Selective Hydrogenation of Ruthenium Acylphosphine Complexes
Gowrisankar, Saravanan; Neumann, Helfried; Spannenberg, Anke; Beller, Matthias; Organometallics 33 (2014) 94–; doi:10.1021/om4008086

data_4082614
_publ_section_title
;
 Selective Hydrogenation of Ruthenium Acylphosphine Complexes
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              94
_journal_paper_doi               10.1021/om4008086
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C26.5 H36.5 Cl6.5 O P Ru'
_chemical_formula_weight         733.52
_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                94.309(2)
_cell_angle_beta                 97.282(2)
_cell_angle_gamma                115.195(2)
_cell_formula_units_Z            4
_cell_length_a                   14.6405(5)
_cell_length_b                   15.2404(5)
_cell_length_c                   16.8663(6)
_cell_measurement_reflns_used    9285
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      2.46
_cell_volume                     3342.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            75677
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Contributions of further disordered solvent were removed from 
the diffraction data with PLATON / SQUEEZE (van der Sluis & Spek, 
1990; Spek, 2009).
;
_refine_diff_density_max         2.709
_refine_diff_density_min         -1.854
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         15344
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0700P)^2^+8.0383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1474
_reflns_number_gt                12152
_reflns_number_total             15344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4008086_si_003.cif
_cod_data_source_block           ax0274
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C26.50 H36.50 Cl6.50 O P Ru'
_cod_database_code               4082614