#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/21/2012146.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_2012146 _journal_name_full 'Acta Crystallographica, Section C' _journal_year 2001 _journal_volume 57 _journal_page_first 929 _journal_page_last 931 _publ_section_title ; Investigations on benzo[1,2]oxaphosphinane derivatives ; loop_ _publ_author_name ' Ma\/lecka, Magdalena' ' Budzisz, El\.zbieta ' _chemical_formula_moiety 'C13 H16 N O5 P' _chemical_formula_sum 'C13 H16 N O5 P' _chemical_formula_weight 297.24 _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.3250(10) _cell_length_b 9.6620(10) _cell_length_c 15.619(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1407.40(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.403 _diffrn_ambient_temperature 293(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_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol O1 1.0085(4) .6457(3) .47913(18) .0567(8) Uani d . 1 . . O P2 .99166(15) .52449(13) .41005(7) .0513(3) Uani d . 1 . . P O21 .9628(5) .3971(4) .4561(2) .0714(11) Uani d . 1 . . O O22 1.1366(4) .5232(5) .3601(2) .0696(11) Uani d . 1 . . O C23 1.2650(7) .4675(9) .4012(5) .101(2) Uani d . 1 . . C H231 1.3069 .5371 .4372 .111 Uiso calc R 1 . . H H232 1.3329 .4404 .3581 .111 Uiso calc R 1 . . H H233 1.2396 .3885 .4352 .111 Uiso calc R 1 . . H C3 .8643(5) .5872(5) .3370(3) .0480(10) Uani d . 1 . . C C4 .8479(5) .7341(5) .3302(3) .0493(11) Uani d . 1 . . C O4 .7573(4) .7897(4) .2813(2) .0639(10) Uani d . 1 . . O C5 .9452(5) .9682(6) .3623(3) .0533(12) Uani d . 1 . . C H5 .890(6) .993(6) .324(3) .059 Uiso d . 1 . . H C6 1.0258(6) 1.0587(6) .4111(4) .0665(14) Uani d . 1 . . C H6 1.025(6) 1.154(6) .402(4) .066(16) Uiso d . 1 . . H C7 1.0992(6) 1.0096(6) .4823(4) .0682(16) Uani d . 1 . . C H7 1.154(6) 1.067(5) .509(3) .055(14) Uiso d . 1 . . H C8 1.0935(6) .8733(6) .5026(4) .0619(13) Uani d . 1 . . C H8 1.155(7) .814(7) .555(4) .09(2) Uiso d . 1 . . H C9 1.0141(5) .7822(5) .4541(3) .0522(11) Uani d . 1 . . C C10 .9371(5) .8295(5) .3819(3) .0454(10) Uani d . 1 . . C C31 .7798(5) .4932(5) .2876(3) .0508(11) Uani d . 1 . . C C311 .8019(6) .3403(6) .2894(4) .0624(13) Uani d . 1 . . C H311 .8980 .3204 .3077 .057(15) Uiso calc R 1 . . H H312 .7869 .3032 .2331 .12(3) Uiso calc R 1 . . H H313 .7351 .2991 .3285 .11(2) Uiso calc R 1 . . H N32 .6769(4) .5415(5) .2383(3) .0568(11) Uani d . 1 . . N H32 .679(6) .642(7) .235(4) .068(17) Uiso d . 1 . . H C33 .5784(6) .4641(7) .1846(4) .0642(14) Uani d . 1 . . C H331 .541(7) .374(7) .214(4) .10(2) Uiso d . 1 . . H H332 .640(5) .445(5) .139(3) .043(12) Uiso d . 1 . . H C34 .4537(6) .5512(6) .1608(4) .0617(14) Uani d . 1 . . C H341 .384(5) .495(5) .118(3) .047(12) Uiso d . 1 . . H H342 .394(6) .571(5) .207(3) .052 Uiso d . 1 . . H O35 .4923(5) .6801(4) .1261(3) .0689(10) Uani d . 1 . . O H35 .541(7) .665(7) .095(4) .07(2) 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 O1 .067(2) .0493(19) .0534(14) .0048(19) -.0097(18) -.0007(13) P2 .0526(7) .0488(6) .0523(5) .0043(6) -.0049(6) -.0009(5) O21 .087(3) .054(2) .073(2) .0046(19) -.021(2) -.0007(17) O22 .057(2) .093(3) .0588(18) .014(2) -.0113(16) -.0076(19) C23 .059(4) .153(7) .090(4) .031(4) -.018(4) -.013(5) C3 .041(2) .053(3) .050(2) -.0034(19) .005(2) -.004(2) C4 .038(2) .064(3) .046(2) .000(2) .0026(19) -.001(2) O4 .064(2) .057(2) .070(2) .0018(18) -.0280(19) .0023(18) C5 .038(2) .060(3) .062(2) .002(2) -.007(2) -.002(2) C6 .058(3) .054(4) .087(3) -.005(2) -.004(3) -.004(3) C7 .059(3) .060(4) .086(3) -.003(3) -.022(3) -.020(3) C8 .055(3) .062(4) .069(3) -.003(2) -.016(3) -.010(3) C9 .040(2) .057(3) .059(2) .007(2) .000(2) -.010(2) C10 .035(2) .047(3) .054(2) .0024(18) -.0015(18) -.0028(19) C31 .039(2) .065(3) .049(2) -.003(2) .0044(18) .002(2) C311 .063(3) .057(4) .067(3) -.002(3) -.003(3) -.002(3) N32 .050(2) .061(3) .059(2) -.002(2) -.0097(18) -.0032(19) C33 .049(3) .078(4) .066(3) -.005(3) -.010(2) -.010(3) C34 .049(3) .075(4) .061(3) -.003(2) -.002(2) -.006(3) O35 .071(3) .068(3) .067(2) .001(2) -.005(2) -.0045(18) 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 O1 C9 . 1.377(6) yes O1 P2 . 1.600(3) yes P2 O21 . 1.451(4) yes P2 O22 . 1.561(4) yes P2 C3 . 1.754(5) yes O22 C23 . 1.461(6) yes C23 H231 . .9600 no C23 H232 . .9600 no C23 H233 . .9600 no C3 C31 . 1.428(6) yes C3 C4 . 1.432(7) yes C4 O4 . 1.259(6) yes C4 C10 . 1.482(6) yes C5 C10 . 1.377(7) no C5 C6 . 1.382(8) no C5 H5 . .82(6) no C6 C7 . 1.389(8) no C6 H6 . .93(6) no C7 C8 . 1.356(9) no C7 H7 . .87(6) no C8 C9 . 1.377(7) no C8 H8 . 1.16(7) no C9 C10 . 1.413(6) yes C31 N32 . 1.316(6) yes C31 C311 . 1.492(8) yes C311 H311 . .9600 no C311 H312 . .9600 no C311 H313 . .9600 no N32 C33 . 1.451(6) yes N32 H32 . .97(6) no C33 C34 . 1.483(8) yes C33 H331 . 1.05(7) no C33 H332 . .94(5) no C34 O35 . 1.405(7) yes C34 H341 . 1.09(5) no C34 H342 . .93(5) no O35 H35 . .68(6) no _cod_database_code 2012146