.16 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme unit _refine_ls_wR_factor_obs 0.055 _reflns_number_observed 1514 _reflns_number_total 1638 _reflns_observed_criterion I>3\s(I) _[local]_cod_data_source_file ta1075.cif _[local]_cod_data_source_block ta1075a _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_original_cell_volume 1082.8(3) _cod_database_code 2005691 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,1/2-y,1/2+z -x,-y,-z -x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv O(1) .8422(2) .2663(1) .9489(3) 3.78(5) O(2) .6251(2) .1862(1) .6082(2) 3.18(4) O(3) .6757(2) .0228(1) .6788(3) 3.45(5) O(4) 1.2283(2) .1216(1) .8429(3) 5.08(6) O(5) .8699(2) .1052(1) 1.1448(3) 4.25(5) N(1) 1.0340(3) .1964(1) .8893(3) 2.89(5) C(2) .8750(3) .2082(2) .8846(3) 2.67(6) C(3) .7317(3) .1506(2) .7807(3) 2.38(5) C(4) .7992(3) .0762(2) .7416(4) 2.63(6) C(5) .9594(3) .0673(2) .7605(4) 3.10(6) C(6) 1.0827(3) .1281(2) .8306(4) 3.19(6) C(7) .6196(3) .1391(2) .8859(4) 2.66(6) C(8) .7152(3) .1093(2) 1.0794(4) 3.07(6) C(9) .6152(4) .0865(2) 1.1862(4) 4.98(8) C(10) 1.1618(4) .2571(2) .9660(5) 4.42(8) C(11) .7226(4) -.0516(2) .6326(5) 4.09(8) HO(2) .678(5) .197(2) .532(5) 4.0 H(5) .996(5) .025(2) .712(5) 4.0 H(7') .533(5) .103(2) .820(5) 4.0 H(7) .564(5) .187(2) .889(5) 4.0 H(9) .675(5) .083(2) 1.317(5) 4.0 H(9') .528(5) .118(2) 1.177(5) 4.0 H(9") .563(5) .041(2) 1.153(5) 4.0 H(10) 1.246(5) .251(2) .911(5) 4.0 H(10') 1.103(5) .302(2) .943(5) 4.0 H(10") 1.207(5) .258(2) 1.104(5) 4.0 H(11') .762(5) -.049(2) .518(5) 4.0 H(11") .801(5) -.077(2) .755(5) 4.0 H(11) .612(5) -.084(2) .596(5) 4.0 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 C(4) O(3) C(11) 117.1(2) yes C(2) N(1) C(6) 123.2(2) yes C(2) N(1) C(10) 118.3(2) yes C(6) N(1) C(10) 118.5(2) yes O(1) C(2) N(1) 120.8(2) yes O(1) C(2) C(3) 119.7(2) yes N(1) C(2) C(3) 119.3(2) yes O(2) C(3) C(2) 106.6(3) yes O(2) C(3) C(4) 109.3(3) yes O(2) C(3) C(7) 105.8(2) yes C(2) C(3) C(4) 112.5(3) yes C(2) C(3) C(7) 110.0(2) yes C(4) C(3) C(7) 112.4(2) yes O(3) C(4) C(3) 111.2(2) yes O(3) C(4) C(5) 125.8(3) yes C(3) C(4) C(5) 122.9(2) yes C(4) C(5) C(6) 121.5(3) yes O(4) C(6) N(1) 119.0(3) yes O(4) C(6) C(5) 122.2(3) yes N(1) C(6) C(5) 118.9(3) yes C(3) C(7) C(8) 113.2(3) yes O(5) C(8) C(7) 120.4(3) yes O(5) C(8) C(9) 121.8(3) yes C(7) C(8) C(9) 117.8(2) yes H(7') C(7) H(7) 108(3) no H(9) C(9) H(9') 102(4) no H(9) C(9) H(9") 104(3) no H(9') C(9) H(9") 103(4) no H(10) C(10) H(10') 117(4) no H(10) C(10) H(10") 117(3) no H(10') C(10) H(10") 99(4) no H(11') C(11) H(11") 120(3) no H(11') C(11) H(11) 111(3) no H(11") C(11) H(11) 102(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag O(1) C(2) 1.217(4) yes O(2) C(3) 1.441(3) yes O(3) C(4) 1.348(4) yes O(3) C(11) 1.449(4) yes O(4) C(6) 1.220(4) yes O(5) C(8) 1.218(3) yes N(1) C(2) 1.366(4) yes N(1) C(6) 1.403(4) yes N(1) C(10) 1.470(3) yes C(2) C(3) 1.544(3) yes C(3) C(4) 1.504(4) yes C(3) C(7) 1.517(4) yes C(4) C(5) 1.332(5) yes C(5) C(6) 1.442(4) yes C(7) C(8) 1.505(4) yes C(8) C(9) 1.480(5) yes O(2) HO(2) .90(5) no C(5) H(5) .94(4) no C(7) H(7') .95(4) no C(7) H(7) .98(4) no C(9) H(9) .95(4) no C(9) H(9') .91(4) no C(9) H(9") .89(4) no C(10) H(10) .99(5) no C(10) H(10') .90(4) no C(10) H(10") 1.00(4) no C(11) H(11') 1.09(5) no C(11) H(11") 1.03(4) no C(11) H(11) 1.05(5) 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 C(6) N(1) C(2) C(3) -10.7(4) yes C(2) N(1) C(6) C(5) 0.4(4) yes N(1) C(2) C(3) C(4) 16.0(3) yes C(2) C(3) C(4) C(5) -12.8(4) yes C(3) C(4) C(5) C(6) 3.6(4) yes C(4) C(5) C(6) N(1) 3.5(4) yes