Ruthenium Complexes of Six-Electron-Donor NUPHOS-Type Diphosphines: Highly Selective Catalysts for the Hydrocarboxylation of Terminal Alkynes
Doherty, Simon; Knight, Julian G.; Rath, Rakesh K.; Clegg, William; Harrington, Ross W.; Newman, Colin R.; Campbell, Robert; Amin, Hiren; Organometallics 24 (2005) 2633–2644; doi:10.1021/om050014j

data_4060499
_publ_section_title
;
Ruthenium Complexes of Six-Electron-Donor NUPHOS-Type Diphosphines: 
Highly Selective Catalysts for the Hydrocarboxylation of Terminal Alkynes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2633
_journal_page_last               2644
_journal_paper_doi               10.1021/om050014j
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         '2 C46 H42 P2 Cl Ru +, 2 Sb F6 -, 4 C H2 Cl2'
_chemical_formula_sum            'C96 H92 Cl10 F12 P4 Ru2 Sb2'
_chemical_formula_weight         2397.72
_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                97.429(1)
_cell_angle_beta                 94.401(2)
_cell_angle_gamma                111.458(1)
_cell_formula_units_Z            2
_cell_length_a                   14.7948(13)
_cell_length_b                   17.8716(15)
_cell_length_c                   19.9255(17)
_cell_measurement_reflns_used    18587
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.28
_cell_volume                     4818.0(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1251
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34203
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.04
_diffrn_standards_decay_%        .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.7845
_exptl_absorpt_correction_T_min  0.7009
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ornage
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.290
_refine_diff_density_min         -1.682
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1167
_refine_ls_number_reflns         34205
_refine_ls_number_restraints     803
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+11.0635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2019
_reflns_number_gt                21606
_reflns_number_total             34205
_reflns_threshold_expression     I>2\s(I)
_cod_database_code               4060499