#------------------------------------------------------------------------------
#$Date: 2015-01-27 19:58:39 +0000 (Tue, 27 Jan 2015) $
#$Revision: 130149 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100877.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_1100877
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
;
_journal_name_full
;
  Organometallics
;
_journal_paper_doi               10.1021/om0489857
_chemical_formula_sum            'C24.5 H34 Cl Os P'
_chemical_formula_weight         585.14
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                103.7850(10)
_cell_angle_beta                 95.9700(10)
_cell_angle_gamma                91.4870(10)
_cell_formula_units_Z            2
_cell_length_a                   7.6298(5)
_cell_length_b                   11.3416(7)
_cell_length_c                   14.0086(8)
_cell_measurement_reflns_used    6550
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2.5
_cell_volume                     1169.30(12)
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14372
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    5.643
_exptl_absorpt_correction_T_max  0.526
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction performed with SADABS program. This is based on the
 method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.
 SADABS: Area-Detector Absorption Correction. Bruker-AXS
  within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         5449
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                4917
_reflns_number_total             5449
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_cif_authors_sg_H-M  P-1
_[local]_cod_chemical_formula_sum_orig 'C24.50 H34 Cl Os P'
_cod_database_code               1100877
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'