#------------------------------------------------------------------------------ #$Date: 2017-10-13 01:08:28 +0100 (Fri, 13 Oct 2017) $ #$Revision: 201955 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/62/2006230.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # 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_2006230 loop_ _publ_author_name 'Bogdan Prelesnik' 'Katarina Andjelkovi\'c' 'Zorica Markovi\'c' 'Tibor Sabo' 'Sre\'cko Trifunovi\'c' _publ_section_title ; Potassium 3-Dithiocarboxy-3-aza-5-aminopentanoate Dihydrate ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 719 _journal_page_last 720 _journal_paper_doi 10.1107/S0108270197001650 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac 'K + , C5 H9 N2 O2 S2 - , 2H2 O' _chemical_formula_sum 'C5 H13 K N2 O4 S2' _chemical_formula_weight 268.39 _chemical_name_systematic ; Potassium 3-Dithiocarboxy-3-Aza-5-Amino Pentanoate Dihydrate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method manually _cell_angle_alpha 90.00 _cell_angle_beta 111.660(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.8156(12) _cell_length_b 6.947(2) _cell_length_c 12.4225(14) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15.96 _cell_measurement_theta_min 9.76 _cell_volume 1108.1(4) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'CAD-4 Software' _computing_molecular_graphics 'ORTEX (McArdle, 1994)' _computing_publication_material SDP _computing_structure_refinement SDP _computing_structure_solution SDP _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\w/2\q scan' _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 0.0228 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 2729 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_min 1.59 _diffrn_standards_decay_% 0.6 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_meas 1.606 _exptl_crystal_density_method 'flotation in a CHBr~3~/m-C~4~H~10~ mixture' _exptl_crystal_description prismatic _exptl_crystal_F_000 560 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.608 _refine_diff_density_min -0.390 _refine_ls_extinction_coef '1.32(2) \\times 10^-6^' _refine_ls_extinction_method 'SDP (Frenz, 1982)' _refine_ls_goodness_of_fit_obs 0.957 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 144 _refine_ls_number_reflns 2031 _refine_ls_number_restraints 0 _refine_ls_restrained_S_obs 0.957 _refine_ls_R_factor_obs .039 _refine_ls_shift/esd_max 0.03 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(Fo)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs .041 _reflns_number_observed 2031 _reflns_number_total 2493 _reflns_observed_criterion >3sigma(I) _cod_data_source_file ka1221.cif _cod_data_source_block zora _cod_depositor_comments ; Changing the _atom_site_occupancy data item value from '.' to '1' for all fully occupied atom sites. Antanas Vaitkus, 2017-02-10 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'YES' changed to 'yes' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'YES' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times). '_geom_angle_publ_flag' value 'YES' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (12 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo)]' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo)]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 1108.0(4) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2006230 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' 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 K .0484(3) .0370(4) .0587(4) .0013(4) .0132(3) .0044(3) S1 .0444(3) .0380(4) .0451(3) .0030(3) .0277(2) -.0048(3) S2 .0393(3) .0368(4) .0371(3) -.0082(3) .0232(2) -.0029(3) O1 .0299(8) .0530(10) .0249(8) .0031(9) .0080(7) .0004(9) Ow1 .0430(10) .068(2) .0480(10) -.0050(10) .0122(9) -.0010(10) O2 .0325(8) .0490(10) .0343(8) -.0057(9) .0186(6) .0029(9) Ow2 .0370(10) .074(2) .107(2) -.042(2) .0040(10) .0090(10) N1 .0247(8) .0320(10) .0207(8) -.0024(9) .0100(6) -.0018(9) N2 .0390(10) .0320(10) .0320(10) .0040(10) .0147(8) -.0020(10) C1 .0230(10) .0360(10) .0210(10) .0020(10) .0075(8) .0020(10) C2 .0280(10) .0350(10) .0290(10) -.0030(10) .0122(8) -.0060(10) C3 .0350(10) .038(2) .0290(10) .0000(10) .0169(8) -.0060(10) C4 .0290(10) .0380(10) .0200(10) -.0040(10) .0103(8) .0010(10) C5 .0290(10) .0270(10) .0290(10) .0000(10) .0134(8) -.0020(10) 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 K .98551(6) .08050(10) .80406(7) .0499(3) Uani d . 1 . K S1 .26832(6) .12180(10) .19533(6) .03930(10) Uani d . 1 . S S2 .40518(5) .16730(10) .05955(6) .03510(10) Uani d . 1 . S O1 .15120(10) .5686(3) .0930(2) .0366(5) Uani d . 1 . O Ow1 .8577(2) .6493(4) .1190(2) .0542(8) Uani d . 1 . O O2 .15450(10) .6202(3) .2710(2) .0367(5) Uani d . 1 . O Ow2 -.0056(2) .7407(5) .4236(3) .0790(10) Uani d . 1 . O N1 .3582(2) .4507(3) .1745(2) .0252(5) Uani d . 1 . N N2 .2781(2) .7684(4) -.0015(2) .0338(6) Uani d . 1 . N C1 .3450(2) .2625(4) .1454(2) .0266(6) Uani d . 1 . C C2 .4238(2) .5770(4) .1339(2) .0300(6) Uani d . 1 . C C3 .3695(2) .6477(5) .0101(2) .0327(8) Uani d . 1 . C C4 .3134(2) .5342(4) .2534(2) .0286(6) Uani d . 1 . C C5 .1975(2) .5754(4) .2011(2) .0274(6) Uani d . 1 . C H21 .484 .507 .139 . . . . 1 . H H22 .443 .686 .183 . . . . 1 . H H31 .417 .720 -.012 . . . . 1 . H H32 .347 .539 -.039 . . . . 1 . H H41 .348 .652 .282 . . . . 1 . H H42 .326 .447 .316 . . . . 1 . H HN21 .283 .905 -.005 . . . . 1 . H HN22 .215 .711 -.005 . . . . 1 . H HW11 .805(3) .695(6) .124(3) . . . . 1 . H HW12 .840(3) .644(8) .070(4) . . . . 1 . H HW21 -.071(3) .767(7) .413(3) . . . . 1 . H HW22 .044(3) .800(7) .489(4) . . . . 1 . H 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' K K 0.2009 0.2494 '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' 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 _geom_angle_publ_flag C1 N1 C2 121.5(2) yes C1 N1 C4 121.1(2) yes C2 N1 C4 117.3(2) yes S1 C1 S2 120.9(2) yes N1 C4 C5 115.5(2) yes S1 C1 N1 119.6(2) yes S2 C1 N1 119.6(2) yes N1 C2 C3 113.6(2) yes N2 C3 C2 111.5(2) yes O1 C5 O2 124.2(2) yes O1 C5 C4 119.4(3) yes O2 C5 C4 116.4(3) yes 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 C1 . 1.717(3) yes S2 C1 . 1.708(3) yes O1 C5 . 1.257(3) yes C2 C3 . 1.523(4) yes O2 C5 . 1.259(4) yes N1 C1 . 1.351(4) yes N1 C2 . 1.477(4) yes C4 C5 . 1.516(3) yes N1 C4 . 1.459(4) yes N2 C3 . 1.478(4) yes 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 OW1 HW12 O1 3_665 0.5670(10) 2.5480(10) 3.0010(10) 139.30(10) no OW2 HW21 O1 4_566 0.8760(10) 2.3600(10) 2.989(5) 129.0(3) no OW2 HW22 O1 2_565 0.941(3) 1.8090(10) 2.738(3) 168.4(2) no N2 HN22 O1 . 0.9440(10) 2.0080(10) 2.8130(10) 142.00(10) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 30652170