#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002915.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_2002915 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1999 _journal_volume B55 _journal_page_first 95 _journal_page_last 103 _chemical_formula_sum 'C58 H64 N2 O12' _chemical_formula_weight 981.11 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/a' 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' _cell_length_a 13.667(4) _cell_length_b 18.647(11) _cell_length_c 20.188(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.72(2) _cell_angle_gamma 90.00 _cell_volume 5145.(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 12 _cell_measurement_temperature 243(2) _exptl_crystal_description Parallelepiped _exptl_crystal_colour Orange _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? loop_ _publ_author_name 'Slimane Dahaoui' 'Christian Jelsch' 'Judith A. K. Howard' 'Claude Lecomte' _chemical_name_systematic ; N-Acetyl-L-tyrosine Ethyl Ester Monohydrate ; _chemical_formula_moiety 'C13 H17 N O4,H2 O' _chemical_formula_sum 'C13 H19 N1 O5' _chemical_formula_weight 269.29 _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.235(2) _cell_length_b 13.056(4) _cell_length_c 14.415(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1361.6(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 512 _cell_measurement_theta_min 11 _cell_measurement_theta_max 45 _cell_measurement_temperature 110(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 110(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'rotating anode tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART-CCD diffractometer' _diffrn_measurement_method '\w scan' _diffrn_reflns_number 98393 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 51.10 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _reflns_number_total 14787 _reflns_number_observed 10189 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0272 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0202 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.650 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? _refine_ls_number_reflns 10189 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)] ' _refine_ls_shift/esd_max -0.006 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.139 _refine_diff_density_min -0.170 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.6(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 .23164(13) .20571(4) .42334(4) .02010(10) Uani d . 1 . O O .57804(8) .03798(4) .37422(5) .01700(10) Uani d . 1 . O O2 .19614(9) .12871(4) .56155(4) .01490(10) Uani d . 1 . O OH -.02619(10) -.44263(4) .32345(4) .01850(10) Uani d . 1 . O HH .031(4) -.491(2) .364(2) .023(2) Uiso d . 1 . H N .27588(7) .01970(3) .33598(3) .01230(10) Uani d . 1 . N H .178(4) .024(4) .284(2) .0154(19) Uiso d . 1 . H CA .21351(6) .01977(3) .43117(3) .01090(10) Uani d . 1 . C HA .311(2) -.024(2) .472(2) .0137(17) Uiso d . 1 . H C .45551(7) .03238(3) .31432(3) .01280(10) Uani d . 1 . C C2 .21534(6) .12880(3) .47020(3) .01180(10) Uani d . 1 . C CG .00760(7) -.13705(3) .40996(3) .01240(10) Uani d . 1 . C CD1 .10085(7) -.21384(4) .45900(3) .01490(10) Uani d . 1 . C HD1 .185(4) -.193(2) .517(2) .019(2) Uiso d . 1 . H C3 .20187(9) .22828(4) .60674(4) .01780(10) Uani d . 1 . C H31 .094(4) .273(2) .573(2) .022(2) Uiso d . 1 . H H32 .336(4) .262(2) .593(2) .022(2) Uiso d . 1 . H CB .01763(6) -.02579(3) .43907(3) .01340(10) Uani d . 1 . C HB1 -.026(5) -.016(2) .510(2) .0168(16) Uiso d . 1 . H HB2 -.076(4) .021(2) .398(2) .0168(16) Uiso d . 1 . H C1 .49913(8) .04026(4) .21235(3) .02050(10) Uani d . 1 . C H11 .636(5) .011(3) .198(2) .025(3) Uiso d . 1 . H H12 .494(5) .121(3) .194(2) .025(3) Uiso d . 1 . H H13 .392(5) .006(3) .169(2) .025(3) Uiso d . 1 . H CZ -.01333(7) -.34367(4) .35433(3) .01360(10) Uani d . 1 . C CE2 -.10879(8) -.26824(4) .30497(4) .01780(10) Uani d . 1 . C HE2 -.187(4) -.288(2) .244(2) .022(2) Uiso d . 1 . H CE1 .09113(7) -.31631(3) .43194(3) .01480(10) Uani d . 1 . C HE1 .161(4) -.375(2) .470(2) .019(2) Uiso d . 1 . H CD2 -.09781(7) -.16620(3) .33312(3) .01650(10) Uani d . 1 . C HD2 -.171(2) -.107(2) .295(2) .021(2) Uiso d . 1 . H C4 .16687(10) .21257(4) .70827(4) .02600(10) Uani d . 1 . C H41 .199(4) .284(2) .743(2) .031(2) Uiso d . 1 . H H42 .255(4) .154(2) .737(2) .031(2) Uiso d . 1 . H H43 .024(4) .190(2) .720(2) .031(2) Uiso d . 1 . H OW .14436(8) .42520(4) .43837(4) .01910(10) Uani d . 1 . O HW1 .118(4) .432(2) .504(2) .024(2) Uiso d . 1 . H HW2 .158(4) .353(2) .426(2) .024(2) 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 O1 .0355(3) .01068(15) .01406(18) .00118(18) .00384(19) .00146(14) O .01324(19) .0218(2) .01590(18) -.00126(16) -.00122(16) -.00271(15) O2 .0239(2) .00970(14) .01103(17) .00023(16) .00065(16) -.00136(13) OH .0253(3) .01128(16) .0184(2) .00086(16) -.00888(19) -.00171(14) N .01215(16) .01438(15) .01019(14) .00012(13) -.00041(13) -.00168(11) CA .01200(14) .01000(12) .01083(13) .00071(11) -.00016(12) -.00123(10) C .01322(17) .01359(16) .01150(15) -.00102(12) .00057(13) -.00267(12) C2 .01517(17) .00907(13) .01110(14) .00049(12) .00059(12) -.00043(11) CG .01322(17) .01120(14) .01278(15) -.00057(12) -.00120(14) -.00101(11) CD1 .01795(19) .01264(16) .01410(15) -.0007(14) -.00543(15) -.00081(12) C3 .0280(3) .01063(14) .01487(17) .00054(15) .00045(17) -.00248(13) CB .01228(15) .01213(14) .01579(15) -.00010(12) .00099(12) -.00257(12) C1 .0227(2) .0254(2) .01337(16) -.00591(17) .00452(15) -.00347(14) CZ .01665(19) .01093(15) .01327(16) -.00017(14) -.00403(15) -.00068(12) CE2 .0242(2) .01213(16) .01714(18) .00123(15) -.01004(17) -.00136(14) CE1 .01790(17) .01205(14) .01452(16) -.00029(16) -.00571(15) .00006(12) CD2 .02070(19) .01174(15) .01705(17) .00096(14) -.00726(16) -.00062(13) C4 .0487(4) .01736(18) .01260(17) .0064(2) -.00312(19) -.00303(14) OW .0274(2) .01407(16) .01584(19) .00282(15) -.00161(16) .00180(13)