#------------------------------------------------------------------------------ #$Date: 2008-03-17 09:03:11 +0000 (Mon, 17 Mar 2008) $ #$Revision: 285 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003549.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_2003549 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1204 _journal_page_last 1207 _publ_section_title ; An Unusual C6-Spiro-Fused Cyclouridine Derivative ; _chemical_formula_moiety 'C13 H16 N2 O8' _chemical_formula_sum 'C13 H16 N2 O8' _chemical_formula_weight 328.28 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,1/2+y,-z' _symmetry_space_group_name_H-M 'P 21' _cell_length_a 7.569(1) _cell_length_b 9.738(2) _cell_length_c 9.503(1) _cell_angle_alpha 90.0 _cell_angle_beta 96.32(1) _cell_angle_gamma 90.0 _cell_volume 696.2(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.55 _cell_measurement_theta_max 19.92 _exptl_absorpt_coefficient_mu 0.123 _cell_measurement_temperature 296 _exptl_crystal_description prism _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour 'pale yellow' _chemical_compound_source ? _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method '\w/2\q scans (rate 2\% min^-1^ in \w)' _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 1405 _reflns_number_total 1302 _reflns_number_observed 1238 _reflns_observed_criterion '[I > \s(I)]' _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.6 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.035 _refine_ls_wR_factor_obs 0.043 _refine_ls_wR_factor_all ? _refine_ls_goodness_of_fit_obs 1.96 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 1238 _refine_ls_number_parameters 207 _refine_ls_hydrogen_treatment ; H atoms riding (C---H, N---H 0.95\%A), except for H7 and H8 which were obtained from a difference map ; _refine_ls_weighting_scheme 'w = 4F~o~^2^/\s^2^(F~o~^2^)' _refine_ls_shift/esd_max 0.0001 _refine_diff_density_max 0.26 _refine_diff_density_min -0.19 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C ? International_Tables_Vol_IV_Table_2.3.1 .002 .002 H ? International_Tables_Vol_IV_Table_2.3.1 0 0 O ? International_Tables_Vol_IV_Table_2.3.1 .008 .006 N ? International_Tables_Vol_IV_Table_2.3.1 .004 .003 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_structure_solution ; TEXSAN PROCESS (Molecular Structure Corporation, 1985) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O2 0.1479(3) 0.3471 0.3925(2) 0.042(1) O4 0.5519(4) 0.6156(4) 0.6423(3) 0.062(1) O7 0.7494(3) 0.4079(4) 0.1546(2) 0.051(1) O8 0.8158(3) 0.4517(5) 0.3907(3) 0.071(1) O2' 0.0507(3) 0.4198(5) -0.0531(2) 0.064(1) O3' 0.2511(3) 0.4079(4) -0.2090(2) 0.040(1) O4' 0.4141(3) 0.3065(4) 0.0764(2) 0.038(1) O5' 0.5477(3) 0.5791(4) 0.1454(2) 0.038(1) N1 0.3550(3) 0.4483(4) 0.2687(2) 0.031(1) N3 0.3714(3) 0.4661(4) 0.5144(2) 0.039(1) C2 0.2824(4) 0.4164(4) 0.3888(3) 0.032(1) C4 0.4949(4) 0.5694(5) 0.5273(3) 0.039(1) C5 0.5449(5) 0.6234(5) 0.3892(4) 0.042(1) C6 0.5312(4) 0.5147(4) 0.2748(3) 0.033(1) C7 0.6853(4) 0.4080(5) 0.2891(3) 0.042(1) C8 0.0647(4) 0.4218(6) -0.2002(3) 0.049(1) C9 -0.0029(6) 0.5546(7) -0.2667(5) 0.072(2) C10 -0.0259(6) 0.2950(6) -0.2660(4) 0.072(2) C1' 0.2820(4) 0.3819(5) 0.1354(3) 0.035(1) C2' 0.2063(4) 0.4811(5) 0.0185(3) 0.041(1) C3' 0.3408(4) 0.4793(4) -0.0911(3) 0.036(1) C4' 0.4930(4) 0.3938(5) -0.0210(3) 0.035(1) C5' 0.6343(4) 0.4834(5) 0.0600(3) 0.041(1) H3 0.3437 0.4244 0.5996 0.047 H7 0.6607 0.3003 0.3357 0.050 H8 0.9393 0.4039 0.3690 0.085 H1' 0.1904 0.3206 0.1553 0.042 H2' 0.1856 0.5707 0.0529 0.050 H3' 0.3772 0.5690 -0.1152 0.044 H4' 0.5439 0.3402 -0.0896 0.043 H5' 0.6995 0.5316 -0.0043 0.051 H5a 0.4677 0.6972 0.3591 0.050 H5b 0.6639 0.6559 0.4031 0.050 H9a 0.0510 0.6296 -0.2142 0.086 H9b 0.0259 0.5589 -0.3614 0.086 H9c -0.1282 0.5592 -0.2664 0.086 H10a 0.0243 0.2155 -0.2197 0.086 H10b -0.0097 0.2914 -0.3637 0.086 H10c -0.1494 0.2988 -0.2561 0.086 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 O2 0.035(1) -0.010(1) 0.010(1) 0.062(2) -0.001(1) 0.032(1) O4 0.063(2) -0.021(2) 0.008(1) 0.091(2) -0.024(1) 0.034(1) O7 0.038(1) 0.019(1) 0.008(1) 0.084(2) -0.003(1) 0.033(1) O8 0.050(1) 0.012(2) -0.005(1) 0.109(3) -0.017(2) 0.051(1) O2' 0.038(1) -0.004(2) 0.0025(9) 0.130(3) -0.003(2) 0.025(1) O3' 0.041(1) -0.000(1) 0.0044(8) 0.056(1) -0.001(1) 0.022(1) O4' 0.053(1) 0.003(1) 0.011(1) 0.036(1) 0.001(1) 0.027(1) O5' 0.048(1) -0.004(1) 0.010(1) 0.039(1) 0.002(1) 0.028(1) N1 0.033(1) -0.003(1) 0.006(1) 0.040(2) -0.000(1) 0.021(1) N3 0.044(1) -0.007(1) 0.006(1) 0.053(2) -0.002(1) 0.020(1) C2 0.032(2) 0.006(2) 0.003(1) 0.040(2) -0.001(1) 0.024(1) C4 0.036(2) 0.001(2) 0.006(1) 0.048(2) -0.009(2) 0.033(2) C5 0.042(2) -0.005(2) 0.008(1) 0.044(2) -0.007(2) 0.040(2) C6 0.039(2) -0.004(1) 0.007(1) 0.038(2) -0.002(1) 0.023(1) C7 0.038(2) 0.008(2) 0.001(1) 0.057(2) -0.001(2) 0.029(1) C8 0.045(2) 0.000(2) 0.005(1) 0.079(3) 0.001(2) 0.024(1) C9 0.069(3) 0.028(3) -0.005(2) 0.098(4) 0.001(2) 0.047(2) C10 0.065(3) -0.030(3) 0.004(2) 0.104(4) 0.002(2) 0.045(2) C1' 0.039(2) -0.006(1) 0.006(1) 0.042(2) -0.002(1) 0.025(1) C2' 0.038(2) 0.010(2) 0.005(1) 0.059(2) -0.003(2) 0.026(1) C3' 0.044(2) 0.003(2) 0.006(1) 0.041(2) 0.001(1) 0.024(1) C4' 0.044(2) 0.005(2) 0.010(1) 0.042(2) -0.002(1) 0.022(1) C5' 0.039(2) 0.003(2) 0.014(1) 0.056(2) -0.001(2) 0.031(2)