A new monoclinic polymorph of 3-diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4H-1 lambda 6,2-thiazete-4-carbonitrile (Articolo in rivista)

Type
Label
  • A new monoclinic polymorph of 3-diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4H-1 lambda 6,2-thiazete-4-carbonitrile (Articolo in rivista) (literal)
Anno
  • 2010-01-01T00:00:00+01:00 (literal)
Alternative label
  • Orlando, Ahmed M.; Lo Presti, Leonardo; Soave, Raffaella (2010)
    A new monoclinic polymorph of 3-diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4H-1 lambda 6,2-thiazete-4-carbonitrile
    in Acta crystallographica. Section E
    (literal)
Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#autori
  • Orlando, Ahmed M.; Lo Presti, Leonardo; Soave, Raffaella (literal)
Pagina inizio
  • o2030 (literal)
Pagina fine
  • o2033 (literal)
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  • PM.P07.002.001 - Nanoingegneria chimica sperimentale e teorica: analisi di distribuzioni di densita' elettronica con metodi computazionali innovativi e tecniche di diffrazione di raggi X ad alta risoluzione. (literal)
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  • 66 (literal)
Rivista
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  • doi:10.1107/S1600536810027558 Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: NK2045 ). (literal)
Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#descrizioneSinteticaDelProdotto
  • ############################################################################## ### ### ### Electronic paper (Acta Crystallographica Section E) ### ### ### ############################################################################## # # # This CIF contains the data in a paper accepted for publication in Acta # # Crystallographica Section E. It conforms to the requirements of Notes # # for Authors for Section E, and has been peer reviewed under the auspices # # of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper \"The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography\" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4. # # # # Software is freely available for graphical display of the structure(s) in # # this CIF. For information consult the CIF home page http://www.iucr.org/ # # cif/home.html # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_global _audit_creation_method 'from SHELXL-97' _journal_date_recd_electronic 2010-06-16 _journal_date_accepted 2010-07-12 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2010 _journal_volume 66 _journal_issue 8 _journal_page_first o2032 _journal_page_last o2033 _journal_paper_category QO _journal_coeditor_code NK2045 _publ_contact_author_name 'Leonardo Lo Presti' _publ_contact_author_address ; Dipartimento di Chimica Fisica ed Elettrochimica Universit\'a degli Studi di Milano Via Golgi 19, 20133 Milano Italy ; _publ_contact_author_email 'leonardo.lopresti@unimi.it' _publ_contact_author_fax '02-50314300' _publ_contact_author_phone '02-50314252' _publ_section_title ;\ A new monoclinic polymorph of 3-diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4H-1\l^6^,2-thiazete-4-\ carbonitrile ; loop_ _publ_author_name _publ_author_address 'Orlando, Ahmed M.' ; Dipartimento di Chimica Fisica ed Elettrochimica Universit\'a degli Studi di Milano Via Golgi 19, 20133 Milano Italy ; 'Lo Presti, Leonardo' ; Dipartimento di Chimica Fisica ed Elettrochimica Universit\'a degli Studi di Milano Via Golgi 19, 20133 Milano Italy ; 'Soave, Raffaella' ; Consiglio Nazionale delle Ricerche Istituto di Scienze e Tecnologie Molecolari Via Golgi 19, 20133 Milano Italy ; _publ_section_synopsis . data_I _chemical_name_systematic ; 3-diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4H-1\l^6^,2-thiazete- 4-carbonitrile ; _chemical_name_common ? _chemical_formula_moiety 'C14 H17 N3 O3 S' _chemical_formula_sum 'C14 H17 N3 O3 S' _chemical_formula_iupac 'C14 H17 N3 O3 S' _chemical_formula_weight 307.37 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.3853(17) _cell_length_b 17.554(4) _cell_length_c 10.458(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.07(3) _cell_angle_gamma 90.00 _cell_volume 1533.4(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2885 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 21.58 _cell_measurement_temperature 293(2) _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2007)' _exptl_absorpt_correction_T_min 0.8549 _exptl_absorpt_correction_T_max 0.9473 _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16661 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.38 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > \s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 2814 _reflns_number_gt 1949 _reflns_threshold_expression I>2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_gt 0.0872 _refine_ls_wR_factor_ref 0.1015 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_number_reflns 2814 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.4078P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.162 _refine_diff_density_min -0.314 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' _computing_data_collection 'SMART (Bruker, 2005)' _computing_cell_refinement 'SAINT (Bruker, 2005)' _computing_data_reduction 'SAINT (Bruker, 2005)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2010)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' loop_ _atom_site_type_symbol _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 S S1 0.46791(6) 0.19850(4) 0.39836(6) 0.0569(2) Uani d . 1 . . O O1 0.1824(2) 0.00687(9) -0.10877(14) 0.0636(5) Uani d . 1 . . O O2 0.57694(19) 0.19314(11) 0.51054(16) 0.0758(5) Uani d . 1 . . O O3 0.53410(19) 0.20903(10) 0.27881(16) 0.0724(5) Uani d . 1 . . N N1 0.0608(2) 0.20205(10) 0.44220(16) 0.0472(4) Uani d . 1 . . N N2 0.3156(2) 0.25469(11) 0.41859(19) 0.0611(5) Uani d . 1 . . N N3 0.3384(3) 0.02616(14) 0.5764(2) 0.0739(6) Uani d . 1 . . C C1 0.2489(4) -0.06433(17) -0.1428(3) 0.0698(8) Uani d . 1 . . C C2 0.2106(2) 0.03021(12) 0.01541(19) 0.0458(5) Uani d . 1 . . C C3 0.2867(3) -0.01266(14) 0.1123(2) 0.0521(6) Uani d . 1 . . C C4 0.3129(3) 0.01743(13) 0.2346(2) 0.0491(5) Uani d . 1 . . C C5 0.1573(3) 0.10253(13) 0.0415(2) 0.0497(5) Uani d . 1 . . C C6 0.1842(3) 0.13239(13) 0.1623(2) 0.0474(5) Uani d . 1 . . C C7 0.2636(2) 0.09019(11) 0.26096(18) 0.0395(5) Uani d . 1 . . C C8 0.3043(2) 0.12520(12) 0.39177(19) 0.0425(5) Uani d . 1 . . C C9 0.2122(2) 0.19738(12) 0.42216(19) 0.0448(5) Uani d . 1 . . C C10 0.3242(2) 0.06955(14) 0.4954(2) 0.0496(5) Uani d . 1 . . C C11 -0.0148(3) 0.27758(15) 0.4525(3) 0.0599(7) Uani d . 1 . . C C12 -0.0724(4) 0.3089(2) 0.3236(3) 0.0769(8) Uani d . 1 . . C C13 -0.0377(3) 0.13436(15) 0.4614(2) 0.0553(6) Uani d . 1 . . C C14 -0.0494(4) 0.1173(2) 0.6015(3) 0.0780(9) Uani d . 1 . . H H1A 0.226(3) -0.0650(17) -0.234(3) 0.105(10) Uiso d . 1 . . H H1B 0.201(3) -0.1077(16) -0.096(3) 0.085(9) Uiso d . 1 . . H H1C 0.364(3) -0.0633(15) -0.122(2) 0.081(9) Uiso d . 1 . . H H3 0.317(3) -0.0621(14) 0.100(2) 0.066(7) Uiso d . 1 . . H H4 0.367(2) -0.0118(12) 0.299(2) 0.055(6) Uiso d . 1 . . H H5 0.100(2) 0.1321(12) -0.027(2) 0.055(6) Uiso d . 1 . . H H6 0.153(3) 0.1815(13) 0.176(2) 0.056(7) Uiso d . 1 . . H H11A -0.101(3) 0.2705(13) 0.502(2) 0.068(7) Uiso d . 1 . . H H11B 0.064(3) 0.3094(15) 0.495(2) 0.078(9) Uiso d . 1 . . H H12A -0.122(3) 0.3602(18) 0.334(3) 0.095(9) Uiso d . 1 . . H H12B -0.152(4) 0.2716(19) 0.279(3) 0.114(12) Uiso d . 1 . . H H12C 0.016(4) 0.3143(15) 0.271(3) 0.088(9) Uiso d . 1 . . H H13A -0.139(3) 0.1458(12) 0.4177(19) 0.053(6) Uiso d . 1 . . H H13B 0.008(2) 0.0906(13) 0.4177(19) 0.052(6) Uiso d . 1 . . H H14A -0.113(4) 0.073(2) 0.613(3) 0.126(12) Uiso d . 1 . . H H14B -0.094(3) 0.1583(18) 0.642(3) 0.095(10) Uiso d . 1 . . H H14C 0.062(4) 0.1065(18) 0.653(3) 0.116(12) Uiso d . 1 . . 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 0.0428(3) 0.0691(4) 0.0599(4) -0.0149(3) 0.0108(3) -0.0137(3) O1 0.0840(12) 0.0642(11) 0.0414(9) 0.0047(9) -0.0024(8) -0.0079(8) O2 0.0492(9) 0.1081(15) 0.0690(11) -0.0171(9) -0.0014(8) -0.0233(10) O3 0.0624(10) 0.0883(13) 0.0705(11) -0.0220(9) 0.0270(9) -0.0068(10) N1 0.0434(10) 0.0506(11) 0.0489(10) -0.0011(8) 0.0116(8) -0.0073(8) N2 0.0559(12) 0.0537(12) 0.0755(14) -0.0126(9) 0.0162(10) -0.0154(10) N3 0.0798(15) 0.0884(17) 0.0534(13) 0.0113(13) 0.0047(11) 0.0129(12) C1 0.092(2) 0.0672(19) 0.0505(17) -0.0020(17) 0.0059(15) -0.0149(14) C2 0.0466(12) 0.0514(13) 0.0392(12) -0.0049(10) 0.0033(9) -0.0013(10) C3 0.0619(14) 0.0448(14) 0.0492(13) 0.0077(11) 0.0032(10) -0.0051(11) C4 0.0510(13) 0.0524(14) 0.0428(13) 0.0089(11) -0.0011(10) 0.0024(11) C5 0.0563(13) 0.0506(14) 0.0417(12) 0.0046(11) 0.0010(10) 0.0066(11) C6 0.0517(13) 0.0415(13) 0.0495(14) 0.0046(10) 0.0072(10) 0.0021(11) C7 0.0355(10) 0.0430(12) 0.0405(11) -0.0034(9) 0.0066(8) -0.0013(9) C8 0.0371(11) 0.0492(13) 0.0415(12) -0.0022(9) 0.0054(9) -0.0042(10) C9 0.0437(11) 0.0491(13) 0.0422(12) -0.0050(10) 0.0064(9) -0.0074(10) C10 0.0447(12) 0.0619(15) 0.0421(13) 0.0007(11) 0.0040(10) -0.0062(12) C11 0.0602(16) 0.0581(16) 0.0635(17) 0.0092(13) 0.0169(13) -0.0099(13) C12 0.083(2) 0.073(2) 0.077(2) 0.0205(18) 0.0162(17) 0.0058(17) C13 0.0408(13) 0.0619(16) 0.0640(16) -0.0094(11) 0.0095(11) -0.0148(13) C14 0.085(2) 0.078(2) 0.077(2) -0.0188(19) 0.0353(18) -0.0019(17) _geom_special_details ; All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. ; 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 O3 . 1.4241(17) ? S1 O2 . 1.4252(18) ? S1 N2 . 1.642(2) yes S1 C8 . 1.878(2) yes O1 C2 . 1.362(2) ? O1 C1 . 1.426(3) ? N1 C9 . 1.307(3) yes N1 C13 . 1.471(3) ? N1 C11 . 1.478(3) ? N2 C9 . 1.331(3) yes N3 C10 . 1.138(3) ? C1 H1A . 0.96(3) ? C1 H1B . 1.01(3) ? C1 H1C . 0.97(3) ? C2 C3 . 1.373(3) ? C2 C5 . 1.381(3) ? C3 C4 . 1.384(3) ? C3 H3 . 0.92(2) ? C4 C7 . 1.377(3) ? C4 H4 . 0.94(2) ? C5 C6 . 1.369(3) ? C5 H5 . 0.98(2) ? C6 C7 . 1.391(3) ? C6 H6 . 0.92(2) ? C7 C8 . 1.511(3) ? C8 C10 . 1.457(3) ? C8 C9 . 1.532(3) ? C11 C12 . 1.496(4) ? C11 H11A . 0.94(2) ? C11 H11B . 0.95(3) ? C12 H12A . 1.00(3) ? C12 H12B . 1.02(3) ? C12 H12C . 0.97(3) ? C13 C14 . 1.508(4) ? C13 H13A . 0.95(2) ? C13 H13B . 0.99(2) ? C14 H14A . 0.95(4) ? C14 H14B . 0.93(3) ? C14 H14C . 1.06(3) ? 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 O3 S1 O2 . . 117.38(11) ? O3 S1 N2 . . 113.77(11) ? O2 S1 N2 . . 112.54(11) ? O3 S1 C8 . . 113.38(10) ? O2 S1 C8 . . 113.47(10) ? N2 S1 C8 . . 80.92(9) ? C2 O1 C1 . . 117.5(2) ? C9 N1 C13 . . 122.43(19) ? C9 N1 C11 . . 119.8(2) ? C13 N1 C11 . . 117.72(19) ? C9 N2 S1 . . 93.77(15) ? O1 C1 H1A . . 102.2(18) ? O1 C1 H1B . . 111.1(15) ? H1A C1 H1B . . 115(2) ? O1 C1 H1C . . 109.3(16) ? H1A C1 H1C . . 109(2) ? H1B C1 H1C . . 110(2) ? O1 C2 C3 . . 124.6(2) ? O1 C2 C5 . . 115.63(19) ? C3 C2 C5 . . 119.7(2) ? C2 C3 C4 . . 119.9(2) ? C2 C3 H3 . . 122.2(15) ? C4 C3 H3 . . 117.9(15) ? C7 C4 C3 . . 120.9(2) ? C7 C4 H4 . . 120.0(13) ? C3 C4 H4 . . 119.1(13) ? C6 C5 C2 . . 120.3(2) ? C6 C5 H5 . . 120.4(12) ? C2 C5 H5 . . 119.3(12) ? C5 C6 C7 . . 120.7(2) ? C5 C6 H6 . . 118.4(14) ? C7 C6 H6 . . 120.8(14) ? C4 C7 C6 . . 118.55(19) ? C4 C7 C8 . . 120.69(18) ? C6 C7 C8 . . 120.64(19) ? C10 C8 C7 . . 113.72(18) ? C10 C8 C9 . . 115.25(17) ? C7 C8 C9 . . 116.52(17) ? C10 C8 S1 . . 113.39(14) ? C7 C8 S1 . . 114.70(13) ? C9 C8 S1 . . 78.81(12) ? N1 C9 N2 . . 127.0(2) ? N1 C9 C8 . . 126.87(18) ? N2 C9 C8 . . 106.11(17) ? N3 C10 C8 . . 179.4(2) ? N1 C11 C12 . . 111.7(2) ? N1 C11 H11A . . 106.2(15) ? C12 C11 H11A . . 110.1(15) ? N1 C11 H11B . . 106.1(16) ? C12 C11 H11B . . 111.2(16) ? H11A C11 H11B . . 111(2) ? C11 C12 H12A . . 109.8(16) ? C11 C12 H12B . . 108.9(18) ? H12A C12 H12B . . 111(2) ? C11 C12 H12C . . 110.2(17) ? H12A C12 H12C . . 109(2) ? H12B C12 H12C . . 108(2) ? N1 C13 C14 . . 112.2(2) ? N1 C13 H13A . . 104.7(13) ? C14 C13 H13A . . 112.1(13) ? N1 C13 H13B . . 108.5(12) ? C14 C13 H13B . . 110.8(12) ? H13A C13 H13B . . 108.2(17) ? C13 C14 H14A . . 111(2) ? C13 C14 H14B . . 110.7(19) ? H14A C14 H14B . . 109(3) ? C13 C14 H14C . . 113.6(17) ? H14A C14 H14C . . 106(3) ? H14B C14 H14C . . 106(3) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O3 S1 N2 C9 . . . . 116.10(15) ? O2 S1 N2 C9 . . . . -107.28(15) ? C8 S1 N2 C9 . . . . 4.46(13) ? C1 O1 C2 C3 . . . . -5.7(3) ? C1 O1 C2 C5 . . . . 174.0(2) ? O1 C2 C3 C4 . . . . 178.3(2) ? C5 C2 C3 C4 . . . . -1.5(3) ? C2 C3 C4 C7 . . . . -0.1(3) ? O1 C2 C5 C6 . . . . -177.87(19) ? C3 C2 C5 C6 . . . . 1.9(3) ? C2 C5 C6 C7 . . . . -0.8(3) ? C3 C4 C7 C6 . . . . 1.2(3) ? C3 C4 C7 C8 . . . . -174.95(19) ? C5 C6 C7 C4 . . . . -0.7(3) ? C5 C6 C7 C8 . . . . 175.38(19) ? C4 C7 C8 C10 . . . . -28.1(3) ? C6 C7 C8 C10 . . . . 155.89(18) ? C4 C7 C8 C9 . . . . -165.80(18) ? C6 C7 C8 C9 . . . . 18.2(3) ? C4 C7 C8 S1 . . . . 104.7(2) ? C6 C7 C8 S1 . . . . -71.3(2) ? O3 S1 C8 C10 . . . . 131.15(16) ? O2 S1 C8 C10 . . . . -6.06(19) ? N2 S1 C8 C10 . . . . -116.78(16) ? O3 S1 C8 C7 . . . . -1.80(19) ? O2 S1 C8 C7 . . . . -139.02(15) ? N2 S1 C8 C7 . . . . 110.27(16) ? O3 S1 C8 C9 . . . . -116.00(13) ? O2 S1 C8 C9 . . . . 106.78(13) ? N2 S1 C8 C9 . . . . -3.94(12) ? C13 N1 C9 N2 . . . . -171.6(2) ? C11 N1 C9 N2 . . . . 5.4(3) ? C13 N1 C9 C8 . . . . 11.5(3) ? C11 N1 C9 C8 . . . . -171.5(2) ? S1 N2 C9 N1 . . . . 176.98(19) ? S1 N2 C9 C8 . . . . -5.62(17) ? C10 C8 C9 N1 . . . . -66.9(3) ? C7 C8 C9 N1 . . . . 70.2(3) ? S1 C8 C9 N1 . . . . -177.6(2) ? C10 C8 C9 N2 . . . . 115.7(2) ? C7 C8 C9 N2 . . . . -107.2(2) ? S1 C8 C9 N2 . . . . 5.00(15) ? C9 N1 C11 C12 . . . . 85.4(3) ? C13 N1 C11 C12 . . . . -97.4(3) ? C9 N1 C13 C14 . . . . 96.4(3) ? C11 N1 C13 C14 . . . . -80.6(3) ? (literal)
Note
  • ISI Web of Science (WOS) (literal)
Http://www.cnr.it/ontology/cnr/pubblicazioni.owl#affiliazioni
  • Dipartimento di Chimica Fisica ed Elettrochimica, Universitá degli Studi di Milano, Via Golgi 19, 20133 Milano, Italy(Orlando, A. M.; Lo Presti, L.) Consiglio Nazionale delle Ricerche, Istituto di Scienze e Tecnologie Molecolari, Via Golgi 19, 20133 Milano, Italy (Soave, R.) (literal)
Titolo
  • A new monoclinic polymorph of 3-diethylamino-4-(4-methoxyphenyl)-1,1-dioxo-4H-1 lambda 6,2-thiazete-4-carbonitrile (literal)
Abstract
  • A new monoclinic form of the title compound, C14H17N3O3S, has been found upon slow crystallization from water. Another monoclinic form of the compound was obtained previously from a mixture of dichloromethane and diethyl ether[Clerici, F.; Gelmi, M. L.; Soave, R.; Lo Presti, L. Tetrahedron 2002, 58, 5173-5178.]. Both phases crystallize in space group P21/n with one molecule in the asymmetric unit. The formally single exocyclic C-N bond that connects the -NEt2 unit with the thiazete ring is considerably shorter than the adjacent, formally double, endocyclic C=N bond. This is likely to be due to the extended conjugated system between the electron-donor diethylammine fragment and the electron-withdrawing sulfonyl group. In the newly discovered polymorph, the methoxy group is rotated by almost 180° around the phenyl-OCH3 bond, resulting in a different molecular conformation. (literal)
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