#------------------------------------------------------------------------------ #$Date: 2009-11-16 02:43:51 +0100 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2100380.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_2100380 _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 'P2(1)/c ' _[local]_cod_cif_authors_sg_Hall '-P 2ybc ' 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 119.15 _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 90.00 _cell_angle_beta 98.4260(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.2339(5) _cell_length_b 7.3703(5) _cell_length_c 9.4771(7) _cell_measurement_reflns_used 4707 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.03 _cell_measurement_theta_min 2.76 _cell_volume 499.83(6) _computing_cell_refinement 'Bruker SMART for WNT/2000 v5.629' _computing_data_collection 'Bruker SMART for WNT/2000 v5.629' _computing_data_reduction 'Bruker SAINT Version 6.45,1997-2003' _computing_molecular_graphics 'Bruker SHELXTL Version 6.14,2000-2003' _computing_publication_material 'Bruker SHELXTL Version 6.14,2000-2003' _computing_structure_refinement 'Bruker SHELXTL Version 6.14,2000-2003' _computing_structure_solution 'Bruker SHELXTL Version 6.14,2000-2003' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega 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 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0111 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 6106 _diffrn_reflns_theta_full 26.03 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_min 2.85 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_T_max 0.9215 _exptl_absorpt_correction_T_min 0.8681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 248 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.196 _refine_diff_density_min -0.262 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 80 _refine_ls_number_reflns 982 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.079 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0245 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.2485P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0648 _refine_ls_wR_factor_ref 0.0653 _reflns_number_gt 953 _reflns_number_total 982 _reflns_threshold_expression >2sigma(I) 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_occupancy _atom_site_type_symbol C2 0.51400(18) 0.29455(17) 0.39851(13) 0.0128(3) Uani d 1 C C6 0.08200(17) 0.23961(18) 0.24985(14) 0.0145(3) Uani d 1 C N4 0.35312(15) 0.21776(16) 0.42325(12) 0.0145(3) Uani d 1 N N5 0.18118(16) 0.29668(15) 0.37321(12) 0.0146(3) Uani d 1 N N3 0.50740(17) 0.44900(16) 0.32790(12) 0.0161(3) Uani d 1 N O7 0.13925(13) 0.13081(13) 0.16897(10) 0.0187(2) Uani d 1 O S1 0.72032(4) 0.19016(4) 0.45953(3) 0.01576(14) Uani d 1 S H3A 0.612(3) 0.499(2) 0.3145(17) 0.024 Uiso d 1 H H3B 0.404(3) 0.498(2) 0.2971(18) 0.024 Uiso d 1 H H4 0.350(2) 0.115(3) 0.4623(19) 0.024 Uiso d 1 H H5 0.134(3) 0.349(2) 0.427(2) 0.024 Uiso d 1 H H6 -0.041(3) 0.297(2) 0.2348(19) 0.021(4) 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 C2 0.0146(6) 0.0141(6) 0.0095(6) -0.0009(4) 0.0010(5) -0.0025(5) C6 0.0121(6) 0.0154(6) 0.0164(6) 0.0002(5) 0.0028(5) 0.0034(5) N4 0.0111(5) 0.0148(5) 0.0172(6) 0.0006(4) 0.0004(4) 0.0037(4) N5 0.0116(6) 0.0169(6) 0.0154(6) 0.0035(4) 0.0029(4) -0.0019(4) N3 0.0130(5) 0.0158(6) 0.0194(6) -0.0001(4) 0.0016(4) 0.0043(4) O7 0.0189(5) 0.0212(5) 0.0160(5) 0.0038(4) 0.0028(4) -0.0023(4) S1 0.0112(2) 0.0163(2) 0.0190(2) -0.00057(11) -0.00037(13) 0.00372(11) 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' 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 N3 C2 N4 118.95(12) N3 C2 S1 121.83(10) N4 C2 S1 119.22(10) O7 C6 N5 124.25(12) O7 C6 H6 125.2(10) N5 C6 H6 110.5(10) C2 N4 N5 121.17(11) C2 N4 H4 122.2(12) N5 N4 H4 116.4(12) C6 N5 N4 120.08(11) C6 N5 H5 120.6(14) N4 N5 H5 116.7(14) C2 N3 H3A 118.4(12) C2 N3 H3B 120.9(12) H3A N3 H3B 120.7(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C2 N3 1.3178(17) C2 N4 1.3452(18) C2 S1 1.7032(13) C6 O7 1.2228(17) C6 N5 1.3464(17) C6 H6 0.974(18) N4 N5 1.3919(16) N4 H4 0.84(2) N5 H5 0.764(19) N3 H3A 0.869(19) N3 H3B 0.843(18)