#------------------------------------------------------------------------------
#$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/4060292.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_4060292
_journal_name_full  'Organometallics'
_journal_year       2005
_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
  'Baya, M.'
  'Buil, M. L.'
  'Esteruelas, M. A.'
  'O\~nate, E.'
_publ_section_title
;
Ene-type reactions between an a-alkenylphosphine and terminal
alkynes promoted by osmium-cyclopentadienyl fragments
;
_chemical_formula_sum 'C22 H30 Cl Os P'
_chemical_formula_weight  551.08
_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  12.3343(10)
_cell_length_b  12.6118(10)
_cell_length_c  13.4358(11)
_cell_angle_alpha  90.00
_cell_angle_beta  95.913(2)
_cell_angle_gamma  90.00
_cell_volume  2078.9(3)
_cell_formula_units_Z  4
_cell_measurement_temperature  296(2)
_exptl_crystal_density_diffrn  1.761
_diffrn_ambient_temperature  296(2)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Os Os 0.840105(14) 0.216209(14) 0.836456(14) 0.03316(6) Uani 1 1 d . . .
Cl Cl 0.88837(10) 0.40251(9) 0.83097(9) 0.0497(3) Uani 1 1 d . . .
P P 0.75584(9) 0.25483(9) 0.97695(9) 0.0375(3) Uani 1 1 d . . .
C1 C 0.6197(3) 0.2903(4) 0.9243(3) 0.0423(12) Uani 1 1 d . . .
C2 C 0.5825(4) 0.2051(5) 0.8499(4) 0.0486(14) Uani 1 1 d . . .
H2A H 0.563(3) 0.134(3) 0.894(3) 0.052(14) Uiso 1 1 d . . .
H2B H 0.514(3) 0.223(3) 0.810(3) 0.048(13) Uiso 1 1 d . . .
C3 C 0.6697(4) 0.1820(4) 0.7798(3) 0.0368(12) Uani 1 1 d . . .
H3 H 0.671(3) 0.109(3) 0.753(3) 0.045(14) Uiso 1 1 d . . .
C4 C 0.7101(3) 0.2659(4) 0.7234(3) 0.0343(12) Uani 1 1 d . . .
H4 H 0.686(3) 0.326(3) 0.738(3) 0.022(12) Uiso 1 1 d . . .
C5 C 0.7370(3) 0.2573(3) 0.6206(3) 0.0367(12) Uani 1 1 d . . .
C6 C 0.7126(4) 0.1689(4) 0.5609(3) 0.0465(13) Uani 1 1 d . . .
H6 H 0.6770 0.1117 0.5867 0.056 Uiso 1 1 calc R . .
C7 C 0.7403(4) 0.1640(4) 0.4635(4) 0.0588(15) Uani 1 1 d . . .
H7 H 0.7232 0.1039 0.4248 0.071 Uiso 1 1 calc R . .
C8 C 0.7928(4) 0.2471(4) 0.4242(4) 0.0583(16) Uani 1 1 d . . .
H8 H 0.8120 0.2434 0.3591 0.070 Uiso 1 1 calc R . .
C9 C 0.8173(4) 0.3366(4) 0.4815(4) 0.0546(14) Uani 1 1 d . . .
H9 H 0.8522 0.3938 0.4550 0.065 Uiso 1 1 calc R . .
C10 C 0.7897(4) 0.3406(4) 0.5784(3) 0.0489(14) Uani 1 1 d . . .
H10 H 0.8069 0.4009 0.6166 0.059 Uiso 1 1 calc R . .
C11 C 0.5697(5) 0.3796(5) 0.9332(5) 0.0592(17) Uani 1 1 d . . .
H11A H 0.598(3) 0.433(3) 0.972(3) 0.042(16) Uiso 1 1 d . . .
H11B H 0.505(3) 0.397(3) 0.892(3) 0.040(13) Uiso 1 1 d . . .
C12 C 0.7317(4) 0.1366(3) 1.0554(3) 0.0472(13) Uani 1 1 d . . .
H12 H 0.7185 0.0781 1.0077 0.057 Uiso 1 1 calc R . .
C13 C 0.6300(4) 0.1410(4) 1.1112(3) 0.0656(16) Uani 1 1 d . . .
H13A H 0.6090 0.0704 1.1276 0.098 Uiso 1 1 calc R . .
H13B H 0.5717 0.1741 1.0696 0.098 Uiso 1 1 calc R . .
H13C H 0.6454 0.1814 1.1716 0.098 Uiso 1 1 calc R . .
C14 C 0.8321(4) 0.1036(4) 1.1237(3) 0.0695(17) Uani 1 1 d . . .
H14A H 0.8397 0.1484 1.1817 0.104 Uiso 1 1 calc R . .
H14B H 0.8956 0.1102 1.0884 0.104 Uiso 1 1 calc R . .
H14C H 0.8244 0.0312 1.1440 0.104 Uiso 1 1 calc R . .
C15 C 0.8073(4) 0.3652(3) 1.0594(3) 0.0463(13) Uani 1 1 d . . .
H15 H 0.7948 0.4295 1.0189 0.056 Uiso 1 1 calc R . .
C16 C 0.7483(4) 0.3837(4) 1.1519(3) 0.0709(18) Uani 1 1 d . . .
H16A H 0.7619 0.3252 1.1972 0.106 Uiso 1 1 calc R . .
H16B H 0.6714 0.3895 1.1325 0.106 Uiso 1 1 calc R . .
H16C H 0.7744 0.4480 1.1842 0.106 Uiso 1 1 calc R . .
C17 C 0.9311(4) 0.3593(4) 1.0860(3) 0.0690(17) Uani 1 1 d . . .
H17A H 0.9558 0.4220 1.1219 0.104 Uiso 1 1 calc R . .
H17B H 0.9664 0.3541 1.0257 0.104 Uiso 1 1 calc R . .
H17C H 0.9487 0.2980 1.1269 0.104 Uiso 1 1 calc R . .
C18 C 0.9057(4) 0.0602(4) 0.8757(4) 0.0532(14) Uani 1 1 d . . .
H18 H 0.8716 0.0161 0.9184 0.064 Uiso 1 1 calc R . .
C19 C 0.9898(4) 0.1328(4) 0.9042(4) 0.0484(14) Uani 1 1 d . . .
H19 H 1.0214 0.1458 0.9688 0.058 Uiso 1 1 calc R . .
C20 C 1.0173(4) 0.1823(4) 0.8151(4) 0.0524(14) Uani 1 1 d . . .
H20 H 1.0711 0.2335 0.8122 0.063 Uiso 1 1 calc R . .
C21 C 0.9512(4) 0.1424(4) 0.7325(4) 0.0472(13) Uani 1 1 d . . .
H21 H 0.9524 0.1620 0.6659 0.057 Uiso 1 1 calc R . .
C22 C 0.8824(4) 0.0664(4) 0.7711(4) 0.0538(15) Uani 1 1 d . . .
H22 H 0.8298 0.0266 0.7331 0.065 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Os 0.03366(10) 0.03158(10) 0.03445(10) -0.00006(11) 0.00445(7) 0.00095(11)
Cl 0.0605(9) 0.0351(7) 0.0533(9) 0.0003(6) 0.0042(7) -0.0115(6)
P 0.0422(8) 0.0361(8) 0.0346(7) -0.0007(6) 0.0059(6) 0.0007(6)
C1 0.039(3) 0.047(3) 0.042(3) 0.001(3) 0.010(2) 0.002(3)
C2 0.039(3) 0.061(4) 0.046(3) -0.001(3) 0.003(3) -0.007(3)
C3 0.032(3) 0.042(3) 0.036(3) -0.002(2) 0.002(2) 0.000(2)
C4 0.029(3) 0.033(3) 0.040(3) -0.008(2) 0.000(2) 0.004(2)
C5 0.028(3) 0.040(3) 0.040(3) 0.009(2) -0.005(2) 0.001(2)
C6 0.050(3) 0.047(3) 0.042(3) 0.002(3) 0.005(3) -0.005(3)
C7 0.083(4) 0.060(4) 0.034(3) -0.004(3) 0.006(3) 0.009(3)
C8 0.072(4) 0.064(4) 0.041(3) 0.014(3) 0.014(3) 0.020(3)
C9 0.059(4) 0.058(4) 0.047(4) 0.018(3) 0.003(3) -0.004(3)
C10 0.058(4) 0.052(3) 0.037(3) 0.009(3) 0.007(3) 0.001(3)
C11 0.047(4) 0.068(5) 0.062(5) -0.005(4) 0.001(3) 0.015(4)
C12 0.062(4) 0.034(3) 0.048(3) 0.004(2) 0.015(3) 0.004(3)
C13 0.081(4) 0.065(4) 0.057(4) 0.004(3) 0.032(3) 0.000(3)
C14 0.093(5) 0.067(4) 0.050(4) 0.020(3) 0.015(3) 0.023(3)
C15 0.064(4) 0.041(3) 0.034(3) -0.009(2) 0.007(3) 0.000(3)
C16 0.114(5) 0.061(4) 0.040(4) -0.016(3) 0.022(3) -0.009(3)
C17 0.060(4) 0.090(4) 0.053(4) -0.011(3) -0.016(3) -0.020(3)
C18 0.061(4) 0.045(3) 0.057(4) -0.002(3) 0.023(3) 0.008(3)
C19 0.045(3) 0.054(4) 0.047(4) -0.004(3) 0.003(3) 0.017(3)
C20 0.031(3) 0.059(4) 0.069(4) -0.005(3) 0.014(3) 0.011(3)
C21 0.041(3) 0.059(4) 0.043(3) 0.000(3) 0.006(3) 0.013(3)
C22 0.054(4) 0.035(3) 0.072(4) -0.010(3) 0.005(3) -0.001(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Os C22 2.170(4) . ?
Os C18 2.171(5) . ?
Os C4 2.184(4) . ?
Os C3 2.203(4) . ?
Os C19 2.236(4) . ?
Os C21 2.256(4) . ?
Os C20 2.274(4) . ?
Os P 2.2990(12) . ?
Os Cl 2.4268(11) . ?
P C1 1.810(4) . ?
P C15 1.850(4) . ?
P C12 1.867(4) . ?
C1 C11 1.296(6) . ?
C1 C2 1.506(6) . ?
C2 C3 1.529(6) . ?
C2 H2A 1.11(4) . ?
C2 H2B 0.98(3) . ?
C3 C4 1.421(6) . ?
C3 H3 0.99(3) . ?
C4 C5 1.456(6) . ?
C4 H4 0.85(3) . ?
C5 C10 1.387(5) . ?
C5 C6 1.389(5) . ?
C6 C7 1.388(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.367(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.383(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.380(6) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11A 0.90(4) . ?
C11 H11B 0.95(4) . ?
C12 C14 1.522(6) . ?
C12 C13 1.528(5) . ?
C12 H12 0.9800 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.522(5) . ?
C15 C17 1.533(6) . ?
C15 H15 0.9800 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.406(6) . ?
C18 C22 1.408(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.421(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.400(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.414(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
_cod_database_code 4060292