#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/70/2007027.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_2007027 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1998 _journal_volume 54 _journal_page_first 206 _journal_page_last 208 _publ_section_title ; trans-[Mo(O)(OH)(dppe)~2~]^+^ as its Perchlorate Salt ; _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 'Bendix, Jesper' 'B\/ogevig, Anders' _chemical_formula_moiety 'C52 H49 Mo O2 P4, Cl O4' _chemical_formula_iupac '[Mo(O)(OH)(C26 H24 P2)2](ClO4)' _chemical_formula_weight 1025.18 _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 16.825(4) _cell_length_b 16.658(3) _cell_length_c 17.162(5) _cell_angle_alpha 90.00(2) _cell_angle_beta 102.18(2) _cell_angle_gamma 90.00(2) _cell_volume 4702(2) _cell_formula_units_Z 4 _cell_measurement_temperature 122(2) _exptl_crystal_density_diffrn 1.448 _diffrn_ambient_temperature 122(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 Mo1 .277854(7) .175981(7) .008868(7) .01353(3) Uani d . 1 . . Mo P1 .20040(2) .04480(2) -.00786(2) .01498(7) Uani d . 1 . . P P2 .18057(2) .19959(2) -.12336(2) .01554(7) Uani d . 1 . . P P3 .36042(2) .15342(2) .14810(2) .01521(7) Uani d . 1 . . P P4 .35197(2) .30977(2) .03401(2) .01447(7) Uani d . 1 . . P O1 .36207(7) .14237(7) -.02649(7) .0186(2) Uani d . 1 . . O O2 .18593(7) .21441(7) .04609(7) .0179(2) Uani d . 1 . . O H1 .1554(18) .2324(19) .0619(18) .055(9) Uiso d . 1 . . H C1 .11184(10) .05432(10) -.09240(10) .0202(3) Uani d . 1 . . C H1A .1241 .0260 -.1392 .024 Uiso calc R 1 . . H H1B .0644 .0276 -.0780 .024 Uiso calc R 1 . . H C11A .24598(10) -.04794(9) -.03280(9) .0185(3) Uani d . 1 . . C C12A .20240(12) -.11994(10) -.03805(11) .0253(3) Uani d . 1 . . C H12A .1503 -.1209 -.0249 .030 Uiso calc R 1 . . H C13A .23488(13) -.19006(10) -.06235(12) .0289(4) Uani d . 1 . . C H13A .2050 -.2388 -.0658 .035 Uiso calc R 1 . . H C14A .31055(13) -.18868(12) -.08141(14) .0358(4) Uani d . 1 . . C H14A .3333 -.2367 -.0971 .043 Uiso calc R 1 . . H C15A .35357(13) -.11713(13) -.07765(17) .0451(6) Uani d . 1 . . C H15A .4051 -.1162 -.0920 .054 Uiso calc R 1 . . H C16A .32169(12) -.04669(11) -.05304(14) .0327(4) Uani d . 1 . . C H16A .3516 .0020 -.0501 .039 Uiso calc R 1 . . H C11B .15700(10) .02082(9) .07773(9) .0182(3) Uani d . 1 . . C C12B .08792(10) .06203(11) .08894(10) .0232(3) Uani d . 1 . . C H12B .0596 .0966 .0484 .028 Uiso calc R 1 . . H C13B .06049(11) .05250(12) .15945(11) .0286(4) Uani d . 1 . . C H13B .0141 .0813 .1672 .034 Uiso calc R 1 . . H C14B .10067(13) .00123(13) .21825(11) .0343(4) Uani d . 1 . . C H14B .0816 -.0053 .2662 .041 Uiso calc R 1 . . H C15B .16877(14) -.04063(12) .20729(11) .0323(4) Uani d . 1 . . C H15B .1960 -.0762 .2475 .039 Uiso calc R 1 . . H C16B .19732(11) -.03057(11) .13718(10) .0245(3) Uani d . 1 . . C H16B .2443 -.0588 .1300 .029 Uiso calc R 1 . . H C2 .08957(9) .14150(10) -.11535(10) .0198(3) Uani d . 1 . . C H2A .0635 .1662 -.0746 .024 Uiso calc R 1 . . H H2B .0500 .1428 -.1670 .024 Uiso calc R 1 . . H C21A .21126(10) .16226(9) -.21215(9) .0182(3) Uani d . 1 . . C C22A .29130(10) .17445(11) -.21932(10) .0231(3) Uani d . 1 . . C H22A .3288 .1997 -.1773 .028 Uiso calc R 1 . . H C23A .31678(12) .14999(12) -.28755(11) .0279(4) Uani d . 1 . . C H23A .3711 .1600 -.2926 .034 Uiso calc R 1 . . H C24A .26335(13) .11116(11) -.34820(11) .0294(4) Uani d . 1 . . C H24A .2811 .0940 -.3945 .035 Uiso calc R 1 . . H C25A .18376(13) .09731(11) -.34127(11) .0295(4) Uani d . 1 . . C H25A .1473 .0700 -.3825 .035 Uiso calc R 1 . . H C26A .15738(11) .12348(11) -.27393(10) .0242(3) Uani d . 1 . . C H26A .1026 .1150 -.2699 .029 Uiso calc R 1 . . H C21B .13985(10) .29944(10) -.14986(10) .0212(3) Uani d . 1 . . C C22B .08398(12) .33212(12) -.10927(12) .0304(4) Uani d . 1 . . C H22B .0638 .3005 -.0717 .036 Uiso calc R 1 . . H C23B .05764(13) .41118(13) -.12374(15) .0388(5) Uani d . 1 . . C H23B .0190 .4330 -.0964 .047 Uiso calc R 1 . . H C24B .08746(13) .45780(12) -.17752(16) .0406(5) Uani d . 1 . . C H24B .0702 .5119 -.1864 .049 Uiso calc R 1 . . H C25B .14211(14) .42585(13) -.21818(15) .0402(5) Uani d . 1 . . C H25B .1622 .4580 -.2554 .048 Uiso calc R 1 . . H C26B .16837(12) .34650(11) -.20528(13) .0302(4) Uani d . 1 . . C H26B .2056 .3247 -.2342 .036 Uiso calc R 1 . . H C3 .45278(9) .21387(9) .15168(10) .0186(3) Uani d . 1 . . C H3A .4869 .2124 .2062 .022 Uiso calc R 1 . . H H3B .4847 .1908 .1148 .022 Uiso calc R 1 . . H C31A .31806(10) .19007(9) .23045(9) .0179(3) Uani d . 1 . . C C32A .23452(11) .18600(12) .22414(10) .0258(3) Uani d . 1 . . C H32A .2014 .1607 .1792 .031 Uiso calc R 1 . . H C33A .19885(12) .21868(13) .28312(11) .0312(4) Uani d . 1 . . C H33A .1415 .2164 .2777 .037 Uiso calc R 1 . . H C34A .24662(12) .25441(11) .34960(11) .0276(4) Uani d . 1 . . C H34A .2221 .2776 .3894 .033 Uiso calc R 1 . . H C35A .33009(12) .25622(11) .35786(11) .0283(4) Uani d . 1 . . C H35A .3631 .2793 .4042 .034 Uiso calc R 1 . . H C36A .36618(11) .22447(11) .29885(10) .0243(3) Uani d . 1 . . C H36A .4236 .2261 .3050 .029 Uiso calc R 1 . . H C31B .39913(10) .05304(10) .17493(10) .0208(3) Uani d . 1 . . C C32B .44383(12) .01457(11) .12627(12) .0286(4) Uani d . 1 . . C H32B .4562 .0420 .0818 .034 Uiso calc R 1 . . H C33B .47047(14) -.06415(12) .14259(14) .0381(5) Uani d . 1 . . C H33B .5016 -.0899 .1097 .046 Uiso calc R 1 . . H C34B .45149(14) -.10471(12) .20672(14) .0389(5) Uani d . 1 . . C H34B .4694 -.1584 .2177 .047 Uiso calc R 1 . . H C35B .40658(13) -.06719(12) .25475(13) .0357(5) Uani d . 1 . . C H35B .3932 -.0954 .2983 .043 Uiso calc R 1 . . H C36B .38075(12) .01187(11) .23976(11) .0271(3) Uani d . 1 . . C H36B .3507 .0377 .2736 .033 Uiso calc R 1 . . H C4 .43046(9) .30124(9) .12807(9) .0184(3) Uani d . 1 . . C H4A .4801 .3301 .1216 .022 Uiso calc R 1 . . H H4B .4100 .3276 .1717 .022 Uiso calc R 1 . . H C41A .40927(9) .32884(9) -.04260(9) .0184(3) Uani d . 1 . . C C42A .37472(12) .37496(12) -.10911(11) .0280(4) Uani d . 1 . . C H42A .3247 .4020 -.1109 .034 Uiso calc R 1 . . H C43A .41378(15) .38122(15) -.17291(13) .0390(5) Uani d . 1 . . C H43A .3900 .4124 -.2182 .047 Uiso calc R 1 . . H C44A .48677(15) .34242(14) -.17056(13) .0379(5) Uani d . 1 . . C H44A .5129 .3467 -.2143 .045 Uiso calc R 1 . . H C45A .52179(13) .29744(12) -.10462(13) .0322(4) Uani d . 1 . . C H45A .5724 .2714 -.1028 .039 Uiso calc R 1 . . H C46A .48332(11) .29016(11) -.04094(11) .0255(3) Uani d . 1 . . C H46A .5075 .2587 .0040 .031 Uiso calc R 1 . . H C41B .30368(10) .40515(9) .04604(9) .0183(3) Uani d . 1 . . C C42B .22208(11) .40722(11) .04903(13) .0295(4) Uani d . 1 . . C H42B .1916 .3588 .0440 .035 Uiso calc R 1 . . H C43B .18426(13) .47980(12) .05931(15) .0371(5) Uani d . 1 . . C H43B .1282 .4806 .0609 .044 Uiso calc R 1 . . H C44B .22810(13) .55033(11) .06717(12) .0319(4) Uani d . 1 . . C H44B .2023 .5998 .0742 .038 Uiso calc R 1 . . H C45B .30950(14) .54885(11) .06484(13) .0336(4) Uani d . 1 . . C H45B .3397 .5974 .0706 .040 Uiso calc R 1 . . H C46B .34774(12) .47688(10) .05412(12) .0270(3) Uani d . 1 . . C H46B .4038 .4765 .0523 .032 Uiso calc R 1 . . H Cl1 -.01557(3) .27849(3) .08221(3) .03095(10) Uani d . 1 . . Cl O3 -.02622(9) .21894(10) .01984(9) .0361(3) Uani d . 1 . . O O4 -.07322(13) .34092(12) .06190(12) .0570(5) Uani d . 1 . . O O5 -.02527(14) .24264(13) .15515(11) .0606(6) Uani d . 1 . . O O6 .06606(11) .30803(15) .09321(15) .0742(8) Uani d . 1 . . O 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 Mo1 .01403(5) .01217(5) .01392(5) -.00203(4) .00189(4) .00003(4) P1 .01578(16) .01342(16) .01604(16) -.00314(12) .00404(13) -.00170(12) P2 .01459(16) .01579(16) .01544(16) -.00047(13) .00136(13) .00007(13) P3 .01530(16) .01396(16) .01547(16) -.00087(13) .00123(13) .00027(12) P4 .01387(15) .01239(15) .01700(16) -.00155(12) .00296(12) -.00062(12) O1 .0177(5) .0173(5) .0214(5) -.0013(4) .0055(4) -.0003(4) O2 .0151(5) .0180(5) .0213(5) .0012(4) .0056(4) -.0017(4) C1 .0190(7) .0212(7) .0195(7) -.0062(6) .0016(5) -.0022(5) C11A .0218(7) .0150(6) .0188(7) -.0017(5) .0043(5) -.0031(5) C12A .0323(9) .0166(7) .0296(8) -.0063(6) .0130(7) -.0040(6) C13A .0395(10) .0156(7) .0325(9) -.0048(7) .0096(8) -.0054(6) C14A .0379(10) .0208(8) .0492(12) .0029(7) .0104(9) -.0126(8) C15A .0283(10) .0292(10) .0825(18) -.0023(8) .0224(11) -.0221(11) C16A .0245(8) .0218(8) .0539(12) -.0041(7) .0132(8) -.0138(8) C11B .0200(7) .0179(6) .0174(6) -.0073(5) .0054(5) -.0030(5) C12B .0202(7) .0267(8) .0236(7) -.0075(6) .0070(6) -.0056(6) C13B .0241(8) .0368(10) .0286(8) -.0132(7) .0138(7) -.0133(7) C14B .0436(11) .0410(11) .0227(8) -.0208(9) .0169(8) -.0093(8) C15B .0452(11) .0317(9) .0205(8) -.0090(8) .0085(7) .0019(7) C16B .0314(8) .0213(7) .0212(7) -.0042(6) .0063(6) -.0006(6) C2 .0140(6) .0232(7) .0211(7) -.0022(5) .0013(5) -.0003(6) C21A .0215(7) .0174(7) .0154(6) -.0004(5) .0028(5) .0006(5) C22A .0234(7) .0266(8) .0198(7) -.0024(6) .0058(6) .0001(6) C23A .0310(9) .0309(9) .0248(8) .0025(7) .0124(7) .0022(7) C24A .0451(11) .0258(8) .0197(7) .0051(8) .0121(7) .0008(6) C25A .0425(10) .0256(8) .0191(7) -.0038(7) .0034(7) -.0037(6) C26A .0282(8) .0251(8) .0183(7) -.0037(6) .0025(6) -.0017(6) C21B .0196(7) .0180(7) .0226(7) .0016(5) -.0032(6) .0009(6) C22B .0309(9) .0263(9) .0329(9) .0098(7) .0043(7) .0028(7) C23B .0328(10) .0296(10) .0504(13) .0138(8) .0005(9) -.0005(9) C24B .0306(10) .0215(9) .0630(15) .0062(7) -.0056(9) .0069(9) C25B .0373(11) .0240(9) .0569(14) -.0003(8) .0044(10) .0147(9) C26B .0279(9) .0229(8) .0390(10) -.0004(7) .0049(7) .0078(7) C3 .0144(6) .0182(7) .0215(7) -.0005(5) .0001(5) .0014(5) C31A .0210(7) .0171(6) .0150(6) -.0018(5) .0025(5) -.0005(5) C32A .0225(7) .0364(10) .0190(7) -.0072(7) .0057(6) -.0059(6) C33A .0267(8) .0442(11) .0251(8) -.0042(8) .0106(7) -.0053(8) C34A .0392(10) .0245(8) .0214(8) -.0013(7) .0116(7) -.0034(6) C35A .0375(10) .0265(8) .0194(7) -.0034(7) .0022(7) -.0060(6) C36A .0244(8) .0276(8) .0188(7) -.0021(6) -.0004(6) -.0031(6) C31B .0215(7) .0163(7) .0217(7) -.0014(5) -.0023(6) .0012(5) C32B .0338(9) .0209(8) .0289(9) .0048(7) .0018(7) -.0004(6) C33B .0450(12) .0235(9) .0406(11) .0105(8) -.0028(9) -.0068(8) C34B .0449(12) .0162(8) .0452(12) .0037(8) -.0144(9) .0006(8) C35B .0400(11) .0217(8) .0390(11) -.0039(8) -.0063(8) .0112(8) C36B .0294(8) .0207(8) .0290(8) -.0012(6) .0007(7) .0066(6) C4 .0170(6) .0166(6) .0199(7) -.0034(5) .0001(5) -.0005(5) C41A .0200(6) .0165(6) .0198(6) -.0047(5) .0070(5) -.0019(5) C42A .0295(9) .0310(9) .0245(8) .0018(7) .0077(7) .0058(7) C43A .0471(12) .0461(12) .0268(9) .0030(10) .0146(9) .0120(9) C44A .0483(12) .0390(11) .0333(10) -.0032(9) .0243(9) .0032(8) C45A .0318(9) .0308(9) .0400(10) .0001(7) .0210(8) .0011(8) C46A .0251(8) .0242(8) .0301(8) .0009(6) .0125(7) .0040(7) C41B .0202(7) .0153(6) .0185(6) .0009(5) .0023(5) -.0011(5) C42B .0214(8) .0187(7) .0484(11) .0013(6) .0069(7) -.0063(7) C43B .0270(9) .0259(9) .0581(14) .0068(7) .0084(9) -.0091(9) C44B .0420(11) .0183(8) .0336(9) .0084(7) .0038(8) -.0046(7) C45B .0441(11) .0153(7) .0412(11) -.0023(7) .0082(9) -.0053(7) C46B .0283(8) .0172(7) .0361(9) -.0033(6) .0084(7) -.0038(7) Cl1 .01998(18) .0411(2) .0331(2) .00122(17) .00860(16) -.01003(19) O3 .0284(7) .0432(8) .0343(7) .0016(6) .0009(6) -.0123(6) O4 .0697(13) .0458(10) .0588(12) .0278(9) .0212(10) .0069(9) O5 .0828(15) .0661(13) .0369(9) .0241(11) .0218(9) .0069(9) O6 .0338(9) .1002(17) .0966(16) -.0256(10) .0317(10) -.0690(14) 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 Mo1 O1 . 1.7471(11) yes Mo1 O2 . 1.9044(12) yes Mo1 P3 . 2.5258(4) yes Mo1 P1 . 2.5294(4) yes Mo1 P2 . 2.5330(4) yes Mo1 P4 . 2.5458(4) yes P1 C11A . 1.8156(16) no P1 C11B . 1.8174(16) no P1 C1 . 1.8542(16) no P2 C21A . 1.8185(16) no P2 C21B . 1.8198(17) no P2 C2 . 1.8408(16) no P3 C31A . 1.8176(16) no P3 C31B . 1.8181(16) no P3 C3 . 1.8419(16) no P4 C41A . 1.8150(16) no P4 C41B . 1.8162(16) no P4 C4 . 1.8629(15) no C1 C2 . 1.530(2) no C11A C16A . 1.389(2) no C11A C12A . 1.399(2) no C12A C13A . 1.390(2) no C13A C14A . 1.380(3) no C14A C15A . 1.389(3) no C15A C16A . 1.392(3) no C11B C16B . 1.394(2) no C11B C12B . 1.398(2) no C12B C13B . 1.392(2) no C13B C14B . 1.384(3) no C14B C15B . 1.388(3) no C15B C16B . 1.397(3) no C21A C22A . 1.393(2) no C21A C26A . 1.399(2) no C22A C23A . 1.390(2) no C23A C24A . 1.384(3) no C24A C25A . 1.389(3) no C25A C26A . 1.392(3) no C21B C26B . 1.394(3) no C21B C22B . 1.393(3) no C22B C23B . 1.395(3) no C23B C24B . 1.379(3) no C24B C25B . 1.373(3) no C25B C26B . 1.396(3) no C3 C4 . 1.536(2) no C31A C32A . 1.388(2) no C31A C36A . 1.400(2) no C32A C33A . 1.392(2) no C33A C34A . 1.384(3) no C34A C35A . 1.382(3) no C35A C36A . 1.391(3) no C31B C32B . 1.392(3) no C31B C36B . 1.396(2) no C32B C33B . 1.395(3) no C33B C34B . 1.385(3) no C34B C35B . 1.380(3) no C35B C36B . 1.394(3) no C41A C46A . 1.397(2) no C41A C42A . 1.397(2) no C42A C43A . 1.395(3) no C43A C44A . 1.381(3) no C44A C45A . 1.381(3) no C45A C46A . 1.388(2) no C41B C42B . 1.385(2) no C41B C46B . 1.398(2) no C42B C43B . 1.395(3) no C43B C44B . 1.379(3) no C44B C45B . 1.379(3) no C45B C46B . 1.391(3) no Cl1 O4 . 1.4147(18) no Cl1 O5 . 1.4271(19) no Cl1 O6 . 1.4334(18) no Cl1 O3 . 1.4425(15) no O2 H1 . .70(3) yes _cod_database_code 2007027