Mixed Phosphane η5-CpRuCl(PR3)2 Complexes as Ambifunctional Catalysts for Anti-Markovnikov Hydration of Terminal Alkynes
Florian Boeck; Thomas Kribber; Li Xiao; Lukas Hintermann; Journal of the American Chemical Society 133 (2011) 8138–8141; doi:10.1021/ja2026823

data_4106191
_publ_contact_author_address
;Department Chemie
Technische Universit\"at M\"unchen
Lichtenbergstrasse 4
85747 Garching bei M\"unchen
Germany
;
_publ_contact_author_email       lukas.hintermann@tum.de
_publ_contact_author_fax         49(0)8928913669
_publ_contact_author_name        'Lukas Hintermann'
_publ_contact_author_phone       49(0)8928913699
_publ_section_title
;
 Mixed Phosphane \h5-CpRuCl(PR3)2 Complexes as Ambifunctional Catalysts
 for Anti-Markovnikov Hydration of Terminal Alkynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8138
_journal_page_last               8141
_journal_paper_doi               10.1021/ja2026823
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C60 H65 F6 N2 P3 Ru'
_chemical_formula_weight         1122.12
_chemical_name_systematic
;(kN-Acetonitrile)(h5-cyclopentadienyl)(kP-2-diphenyl-
phosphanyl-6-(2,4,6-triphenylphenyl)pyridine)-
(kP-tributylphosphine)ruthenium(II) hexafluorophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 111.7290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3756(11)
_cell_length_b                   14.6058(9)
_cell_length_c                   22.0886(13)
_cell_measurement_reflns_used    5982
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      21.48
_cell_measurement_theta_min      2.29
_cell_volume                     5507.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max .966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_sigmaI/netI    0.1111
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            81939
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.29
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.9663
_exptl_absorpt_correction_T_min  0.8670
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.161
_refine_diff_density_min         -.588
_refine_diff_density_rms         .089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         16265
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1234
_reflns_number_gt                9259
_reflns_number_total             16265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2026823_si_002.cif
_cod_data_source_block           TK513_1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4106191