#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006199.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_2006199 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 773 _journal_page_last 775 _publ_section_title ; A Tricyclic Phosphorus(V)-Hydrazine System with Twist Conformation of the Central Heterocycle ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _publ_author_name 'Engelhardt, Udo' 'Rosefid, Mehdi' _chemical_formula_sum 'C15 H21 N4 O2 P S' _chemical_formula_weight 352.14 _chemical_melting_point '112\%C' _symmetry_cell_setting monoclinic 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 8.002(5) _cell_length_b 12.286(2) _cell_length_c 17.380(4) _cell_angle_alpha 90.0 _cell_angle_beta 91.10(2) _cell_angle_gamma 90.0 _cell_volume 1708.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293 _exptl_crystal_density_diffrn 1.371 _diffrn_ambient_temperature '293 K' _refine_ls_R_factor_obs .048 _refine_ls_wR_factor_obs .029 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 _atom_site_refinement_flags _atom_site_disorder_group _atom_site_type_symbol S .12237(9) .59818(5) .24318(4) .0595(5) Ueq ? ? ? ? ? P2 .31535(9) .64953(5) .19106(4) .0451(4) Ueq ? ? ? ? ? O1 .4067(2) .56070(10) .14000(10) .0580(10) Ueq ? ? ? ? ? O2 .6413(2) .91770(10) .14430(10) .0730(10) Ueq ? ? ? ? ? N1 .2815(3) .7554(2) .13470(10) .0440(10) Ueq ? ? ? ? ? N3 .4800(3) .69130(10) .24330(10) .0470(10) Ueq ? ? ? ? ? N8 .5317(3) .8005(2) .23200(10) .056(2) Ueq ? ? ? ? ? N10 .4346(3) .7983(2) .10670(10) .0500(10) Ueq ? ? ? ? ? C1 .3258(3) .4863(2) .0905(2) .051(2) Ueq ? ? ? ? ? C2 .3157(4) .3804(2) .1129(2) .064(2) Ueq ? ? ? ? ? C3 .2502(5) .3046(3) .0609(3) .085(3) Ueq ? ? ? ? ? C8 .1995(5) .3355(4) -.0104(3) .096(3) Ueq ? ? ? ? ? C10 .2066(6) .4434(4) -.0305(2) .112(3) Ueq ? ? ? ? ? C15 .2730(5) .5185(3) .0200(2) .089(3) Ueq ? ? ? ? ? C4 .6198(4) .6200(2) .2653(2) .059(2) Ueq ? ? ? ? ? C5 .7062(5) .6634(3) .3368(2) .067(2) Ueq ? ? ? ? ? C6 .7622(4) .7794(3) .3248(2) .060(2) Ueq ? ? ? ? ? C7 .6164(4) .8483(2) .2986(2) .059(2) Ueq ? ? ? ? ? C9 .5451(3) .8446(2) .1600(2) .058(2) Ueq ? ? ? ? ? C11 .4075(4) .8547(3) .0328(2) .062(2) Ueq ? ? ? ? ? C12 .2788(5) .9448(2) .0403(2) .066(3) Ueq ? ? ? ? ? C13 .1178(4) .9000(3) .0728(2) .065(2) Ueq ? ? ? ? ? C14 .1533(4) .8397(2) .1477(2) .053(2) Ueq ? ? ? ? ? H2 .347(4) .362(2) .1600(10) .080(10) Uiso ? ? ? ? ? H3 .249(4) .240(2) .072(2) .090(10) Uiso ? ? ? ? ? H8 .156(4) .283(3) -.047(2) .130(10) Uiso ? ? ? ? ? H10 .167(4) .465(3) -.088(2) .15(2) Uiso ? ? ? ? ? H15 .266(4) .593(3) .009(2) .130(10) Uiso ? ? ? ? ? H41 .572(3) .545(2) .2730(10) .077(9) Uiso ? ? ? ? ? H42 .694(3) .617(2) .2190(10) .070(9) Uiso ? ? ? ? ? H51 .623(3) .664(2) .3790(10) .068(9) Uiso ? ? ? ? ? H52 .791(3) .616(2) .3480(10) .071(9) Uiso ? ? ? ? ? H61 .810(3) .807(2) .3750(10) .058(8) Uiso ? ? ? ? ? H62 .847(3) .778(2) .2860(10) .080(10) Uiso ? ? ? ? ? H71 .534(3) .854(2) .3420(10) .090(10) Uiso ? ? ? ? ? H72 .648(3) .918(2) .2810(10) .080(10) Uiso ? ? ? ? ? H111 .364(3) .796(2) -.0030(10) .052(7) Uiso ? ? ? ? ? H112 .524(3) .881(2) .0210(10) .063(8) Uiso ? ? ? ? ? H121 .251(3) .982(2) -.0110(10) .058(7) Uiso ? ? ? ? ? H122 .333(3) .998(2) .0760(10) .061(8) Uiso ? ? ? ? ? H131 .069(3) .845(2) .0320(10) .080(10) Uiso ? ? ? ? ? H132 .034(3) .956(2) .0810(10) .090(10) Uiso ? ? ? ? ? H141 .058(3) .805(2) .1630(10) .055(8) Uiso ? ? ? ? ? H142 .195(3) .890(2) .1900(10) .051(7) Uiso ? ? ? ? ? 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 _atom_site_aniso_type_symbol S .0595(5) .0467(4) .0723(5) -.0100(4) .0100(4) .0091(4) U P2 .0497(4) .0325(3) .0531(4) -.0044(3) .0015(3) -.0005(3) U O1 .0530(10) .0460(10) .0750(10) -.0072(9) .0040(10) -.0168(9) U O2 .0700(10) .0570(10) .0910(10) -.0300(10) .0010(10) .0060(10) U N1 .0480(10) .0390(10) .0460(10) -.0070(10) .0000(10) .0039(9) U N3 .0510(10) .0320(10) .0590(10) -.0030(10) -.0080(10) .0020(10) U N8 .068(2) .0340(10) .0660(10) -.0120(10) -.0250(10) .0050(10) U N10 .0550(10) .0460(10) .0500(10) -.0120(10) .0050(10) .0050(10) U C1 .051(2) .042(2) .059(2) -.0050(10) .0030(10) -.0100(10) U C2 .074(2) .046(2) .073(2) .001(2) .004(2) -.004(2) U C3 .096(3) .044(2) .115(3) -.018(2) .028(3) -.024(2) U C8 .100(3) .104(3) .084(3) -.035(3) .011(2) -.046(3) U C10 .166(4) .102(3) .069(3) -.023(3) -.021(3) -.011(2) U C15 .141(4) .059(2) .068(2) -.009(2) -.015(2) .000(2) U C4 .070(2) .041(2) .067(2) .008(2) -.012(2) .0000(10) U C5 .077(3) .055(2) .069(2) .017(2) -.023(2) .000(2) U C6 .055(2) .065(2) .060(2) .005(2) -.013(2) -.010(2) U C7 .065(2) .042(2) .069(2) -.002(2) -.019(2) -.005(2) U C9 .051(2) .0390(10) .065(2) -.0030(10) -.0010(10) .0000(10) U C11 .079(2) .061(2) .046(2) -.018(2) .005(2) .004(2) U C12 .097(3) .048(2) .054(2) -.010(2) -.012(2) .014(2) U C13 .071(2) .058(2) .068(2) .005(2) -.008(2) .014(2) U C14 .056(2) .049(2) .055(2) -.005(2) .002(2) .005(2) U loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S P2 1.9130(10) yes P2 O1 1.594(2) yes P2 N1 1.647(2) yes P2 N3 1.663(2) yes N1 N10 1.429(3) yes N1 C14 1.479(4) no N3 N8 1.420(3) yes N3 C4 1.468(4) no O1 C1 1.404(3) no O2 C9 1.218(3) yes N8 C7 1.453(4) no N8 C9 1.370(3) yes N10 C11 1.471(4) no N10 C9 1.390(3) yes C1 C2 1.361(4) no C1 C15 1.348(4) no C2 C3 1.392(5) no C3 C8 1.351(6) no C8 C10 1.373(6) no C10 C15 1.372(6) no C C(phenyl)mean 1.370(10) no C4 C5 1.507(5) no C5 C6 1.510(5) no C6 C7 1.504(5) no C11 C12 1.520(5) no C12 C13 1.520(5) no C13 C14 1.519(4) no C C(hexahydropyridazine)mean 1.513(7) no C2 H2 .88(3) no C3 H3 .82(3) no C8 H8 .97(3) no C10 H10 1.08(3) no C15 H15 .94(3) no C4 H41 1.00(2) no C4 H42 1.01(2) no C5 H51 1.00(2) no C5 H52 .91(3) no C6 H61 1.01(2) no C6 H62 .96(3) no C7 H71 1.02(3) no C7 H72 .95(3) no C11 H111 1.01(2) no C11 H112 1.01(2) no C12 H121 1.03(2) no C12 H122 .99(2) no C13 H131 1.06(2) no C13 H132 .98(3) no C14 H141 .91(2) no C14 H142 1.01(2) no _cod_database_code 2006199