P−C Bond Splitting Reactions in Ruthenium(II) Complexes of Binap and MeO−Biphep Using CF3SO3H and HBF4. A Novel Ru−F−H Interaction
den Reijer, Carolien J.; Wörle, Michael; Pregosin, Paul S.; Organometallics 19 (2000) 309–; doi:10.1021/om990714m

data_4077673
_publ_contact_author
;
 Pregosin, Paul S.
 Laboratory of Inorganic Chemistry,
 Universit\"atstr. 6
 CH-8092 Z\"urich,
 Switzerland
;
_publ_section_title
;
 P&#x2212;C Bond Splitting Reactions in Ruthenium(II) Complexes of Binap
 and MeO&#x2212;Biphep Using CF3SO3H and HBF4. A Novel
 Ru&#x2212;F&#x2212;H Interaction
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              309
_journal_paper_doi               10.1021/om990714m
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C46.73 H34 F6 O7 P2 Ru S2'
_chemical_formula_weight         1048.66
_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                108.20(3)
_cell_angle_beta                 103.14(3)
_cell_angle_gamma                94.34(3)
_cell_formula_units_Z            4
_cell_length_a                   15.099(2)
_cell_length_b                   16.131(2)
_cell_length_c                   19.817(3)
_cell_measurement_reflns_used    6196
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      49.5
_cell_measurement_theta_min      3
_cell_volume                     4408.7(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SMART PLATFORM, CCD Detector'
_diffrn_measurement_method       '\w scans'
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0926
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24430
_diffrn_reflns_theta_full        24.74
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.9535
_exptl_absorpt_correction_T_min  0.7533
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Program Sadabs, G. Sheldrick, 1997, G\"ottingen'
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2122
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1156
_refine_ls_number_reflns         14887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          1.444
_refine_ls_shift/su_mean         0.021
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                9843
_reflns_number_total             14887
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990714m.cif
_cod_data_source_block           7a
_cod_original_cell_volume        4408.7(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077673