Access to Ruthenium(0) Carbonyl Complexes via Dehydrogenation of a Tricyclopentylphosphine Ligand and Decarbonylation of Alcohols
Bolton, Paul D.; Grellier, Mary; Vautravers, Nicolas; Vendier, Laure; Sabo-Etienne, Sylviane; Organometallics 27 (2008) 5088–; doi:10.1021/om8005118

data_4072005
_publ_contact_author
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_publ_section_title
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 Access to Ruthenium(0) Carbonyl Complexes via Dehydrogenation of a
 Tricyclopentylphosphine Ligand and Decarbonylation of Alcohols
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_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5088
_journal_paper_doi               10.1021/om8005118
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C31 H54 O P2 Ru'
_chemical_formula_sum            'C31 H54 O P2 Ru'
_chemical_formula_weight         605.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.27(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.835(3)
_cell_length_b                   8.3164(17)
_cell_length_c                   22.417(5)
_cell_measurement_reflns_used    6500
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.0896
_cell_measurement_theta_min      2.7492
_cell_measurement_wavelength     0.71073
_cell_volume                     2921.4(11)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0223209751
_diffrn_orient_matrix_UB_12      -0.0065410841
_diffrn_orient_matrix_UB_13      -0.0296690375
_diffrn_orient_matrix_UB_21      -0.0368784664
_diffrn_orient_matrix_UB_22      -0.0260118603
_diffrn_orient_matrix_UB_23      0.0118409678
_diffrn_orient_matrix_UB_31      -0.0136866032
_diffrn_orient_matrix_UB_32      0.0808989773
_diffrn_orient_matrix_UB_33      0.0014254881
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5937
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.263
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         5937
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+30.4568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1405
_reflns_number_gt                5015
_reflns_number_total             5937
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om8005118_si_003.cif
_cod_data_source_block           global
_cod_original_cell_volume        2921.3(10)
_cod_database_code               4072005