#------------------------------------------------------------------------------ #$Date: 2014-08-05 19:20:29 +0300 (Tue, 05 Aug 2014) $ #$Revision: 121325 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/68/1516804.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_1516804 loop_ _publ_author_name 'Minkov, Vasily S.' 'Boldyreva, Elena V.' _publ_section_title ; Contribution of Weak S-H···O Hydrogen Bonds to the Side Chain Motions in d,l-Homocysteine on Cooling. ; _journal_issue 29 _journal_name_full 'The journal of physical chemistry. B' _journal_page_first 8513 _journal_page_last 8523 _journal_paper_doi 10.1021/jp503154x _journal_volume 118 _journal_year 2014 _chemical_formula_moiety 'C4 H9 N O2 S' _chemical_formula_sum 'C4 H9 N O2 S' _chemical_formula_weight 135.19 _chemical_name_common DL-homocysteine _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 102.934(8) _cell_angle_beta 91.190(9) _cell_angle_gamma 107.073(8) _cell_formula_units_Z 2 _cell_length_a 5.1838(6) _cell_length_b 5.5014(6) _cell_length_c 11.3669(12) _cell_measurement_reflns_used 6402 _cell_measurement_temperature 215(2) _cell_measurement_theta_max 29.55 _cell_measurement_theta_min 1.85 _cell_volume 300.71(6) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 215(2) _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector_type STOE _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 3821 _diffrn_reflns_theta_full 29.16 _diffrn_reflns_theta_max 29.16 _diffrn_reflns_theta_min 1.85 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_T_max 0.9569 _exptl_absorpt_correction_T_min 0.7580 _exptl_absorpt_correction_type numerical _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 144 _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.379 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.063 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1619 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0369 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.0957P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.1006 _reflns_number_gt 1395 _reflns_number_total 1619 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file jp503154x_si_001.cif _[local]_cod_data_source_block DL-homocysteine-215K _cod_depositor_comments 'Adding full bibliography for 1516800--1516810.cif.' _cod_database_code 1516804 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -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 S1 S 1.20427(8) 0.88390(9) 0.11881(4) 0.03700(16) Uani 1 1 d H1S H 1.271(5) 1.020(5) 0.224(2) 0.044 Uiso 1 1 d O1 O 0.6626(2) 0.1959(2) 0.39011(10) 0.0260(2) Uani 1 1 d O2 O 1.1107(2) 0.3176(2) 0.37240(10) 0.0253(2) Uani 1 1 d N1 N 0.6566(2) 0.6967(2) 0.39908(12) 0.0219(2) Uani 1 1 d H3N H 0.695(4) 0.722(4) 0.4771(19) 0.026 Uiso 1 1 d H2N H 0.655(4) 0.854(4) 0.3874(17) 0.026 Uiso 1 1 d H1N H 0.494(4) 0.590(4) 0.3813(17) 0.026 Uiso 1 1 d C4 C 0.8452(3) 0.7474(3) 0.13155(14) 0.0269(3) Uani 1 1 d H41 H 0.772(4) 0.683(4) 0.0461(19) 0.032 Uiso 1 1 d H42 H 0.783(4) 0.895(4) 0.1755(18) 0.032 Uiso 1 1 d C1 C 0.8800(3) 0.3498(3) 0.36904(12) 0.0194(3) Uani 1 1 d C3 C 0.7778(3) 0.5191(3) 0.19248(13) 0.0260(3) Uani 1 1 d H31 H 0.874(4) 0.391(4) 0.1532(18) 0.031 Uiso 1 1 d H32 H 0.590(4) 0.432(4) 0.1779(18) 0.031 Uiso 1 1 d C2 C 0.8594(3) 0.5934(3) 0.32964(12) 0.0199(3) Uani 1 1 d H21 H 1.029(4) 0.726(4) 0.3490(16) 0.024 Uiso 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 S1 0.0283(2) 0.0414(3) 0.0350(2) 0.00870(18) 0.00897(16) 0.00107(17) O1 0.0236(5) 0.0193(5) 0.0392(6) 0.0119(4) 0.0076(4) 0.0086(4) O2 0.0215(5) 0.0253(5) 0.0322(6) 0.0069(4) 0.0027(4) 0.0117(4) N1 0.0228(6) 0.0175(5) 0.0297(6) 0.0095(5) 0.0067(5) 0.0094(5) C4 0.0251(7) 0.0288(8) 0.0283(7) 0.0117(6) 0.0024(5) 0.0070(6) C1 0.0213(6) 0.0176(6) 0.0203(6) 0.0033(5) 0.0017(5) 0.0083(5) C3 0.0284(7) 0.0212(7) 0.0261(7) 0.0066(5) 0.0012(5) 0.0037(6) C2 0.0189(6) 0.0172(6) 0.0254(6) 0.0071(5) 0.0042(5) 0.0063(5) 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C4 S1 H1S 98.4(11) C2 N1 H3N 110.4(13) C2 N1 H2N 112.7(12) H3N N1 H2N 105.9(18) C2 N1 H1N 112.5(13) H3N N1 H1N 107.0(18) H2N N1 H1N 108.0(18) C3 C4 S1 113.80(11) C3 C4 H41 109.2(12) S1 C4 H41 101.8(12) C3 C4 H42 112.2(12) S1 C4 H42 106.5(12) H41 C4 H42 113.0(17) O1 C1 O2 126.25(13) O1 C1 C2 116.77(11) O2 C1 C2 116.91(12) C4 C3 C2 115.20(12) C4 C3 H31 108.5(12) C2 C3 H31 107.6(11) C4 C3 H32 108.7(12) C2 C3 H32 109.1(12) H31 C3 H32 107.4(17) N1 C2 C1 109.43(11) N1 C2 C3 111.17(12) C1 C2 C3 109.01(11) N1 C2 H21 107.4(11) C1 C2 H21 109.3(11) C3 C2 H21 110.6(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C4 1.8136(16) S1 H1S 1.24(2) O1 C1 1.2590(17) O2 C1 1.2605(16) N1 C2 1.4952(17) N1 H3N 0.88(2) N1 H2N 0.91(2) N1 H1N 0.86(2) C4 C3 1.524(2) C4 H41 0.98(2) C4 H42 0.99(2) C1 C2 1.5358(18) C3 C2 1.537(2) C3 H31 1.01(2) C3 H32 0.94(2) C2 H21 0.95(2) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O2 0.86(2) 2.09(2) 2.9435(17) 168.5(18) 1_455 N1 H2N O1 0.91(2) 1.86(2) 2.7625(15) 170.9(18) 1_565 N1 H3N O2 0.88(2) 2.05(2) 2.8678(17) 154.7(18) 2_766 N1 H3N O1 0.88(2) 2.496(19) 2.9891(16) 116.3(15) 2_666 S1 H1S O1 1.24(2) 2.55(2) 3.6102(13) 142.4(15) 1_665 S1 H1S O2 1.24(2) 2.42(2) 3.4490(12) 138.9(15) 1_565 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 S1 C4 C3 C2 71.74(15) O1 C1 C2 N1 38.27(16) O2 C1 C2 N1 -144.52(12) O1 C1 C2 C3 -83.50(15) O2 C1 C2 C3 93.71(14) C4 C3 C2 N1 80.27(15) C4 C3 C2 C1 -159.02(12)