#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/72/2007223.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_2007223 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1998 _journal_volume 54 _journal_page_first 608 _journal_page_last 609 _publ_section_title ; Tetraphenylphosphonium Hexatungstate(VI) Acetonitrile Solvate ; _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 'Parvez, Masood' 'Boorman, P. Michael' 'Langdon, Naomi' _chemical_formula_sum 'C52 H40 D6 N2 O19 P2 W6' _[local]_cod_chemical_formula_sum_orig 'C52 H40 D6 N2 O19 P2 W6 ' _chemical_formula_structural '(W6 O19), (C24 H20 P)2, 2(C2 D3 N) ' _chemical_formula_analytical 'C52 H40 D6 N2 O19 P2 W6 ' _chemical_formula_iupac '(C24 H20 P)2 [W6 O19], 2C2 D3 N' _chemical_formula_weight 2174.04 _symmetry_cell_setting monoclinic loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' _cell_length_a 13.102(3) _cell_length_b 11.570(2) _cell_length_c 19.345(3) _cell_angle_alpha 90 _cell_angle_beta 101.126(12) _cell_angle_gamma 90 _cell_volume 2877.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 170 _exptl_crystal_density_diffrn 2.509 _diffrn_ambient_temperature 170 _refine_ls_R_factor_obs .035 _refine_ls_wR_factor_obs .022 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_occupancy W(1) .90621(5) .04862(6) .08598(3) .0415(2) Uani d ? . 1.000 W(2) .89583(5) .12303(6) -.07912(3) .04004(19) Uani d ? . 1.000 W(3) 1.11388(5) .15132(6) .03613(3) .0437(2) Uani d ? . 1.000 P(1) .9620(3) .2556(3) .34048(18) .0302(11) Uani d ? . 1.000 O(1) 1.0000 .0000 .0000 .028(4) Uani d ? S 1.000 O(2) .8415(6) .1376(8) .0051(4) .045(3) Uani d ? . 1.000 O(3) 1.0162(7) .1614(8) .0966(4) .051(3) Uani d ? . 1.000 O(4) 1.0054(7) .2218(8) -.0339(4) .045(3) Uani d ? . 1.000 O(5) 1.0064(6) -.0598(8) .1311(4) .049(3) Uani d ? . 1.000 O(6) .8390(7) .0860(9) .1493(4) .065(4) Uani d ? . 1.000 O(7) .8336(7) -.0813(8) .0406(4) .048(3) Uani d ? . 1.000 O(8) .8239(6) -.0242(9) -.0910(4) .045(3) Uani d ? . 1.000 O(9) .8156(7) .2123(9) -.1373(5) .059(4) Uani d ? . 1.000 O(10) 1.1995(8) .2618(9) .0643(6) .079(4) Uani d ? . 1.000 N(1) .2405(14) .0769(16) .5793(9) .119(8) Uani d ? . 1.000 C(1) .9856(10) .3011(12) .4304(6) .031(4) Uani d ? . 1.000 C(2) 1.0838(9) .2924(12) .4712(7) .039(5) Uani d ? . 1.000 C(3) 1.1042(10) .3255(11) .5423(7) .036(4) Uani d ? . 1.000 C(4) 1.0215(10) .3694(13) .5706(6) .038(4) Uani d ? . 1.000 C(5) .9245(10) .3777(12) .5294(6) .037(4) Uani d ? . 1.000 C(6) .9068(9) .3436(11) .4592(6) .032(4) Uani d ? . 1.000 C(7) .8248(9) .2482(12) .3080(6) .028(4) Uani d ? . 1.000 C(8) .7697(10) .3454(13) .2814(7) .048(5) Uani d ? . 1.000 C(9) .6647(12) .3422(15) .2625(8) .064(6) Uani d ? . 1.000 C(10) .6117(11) .2381(14) .2689(8) .050(5) Uani d ? . 1.000 C(11) .6659(13) .1453(16) .2949(8) .069(6) Uani d ? . 1.000 C(12) .7727(10) .1500(14) .3147(7) .050(5) Uani d ? . 1.000 C(13) 1.0189(9) .3571(11) .2866(6) .028(4) Uani d ? . 1.000 C(14) 1.0868(10) .4385(12) .3159(6) .037(4) Uani d ? . 1.000 C(15) 1.1322(10) .5168(12) .2770(8) .047(5) Uani d ? . 1.000 C(16) 1.0989(11) .5067(13) .2037(8) .050(5) Uani d ? . 1.000 C(17) 1.0282(11) .4251(13) .1715(7) .052(6) Uani d ? . 1.000 C(18) .9866(9) .3487(12) .2132(6) .035(4) Uani d ? . 1.000 C(19) 1.0212(9) .1162(11) .3398(6) .027(4) Uani d ? . 1.000 C(20) 1.0781(10) .0836(11) .2893(6) .035(4) Uani d ? . 1.000 C(21) 1.1234(11) -.0271(14) .2930(8) .059(6) Uani d ? . 1.000 C(22) 1.1136(12) -.1022(14) .3432(8) .060(6) Uani d ? . 1.000 C(23) 1.0601(12) -.0696(14) .3956(8) .062(6) Uani d ? . 1.000 C(24) 1.0127(11) .0362(14) .3930(7) .050(5) Uani d ? . 1.000 C(25) .2809(15) .0585(17) .5358(10) .080(8) Uani d ? . 1.000 C(26) .3308(15) .0402(18) .4787(10) .123(10) Uani d ? . 1.000 H(2) 1.1388 .2634 .4507 .047 Uiso c ? . 1.000 H(3) 1.1720 .3182 .5703 .043 Uiso c ? . 1.000 H(4) 1.0329 .3935 .6184 .045 Uiso c ? . 1.000 H(5) .8685 .4071 .5489 .045 Uiso c ? . 1.000 H(6) .8390 .3500 .4311 .039 Uiso c ? . 1.000 H(8) .8057 .4151 .2763 .058 Uiso c ? . 1.000 H(9) .6271 .4097 .2451 .077 Uiso c ? . 1.000 H(10) .5382 .2341 .2548 .060 Uiso c ? . 1.000 H(11) .6306 .0751 .3000 .082 Uiso c ? . 1.000 H(12) .8099 .0830 .3334 .060 Uiso c ? . 1.000 H(14) 1.1047 .4424 .3658 .044 Uiso c ? . 1.000 H(15) 1.1815 .5727 .2982 .056 Uiso c ? . 1.000 H(16) 1.1268 .5592 .1745 .060 Uiso c ? . 1.000 H(17) 1.0088 .4220 .1217 .063 Uiso c ? . 1.000 H(18) .9376 .2919 .1927 .041 Uiso c ? . 1.000 H(20) 1.0863 .1354 .2527 .042 Uiso c ? . 1.000 H(21) 1.1624 -.0487 .2585 .071 Uiso c ? . 1.000 H(22) 1.1422 -.1775 .3430 .072 Uiso c ? . 1.000 H(23) 1.0568 -.1208 .4335 .075 Uiso c ? . 1.000 H(24) .9734 .0558 .4277 .060 Uiso c ? . 1.000 D(1) .3608 -.0350 .4821 .147 Uiso c ? . 1.000 D(2) .2818 .0468 .4359 .147 Uiso c ? . 1.000 D(3) .3842 .0963 .4798 .147 Uiso c ? . 1.000 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 W(1) .0338(4) .0529(5) .0395(4) .0064(4) .0115(3) -.0093(4) W(2) .0310(4) .0432(4) .0438(4) .0074(3) .0017(3) .0018(3) W(3) .0277(4) .0362(4) .0639(4) -.0066(3) .0003(3) -.0153(4) P(1) .030(2) .030(2) .031(2) -.0021(18) .0078(17) -.0041(18) O(1) .019(7) .042(9) .024(7) .005(6) .006(6) -.010(6) O(2) .036(6) .043(7) .061(6) .008(5) .019(5) -.014(6) O(3) .041(6) .046(7) .066(7) -.004(6) .011(5) -.021(6) O(4) .032(6) .035(6) .066(7) -.005(5) .006(5) -.005(5) O(5) .039(6) .063(8) .046(6) .008(6) .015(5) -.001(6) O(6) .074(8) .077(9) .051(7) .001(7) .029(6) -.009(6) O(7) .042(6) .049(7) .060(7) -.010(5) .026(5) -.004(6) O(8) .027(5) .065(8) .040(6) -.001(5) -.001(5) -.007(6) O(9) .055(7) .057(8) .062(7) .024(6) .005(5) .008(6) O(10) .052(7) .058(8) .125(10) -.030(7) .014(7) -.048(8) N(1) .138(17) .118(17) .116(16) .046(13) .060(13) .027(13) C(1) .029(8) .042(9) .021(7) .008(7) .004(6) -.002(7) C(2) .020(8) .048(10) .050(10) -.005(7) .012(7) -.009(8) C(3) .031(8) .039(10) .036(8) -.003(7) .005(7) -.003(8) C(4) .037(8) .040(10) .036(8) -.003(8) .006(7) .004(8) C(5) .039(9) .043(10) .033(8) .004(8) .014(7) .002(8) C(6) .029(8) .029(8) .036(8) -.005(7) -.002(6) .003(7) C(7) .031(8) .029(9) .026(8) -.001(7) .011(6) .008(7) C(8) .033(9) .042(10) .067(10) .008(8) .005(8) .023(9) C(9) .042(10) .062(13) .083(13) .008(10) -.004(9) .021(11) C(10) .041(10) .054(12) .056(11) -.012(9) .009(8) -.018(9) C(11) .068(13) .049(12) .088(13) -.008(11) .012(11) .002(11) C(12) .029(9) .046(11) .075(11) .004(9) .012(8) -.001(10) C(13) .043(8) .022(8) .021(7) .008(7) .013(6) -.009(7) C(14) .033(8) .042(10) .033(8) .009(8) -.002(7) -.007(8) C(15) .043(9) .037(10) .061(11) -.015(8) .012(8) .000(9) C(16) .061(11) .039(10) .055(11) .003(9) .025(9) .016(9) C(17) .059(11) .053(12) .045(10) .013(9) .009(8) .019(9) C(18) .038(8) .043(10) .022(7) .007(8) .004(6) -.014(7) C(19) .031(8) .026(8) .025(7) -.005(7) .006(6) -.006(7) C(20) .042(9) .036(10) .028(8) .003(7) .005(7) .003(7) C(21) .051(10) .049(12) .074(13) .024(9) .004(9) -.028(10) C(22) .062(12) .047(12) .063(12) .026(10) -.008(9) .002(10) C(23) .073(13) .039(11) .068(12) .011(10) -.005(10) .032(10) C(24) .047(10) .057(12) .048(10) .004(9) .012(8) -.007(10) C(25) .097(17) .065(14) .080(16) .016(13) .022(12) .015(13) C(26) .16(2) .106(19) .127(19) -.031(17) .078(17) -.032(16) 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 W(1) O(1) . . 2.3198(6) y W(1) O(2) . . 1.928(9) y W(1) O(3) . . 1.925(9) y W(1) O(5) . . 1.901(9) y W(1) O(6) . . 1.697(8) y W(1) O(7) . . 1.901(9) y W(2) O(1) . . 2.3292(6) y W(2) O(2) . . 1.907(7) y W(2) O(4) . . 1.910(9) y W(2) O(5) . 3_755 1.919(7) y W(2) O(8) . . 1.939(9) y W(2) O(9) . . 1.727(9) y W(3) O(1) . . 2.3189(6) y W(3) O(3) . . 1.896(8) y W(3) O(4) . . 1.944(9) y W(3) O(7) . 3_755 1.930(8) y W(3) O(8) . 3_755 1.903(9) y W(3) O(10) . . 1.718(10) y P(1) C(1) . . 1.786(12) no P(1) C(7) . . 1.788(12) no P(1) C(13) . . 1.822(12) no P(1) C(19) . . 1.791(13) no N(1) C(25) . . 1.099(17) no C(1) C(2) . . 1.377(16) no C(1) C(6) . . 1.355(15) no C(2) C(3) . . 1.404(15) no C(3) C(4) . . 1.400(15) no C(4) C(5) . . 1.367(16) no C(5) C(6) . . 1.391(15) no C(7) C(8) . . 1.381(17) no C(7) C(12) . . 1.345(17) no C(8) C(9) . . 1.353(17) no C(9) C(10) . . 1.41(2) no C(10) C(11) . . 1.33(2) no C(11) C(12) . . 1.379(18) no C(13) C(14) . . 1.344(16) no C(13) C(18) . . 1.406(14) no C(14) C(15) . . 1.382(16) no C(15) C(16) . . 1.405(17) no C(16) C(17) . . 1.384(19) no C(17) C(18) . . 1.378(16) no C(19) C(20) . . 1.390(14) no C(19) C(24) . . 1.404(17) no C(20) C(21) . . 1.407(18) no C(21) C(22) . . 1.329(18) no C(22) C(23) . . 1.390(18) no C(23) C(24) . . 1.368(19) no C(25) C(26) . . 1.403(19) no _cod_database_code 2007223