#------------------------------------------------------------------------------ #$Date: 2009-11-16 02:43:51 +0100 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100379.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_2100379 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Munshi, Parthapratim' 'Thakur, T. S.' 'Guru Row, T. N.' 'Desiraju, G. R.' _publ_section_title ; ? ; _journal_coeditor_code LC5030 _journal_issue 1 _journal_name_full 'Acta Crystallographica, Section B' _journal_page_first 118 _journal_page_last 127 _journal_volume 62 _journal_year 2006 _chemical_formula_moiety 'C2 H5 N3 O S' _chemical_formula_sum 'C2 H5 N3 O S' _chemical_formula_weight 119.16 _chemical_name_common 1-formyl-3-thiosemicarbazide _chemical_name_systematic ; 1-formyl-3-thiosemicarbazide ; _symmetry_cell_setting Monoclinic _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 98.606(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.2569(17) _cell_length_b 7.4263(18) _cell_length_c 9.593(2) _cell_measurement_reflns_used 3850 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.4 _cell_measurement_theta_min 2.84 _cell_volume 511.2(2) _computing_cell_refinement 'SMART (Bruker, 2004)' _computing_data_collection 'SMART (Bruker, 2004)' _computing_data_reduction 'SMART (Bruker, 2004)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'PLATON (Spek, 2001)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\f & \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 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0126 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3850 _diffrn_reflns_reduction_process ' ?' _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.84 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_T_max 0.9231 _exptl_absorpt_correction_T_min 0.8272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_description prism _exptl_crystal_F_000 248 _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.242 _refine_diff_density_min -0.265 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 80 _refine_ls_number_reflns 1012 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.075 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0288 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.1699P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.0764 _reflns_number_gt 961 _reflns_number_total 1012 _reflns_threshold_expression >2sigma(I) loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z 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_type_symbol S1 0.78081(5) 0.18924(5) 0.54094(4) 0.03944(17) Uani d . 1 S C2 0.9854(2) 0.29268(18) 0.60197(14) 0.0286(3) Uani d . 1 C N3 0.9916(2) 0.44516(19) 0.67164(15) 0.0395(3) Uani d . 1 N N4 1.14576(17) 0.21758(18) 0.57826(14) 0.0340(3) Uani d . 1 N N5 1.31717(17) 0.29497(17) 0.62762(13) 0.0347(3) Uani d . 1 N H5 1.3606 0.3785 0.5796 0.042 Uiso calc R 1 H C6 1.4154(2) 0.2403(2) 0.74972(16) 0.0340(3) Uani d . 1 C O7 1.35930(16) 0.13404(17) 0.82965(12) 0.0465(3) Uani d . 1 O H3A 0.888(3) 0.498(3) 0.6861(19) 0.052(5) Uiso d . 1 H H3B 1.091(3) 0.492(3) 0.702(2) 0.052(6) Uiso d . 1 H H4 1.149(3) 0.116(3) 0.5415(19) 0.039(5) Uiso d . 1 H H6 1.537(3) 0.297(2) 0.763(2) 0.046(5) Uiso d . 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 0.0244(2) 0.0430(3) 0.0486(3) 0.00265(14) -0.00218(16) -0.01180(16) C2 0.0283(7) 0.0320(7) 0.0249(6) 0.0028(5) 0.0024(5) 0.0014(5) N3 0.0311(7) 0.0377(7) 0.0490(8) 0.0015(6) 0.0035(6) -0.0126(6) N4 0.0245(6) 0.0357(7) 0.0408(7) 0.0004(5) 0.0016(5) -0.0086(6) N5 0.0250(6) 0.0412(7) 0.0380(7) -0.0058(5) 0.0055(5) 0.0043(5) C6 0.0247(7) 0.0398(8) 0.0375(8) -0.0035(6) 0.0052(6) -0.0039(7) O7 0.0417(6) 0.0565(7) 0.0401(6) -0.0130(6) 0.0026(5) 0.0082(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source S S 0.1246 0.1234 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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 N3 C2 N4 118.74(14) N3 C2 S1 121.89(12) N4 C2 S1 119.37(11) C2 N3 H3A 120.0(13) C2 N3 H3B 121.0(14) H3A N3 H3B 119(2) C2 N4 N5 121.78(13) C2 N4 H4 121.7(13) N5 N4 H4 116.2(13) C6 N5 N4 120.36(13) C6 N5 H5 119.8 N4 N5 H5 119.8 O7 C6 N5 124.40(14) O7 C6 H6 125.5(12) N5 C6 H6 110.1(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C2 1.6959(15) C2 N3 1.312(2) C2 N4 1.3405(19) N3 H3A 0.88(2) N3 H3B 0.82(2) N4 N5 1.3876(17) N4 H4 0.83(2) N5 C6 1.340(2) N5 H5 0.8600 C6 O7 1.212(2) C6 H6 0.97(2)