#------------------------------------------------------------------------------
#$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $
#$Revision: 26848 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/23/2202337.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_2202337
_journal_name_full  'Acta Crystallographica, Section E'
_journal_year  2003
_journal_volume  59
_journal_page_first  m644
_journal_page_last  m646
_publ_section_title
;
Tetraethylammonium
dicarbonyl(dicyanomethylene)[tris(3,5-dimethyl-1-
pyrazolyl)hydroborato]molybdenum(0)
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_[local]_cod_cif_authors_sg_H-M  'C 2/c'
loop_
_publ_author_name
  'Ferguson, George'
  'Lalor, Fergus J.'
  "O'Neill, S. A."
_chemical_formula_moiety  'C8 H20 N 1+, C20 H22 B Mo N8 O2 1-'
_chemical_formula_sum  'C28 H42 B Mo N9 O2'
_chemical_formula_iupac  '(C8 H20 N) [Mo (C15 H22 B N6) (C3 N2) (C1 O1)2]'
_chemical_formula_weight  643.46
_symmetry_cell_setting  monoclinic
loop_
_symmetry_equiv_pos_as_xyz
  'x, y, z'
  '-x, y, -z+1/2'
  'x+1/2, y+1/2, z'
  '-x+1/2, y+1/2, -z+1/2'
  '-x, -y, -z'
  'x, -y, z-1/2'
  '-x+1/2, -y+1/2, -z'
  'x+1/2, -y+1/2, z-1/2'
_cell_length_a  40.153(3)
_cell_length_b  8.113(2)
_cell_length_c  20.161(3)
_cell_angle_alpha  90.00
_cell_angle_beta  109.989(8)
_cell_angle_gamma  90.00
_cell_volume  6172.0(18)
_cell_formula_units_Z  8
_cell_measurement_temperature  294.0(10)
_exptl_crystal_density_diffrn  1.385
_diffrn_ambient_temperature  294.0(10)
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 0.358557(6) 0.17635(3) 0.320422(12) 0.02968(8) Uani d . 1 . . Mo
  O1 0.34972(7) 0.3246(4) 0.44869(11) 0.0602(7) Uani d . 1 . . O
  O2 0.37920(7) -0.0763(3) 0.43723(12) 0.0574(7) Uani d . 1 . . O
  N11 0.33736(7) 0.3799(3) 0.24569(12) 0.0356(6) Uani d . 1 . . N
  N12 0.31938(6) 0.3427(4) 0.17908(12) 0.0377(6) Uani d . 1 . . N
  N21 0.36922(7) 0.0483(3) 0.23396(13) 0.0382(6) Uani d . 1 . . N
  N22 0.34514(7) 0.0655(3) 0.16950(12) 0.0391(6) Uani d . 1 . . N
  N31 0.30455(6) 0.0766(3) 0.26795(12) 0.0346(6) Uani d . 1 . . N
  N32 0.29019(6) 0.0831(3) 0.19871(12) 0.0374(6) Uani d . 1 . . N
  N4 0.43847(10) 0.3891(7) 0.27592(19) 0.1009(16) Uani d . 1 . . N
  N5 0.44759(9) 0.2422(5) 0.47857(16) 0.0668(10) Uani d . 1 . . N
  N6 0.44955(6) 0.3337(4) 0.08250(13) 0.0433(6) Uani d . 1 . . N
  B1 0.31107(10) 0.1629(5) 0.15768(16) 0.0405(9) Uani d . 1 . . B
  H1 0.2969 0.1589 0.1073 0.049 Uiso calc R 1 . . H
  C1 0.35118(8) 0.2752(4) 0.39828(16) 0.0368(7) Uani d . 1 . . C
  C2 0.37173(8) 0.0091(4) 0.39057(15) 0.0383(7) Uani d . 1 . . C
  C3 0.40858(8) 0.2643(4) 0.35400(15) 0.0386(7) Uani d . 1 . . C
  C4 0.42592(9) 0.3344(6) 0.31163(18) 0.0591(10) Uani d . 1 . . C
  C5 0.43110(8) 0.2555(5) 0.42307(18) 0.0442(8) Uani d . 1 . . C
  C13 0.30931(9) 0.4846(5) 0.14415(17) 0.0452(8) Uani d . 1 . . C
  C14 0.32054(10) 0.6120(5) 0.18795(19) 0.0531(9) Uani d . 1 . . C
  H14 0.3172 0.7237 0.1773 0.064 Uiso calc R 1 . . H
  C15 0.33767(9) 0.5432(4) 0.25062(17) 0.0427(8) Uani d . 1 . . C
  C16 0.29008(10) 0.4878(6) 0.06957(17) 0.0666(12) Uani d . 1 . . C
  H16A 0.2852 0.6000 0.0542 0.100 Uiso calc R 1 . . H
  H16B 0.2682 0.4290 0.0598 0.100 Uiso calc R 1 . . H
  H16C 0.3040 0.4366 0.0450 0.100 Uiso calc R 1 . . H
  C17 0.35373(11) 0.6300(5) 0.31612(19) 0.0643(11) Uani d . 1 . . C
  H17A 0.3521 0.7466 0.3075 0.096 Uiso calc R 1 . . H
  H17B 0.3782 0.5988 0.3363 0.096 Uiso calc R 1 . . H
  H17C 0.3416 0.6023 0.3482 0.096 Uiso calc R 1 . . H
  C23 0.35653(11) -0.0209(5) 0.12611(18) 0.0517(9) Uani d . 1 . . C
  C24 0.38756(11) -0.0941(5) 0.1621(2) 0.0567(10) Uani d . 1 . . C
  H24 0.4011 -0.1612 0.1438 0.068 Uiso calc R 1 . . H
  C25 0.39486(9) -0.0505(4) 0.22925(19) 0.0467(8) Uani d . 1 . . C
  C26 0.33562(13) -0.0286(6) 0.05210(18) 0.0821(15) Uani d . 1 . . C
  H26A 0.3475 -0.0962 0.0281 0.123 Uiso calc R 1 . . H
  H26B 0.3326 0.0805 0.0325 0.123 Uiso calc R 1 . . H
  H26C 0.3128 -0.0752 0.0465 0.123 Uiso calc R 1 . . H
  C27 0.42546(10) -0.1034(6) 0.2889(2) 0.0679(12) Uani d . 1 . . C
  H27A 0.4211 -0.0827 0.3321 0.102 Uiso calc R 1 . . H
  H27B 0.4461 -0.0432 0.2889 0.102 Uiso calc R 1 . . H
  H27C 0.4293 -0.2192 0.2849 0.102 Uiso calc R 1 . . H
  C33 0.25857(9) 0.0080(5) 0.17815(17) 0.0481(9) Uani d . 1 . . C
  C34 0.25159(9) -0.0468(5) 0.23328(18) 0.0545(10) Uani d . 1 . . C
  H34 0.2316 -0.1032 0.2343 0.065 Uiso calc R 1 . . H
  C35 0.28068(8) -0.0013(4) 0.28848(17) 0.0418(8) Uani d . 1 . . C
  C36 0.23614(11) -0.0101(7) 0.10529(19) 0.0790(14) Uani d . 1 . . C
  H36A 0.2492 -0.0633 0.0793 0.118 Uiso calc R 1 . . H
  H36B 0.2285 0.0966 0.0853 0.118 Uiso calc R 1 . . H
  H36C 0.2159 -0.0758 0.1028 0.118 Uiso calc R 1 . . H
  C37 0.28574(10) -0.0313(6) 0.36034(18) 0.0620(11) Uani d . 1 . . C
  H37A 0.2641 -0.0721 0.3646 0.093 Uiso calc R 1 . . H
  H37B 0.2924 0.0695 0.3865 0.093 Uiso calc R 1 . . H
  H37C 0.3042 -0.1115 0.3787 0.093 Uiso calc R 1 . . H
  C61 0.41331(9) 0.4083(5) 0.04920(19) 0.0562(10) Uani d . 1 . . C
  H61A 0.4163 0.5207 0.0359 0.067 Uiso calc R 1 . . H
  H61B 0.4013 0.3483 0.0060 0.067 Uiso calc R 1 . . H
  C62 0.38977(11) 0.4118(7) 0.0917(2) 0.0791(14) Uani d . 1 . . C
  H62A 0.3679 0.4647 0.0653 0.119 Uiso calc R 1 . . H
  H62B 0.4011 0.4718 0.1346 0.119 Uiso calc R 1 . . H
  H62C 0.3851 0.3011 0.1029 0.119 Uiso calc R 1 . . H
  C63 0.44504(11) 0.1541(5) 0.0947(2) 0.0715(12) Uani d . 1 . . C
  H63A 0.4306 0.1047 0.0503 0.086 Uiso calc R 1 . . H
  H63B 0.4322 0.1436 0.1274 0.086 Uiso calc R 1 . . H
  C64 0.47940(14) 0.0577(6) 0.1235(3) 0.114(2) Uani d . 1 . . C
  H64A 0.4743 -0.0538 0.1327 0.171 Uiso calc R 1 . . H
  H64B 0.4943 0.1078 0.1665 0.171 Uiso calc R 1 . . H
  H64C 0.4913 0.0581 0.0895 0.171 Uiso calc R 1 . . H
  C65 0.46916(10) 0.4157(5) 0.14930(18) 0.0576(10) Uani d . 1 . . C
  H65A 0.4928 0.3688 0.1669 0.069 Uiso calc R 1 . . H
  H65B 0.4577 0.3890 0.1831 0.069 Uiso calc R 1 . . H
  C66 0.47276(13) 0.5990(6) 0.1478(2) 0.0785(14) Uani d . 1 . . C
  H66A 0.4842 0.6390 0.1949 0.118 Uiso calc R 1 . . H
  H66B 0.4497 0.6479 0.1284 0.118 Uiso calc R 1 . . H
  H66C 0.4867 0.6277 0.1191 0.118 Uiso calc R 1 . . H
  C67 0.47131(9) 0.3605(5) 0.03700(19) 0.0576(11) Uani d . 1 . . C
  H67A 0.4724 0.4776 0.0284 0.069 Uiso calc R 1 . . H
  H67B 0.4953 0.3225 0.0617 0.069 Uiso calc R 1 . . H
  C68 0.45733(12) 0.2749(7) -0.0304(2) 0.0906(17) Uani d . 1 . . C
  H68A 0.4727 0.2935 -0.0571 0.136 Uiso calc R 1 . . H
  H68B 0.4341 0.3160 -0.0562 0.136 Uiso calc R 1 . . H
  H68C 0.4560 0.1589 -0.0222 0.136 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
  Mo1 0.03031(12) 0.03440(14) 0.02363(11) -0.00140(14) 0.00831(8) -0.00083(14)
  O1 0.0826(18) 0.0687(18) 0.0358(12) 0.0135(16) 0.0287(12) -0.0046(14)
  O2 0.0735(17) 0.0539(17) 0.0407(13) 0.0115(14) 0.0143(12) 0.0144(13)
  N11 0.0405(14) 0.0369(16) 0.0271(12) -0.0026(12) 0.0086(11) 0.0009(11)
  N12 0.0415(14) 0.0431(17) 0.0253(11) -0.0019(13) 0.0073(10) 0.0042(12)
  N21 0.0397(14) 0.0441(17) 0.0337(13) -0.0008(13) 0.0163(11) -0.0054(12)
  N22 0.0504(16) 0.0420(17) 0.0289(13) -0.0075(13) 0.0190(12) -0.0083(12)
  N31 0.0342(13) 0.0413(16) 0.0287(12) -0.0042(12) 0.0112(10) -0.0002(11)
  N32 0.0350(14) 0.0473(17) 0.0278(12) -0.0068(13) 0.0081(10) -0.0034(12)
  N4 0.071(2) 0.185(5) 0.055(2) -0.035(3) 0.0309(19) 0.010(3)
  N5 0.0552(19) 0.095(3) 0.0391(17) -0.0068(19) 0.0016(15) -0.0095(17)
  N6 0.0355(13) 0.0501(18) 0.0433(14) -0.0016(14) 0.0121(11) 0.0040(15)
  B1 0.0454(19) 0.053(2) 0.0206(14) -0.009(2) 0.0074(13) -0.0031(18)
  C1 0.0365(16) 0.040(2) 0.0327(16) 0.0016(14) 0.0099(13) 0.0032(14)
  C2 0.0432(17) 0.0396(19) 0.0294(15) 0.0001(16) 0.0092(13) -0.0021(15)
  C3 0.0350(16) 0.051(2) 0.0302(15) -0.0059(15) 0.0114(13) -0.0062(14)
  C4 0.0402(18) 0.096(3) 0.0406(18) -0.012(2) 0.0129(15) -0.007(2)
  C5 0.0373(17) 0.053(2) 0.0415(19) -0.0044(16) 0.0122(15) -0.0095(16)
  C13 0.0447(19) 0.054(2) 0.0363(17) 0.0016(18) 0.0134(14) 0.0143(17)
  C14 0.063(2) 0.042(2) 0.053(2) 0.0040(19) 0.0175(18) 0.0164(18)
  C15 0.052(2) 0.035(2) 0.0423(18) -0.0017(16) 0.0172(15) 0.0032(15)
  C16 0.067(2) 0.087(3) 0.0397(19) 0.009(2) 0.0106(18) 0.025(2)
  C17 0.093(3) 0.039(2) 0.055(2) -0.013(2) 0.017(2) -0.0105(19)
  C23 0.074(3) 0.049(2) 0.0436(19) -0.013(2) 0.0360(19) -0.0097(17)
  C24 0.070(3) 0.052(2) 0.066(2) -0.004(2) 0.046(2) -0.019(2)
  C25 0.047(2) 0.044(2) 0.057(2) -0.0051(17) 0.0288(17) -0.0077(17)
  C26 0.120(4) 0.098(4) 0.038(2) -0.013(3) 0.039(2) -0.026(2)
  C27 0.053(2) 0.074(3) 0.078(3) 0.018(2) 0.023(2) -0.004(2)
  C33 0.0425(19) 0.055(2) 0.0411(18) -0.0170(18) 0.0066(15) -0.0077(17)
  C34 0.0416(19) 0.064(3) 0.056(2) -0.0181(19) 0.0144(17) -0.0032(19)
  C35 0.0405(17) 0.047(2) 0.0426(17) -0.0049(16) 0.0202(14) 0.0012(16)
  C36 0.064(3) 0.110(4) 0.050(2) -0.034(3) 0.003(2) -0.016(3)
  C37 0.059(2) 0.087(3) 0.048(2) -0.018(2) 0.0273(18) 0.010(2)
  C61 0.0376(18) 0.070(3) 0.057(2) 0.0035(19) 0.0109(16) 0.012(2)
  C62 0.051(2) 0.103(4) 0.093(3) 0.011(3) 0.038(2) 0.017(3)
  C63 0.063(3) 0.055(3) 0.093(3) -0.003(2) 0.023(2) 0.014(2)
  C64 0.100(4) 0.061(3) 0.154(6) 0.016(3) 0.009(4) 0.018(4)
  C65 0.060(2) 0.071(3) 0.0375(18) -0.003(2) 0.0116(17) 0.0023(19)
  C66 0.099(4) 0.074(3) 0.060(3) -0.013(3) 0.025(2) -0.022(2)
  C67 0.050(2) 0.075(3) 0.055(2) -0.010(2) 0.0268(17) -0.012(2)
  C68 0.083(3) 0.136(5) 0.066(3) -0.034(3) 0.043(2) -0.039(3)
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 C1 . 1.874(3) y
  Mo1 C2 . 1.900(3) y
  Mo1 C3 . 2.018(3) y
  Mo1 N11 . 2.201(3) y
  Mo1 N21 . 2.193(2) y
  Mo1 N31 . 2.215(2) y
  O1 C1 . 1.113(3) y
  O2 C2 . 1.124(4) y
  N11 N12 . 1.324(3) ?
  N11 C15 . 1.328(4) ?
  N12 C13 . 1.337(4) ?
  N12 B1 . 1.526(5) ?
  N21 C25 . 1.334(4) ?
  N21 N22 . 1.336(3) ?
  N22 C23 . 1.319(4) ?
  N22 B1 . 1.526(5) ?
  N31 N32 . 1.317(3) ?
  N31 C35 . 1.327(4) ?
  N32 C33 . 1.340(4) ?
  N32 B1 . 1.510(4) ?
  N4 C4 . 1.104(5) y
  N5 C5 . 1.093(4) y
  N6 C65 . 1.467(4) ?
  N6 C67 . 1.483(4) ?
  N6 C63 . 1.499(5) ?
  N6 C61 . 1.506(4) ?
  B1 H1 . 0.98 ?
  C3 C5 . 1.379(4) y
  C3 C4 . 1.394(5) y
  C13 C14 . 1.334(5) ?
  C13 C16 . 1.437(4) ?
  C14 C15 . 1.337(4) ?
  C14 H14 . 0.93 ?
  C15 C17 . 1.440(5) ?
  C16 H16A . 0.96 ?
  C16 H16B . 0.96 ?
  C16 H16C . 0.96 ?
  C17 H17A . 0.96 ?
  C17 H17B . 0.96 ?
  C17 H17C . 0.96 ?
  C23 C24 . 1.347(5) ?
  C23 C26 . 1.442(5) ?
  C24 C25 . 1.331(5) ?
  C24 H24 . 0.93 ?
  C25 C27 . 1.459(5) ?
  C26 H26A . 0.96 ?
  C26 H26B . 0.96 ?
  C26 H26C . 0.96 ?
  C27 H27A . 0.96 ?
  C27 H27B . 0.96 ?
  C27 H27C . 0.96 ?
  C33 C34 . 1.313(5) ?
  C33 C36 . 1.444(4) ?
  C34 C35 . 1.360(4) ?
  C34 H34 . 0.93 ?
  C35 C37 . 1.413(4) ?
  C36 H36A . 0.96 ?
  C36 H36B . 0.96 ?
  C36 H36C . 0.96 ?
  C37 H37A . 0.96 ?
  C37 H37B . 0.96 ?
  C37 H37C . 0.96 ?
  C61 C62 . 1.477(5) ?
  C61 H61A . 0.97 ?
  C61 H61B . 0.97 ?
  C62 H62A . 0.96 ?
  C62 H62B . 0.96 ?
  C62 H62C . 0.96 ?
  C63 C64 . 1.518(6) ?
  C63 H63A . 0.97 ?
  C63 H63B . 0.97 ?
  C64 H64A . 0.96 ?
  C64 H64B . 0.96 ?
  C64 H64C . 0.96 ?
  C65 C66 . 1.495(6) ?
  C65 H65A . 0.97 ?
  C65 H65B . 0.97 ?
  C66 H66A . 0.96 ?
  C66 H66B . 0.96 ?
  C66 H66C . 0.96 ?
  C67 C68 . 1.456(5) ?
  C67 H67A . 0.97 ?
  C67 H67B . 0.97 ?
  C68 H68A . 0.96 ?
  C68 H68B . 0.96 ?
  C68 H68C . 0.96 ?
_cod_database_code 2202337