#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/69/2006964.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_2006964 loop_ _publ_author_name 'Ojala, Charles R.' 'Ojala, William H.' 'Pennamon, Shanieka Y.' 'Gleason, William B.' _publ_section_title ; Conformational Polymorphs of Acetone Tosylhydrazone ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 57 _journal_page_last 60 _journal_paper_doi 10.1107/S0108270197011669 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety 'C10 H14 N2 O2 S ' _chemical_formula_sum 'C10 H14 N2 O2 S' _chemical_formula_weight 226.29 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 76.280(10) _cell_angle_beta 79.130(10) _cell_angle_gamma 61.790(10) _cell_formula_units_Z 2 _cell_length_a 8.1150(10) _cell_length_b 8.2710(10) _cell_length_c 10.035(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 173 _cell_measurement_theta_max 50.0 _cell_measurement_theta_min 40.0 _cell_volume 574.30(16) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1985)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 173 _diffrn_measurement_device CAD4 _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max -5 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2552 _diffrn_reflns_theta_max 70 _diffrn_standards_decay_% <1.0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.331 _exptl_absorpt_correction_T_max 0.689 _exptl_absorpt_correction_T_min 0.569 _exptl_absorpt_correction_type '\y scans (North, Phillips & Mathews, 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_meas ? _exptl_crystal_description prism _exptl_crystal_F_000 240.00 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.47 _refine_diff_density_min -0.40 _refine_ls_extinction_coef 0.1486E-04 _refine_ls_extinction_method Zachariasen_(1963)_type_2_Gaussian_isotropic _refine_ls_goodness_of_fit_obs 3.166 _refine_ls_matrix_type full _refine_ls_number_parameters 140 _refine_ls_number_reflns 2005 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs .040 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 4Fo^2^/\s^2^(Fo^2^)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs .062 _reflns_number_observed 2005 _reflns_number_total 2103 _reflns_observed_criterion '[ I>3\s(I) ]' _cod_data_source_file sx1030.cif _cod_data_source_block 1 _cod_depositor_comments ; The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 29 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z 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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 4Fo^2^/\s^2^(Fo^2^)' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 4Fo^2^/\s^2^(Fo^2^)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 574.3(3) _cod_original_sg_symbol_H-M 'P -1 ' _cod_original_formula_sum 'C10 H14 N2 O2 S ' _cod_database_code 2006964 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' 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 .0229(3) .0238(3) .0324(3) -.0088(2) .0029(2) -.0047(2) O1 .0279(7) .0392(7) .0426(8) -.0168(6) .0052(6) -.0066(6) O2 .0284(6) .0228(6) .0398(7) -.0063(5) .0018(5) -.0033(5) N1 .0293(7) .0224(7) .0356(8) -.0098(6) -.0070(6) -.0021(6) N2 .0281(7) .0220(7) .0317(8) -.0087(6) -.0003(6) -.0030(5) C1 .0276(8) .0254(8) .0399(10) -.0118(7) -.0071(7) -.0057(7) C2 .0390(10) .0324(9) .0430(10) -.0143(8) .0053(8) -.0130(8) C3 .0358(10) .0255(9) .0580(10) -.0074(8) -.0118(9) -.0049(8) C4 .0273(8) .0252(8) .0295(9) -.0104(6) .0050(7) -.0069(6) C5 .0370(10) .0470(10) .0314(10) -.0219(9) .0058(8) -.0043(8) C6 .0470(10) .0560(10) .0276(9) -.0250(10) .0045(8) -.0033(8) C7 .0358(10) .0343(9) .0323(9) -.0104(8) .0020(8) -.0115(7) C8 .0329(9) .0349(9) .0380(10) -.0167(8) .0019(8) -.0054(7) C9 .0362(10) .0369(9) .0308(9) -.0200(8) .0027(7) -.0028(7) C10 .0450(10) .0530(10) .0390(10) -.0169(10) -.0047(9) -.0118(9) 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_calc_attached_atom S1 .61682(5) .64163(5) .30586(4) .02790(10) Uani ? ? O1 .7564(2) .6966(2) .2336(2) .0371(4) Uani ? ? O2 .6755(2) .4563(2) .38530(10) .0336(3) Uani ? ? N1 .4004(2) .9657(2) .3597(2) .0298(4) Uani ? ? N2 .4939(2) .7770(2) .4208(2) .0290(4) Uani ? ? C1 .2649(2) 1.0716(2) .4346(2) .0304(4) Uani ? ? C2 .1979(3) 1.0126(3) .5778(2) .0392(5) Uani ? ? C3 .1661(3) 1.2720(3) .3711(2) .0416(5) Uani ? ? C4 .4607(2) .6803(2) .1890(2) .0286(4) Uani ? ? C5 .4841(3) .7556(3) .0518(2) .0389(5) Uani ? ? C6 .3573(3) .7846(3) -.0362(2) .0447(6) Uani ? ? C7 .2067(3) .7424(3) .0097(2) .0360(5) Uani ? ? C8 .1863(3) .6690(3) .1488(2) .0355(5) Uani ? ? C9 .3119(3) .6376(3) .2375(2) .0346(5) Uani ? ? C10 .0683(3) .7734(3) -.0851(2) .0467(6) Uani ? ? H2N .422(3) .733(3) .471(2) .0325 Uani ? ? H2A .2939 .9709 .6371 .0470 Uani ? ? H2B .0894 1.1151 .6082 .0470 Uani ? ? H2C .1678 .9142 .5795 .0470 Uani ? ? H3A .1748 1.3470 .4253 .0500 Uani ? ? H3B .0377 1.3053 .3668 .0500 Uani ? ? H3C .2228 1.2910 .2807 .0500 Uani ? ? H5 .5852 .7865 .0191 .0466 Uani ? ? H6 .3730 .8347 -.1305 .0537 Uani ? ? H8 .0839 .6404 .1824 .0426 Uani ? ? H9 .2969 .5869 .3318 .0415 Uani ? ? H10A .1334 .7139 -.1623 .0560 Uani ? ? H10B -.0144 .7228 -.0374 .0560 Uani ? ? H10C -.0021 .9032 -.1155 .0560 Uani ? ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.018 0.009 'International Tables' H 0.000 0.000 'International Tables' N 0.031 0.018 'International Tables' S 0.333 0.557 'International Tables' O 0.049 0.032 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -2 1 -2 -4 -1 -1 -3 -1 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 O1 S1 O2 119.01(8) yes O1 S1 N2 108.82(8) yes O1 S1 C4 108.60(8) yes O2 S1 N2 103.42(8) yes O2 S1 C4 109.53(8) yes N2 S1 C4 106.75(8) yes N2 N1 C1 115.8(2) yes S1 N2 N1 112.10(10) yes S1 N2 H2N 107.0(10) no N1 N2 H2N 114.0(10) no N1 C1 C2 125.9(2) yes N1 C1 C3 116.2(2) yes C2 C1 C3 117.9(2) yes C1 C2 H2A 109.5 no C1 C2 H2B 109.5 no C1 C2 H2C 109.5 no H2A C2 H2B 109.5 no H2A C2 H2C 109.5 no H2B C2 H2C 109.5 no C1 C3 H3A 109.5 no C1 C3 H3B 109.5 no C1 C3 H3C 109.5 no H3A C3 H3B 109.5 no H3A C3 H3C 109.5 no H3B C3 H3C 109.5 no S1 C4 C5 120.60(10) yes S1 C4 C9 118.50(10) yes C5 C4 C9 120.9(2) yes C4 C5 C6 118.5(2) yes C4 C5 H5 120.7 no C6 C5 H5 120.7 no C5 C6 C7 121.8(2) yes C5 C6 H6 119.1 no C7 C6 H6 119.1 no C6 C7 C8 118.1(2) yes C6 C7 C10 122.1(2) yes C8 C7 C10 119.8(2) yes C7 C8 C9 121.0(2) yes C7 C8 H8 119.5 no C9 C8 H8 119.5 no C4 C9 C8 119.7(2) yes C4 C9 H9 120.2 no C8 C9 H9 120.2 no C7 C10 H10A 109.5 no C7 C10 H10B 109.5 no C7 C10 H10C 109.5 no H10A C10 H10B 109.5 no H10A C10 H10C 109.5 no H10B C10 H10C 109.5 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 O1 ? ? 1.4280(10) yes S1 O2 ? ? 1.4440(10) yes S1 N2 ? ? 1.644(2) yes S1 C4 ? ? 1.755(2) yes N1 N2 ? ? 1.411(2) yes N1 C1 ? ? 1.277(2) yes N2 H2N ? ? .85(2) no C1 C2 ? ? 1.490(3) yes C1 C3 ? ? 1.494(2) yes C2 H2A ? ? .950 no C2 H2B ? ? .950 no C2 H2C ? ? .950 no C3 H3A ? ? .950 no C3 H3B ? ? .950 no C3 H3C ? ? .950 no C4 C5 ? ? 1.388(3) yes C4 C9 ? ? 1.385(2) yes C5 C6 ? ? 1.380(3) yes C5 H5 ? ? .950 no C6 C7 ? ? 1.393(3) yes C6 H6 ? ? .950 no C7 C8 ? ? 1.396(3) yes C7 C10 ? ? 1.499(3) yes C8 C9 ? ? 1.372(3) yes C8 H8 ? ? .950 no C9 H9 ? ? .950 no C10 H10A ? ? .950 no C10 H10B ? ? .950 no C10 H10C ? ? .950 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag S1 N2 N1 C1 161.90(10) yes O1 S1 N2 N1 61.20(10) yes O1 S1 C4 C5 -0.9(2) yes O1 S1 C4 C9 -179.50(10) yes O2 S1 N2 N1 -171.30(10) yes O2 S1 C4 C5 -132.3(2) yes O2 S1 C4 C9 49.0(2) yes N1 N2 S1 C4 -55.80(10) yes N2 S1 C4 C5 116.3(2) yes N2 S1 C4 C9 -62.3(2) yes N2 N1 C1 C2 -0.7(3) yes N2 N1 C1 C3 179.50(10) yes