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_4066681
_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            'C23 H38 B N6 Os P'
_chemical_formula_weight         630.57
_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                89.467(5)
_cell_angle_beta                 77.641(3)
_cell_angle_gamma                78.370(3)
_cell_formula_units_Z            2
_cell_length_a                   8.2181(15)
_cell_length_b                   8.7108(15)
_cell_length_c                   19.098(4)
_cell_measurement_reflns_used    1715
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     1307.2(4)
_computing_cell_refinement       'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.1 (Bruker AXS, 2000)'
_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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_sigmaI/netI    0.1046
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17539
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.79
_diffrn_reflns_theta_min         1.09
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.960
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.60
_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            orange
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.493
_refine_diff_density_min         -1.446
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         6231
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+4.2349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                4848
_reflns_number_total             6231
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100568r_si_001.cif
_cod_data_source_block           mae455cs
_cod_original_cell_volume        1307.3(4)
_cod_database_code               4066681