#------------------------------------------------------------------------------ #$Date: 2017-10-13 03:48:21 +0300 (Fri, 13 Oct 2017) $ #$Revision: 201957 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/06/2010600.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_2010600 loop_ _publ_author_name 'Parsons, Simon' 'Smith, Andrew G.' 'Tasker, Peter A.' 'White, David J.' _publ_section_title ; Acetone-4-methylthiosemicarbazone at 220K ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 237 _journal_page_last 238 _journal_paper_doi 10.1107/S0108270199014559 _journal_volume 56 _journal_year 2000 _chemical_formula_sum 'C5 H11 N3 S' _chemical_formula_weight 145.23 _chemical_name_systematic ; ? ; _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 SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 103.43(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.067(4) _cell_length_b 9.783(5) _cell_length_c 11.440(6) _cell_measurement_reflns_used 31 _cell_measurement_temperature 220(2) _cell_measurement_theta_max 22 _cell_measurement_theta_min 20 _cell_volume 769.3(7) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1990a)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1990b)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997b)' _diffrn_ambient_temperature 220(2) _diffrn_measured_fraction_theta_full .925 _diffrn_measured_fraction_theta_max .925 _diffrn_measurement_device_type ; Stoe Stadi-4 diffractometer equipped with an Oxford Cryosystems open flow cryostat device. ; _diffrn_measurement_method \w-\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents .0132 _diffrn_reflns_av_sigmaI/netI .0190 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2687 _diffrn_reflns_theta_full 69.93 _diffrn_reflns_theta_max 69.93 _diffrn_reflns_theta_min 6.02 _diffrn_standards_decay_% +/-1 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 3.092 _exptl_absorpt_correction_T_max .658 _exptl_absorpt_correction_T_min .302 _exptl_absorpt_correction_type 'Optimised numerical' _exptl_absorpt_process_details ; A numerical absorption was performed by Gaussian integration after refinement of the crystal form and dimensions against a set of psi-scans (X-shape; Stoe & Cie, 1997). ; _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'plate developed in (001)' _exptl_crystal_F_000 312 _exptl_crystal_size_max .42 _exptl_crystal_size_mid .31 _exptl_crystal_size_min .12 _refine_diff_density_max .300 _refine_diff_density_min -.401 _refine_ls_extinction_coef .0144(15) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997a)' _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 94 _refine_ls_number_reflns 1348 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all .0495 _refine_ls_R_factor_gt .0431 _refine_ls_shift/su_max .018 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.7050P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1221 _reflns_number_gt 1181 _reflns_number_total 1348 _reflns_threshold_expression I>2\s(I) _cod_data_source_file bm1372.cif _cod_data_source_block I _cod_depositor_comments ; 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. 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. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'Not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2010600 _cod_database_fobs_code 2010600 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_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_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol S1 .26869(10) .14281(6) .64775(5) .0360(3) Uani d . 1 . . S C1 .2538(3) .2408(2) .5243(2) .0290(6) Uani d . 1 . . C N1 .2563(3) .3793(2) .53596(19) .0332(5) Uani d . 1 . . N H1 .270(4) .415(3) .603(3) .036(8) Uiso d . 1 . . H N2 .2411(3) .4609(2) .43562(18) .0306(5) Uani d . 1 . . N C3 .2443(3) .5906(2) .4509(2) .0288(6) Uani d . 1 . . C C31 .2621(4) .6599(3) .5697(2) .0402(7) Uani d . 1 . . C H31A .2545 .7581 .5580 .060 Uiso calc R 1 . . H H31B .3861 .6365 .6227 .060 Uiso calc R 1 . . H H31C .1572 .6300 .6053 .060 Uiso calc R 1 . . H C32 .2273(4) .6770(3) .3415(2) .0365(6) Uani d . 1 . . C H32A .3421 .7340 .3506 .055 Uiso calc R 1 . . H H32B .1127 .7345 .3311 .055 Uiso calc R 1 . . H H32C .2159 .6187 .2716 .055 Uiso calc R 1 . . H N4 .2394(3) .1933(2) .41414(19) .0335(5) Uani d . 1 . . N H4 .247(4) .255(3) .363(2) .027(7) Uiso d . 1 . . H C41 .2341(5) .0490(3) .3840(3) .0428(7) Uani d . 1 . . C H41A .3637 .0107 .4099 .064 Uiso calc R 1 . . H H41B .1889 .0381 .2977 .064 Uiso calc R 1 . . H H41C .1463 .0019 .4241 .064 Uiso calc R 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 S1 .0502(5) .0286(4) .0314(4) .0003(3) .0141(3) .0064(2) C1 .0300(14) .0261(12) .0318(12) .0002(9) .0090(9) .0000(9) N1 .0514(15) .0223(10) .0269(11) -.0003(9) .0115(9) .0003(8) N2 .0416(13) .0240(10) .0273(10) -.0004(8) .0103(9) .0014(8) C3 .0298(14) .0243(12) .0324(12) -.0010(9) .0076(10) .0000(9) C31 .0527(19) .0291(14) .0385(14) -.0016(11) .0102(12) -.0068(11) C32 .0479(17) .0243(12) .0377(14) -.0007(11) .0108(12) .0026(10) N4 .0496(14) .0217(10) .0314(11) -.0007(9) .0139(9) .0011(9) C41 .062(2) .0254(14) .0422(14) .0016(12) .0140(13) -.0060(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .3331 .5567 '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 N4 C1 N1 116.0(2) yes N4 C1 S1 124.93(19) yes N1 C1 S1 119.08(18) yes C1 N1 N2 119.8(2) yes C3 N2 N1 117.6(2) yes N2 C3 C32 116.8(2) yes N2 C3 C31 124.6(2) yes C32 C3 C31 118.6(2) yes C1 N4 C41 124.0(2) 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 . 1.689(2) yes C1 N4 . 1.325(3) yes C1 N1 . 1.361(3) yes N1 N2 . 1.382(3) yes N2 C3 . 1.281(3) yes C3 C32 . 1.492(3) yes C3 C31 . 1.497(3) yes N4 C41 . 1.451(3) yes loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 10302189