C−H Bond Activation Reactions in π-Allene−Osmium−Triisopropylphosphine Complexes with Cyclopentadienyl or Hydridotris(pyrazolyl)borate Ligands: Formation of Isopropenyldiisopropylphosphine versus Hydride−Alkenylcarbyne Derivatives
Castro-Rodrigo, Ruth; Esteruelas, Miguel A.; López, Ana M.; Mozo, Silvia; Oñate, Enrique; Organometallics 29 (2010) 4071–; doi:10.1021/om100568r

data_4066678
_publ_section_title
;
 C&#x2212;H Bond Activation Reactions in
 \p-Allene&#x2212;Osmium&#x2212;Triisopropylphosphine Complexes with
 Cyclopentadienyl or Hydridotris(pyrazolyl)borate Ligands: Formation of
 Isopropenyldiisopropylphosphine versus Hydride&#x2212;Alkenylcarbyne
 Derivatives
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4071
_journal_paper_doi               10.1021/om100568r
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C24 H45 Cl2 F6 N Os P2 Si'
_chemical_formula_weight         812.74
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.589(6)
_cell_angle_beta                 72.938(11)
_cell_angle_gamma                87.127(7)
_cell_formula_units_Z            2
_cell_length_a                   10.3264(15)
_cell_length_b                   12.0488(6)
_cell_length_c                   13.6302(15)
_cell_measurement_reflns_used    3634
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.3668
_cell_measurement_theta_min      2.7468
_cell_volume                     1619.2(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
;
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3990
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type
;
Oxford Diffraction Excalibur (TM) single-crystal X-ray diffractometer
with Sapphire CCD detector
;
_diffrn_measurement_method
;
Rotation method data acquisition using \w 
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1633
_diffrn_reflns_av_sigmaI/netI    0.3267
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            33636
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    4.289
_exptl_absorpt_correction_T_max  0.9191
_exptl_absorpt_correction_T_min  0.6498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.19 (release 28-02-2008 CrysAlis171 .NET)
(compiled Feb 28 2008,12:10:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.284
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.702
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         7375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.702
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                3519
_reflns_number_total             7375
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100568r_si_001.cif
_cod_data_source_block           est6
_cod_database_code               4066678