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#$Date: 2012-02-24 19:13:23 +0200 (Fri, 24 Feb 2012) $
#$Revision: 34330 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/02/4060293.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_4060293
_journal_name_full  'Organometallics'
_journal_year       2005
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            'C24.5 H34 Cl Os P'
_[local]_cod_chemical_formula_sum_orig 'C24.50 H34 Cl Os P'
_chemical_formula_weight  585.14
_symmetry_cell_setting  'triclinic'
_symmetry_space_group_name_H-M  'P -1'
loop_
_symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
_cell_length_a  7.6298(5)
_cell_length_b  11.3416(7)
_cell_length_c  14.0086(8)
_cell_angle_alpha  103.7850(10)
_cell_angle_beta  95.9700(10)
_cell_angle_gamma  91.4870(10)
_cell_volume  1169.30(12)
_cell_formula_units_Z  2
_cell_measurement_temperature  100(2)
_exptl_crystal_density_diffrn  1.662
_diffrn_ambient_temperature  100(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 0.21702(2) 0.115328(15) 0.188806(12) 0.02046(6) Uani 1 1 d . A .
Cl Cl -0.05632(13) 0.21374(11) 0.19494(9) 0.0330(3) Uani 1 1 d . . .
P P 0.29625(14) 0.21829(10) 0.35097(8) 0.0217(2) Uani 1 1 d . . .
C1 C 0.1706(5) -0.0208(4) 0.2307(3) 0.0267(10) Uani 1 1 d . . .
C2 C 0.1558(6) -0.1289(4) 0.2511(3) 0.0270(10) Uani 1 1 d . A .
H2 H 0.258(5) -0.162(4) 0.275(3) 0.026(12) Uiso 1 1 d . . .
C3 C -0.0080(6) -0.2020(4) 0.2425(3) 0.0257(9) Uani 1 1 d . . .
C4 C -0.0036(6) -0.3209(4) 0.2531(4) 0.0365(11) Uani 1 1 d . A .
H4 H 0.1071 -0.3525 0.2685 0.044 Uiso 1 1 calc R . .
C5 C -0.1551(7) -0.3941(5) 0.2419(4) 0.0438(13) Uani 1 1 d . . .
H5 H -0.1478 -0.4755 0.2483 0.053 Uiso 1 1 calc R A .
C6 C -0.3145(7) -0.3497(4) 0.2218(4) 0.0386(12) Uani 1 1 d . A .
H6 H -0.4192 -0.3997 0.2146 0.046 Uiso 1 1 calc R . .
C7 C -0.3246(6) -0.2314(4) 0.2116(3) 0.0353(11) Uani 1 1 d . . .
H7 H -0.4364 -0.2004 0.1976 0.042 Uiso 1 1 calc R A .
C8 C -0.1731(6) -0.1583(4) 0.2218(3) 0.0288(10) Uani 1 1 d . A .
H8 H -0.1815 -0.0774 0.2146 0.035 Uiso 1 1 calc R . .
C9 C 0.3958(6) 0.3734(4) 0.3707(3) 0.0307(10) Uani 1 1 d . A .
H9 H 0.4042 0.4116 0.4433 0.037 Uiso 1 1 calc R . .
C10 C 0.5802(6) 0.3759(4) 0.3413(4) 0.0367(11) Uani 1 1 d . . .
H10A H 0.5771 0.3398 0.2702 0.055 Uiso 1 1 calc R A .
H10B H 0.6555 0.3293 0.3781 0.055 Uiso 1 1 calc R . .
H10C H 0.6278 0.4602 0.3564 0.055 Uiso 1 1 calc R . .
C11 C 0.2792(6) 0.4513(4) 0.3186(4) 0.0359(11) Uani 1 1 d . . .
H11A H 0.3328 0.5340 0.3331 0.054 Uiso 1 1 calc R A .
H11B H 0.1624 0.4537 0.3420 0.054 Uiso 1 1 calc R . .
H11C H 0.2673 0.4162 0.2470 0.054 Uiso 1 1 calc R . .
C12 C 0.4598(6) 0.1448(4) 0.4204(3) 0.0308(10) Uani 1 1 d . A .
C13 C 0.5265(7) 0.2130(5) 0.5243(3) 0.0395(12) Uani 1 1 d . . .
H13A H 0.6102 0.1640 0.5539 0.059 Uiso 1 1 calc R A .
H13B H 0.4271 0.2291 0.5637 0.059 Uiso 1 1 calc R . .
H13C H 0.5858 0.2902 0.5230 0.059 Uiso 1 1 calc R . .
C14 C 0.5561(9) 0.0586(6) 0.3720(5) 0.062(2) Uani 1 1 d . . .
H14A H 0.633(6) 0.025(4) 0.406(3) 0.033(13) Uiso 1 1 d . . .
H14B H 0.525(6) 0.019(4) 0.308(4) 0.040(14) Uiso 1 1 d . . .
C15A C 0.1031(12) 0.2385(7) 0.4241(6) 0.029(2) Uiso 0.74(2) 1 d PD A 1
C16A C 0.1074(13) 0.3494(7) 0.5059(7) 0.043(2) Uiso 0.74(2) 1 d PD A 1
C17A C 0.0602(12) 0.1193(6) 0.4564(7) 0.038(2) Uiso 0.74(2) 1 d PD A 1
C15B C 0.141(3) 0.2328(17) 0.4438(18) 0.029(6) Uiso 0.26(2) 1 d PD A 2
C16B C -0.001(2) 0.1307(14) 0.4257(14) 0.021(5) Uiso 0.26(2) 1 d PD A 2
C17B C 0.061(3) 0.3526(15) 0.4801(18) 0.030(6) Uiso 0.26(2) 1 d PD A 2
C18 C 0.3838(5) 0.0102(4) 0.0844(3) 0.0278(10) Uani 1 1 d . . .
H18 H 0.4209 -0.0667 0.0920 0.033 Uiso 1 1 calc R A .
C19 C 0.2329(6) 0.0301(4) 0.0247(3) 0.0316(11) Uani 1 1 d . A .
H19 H 0.1496 -0.0303 -0.0148 0.038 Uiso 1 1 calc R . .
C20 C 0.2289(6) 0.1560(5) 0.0347(3) 0.0352(11) Uani 1 1 d . . .
H20 H 0.1398 0.1955 0.0034 0.042 Uiso 1 1 calc R A .
C21 C 0.3757(6) 0.2148(4) 0.0978(3) 0.0337(11) Uani 1 1 d . A .
H21 H 0.4055 0.2996 0.1149 0.040 Uiso 1 1 calc R . .
C22 C 0.4716(5) 0.1247(4) 0.1315(3) 0.0305(10) Uani 1 1 d . A .
H22 H 0.5756 0.1381 0.1771 0.037 Uiso 1 1 calc R . .
C23 C 1.0000 0.5000 1.0000 0.076(3) Uiso 1 2 d SD . .
C24A C 0.8086(11) 0.4667(9) 0.9757(8) 0.046(3) Uiso 0.50 1 d PD . .
C25A C 0.7210(15) 0.3524(10) 0.9864(9) 0.049(3) Uiso 0.50 1 d PD . .
C24B C 0.8933(13) 0.3982(10) 1.0005(10) 0.065(3) Uiso 0.50 1 d PD . .
C25B C 0.7014(15) 0.4031(14) 0.9694(10) 0.063(4) Uiso 0.50 1 d PD . .
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 0.01852(9) 0.02152(10) 0.02139(9) 0.00522(6) 0.00296(6) -0.00098(6)
Cl 0.0207(5) 0.0354(6) 0.0418(7) 0.0086(5) -0.0001(5) 0.0041(4)
P 0.0248(5) 0.0176(5) 0.0230(6) 0.0046(4) 0.0051(4) -0.0002(4)
C1 0.019(2) 0.033(3) 0.023(2) -0.0024(19) -0.0001(17) -0.0023(18)
C2 0.029(2) 0.023(2) 0.030(2) 0.0072(19) 0.0053(19) 0.0032(19)
C3 0.034(2) 0.021(2) 0.023(2) 0.0051(18) 0.0082(18) -0.0002(18)
C4 0.038(3) 0.032(3) 0.044(3) 0.016(2) 0.007(2) 0.005(2)
C5 0.051(3) 0.028(3) 0.056(3) 0.017(3) 0.009(3) -0.004(2)
C6 0.042(3) 0.031(3) 0.044(3) 0.009(2) 0.010(2) -0.009(2)
C7 0.032(2) 0.036(3) 0.038(3) 0.009(2) 0.004(2) -0.001(2)
C8 0.033(2) 0.024(2) 0.031(2) 0.009(2) 0.007(2) 0.0009(19)
C9 0.039(3) 0.020(2) 0.031(2) 0.0041(19) 0.002(2) -0.0065(19)
C10 0.039(3) 0.027(3) 0.043(3) 0.008(2) 0.006(2) -0.010(2)
C11 0.050(3) 0.020(2) 0.039(3) 0.010(2) 0.007(2) 0.000(2)
C12 0.036(3) 0.033(3) 0.025(2) 0.010(2) 0.0004(19) 0.005(2)
C13 0.047(3) 0.037(3) 0.031(3) 0.007(2) -0.008(2) -0.003(2)
C14 0.078(5) 0.050(4) 0.044(4) -0.004(3) -0.030(3) 0.032(3)
C18 0.029(2) 0.032(3) 0.022(2) 0.0027(19) 0.0098(18) 0.0035(19)
C19 0.026(2) 0.045(3) 0.020(2) 0.000(2) 0.0048(18) -0.004(2)
C20 0.038(3) 0.050(3) 0.024(2) 0.018(2) 0.010(2) 0.007(2)
C21 0.045(3) 0.031(3) 0.029(2) 0.010(2) 0.017(2) -0.006(2)
C22 0.020(2) 0.043(3) 0.027(2) 0.005(2) 0.0077(18) -0.0052(19)
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 C1 1.817(5) . ?
Os C22 2.188(4) . ?
Os C18 2.195(4) . ?
Os C19 2.289(4) . ?
Os C21 2.302(4) . ?
Os P 2.3028(11) . ?
Os C20 2.322(4) . ?
Os Cl 2.3906(10) . ?
P C15B 1.83(2) . ?
P C12 1.840(4) . ?
P C9 1.845(4) . ?
P C15A 1.869(8) . ?
C1 C2 1.328(6) . ?
C2 C3 1.460(6) . ?
C2 H2 0.94(4) . ?
C3 C4 1.392(6) . ?
C3 C8 1.394(6) . ?
C4 C5 1.379(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.357(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.379(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.508(6) . ?
C9 C11 1.523(6) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.334(7) . ?
C12 C13 1.505(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.87(5) . ?
C14 H14B 0.90(5) . ?
C15A C16A 1.483(10) . ?
C15A C17A 1.562(11) . ?
C15B C17B 1.503(19) . ?
C15B C16B 1.521(19) . ?
C18 C19 1.407(6) . ?
C18 C22 1.423(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.403(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.398(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.413(6) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24B 1.398(9) 2_767 ?
C23 C24B 1.398(9) . ?
C23 C24A 1.483(8) 2_767 ?
C23 C24A 1.483(8) . ?
C24A C25B 1.059(14) . ?
C24A C24B 1.119(15) . ?
C24A C25A 1.490(9) . ?
C25A C25B 0.687(16) . ?
C25A C24B 1.378(14) . ?
C24B C25B 1.490(10) . ?
_cod_database_code 4060293