Synthesis and Reactions of Diphosphinidenecyclobutene Ruthenium Complexes Relevant to Catalytic Hydrosilylation of Terminal Alkynes
Hayashi, Akito; Yoshitomi, Takahiko; Umeda, Kazutoshi; Okazaki, Masaaki; Ozawa, Fumiyuki; Organometallics 27 (2008) 2321–; doi:10.1021/om800119f

data_4071341
_publ_section_title
;
 Synthesis and Reactions of Diphosphinidenecyclobutene Ruthenium Complexes
 Relevant to Catalytic Hydrosilylation of Terminal Alkynes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2321
_journal_paper_doi               10.1021/om800119f
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C56 H76 Cl4 O4 P2 Ru'
_chemical_formula_sum            'C56 H76 Cl4 O4 P2 Ru'
_chemical_formula_weight         1117.98
_chemical_melting_point          528
_chemical_name_common            'complex 8a'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                81.08(11)
_cell_angle_beta                 64.64(9)
_cell_angle_gamma                71.75(10)
_cell_formula_units_Z            2
_cell_length_a                   14.556(15)
_cell_length_b                   14.86(2)
_cell_length_c                   15.45(2)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.15
_cell_volume                     2867(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  RigakuMercuryCCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22289
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.9727
_exptl_absorpt_correction_T_min  0.9464
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.167
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         12235
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2292
_refine_ls_wR_factor_ref         0.3074
_reflns_number_gt                8335
_reflns_number_total             12235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800119f-file003.cif
_cod_data_source_block           ruoh2
_cod_original_cell_volume        2869(6)
_cod_database_code               4071341