C−H Bond Activation of Terminal Allenes: Formation of Hydride-Alkenylcarbyne-Osmium and Disubstituted Vinylidene-Ruthenium Derivatives∥
Collado, Alba; Esteruelas, Miguel A.; López, Fernando; Mascareñas, José L.; Oñate, Enrique; Trillo, Beatriz; Organometallics 29 (2010) 4966–; doi:10.1021/om100192t

data_4065921
_publ_section_title
;
 C&#x2212;H Bond Activation of Terminal Allenes: Formation of
 Hydride-Alkenylcarbyne-Osmium and Disubstituted Vinylidene-Ruthenium
 Derivatives&#x2225;
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4966
_journal_paper_doi               10.1021/om100192t
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C24 H54 Cl2 P2 Ru Si'
_chemical_formula_weight         604.67
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.064(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.498(7)
_cell_length_b                   12.003(4)
_cell_length_c                   15.441(6)
_cell_measurement_reflns_used    2435
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3128(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.942
_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  0.0724
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18724
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.850
_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            'dark orange'
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3854
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+3.3827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                2992
_reflns_number_total             3854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100192t_si_002.cif
_cod_data_source_block           mae436bs
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4065921