#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008584.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_2008584 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1999 _journal_volume 55 _journal_page_first 916 _journal_page_last 918 _publ_section_title ; Dibenzylbis(tert-butylimido)molybdenum(VI), containing both \h^1^- and \h^2^-benzyl ligands ; _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 'Clegg, William' 'Elsegood, Mark R. J.' 'Dyer, Philip W.' 'Gibson, Vernon C.' 'Marshall, Edward L.' _chemical_formula_sum 'C22 H32 Mo N2' _chemical_formula_iupac '[Mo (C~7~H~7~)~2~(C~4~H~9~N)~2~]' _chemical_formula_weight 420.44 _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 9.733(3) _cell_length_b 17.579(4) _cell_length_c 13.016(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.12(2) _cell_angle_gamma 90.00 _cell_volume 2209.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _exptl_crystal_density_diffrn 1.264 _diffrn_ambient_temperature 160(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 Mo .134804(13) .265493(7) .098781(9) .02181(6) Uani d . 1 . . Mo N1 .23454(14) .19219(8) .15968(9) .0273(3) Uani d . 1 . . N C1 .27044(17) .11882(9) .20734(12) .0299(3) Uani d . 1 . . C C2 .19142(19) .05632(10) .14285(15) .0394(4) Uani d . 1 . . C H2A .2140 .0067 .1750 .059 Uiso calc R 1 . . H H2B .2180 .0567 .0726 .059 Uiso calc R 1 . . H H2C .0917 .0655 .1396 .059 Uiso calc R 1 . . H C3 .2333(2) .12004(12) .31843(14) .0517(5) Uani d . 1 . . C H3A .2568 .0709 .3516 .077 Uiso calc R 1 . . H H3B .1338 .1295 .3171 .077 Uiso calc R 1 . . H H3C .2854 .1605 .3576 .077 Uiso calc R 1 . . H C4 .42592(19) .10643(12) .20788(16) .0460(5) Uani d . 1 . . C H4A .4525 .0578 .2413 .069 Uiso calc R 1 . . H H4B .4767 .1478 .2461 .069 Uiso calc R 1 . . H H4C .4483 .1058 .1365 .069 Uiso calc R 1 . . H N2 -.04274(15) .24859(8) .08815(10) .0288(3) Uani d . 1 . . N C5 -.17756(16) .21728(10) .10232(12) .0305(3) Uani d . 1 . . C C6 -.2237(2) .16397(14) .01228(15) .0499(5) Uani d . 1 . . C H6A -.3140 .1421 .0212 .075 Uiso calc R 1 . . H H6B -.1556 .1230 .0106 .075 Uiso calc R 1 . . H H6C -.2310 .1925 -.0528 .075 Uiso calc R 1 . . H C7 -.16578(18) .17478(10) .20528(13) .0349(4) Uani d . 1 . . C H7A -.2575 .1566 .2177 .052 Uiso calc R 1 . . H H7B -.1291 .2091 .2614 .052 Uiso calc R 1 . . H H7C -.1032 .1313 .2029 .052 Uiso calc R 1 . . H C8 -.2784(2) .28415(13) .10442(17) .0496(5) Uani d . 1 . . C H8A -.3711 .2647 .1116 .074 Uiso calc R 1 . . H H8B -.2813 .3131 .0398 .074 Uiso calc R 1 . . H H8C -.2471 .3174 .1632 .074 Uiso calc R 1 . . H C9 .1628(2) .36249(10) .20446(14) .0374(4) Uani d . 1 . . C H9A .222(2) .3542(13) .2644(19) .056 Uiso d . 1 . . H H9B .075(2) .3799(14) .2154(17) .056 Uiso d . 1 . . H C10 .22237(18) .39708(9) .11823(12) .0292(3) Uani d . 1 . . C C11 .13650(18) .42782(9) .03293(13) .0316(4) Uani d . 1 . . C H11 .0396 .4315 .0354 .038 Uiso calc R 1 . . H C12 .19165(19) .45266(9) -.05445(13) .0357(4) Uani d . 1 . . C H12 .1327 .4747 -.1102 .043 Uiso calc R 1 . . H C13 .3313(2) .44568(10) -.06108(14) .0378(4) Uani d . 1 . . C H13 .3683 .4628 -.1212 .045 Uiso calc R 1 . . H C14 .41750(19) .41366(10) .02026(15) .0394(4) Uani d . 1 . . C H14 .5137 .4085 .0155 .047 Uiso calc R 1 . . H C15 .36442(18) .38916(10) .10819(13) .0347(4) Uani d . 1 . . C H15 .4245 .3666 .1628 .042 Uiso calc R 1 . . H C16 .18291(19) .25914(9) -.06142(12) .0262(3) Uani d . 1 . . C H16A .255(2) .2927(12) -.0663(15) .039 Uiso d . 1 . . H H16B .107(2) .2790(11) -.1014(16) .039 Uiso d . 1 . . H C17 .21836(15) .18155(9) -.09541(10) .0232(3) Uani d . 1 . . C C18 .11671(16) .13065(9) -.13714(12) .0285(3) Uani d . 1 . . C H18 .0223 .1458 -.1442 .034 Uiso calc R 1 . . H C19 .15010(18) .05848(10) -.16849(13) .0348(4) Uani d . 1 . . C H19 .0788 .0251 -.1975 .042 Uiso calc R 1 . . H C20 .28669(19) .03445(10) -.15798(13) .0364(4) Uani d . 1 . . C H20 .3094 -.0153 -.1788 .044 Uiso calc R 1 . . H C21 .38977(18) .08412(10) -.11667(13) .0343(4) Uani d . 1 . . C H21 .4838 .0683 -.1090 .041 Uiso calc R 1 . . H C22 .35598(16) .15675(10) -.08653(12) .0284(3) Uani d . 1 . . C H22 .4278 .1904 -.0593 .034 Uiso calc R 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 Mo .02773(9) .01892(9) .01963(8) .00094(5) .00638(5) .00024(4) N1 .0333(7) .0262(7) .0227(6) .0013(6) .0052(5) -.0003(5) C1 .0338(8) .0295(8) .0261(8) .0087(7) .0026(6) .0059(7) C2 .0427(10) .0269(9) .0476(10) .0002(8) .0022(8) .0067(8) C3 .0782(15) .0480(12) .0313(9) .0228(11) .0166(9) .0156(9) C4 .0348(10) .0524(12) .0486(11) .0103(9) -.0043(8) -.0006(9) N2 .0320(7) .0301(7) .0254(7) .0035(6) .0082(6) .0000(6) C5 .0245(8) .0393(9) .0289(8) .0029(7) .0082(6) -.0001(7) C6 .0394(10) .0721(15) .0388(10) -.0122(10) .0067(8) -.0148(10) C7 .0346(9) .0367(9) .0353(9) -.0012(7) .0119(7) .0030(7) C8 .0418(11) .0608(13) .0493(11) .0220(10) .0178(9) .0138(10) C9 .0582(12) .0276(9) .0274(8) -.0017(8) .0090(8) -.0064(7) C10 .0429(9) .0168(7) .0270(8) -.0020(7) .0008(7) -.0048(6) C11 .0350(9) .0226(8) .0362(9) .0051(7) .0003(7) -.0044(7) C12 .0512(10) .0230(8) .0304(8) .0017(7) -.0048(7) .0023(7) C13 .0522(11) .0266(9) .0354(9) -.0103(8) .0087(8) .0019(7) C14 .0347(9) .0313(9) .0520(11) -.0077(7) .0046(8) .0012(8) C15 .0380(9) .0267(8) .0361(9) -.0035(7) -.0091(7) .0004(7) C16 .0356(9) .0217(8) .0225(8) -.0013(7) .0077(7) .0001(6) C17 .0301(8) .0241(8) .0165(6) -.0016(6) .0075(6) .0004(6) C18 .0265(8) .0335(9) .0262(8) -.0032(7) .0066(6) -.0037(7) C19 .0392(9) .0315(9) .0350(9) -.0115(7) .0094(7) -.0101(7) C20 .0487(10) .0256(8) .0378(9) .0000(7) .0169(8) -.0079(7) C21 .0316(8) .0370(10) .0361(9) .0057(7) .0115(7) -.0011(7) C22 .0278(8) .0303(9) .0278(8) -.0056(6) .0063(6) -.0032(6) 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 Mo N2 . 1.7420(15) yes Mo N1 . 1.7437(14) yes Mo C9 . 2.1866(17) yes Mo C16 . 2.1958(16) yes Mo C10 . 2.4673(16) yes N1 C1 . 1.455(2) yes C1 C4 . 1.528(2) no C1 C2 . 1.531(2) no C1 C3 . 1.534(2) no N2 C5 . 1.456(2) yes C5 C6 . 1.524(2) no C5 C7 . 1.526(2) no C5 C8 . 1.534(2) no C9 C10 . 1.459(2) yes C10 C15 . 1.412(2) yes C10 C11 . 1.412(2) yes C11 C12 . 1.387(3) no C12 C13 . 1.378(3) no C13 C14 . 1.386(3) no C14 C15 . 1.382(3) no C16 C17 . 1.488(2) yes C17 C18 . 1.393(2) no C17 C22 . 1.400(2) no C18 C19 . 1.384(2) no C19 C20 . 1.385(3) no C20 C21 . 1.387(3) no C21 C22 . 1.387(2) no C9 H9A . .92(2) no C9 H9B . .94(2) no C16 H16A . .93(2) no C16 H16B . .92(2) no C2 H2A . .980 no C2 H2B . .980 no C2 H2C . .980 no C3 H3A . .980 no C3 H3B . .980 no C3 H3C . .980 no C4 H4A . .980 no C4 H4B . .980 no C4 H4C . .980 no C6 H6A . .980 no C6 H6B . .980 no C6 H6C . .980 no C7 H7A . .980 no C7 H7B . .980 no C7 H7C . .980 no C8 H8A . .980 no C8 H8B . .980 no C8 H8C . .980 no C11 H11 . .950 no C12 H12 . .950 no C13 H13 . .950 no C14 H14 . .950 no C15 H15 . .950 no C18 H18 . .950 no C19 H19 . .950 no C20 H20 . .950 no C21 H21 . .950 no C22 H22 . .950 no _cod_database_code 2008584