#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007269.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_2007269 _journal_name_full 'Acta Crystallographica' _journal_year 1998 _journal_volume C54 _publ_section_title ; Bis(tetra-n-butylammonium) Nonadecaoxohexamolybdenum(VI): a Redetermination at 148 K ; loop_ _publ_author_name 'Boyle, Paul D.' 'Stauffer, Thad C.' 'Wirgau, Joseph I.' 'Cornman, Charles R.' _chemical_formula_moiety '2(C16 H36 N). (Mo6 O19)' _chemical_formula_sum 'C32 H72 Mo6 N2 O19 ' _chemical_formula_weight 1364.55 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 1/2+x,1/2+y,z 1/2-x,1/2-y,-z -x,y,1/2-z x,-y,1/2+z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 15.9935(7) _cell_length_b 17.3378(6) _cell_length_c 17.5073(7) _cell_angle_alpha 90.0 _cell_angle_beta 101.542(5) _cell_angle_gamma 90.0 _cell_volume 4756.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 148 _exptl_crystal_density_diffrn 1.906 _diffrn_ambient_temperature 148 _refine_ls_R_factor_obs .035 _refine_ls_wR_factor_obs .042 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_refinement_flags _atom_site_type_symbol Mo1 .562919(19) .291128(18) .141361(19) .02354(16) Uij ? . Mo Mo2 .50000 .15640(2) .25000 .0187(2) Uij ? S Mo Mo3 .634029(18) .290873(18) .33055(2) .02445(15) Uij ? . Mo Mo4 .50000 .42544(3) .25000 .0325(3) Uij ? S Mo O1 .50000 .29098(19) .25000 .0197(16) Uij ? S O O2 .61207(17) .29290(16) .06473(17) .0320(14) Uij ? . O O3 .55384(15) .18238(14) .16405(15) .0227(12) Uij ? . O O4 .66001(15) .29146(14) .23013(16) .0257(13) Uij ? . O O5 .55320(16) .40001(15) .16363(18) .0315(15) Uij ? . O O6 .50000 .05850(19) .25000 .0228(17) Uij ? S O O7 .39312(14) .18201(14) .18236(14) .0209(11) Uij ? . O O8 .73003(16) .28860(16) .39084(17) .0325(14) Uij ? . O O9 .60803(16) .39941(14) .31769(19) .0334(15) Uij ? . O O10 .50000 .5226(2) .25000 .043(3) Uij ? S O O11 .44508(16) .29158(15) .09686(16) .0277(13) Uij ? . O N1 .25249(18) .48387(17) .94375(18) .0239(14) Uij ? . N C1 .2451(2) .5610(2) .9835(2) .0281(17) Uij ? . C C2 .2764(2) .5632(2) 1.0716(2) .0318(19) Uij ? . C C3 .2620(3) .6430(2) 1.1025(3) .040(2) Uij ? . C C4 .2878(3) .6458(3) 1.1908(3) .045(2) Uij ? . C C5 .3472(2) .4662(2) .9494(2) .0271(17) Uij ? . C C6 .3667(2) .3932(2) .9091(3) .0333(19) Uij ? . C C7 .4634(3) .3861(3) .9154(2) .038(2) Uij ? . C C8 .4873(3) .3179(3) .8715(3) .042(2) Uij ? . C C9 .2062(2) .4897(2) .8584(2) .0296(17) Uij ? . C C10 .2468(2) .5423(3) .8066(2) .0317(18) Uij ? . C C11 .1806(2) .5639(3) .7340(2) .0343(19) Uij ? . C C12 .1186(3) .6249(3) .7508(3) .050(3) Uij ? . C C13 .2122(2) .4190(2) .9827(2) .0229(16) Uij ? . C C14 .1200(2) .4324(2) .9887(2) .0257(16) Uij ? . C C15 .0832(2) .3629(2) 1.0245(2) .0259(16) Uij ? . C C16 -.0094(2) .3780(2) 1.0318(3) .034(2) Uij ? . C H1a .186 .576 .973 .0368 Uiso ? . H H1b .277 .598 .961 .0368 Uiso ? . H H2a .246 .526 1.095 .0400 Uiso ? . H H2b .336 .552 1.084 .0400 Uiso ? . H H3a .203 .656 1.088 .0473 Uiso ? . H H3b .295 .680 1.081 .0473 Uiso ? . H H4a .278 .697 1.209 .0530 Uiso ? . H H4b .255 .609 1.213 .0530 Uiso ? . H H4c .347 .633 1.206 .0530 Uiso ? . H H5a .373 .462 1.004 .0358 Uiso ? . H H5b .372 .509 .927 .0358 Uiso ? . H H6a .346 .349 .934 .0418 Uiso ? . H H6b .339 .395 .855 .0418 Uiso ? . H H7a .490 .381 .969 .0480 Uiso ? . H H7b .484 .432 .895 .0480 Uiso ? . H H8a .548 .316 .877 .0507 Uiso ? . H H8b .468 .271 .892 .0507 Uiso ? . H H8c .462 .323 .817 .0507 Uiso ? . H H9a .149 .508 .858 .0378 Uiso ? . H H9b .203 .439 .836 .0378 Uiso ? . H H10a .267 .588 .835 .0400 Uiso ? . H H10b .294 .516 .791 .0400 Uiso ? . H H11a .149 .518 .715 .0433 Uiso ? . H H11b .210 .583 .695 .0433 Uiso ? . H H12a .078 .637 .704 .0585 Uiso ? . H H12b .089 .606 .789 .0585 Uiso ? . H H12c .150 .671 .770 .0585 Uiso ? . H H13a .245 .412 1.034 .0321 Uiso ? . H H13b .215 .373 .953 .0321 Uiso ? . H H14a .117 .477 1.021 .0346 Uiso ? . H H14b .087 .441 .937 .0346 Uiso ? . H H15a .085 .318 .992 .0347 Uiso ? . H H15b .117 .353 1.075 .0347 Uiso ? . H H16a -.031 .334 1.055 .0431 Uiso ? . H H16b -.012 .422 1.064 .0431 Uiso ? . H H16c -.044 .387 .981 .0431 Uiso ? . 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 _atom_site_aniso_type_symbol Mo1 .01801(15) .01962(16) .03502(18) -.00050(12) .01021(12) .00257(13) Mo Mo2 .01594(19) .01038(18) .0281(2) .00000 .00027(16) .00000 Mo Mo3 .01395(14) .02167(16) .03732(19) -.00398(12) .00416(12) -.00954(13) Mo Mo4 .0315(3) .0098(2) .0616(4) .00000 .0224(2) .00000 Mo O1 .0142(15) .0139(15) .0314(18) .00000 .0053(13) .00000 O O2 .0255(13) .0336(15) .0402(16) -.0011(11) .0143(12) .0101(12) O O3 .0203(12) .0178(12) .0315(14) .0017(9) .0087(10) -.0022(10) O O4 .0158(11) .0205(12) .0422(15) .0000(10) .0096(10) .0031(11) O O5 .0226(13) .0153(12) .0600(19) -.0005(10) .0167(13) .0067(12) O O6 .0225(17) .0131(16) .032(2) .00000 .0036(14) .00000 O O7 .0166(11) .0164(11) .0286(13) -.0013(9) .0017(10) .0013(10) O O8 .0195(12) .0293(14) .0472(17) -.0050(11) .0030(11) -.0153(13) O O9 .0223(13) .0142(12) .066(2) -.0040(10) .0129(13) -.0094(12) O O10 .040(2) .0123(18) .083(4) .00000 .026(2) .00000 O O11 .0208(12) .0292(14) .0336(14) .0029(11) .0069(10) .0133(11) O N1 .0162(13) .0242(15) .0272(16) -.0082(11) -.0057(11) .0115(12) N C1 .0183(16) .0248(19) .037(2) -.0047(14) -.0042(15) .0153(16) C C2 .0256(18) .027(2) .037(2) -.0027(15) -.0067(16) .0067(16) C C3 .0252(19) .025(2) .062(3) -.0024(15) -.0084(19) .0020(19) C C4 .031(2) .032(2) .066(3) -.0001(17) -.005(2) -.015(2) C C5 .0149(15) .036(2) .0261(19) -.0056(14) -.0054(13) .0143(16) C C6 .0202(17) .032(2) .043(2) -.0040(15) -.0044(16) .0154(18) C C7 .0233(18) .067(3) .024(2) -.0070(19) .0048(15) .0087(19) C C8 .030(2) .037(2) .055(3) .0054(18) .0012(19) .024(2) C C9 .0196(16) .037(2) .0271(19) -.0097(15) -.0082(14) .0182(16) C C10 .0202(17) .039(2) .031(2) -.0090(16) -.0069(15) .0206(17) C C11 .0208(18) .044(2) .035(2) -.0093(16) -.0017(16) .0232(18) C C12 .037(2) .060(3) .048(3) .002(2) -.002(2) .032(3) C C13 .0212(16) .0205(17) .0246(18) -.0057(13) -.0012(13) .0103(14) C C14 .0210(16) .0230(18) .0299(19) -.0017(14) -.0024(14) .0112(15) C C15 .0172(15) .0234(18) .034(2) -.0056(13) -.0033(14) .0094(15) C C16 .0196(17) .034(2) .046(2) -.0029(16) .0001(16) .0193(19) C 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 Mo1 O1 ? ? 2.3229(3) yes Mo1 O2 ? ? 1.686(3) yes Mo1 O3 ? ? 1.938(3) yes Mo1 O4 ? ? 1.965(3) yes Mo1 O5 ? ? 1.940(3) yes Mo1 O11 ? ? 1.890(3) yes Mo2 O1 ? ? 2.333(3) yes Mo2 O3 ? ? 1.931(2) yes Mo2 O3 ? 5_655 1.931(2) yes Mo2 O6 ? ? 1.697(3) yes Mo2 O7 ? ? 1.927(2) yes Mo2 O7 ? 5_655 1.927(2) yes Mo3 O1 ? ? 2.3182(3) yes Mo3 O4 ? ? 1.886(3) yes Mo3 O7 ? 5_655 1.940(2) yes Mo3 O8 ? ? 1.681(3) yes Mo3 O9 ? ? 1.931(3) yes Mo3 O11 ? 5_655 1.965(3) yes Mo4 O1 ? ? 2.331(3) yes Mo4 O5 ? ? 1.929(3) yes Mo4 O5 ? 5_655 1.929(3) yes Mo4 O9 ? ? 1.943(3) yes Mo4 O9 ? 5_655 1.943(3) yes Mo4 O10 ? ? 1.684(4) yes O1 Mo1 ? 5_655 2.3229(3) yes O1 Mo3 ? 5_655 2.3182(3) yes O7 Mo3 ? 5_655 1.940(2) yes O11 Mo3 ? 5_655 1.965(3) yes N1 C1 ? ? 1.523(5) ? N1 C5 ? ? 1.530(5) ? N1 C9 ? ? 1.532(5) ? N1 C13 ? ? 1.523(4) ? C1 C2 ? ? 1.523(6) ? C2 C3 ? ? 1.520(6) ? C3 C4 ? ? 1.519(7) ? C5 C6 ? ? 1.511(6) ? C6 C7 ? ? 1.534(5) ? C7 C8 ? ? 1.501(7) ? C9 C10 ? ? 1.522(5) ? C10 C11 ? ? 1.529(5) ? C11 C12 ? ? 1.519(7) ? C13 C14 ? ? 1.518(5) ? C14 C15 ? ? 1.528(5) ? C15 C16 ? ? 1.534(5) ?