#------------------------------------------------------------------------------ #$Date: 2008-01-26 15:05:32 +0200 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2003648.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_2003648 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1462 _journal_page_last 1464 _publ_section_title ; 2',3'-Dideoxy-3'-C,2'-N-[(3R,5R)-5-ethoxycarbonyl-2-methyl-1,2- isoxazolidine]ribothymidine\\dag ; _chemical_formula_moiety 'C15 H21 N3 O7' _chemical_formula_sum 'C15 H21 N3 O7' _chemical_formula_weight 355.35 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _symmetry_space_group_name_H-M 'P21' _cell_length_a 5.5020(10) _cell_length_b 15.3840(10) _cell_length_c 9.918(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.43(2) _cell_angle_gamma 90.00 _cell_volume 838.0(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71070 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22 _cell_measurement_theta_max 30 _exptl_absorpt_coefficient_mu 0.113 _cell_measurement_temperature 295(2) _exptl_crystal_description trapezoid _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.27 _exptl_crystal_colour colorless _chemical_compound_source ? _diffrn_measurement_device 'Rigaku AFC5S four-circle' _diffrn_measurement_method \w/2\q _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2010 _reflns_number_total 2010 _reflns_number_observed 1447 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 27.56 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 6 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.5 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0369 _refine_ls_wR_factor_obs 0.0834 _refine_ls_wR_factor_all 0.1311 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_number_reflns 2003 _refine_ls_number_parameters 291 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0279P)^2^ + 0.1537P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.165 _refine_diff_density_min -0.144 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0037(25) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -0.74(161) ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1' 1 0.0701(5) 0.8156(2) 0.7464(3) 0.0303(7) H1' 1 0.2135(54) 0.7828(12) 0.7238(9) 0.033(9) C2' 1 -0.1569(6) 0.7657(2) 0.6944(3) 0.0321(7) H2' 1 -0.2946(48) 0.7758(4) 0.7506(20) 0.034(9) C3' 1 -0.2028(6) 0.8039(2) 0.5513(3) 0.0314(7) H3' 1 -0.3716(55) 0.8020(2) 0.5224(10) 0.030(8) C4' 1 -0.1088(6) 0.8963(2) 0.5606(3) 0.0355(7) H4' 1 -0.0295(32) 0.9094(6) 0.4821(32) 0.036(9) O4' 1 0.0693(4) 0.8969(2) 0.6760(2) 0.0375(6) C5' 1 -0.2996(7) 0.9640(3) 0.5808(4) 0.0454(9) H5'1 1 -0.2223(22) 1.0200(16) 0.5951(5) 0.071(14) H5'2 1 -0.4075(31) 0.9679(3) 0.5004(23) 0.052(11) O5' 1 -0.4374(5) 0.9435(2) 0.6936(3) 0.0538(7) H5' 1 -0.5763(89) 0.9381(33) 0.6693(18) 0.072(16) C2" 1 -0.3274(9) 0.6231(3) 0.6558(5) 0.0605(12) H2" 1 -0.2858(12) 0.5641(15) 0.6391(28) 0.071(14) H2"2 1 -0.4197(36) 0.6458(13) 0.5794(26) 0.055(11) H2"3 1 -0.4216(36) 0.6260(15) 0.7332(23) 0.116(23) N2" 1 -0.1052(5) 0.6741(2) 0.6798(3) 0.0402(7) O3" 1 0.0313(5) 0.6722(2) 0.5580(2) 0.0485(7) C3" 1 -0.0533(7) 0.7417(2) 0.4698(3) 0.0405(9) H3" 1 0.0970(59) 0.7751(13) 0.4406(12) 0.048(11) C4" 1 -0.1931(7) 0.7091(3) 0.3424(3) 0.0504(10) O4"A 0.874(8) -0.3438(10) 0.7521(4) 0.2842(4) 0.084(2) O5"A 0.874(8) -0.1229(8) 0.6321(3) 0.3015(3) 0.0661(14) C5"A 0.874(8) -0.2284(12) 0.5992(4) 0.1729(4) 0.064(2) H5" 0.874(8) -0.3957(74) 0.6165(8) 0.1621(6) 0.052(14) H5"2 0.874(8) -0.2226(12) 0.5370(27) 0.1733(4) 0.101(22) C6"A 0.874(8) -0.0975(11) 0.6323(4) 0.0591(5) 0.068(2) H6" 0.874(8) -0.1247(62) 0.6937(6) 0.0499(27) 0.140(31) H6"2 0.874(8) -0.1555(55) 0.6034(20) -0.0223(8) 0.087(20) H6"3 0.874(8) 0.0736(14) 0.6214(25) 0.0753(20) 0.112(25) O4"B 0.126(8) -0.4014(19) 0.7157(20) 0.308(3) 0.055(8) O5"B 0.126(8) -0.0235(24) 0.6755(16) 0.2685(16) 0.046(6) C5"B 0.126(8) -0.0908(52) 0.6546(20) 0.1277(16) 0.060(11) H5"3 0.126(8) 0.0541(52) 0.6385(20) 0.0825(16) 0.072 H5"4 0.126(8) -0.1604(52) 0.7057(20) 0.0830(16) 0.072 C6"B 0.126(8) -0.2665(79) 0.583(3) 0.116(4) 0.078(16) H6"4 0.126(8) -0.2032(247) 0.5341(71) 0.1662(257) 0.117 H6"5 0.126(8) -0.2949(435) 0.5677(138) 0.0228(48) 0.117 H6"6 0.126(8) -0.4169(192) 0.6015(70) 0.1516(285) 0.117 N1 1 0.0879(5) 0.8341(2) 0.8906(2) 0.0319(6) C2 1 0.2818(6) 0.7984(2) 0.9681(3) 0.0340(7) O2 1 0.4308(4) 0.7500(2) 0.9237(2) 0.0479(7) N3 1 0.2926(5) 0.8240(2) 1.1009(3) 0.0410(7) H3 1 0.4112(52) 0.8017(10) 1.1525(22) 0.042(10) C4 1 0.1402(6) 0.8806(2) 1.1633(3) 0.0368(8) O4 1 0.1812(5) 0.8982(2) 1.2825(2) 0.0550(7) C5 1 -0.0610(6) 0.9142(2) 1.0766(3) 0.0375(8) C5M 1 -0.2368(7) 0.9754(3) 1.1377(4) 0.0514(10) H5M1 1 -0.1450(22) 1.0273(14) 1.1776(24) 0.060(12) H5M2 1 -0.3224(39) 0.9443(9) 1.2113(24) 0.066(13) H5M3 1 -0.3614(40) 0.9958(14) 1.0654(17) 0.074(14) C6 1 -0.0762(6) 0.8892(2) 0.9475(3) 0.0337(7) H6 1 -0.2166(46) 0.9120(8) 0.8875(20) 0.030(8) 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 C1' 0.0284(15) 0.0017(14) 0.0011(11) 0.043(2) -0.0017(13) 0.0197(14) C2' 0.0290(15) 0.0028(14) -0.0004(12) 0.041(2) -0.0007(13) 0.0259(14) C3' 0.0268(14) 0.0047(13) -0.0050(11) 0.041(2) -0.0028(13) 0.0259(14) C4' 0.034(2) 0.000(2) -0.0001(12) 0.048(2) 0.0066(15) 0.0249(14) O4' 0.0324(11) -0.0089(11) -0.0030(8) 0.0487(15) 0.0059(11) 0.0308(10) C5' 0.046(2) 0.006(2) -0.004(2) 0.041(2) 0.006(2) 0.048(2) O5' 0.0311(13) 0.0105(14) 0.0019(11) 0.072(2) -0.0034(14) 0.058(2) C2" 0.073(3) -0.008(2) -0.018(2) 0.040(2) -0.002(2) 0.066(3) N2" 0.047(2) 0.0036(14) -0.0047(12) 0.039(2) -0.0014(13) 0.0342(15) O3" 0.057(2) 0.0256(14) -0.0072(11) 0.055(2) -0.0050(12) 0.0325(12) C3" 0.043(2) 0.012(2) -0.0056(13) 0.051(2) -0.0014(15) 0.027(2) C4" 0.063(2) 0.014(2) -0.011(2) 0.056(2) -0.006(2) 0.031(2) O4"A 0.115(3) 0.045(3) -0.055(2) 0.075(4) -0.020(2) 0.054(2) O5"A 0.103(3) 0.021(2) -0.015(2) 0.061(2) -0.014(2) 0.032(2) C5"A 0.099(5) -0.012(3) -0.002(3) 0.057(4) -0.012(2) 0.036(3) C6"A 0.083(4) -0.001(3) 0.007(3) 0.077(4) -0.007(3) 0.045(3) N1 0.0296(13) 0.0010(12) -0.0001(10) 0.040(2) -0.0028(11) 0.0256(13) C2 0.032(2) -0.0001(15) 0.0019(12) 0.045(2) 0.0023(13) 0.0257(15) O2 0.0413(14) 0.0170(13) -0.0026(10) 0.067(2) -0.0019(12) 0.0346(12) N3 0.0371(14) 0.0025(15) -0.0064(11) 0.057(2) -0.0010(14) 0.0274(13) C4 0.041(2) -0.011(2) 0.0081(13) 0.042(2) -0.0023(15) 0.028(2) O4 0.064(2) -0.004(2) 0.0037(10) 0.075(2) -0.0103(13) 0.0261(11) C5 0.036(2) -0.003(2) 0.0089(13) 0.043(2) -0.0039(15) 0.034(2) C5M 0.049(2) 0.004(2) 0.012(2) 0.059(3) -0.014(2) 0.047(2) C6 0.029(2) 0.0017(15) 0.0025(12) 0.041(2) -0.0007(15) 0.0308(14)