#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100379.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_2100379 loop_ _publ_author_name 'Munshi, Parthapratim' 'Thakur, T. S.' 'Guru Row, T. N.' 'Desiraju, G. R.' _publ_section_title ; ? ; _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_iupac ? _chemical_formula_moiety 'C2 H5 N3 O S' _chemical_formula_structural ? _chemical_formula_sum 'C2 H5 N3 O S' _chemical_formula_weight 119.16 _chemical_melting_point ? _chemical_name_common 1-formyl-3-thiosemicarbazide _chemical_name_systematic ; 1-formyl-3-thiosemicarbazide ; _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _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_detector_area_resol_mean ? _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_interval_count ? _diffrn_standards_interval_time ? _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_meas ? _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_coef ? _refine_ls_extinction_expression ? _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_disorder_assembly _atom_site_disorder_group _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_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? 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_site_symmetry_3 _geom_angle _geom_angle_publ_flag 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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag 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) ?