#------------------------------------------------------------------------------ #$Date: 2014-01-30 13:15:25 +0200 (Thu, 30 Jan 2014) $ #$Revision: 99302 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/33/1513331.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided the Crystal Eye server at # http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the # Peter Murray-Rust laboratory. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_1513331 loop_ _publ_author_name 'Moggach, Stephen A.' 'Allan, David R.' 'Parsons, Simon' 'Sawyer, Lindsay' 'Warren, John E.' _publ_section_title ; The effect of pressure on the crystal structure of hexagonalL-cystine ; _journal_coeditor_code XD5007 _journal_issue 5 _journal_name_full 'Journal of Synchrotron Radiation' _journal_page_first 598 _journal_page_last 607 _journal_paper_doi 10.1107/S0909049505019850 _journal_volume 12 _journal_year 2005 _chemical_formula_moiety 'C6 H12 N2 O4 S2' _chemical_formula_sum 'C6 H12 N2 O4 S2' _chemical_formula_weight 240.30 _chemical_name_common L-cystine _chemical_name_systematic 'L-(-)-3,3'-Dithiobis(2-aminopropanoic acid)' _space_group_IT_number 178 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P 61 2 (0 0 5)' _symmetry_space_group_name_H-M 'P 61 2 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method CRYSTALS_ver_12.80 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 5.31410(10) _cell_length_b 5.31410(10) _cell_length_c 54.291(3) _cell_measurement_reflns_used 3365 _cell_measurement_temperature 293 _cell_measurement_theta_max 53 _cell_measurement_theta_min 9 _cell_volume 1327.75(8) _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_collection 'SMART (Siemens, 1993)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _diffrn_ambient_temperature 293 _diffrn_measured_fraction_theta_full 0.455 _diffrn_measured_fraction_theta_max 0.422 _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method \w _diffrn_radiation_monochromator 'Silicon (111)' _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.6774 _diffrn_reflns_av_R_equivalents 0.053 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 4229 _diffrn_reflns_theta_full 25.309 _diffrn_reflns_theta_max 28.121 _diffrn_reflns_theta_min 4.492 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.592 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.803 _exptl_crystal_description 'hexagonal block' _exptl_crystal_F_000 756 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.27 _refine_diff_density_min -0.21 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0538 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 64 _refine_ls_number_reflns 458 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0483 _refine_ls_shift/su_max 0.000120 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(F^2^) + 0.03 + 3.33P] where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1122 _refine_ls_wR_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.1122 _reflns_number_gt 438 _reflns_number_total 492 _reflns_threshold_expression I>2.00u(I) _[local]_cod_data_source_file xd5007sup1.cif _[local]_cod_data_source_block cystin23 _cod_database_code 1513331 loop_ _symmetry_equiv_pos_as_xyz x,y,z x-y,x,z+1/6 -y,x-y,z+1/3 -x,-y,z+1/2 -x+y,-x,z+2/3 y,-x+y,z+5/6 x-y,-y,-z -y,-x,-z+5/6 -x,-x+y,-z+2/3 -x+y,y,-z+1/2 y,x,-z+1/3 x,x-y,-z+1/6 loop_ _atom_site_label _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_type_symbol S1 0.0379(2) 0.8292(2) 0.08036(6) 0.0316 Uani 1.0000 S O1 0.0899(5) 1.2288(4) 0.02371(12) 0.0218 Uani 1.0000 O C3 -0.1619(4) 1.0333(4) 0.02859(10) 0.0256 Uani 1.0000 C O2 -0.3791(5) 1.0675(5) 0.03148(11) 0.0331 Uani 1.0000 O C2 -0.2098(4) 0.7269(3) 0.03295(7) 0.0247 Uani 1.0000 C C1 -0.2695(6) 0.6317(6) 0.05979(6) 0.0291 Uani 1.0000 C N1 0.0390(6) 0.7081(5) 0.02292(10) 0.0255 Uani 1.0000 N H2 -0.4323 0.6592 0.0657 0.0330 Uiso 1.0000 H H1 -0.3298 0.4210 0.0606 0.0330 Uiso 1.0000 H H3 -0.3855 0.5889 0.0233 0.0285 Uiso 1.0000 H H6 0.0676 0.7658 0.0071 0.0295 Uiso 1.0000 H H5 0.1997 0.8237 0.0317 0.0295 Uiso 1.0000 H H4 0.0011 0.5232 0.0238 0.0295 Uiso 1.0000 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 S1 0.0322(6) 0.0292(6) 0.041(3) 0.0209(5) -0.0013(9) -0.0005(8) O1 0.0224(14) 0.0147(12) 0.028(9) 0.0086(11) 0.007(2) 0.0037(17) C3 0.0187(16) 0.0163(16) 0.043(10) 0.0099(13) 0.001(3) -0.001(3) O2 0.0225(14) 0.0244(15) 0.058(10) 0.0157(12) 0.000(2) 0.001(2) C2 0.0157(16) 0.0127(14) 0.043(4) 0.0049(13) 0.002(2) 0.001(2) C1 0.0240(19) 0.0153(17) 0.043(4) 0.0063(15) 0.0057(19) 0.002(2) N1 0.0183(16) 0.0112(14) 0.044(7) 0.0054(13) 0.003(2) -0.001(2) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 'International Tables Vol C 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_site_symmetry_1 _geom_angle _geom_angle_publ_flag S1 S1 C1 12_575 102.90(16) yes O1 C3 O2 . 125.73(5) yes O1 C3 C2 . 117.19(5) yes O2 C3 C2 . 116.98(5) yes C3 C2 C1 . 113.36(5) yes C3 C2 N1 . 109.56(5) yes C1 C2 N1 . 112.03(5) yes C3 C2 H3 . 107.2 no C1 C2 H3 . 107.2 no N1 C2 H3 . 107.2 no C2 C1 S1 . 114.7(2) yes C2 C1 H2 . 108.1 no S1 C1 H2 . 108.1 no C2 C1 H1 . 108.1 no S1 C1 H1 . 108.1 no H2 C1 H1 . 109.5 no C2 N1 H6 . 109.5 no C2 N1 H5 . 109.5 no H6 N1 H5 . 109.5 no C2 N1 H4 . 109.5 no H6 N1 H4 . 109.5 no H5 N1 H4 . 109.5 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 S1 12_575 2.043(2) yes S1 C1 . 1.8177(7) yes O1 C3 . 1.2446(9) yes C3 O2 . 1.2651(9) yes C3 C2 . 1.5359(8) yes C2 C1 . 1.5226(9) yes C2 N1 . 1.4791(9) yes C2 H3 . 1.000 no C1 H2 . 1.000 no C1 H1 . 1.000 no N1 H6 . 0.900 no N1 H5 . 0.900 no N1 H4 . 0.900 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H6 O1 7_675 0.900 2.007 2.780 143.1 yes N1 H5 O2 1_655 0.900 1.946 2.742 146.5 yes N1 H4 O1 1_545 0.900 1.846 2.693 155.8 yes