#------------------------------------------------------------------------------ #$Date: 2012-02-24 17:13:23 +0000 (Fri, 24 Feb 2012) $ #$Revision: 34330 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/02/4060204.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_4060204 loop_ _publ_author_name ' Chekmenev , Eduard' ' Zhang , Qianwen' ' Waddell , Kevin' ' Mashuta, Mark S.' 'Wittebort, Richard J.' _publ_section_title ; Glycyl 15N Chemical Shielding in Tripeptides: ; _journal_name_full Organometallics _journal_year 2004 _chemical_formula_moiety 'C7 H14 N3 O4, Cl' _chemical_formula_sum 'C7 H14 Cl N3 O4' _chemical_formula_weight 239.66 _chemical_name_common 'ala-gly-gly HCl' _chemical_name_systematic ; alanyl-glycyl-glycine hydrochloride ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M P2(1)2(1)2(1) _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.2258(5) _cell_length_b 8.7007(9) _cell_length_c 22.970(2) _cell_measurement_reflns_used 4816 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.32 _cell_measurement_theta_min 2.50 _cell_volume 1044.42(18) _diffrn_ambient_temperature 100(2) _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method \w-scans _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 8593 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 1.77 _diffrn_standards_decay_% <0.1 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Sheldrick, G. M.; SADABS (1996). ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 504 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _refine_ls_abs_structure_details ad _refine_ls_abs_structure_Flack 0.05(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 165 _refine_ls_number_reflns 2214 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.05 _refine_ls_R_factor_all 0.053 _refine_ls_R_factor_gt 0.048 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+0.9950P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.106 _refine_ls_wR_factor_ref 0.109 _reflns_number_gt 2065 _reflns_number_total 2214 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4060204 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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.6354(4) 0.2185(2) 0.04697(9) 0.0129(4) Uani 1 1 d . . . O2 O 0.8267(4) 0.0131(3) 0.21160(9) 0.0125(5) Uani 1 1 d . . . O3 O 0.6092(5) -0.2594(3) 0.32138(9) 0.0168(5) Uani 1 1 d . . . O4 O 0.8237(4) -0.3303(3) 0.24111(10) 0.0147(5) Uani 1 1 d . . . H4O H 0.923(10) -0.382(6) 0.268(2) 0.022(16) Uiso 1 1 d . . . N1 N 0.8832(6) 0.4909(3) 0.02787(12) 0.0112(5) Uani 1 1 d . . . H1NC H 0.983(8) 0.576(5) 0.0258(16) 0.015(10) Uiso 1 1 d . . . H1NB H 0.917(9) 0.438(5) -0.0021(17) 0.021(11) Uiso 1 1 d . . . H1NA H 0.718(9) 0.525(5) 0.0307(18) 0.025(11) Uiso 1 1 d . . . N2 N 0.9685(5) 0.1235(3) 0.10041(11) 0.0102(6) Uani 1 1 d . . . H2N H 1.113(8) 0.149(4) 0.1190(16) 0.020(10) Uiso 1 1 d . . . N3 N 0.5483(5) -0.1490(3) 0.17117(12) 0.0117(6) Uani 1 1 d . . . H3N H 0.500(7) -0.197(4) 0.1396(16) 0.012(9) Uiso 1 1 d . . . C1 C 0.8402(6) 0.2354(3) 0.07299(13) 0.0091(6) Uani 1 1 d . . . C2 C 0.9669(6) 0.3926(4) 0.07771(14) 0.0095(6) Uani 1 1 d . . . H2 H 1.138(7) 0.385(3) 0.0728(13) 0.016(7) Uiso 1 1 d . . . C3 C 0.8968(7) 0.4721(4) 0.13423(13) 0.0130(6) Uani 1 1 d . . . H3C H 0.9732 0.5749 0.1350 0.020 Uiso 1 1 calc R . . H3B H 0.9615 0.4118 0.1671 0.020 Uiso 1 1 calc R . . H3A H 0.7102 0.4808 0.1371 0.020 Uiso 1 1 calc R . . C4 C 0.8645(7) -0.0304(3) 0.10781(13) 0.0120(6) Uani 1 1 d . . . H4B H 1.0033 -0.1067 0.1027 0.014 Uiso 1 1 calc R . . H4A H 0.7342 -0.0496 0.0774 0.014 Uiso 1 1 calc R . . C5 C 0.7433(6) -0.0517(3) 0.16751(13) 0.0102(6) Uani 1 1 d . . . C6 C 0.4426(5) -0.1887(4) 0.22775(13) 0.0132(6) Uani 1 1 d . . . H6B H 0.2982 -0.2608 0.2220 0.016 Uiso 1 1 calc R . . H6A H 0.3736 -0.0945 0.2461 0.016 Uiso 1 1 calc R . . C7 C 0.6342(7) -0.2616(3) 0.26888(13) 0.0117(6) Uani 1 1 d . . . Cl1 Cl 0.37687(14) 0.68926(8) 0.05423(3) 0.01184(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0143(10) 0.0133(10) 0.0113(10) -0.0011(8) -0.0028(10) -0.0009(9) O2 0.0104(11) 0.0144(11) 0.0128(10) -0.0013(9) 0.0003(9) -0.0037(9) O3 0.0140(11) 0.0238(12) 0.0128(11) -0.0003(9) -0.0006(10) 0.0026(11) O4 0.0125(11) 0.0172(12) 0.0145(11) 0.0009(10) 0.0000(9) 0.0043(9) N1 0.0100(13) 0.0107(13) 0.0130(13) -0.0006(10) 0.0032(12) -0.0006(13) N2 0.0102(13) 0.0102(13) 0.0101(13) 0.0019(10) -0.0032(10) -0.0025(10) N3 0.0119(13) 0.0115(13) 0.0115(13) 0.0030(11) -0.0035(10) -0.0009(10) C1 0.0101(15) 0.0109(14) 0.0063(12) -0.0012(11) 0.0038(12) -0.0017(12) C2 0.0048(13) 0.0121(15) 0.0117(15) 0.0028(12) -0.0004(12) -0.0024(12) C3 0.0151(16) 0.0127(14) 0.0113(14) -0.0011(12) 0.0009(14) -0.0019(14) C4 0.0149(15) 0.0092(14) 0.0118(14) 0.0018(11) -0.0005(14) 0.0014(14) C5 0.0120(15) 0.0075(14) 0.0110(15) -0.0010(12) -0.0018(12) 0.0037(12) C6 0.0075(14) 0.0174(16) 0.0146(15) 0.0011(13) -0.0009(11) -0.0022(13) C7 0.0119(14) 0.0089(13) 0.0143(14) 0.0001(11) 0.0008(13) -0.0053(13) Cl1 0.0089(3) 0.0134(3) 0.0133(3) 0.0006(3) -0.0014(3) -0.0014(3)