#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006967.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_2006967 _journal_name_full 'Acta Crystallographica' _journal_year 1998 _journal_volume C54 _journal_page_first 60 _journal_page_last 63 _publ_section_title ; Byproducts from the Preparation of Acetone Tosylhydrazone: 4,5-Dihydro-3,5,5-trimethyl-1-[(4-methylphenyl)sulfonyl]-1H-pyrazole and 1,2-Bis(p-toluenesulfono)hydrazide ; loop_ _publ_author_name 'Charles R. Ojala' ' William H. Ojala' ' William B. Gleason' _chemical_formula_moiety 'C14 H16 N2 O4 S2 ' _chemical_formula_sum 'C14 H16 N2 O4 S2 ' _chemical_formula_weight 340.41 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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' _cell_length_a 15.7850(10) _cell_length_b 10.7397(9) _cell_length_c 9.492(2) _cell_angle_alpha 90 _cell_angle_beta 90.168(10) _cell_angle_gamma 90 _cell_volume 1609.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296 _exptl_crystal_density_diffrn 1.405 _diffrn_ambient_temperature 296.2 _refine_ls_R_factor_obs .082 _refine_ls_wR_factor_obs .121 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 S1A .79898(8) .91540(10) -.01280(10) .0549(4) Uij ? ? S1 .67920(7) .60720(10) -.00420(10) .0504(4) Uij ? ? O1A .8161(2) .8615(4) -.1473(3) .0660(10) Uij ? ? O1 .6774(2) .6444(4) -.1495(3) .0620(10) Uij ? ? O2A .7666(2) 1.0383(4) -.0012(4) .0750(10) Uij ? ? O2 .7079(2) .4855(4) .0343(4) .0660(10) Uij ? ? N1 .7496(2) .7003(4) .0739(4) .0490(10) Uij ? ? N1A .7274(2) .8275(4) .0644(4) .0510(10) Uij ? ? C1 .5797(3) .6374(5) .0678(4) .0450(10) Uij ? ? C1A .8926(3) .9038(5) .0880(5) .0490(10) Uij ? ? C2A .9566(4) .8293(6) .0460(6) .078(2) Uij ? ? C2 .5333(3) .7391(5) .0200(5) .057(2) Uij ? ? C3 .4539(3) .7626(6) .0758(6) .064(2) Uij ? ? C3A 1.0286(4) .8241(6) .1269(7) .087(2) Uij ? ? C4A 1.0378(3) .8883(6) .2476(6) .064(2) Uij ? ? C4 .4182(3) .6869(5) .1789(5) .055(2) Uij ? ? C5 .4658(3) .5866(5) .2234(5) .058(2) Uij ? ? C5A .9740(4) .9625(7) .2882(7) .097(3) Uij ? ? C6A .8999(4) .9710(6) .2090(7) .087(2) Uij ? ? C6 .5473(3) .5602(5) .1698(5) .052(2) Uij ? ? C7 .3298(3) .7136(6) .2351(6) .078(2) Uij ? ? C7A 1.1167(4) .8800(7) .3345(7) .093(2) Uij ? ? H1N .7535 .6781 .1706 .0592 Uij ? ? H1NA .7188 .8583 .1571 .0617 Uij ? ? H2A .9518 .7815 -.0379 .0934 Uij ? ? H2 .5560 .7922 -.0505 .0690 Uij ? ? H3 .4228 .8324 .0426 .0770 Uij ? ? H3A 1.0741 .7729 .0963 .1040 Uij ? ? H5A .9794 1.0099 .3722 .1168 Uij ? ? H5 .4428 .5329 .2930 .0695 Uij ? ? H6 .5789 .4909 .2033 .0623 Uij ? ? H6A .8548 1.0232 .2391 .1044 Uij ? ? H7AA 1.1179 .9467 .4003 .1116 Uij ? ? H7BA 1.1175 .8030 .3836 .1116 Uij ? ? H7CA 1.1647 .8852 .2748 .1116 Uij ? ? H7A .3114 .6454 .2909 .0942 Uij ? ? H7B .3311 .7869 .2910 .0942 Uij ? ? H7C .2918 .7251 .1584 .0942 Uij ? ? 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 S1A .0596(8) .0670(10) .0380(7) -.0079(7) -.0029(5) .0036(7) S1 .0445(6) .0685(9) .0382(7) -.0047(7) -.0034(5) -.0023(7) O1A .070(2) .101(3) .029(2) -.022(2) .004(2) -.003(2) O1 .056(2) .097(3) .032(2) -.012(2) -.001(2) -.004(2) O2A .083(3) .066(3) .077(3) .005(2) -.013(2) .007(2) O2 .059(2) .060(3) .078(3) .007(2) -.005(2) -.001(2) N1 .050(2) .064(3) .034(2) -.011(2) -.006(2) .000(2) N1A .046(2) .071(3) .038(2) -.005(2) .000(2) -.004(2) C1 .042(2) .056(3) .036(3) -.009(2) -.004(2) .003(2) C1A .049(3) .054(3) .045(3) -.012(3) -.007(2) .000(3) C2A .063(4) .093(5) .078(4) .003(3) .003(3) -.034(4) C2 .047(3) .072(4) .053(3) -.004(3) .001(2) .017(3) C3 .052(3) .075(4) .065(4) .003(3) -.011(3) .004(3) C3A .049(3) .120(6) .091(5) .017(4) -.007(3) -.027(4) C4A .046(3) .089(5) .058(3) -.020(3) -.001(3) .012(4) C4 .051(3) .060(4) .052(3) -.011(3) -.003(2) -.015(3) C5 .063(3) .064(4) .047(3) -.021(3) .012(2) -.002(3) C5A .089(5) .134(6) .069(4) .007(5) -.036(4) -.039(4) C6A .086(4) .102(5) .072(4) .024(4) -.014(4) -.037(4) C6 .055(3) .053(4) .048(3) -.008(2) -.003(2) .000(2) C7 .055(3) .097(5) .084(4) -.003(3) .011(3) -.016(4) C7A .064(4) .136(6) .080(4) -.022(4) -.015(3) .024(5) 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 S1A O1A ? ? 1.428(3) yes S1A O2A ? ? 1.420(4) yes S1A N1A ? ? 1.646(4) yes S1A C1A ? ? 1.762(4) yes S1 O1 ? ? 1.436(3) yes S1 O2 ? ? 1.430(4) yes S1 N1 ? ? 1.667(4) yes S1 C1 ? ? 1.744(4) yes N1 N1A ? ? 1.413(5) yes N1 H1N ? ? .953 ? N1A H1NA ? ? .955 ? C1 C2 ? ? 1.390(7) yes C1 C6 ? ? 1.375(6) yes C1A C2A ? ? 1.350(7) yes C1A C6A ? ? 1.361(7) yes C2A C3A ? ? 1.372(7) yes C2A H2A ? ? .950 ? C2 C3 ? ? 1.386(6) yes C2 H2 ? ? .951 ? C3 C4 ? ? 1.393(7) yes C3 H3 ? ? .950 ? C3A C4A ? ? 1.345(8) yes C3A H3A ? ? .950 ? C4A C5A ? ? 1.342(8) yes C4A C7A ? ? 1.493(7) yes C4 C5 ? ? 1.379(7) yes C4 C7 ? ? 1.522(7) yes C5 C6 ? ? 1.414(6) yes C5 H5 ? ? .950 no C5A C6A ? ? 1.391(8) yes C5A H5A ? ? .951 no C6A H6A ? ? .949 no C6 H6 ? ? .950 no C7 H7A ? ? .948 no C7 H7B ? ? .950 no C7 H7C ? ? .954 no C7A H7AA ? ? .950 no C7A H7BA ? ? .952 no C7A H7CA ? ? .946 no