Reactions of Ruthenium Cp Phosphine Complex with 4,4-Disubstituted-1,6-Enynes: Effect of Methyl Substituents in the Olefinic Fraction
Chia-Pei Chung; Chien-Chih Chen; Ying-Chih Lin; Yi-Hong Liu; Yu Wang; Journal of the American Chemical Society 131 (2009) 18366–18375; doi:10.1021/ja906745j

data_4105496
_publ_section_title
;
 Reactions of Ruthenium Cp Phosphine Complex with
 4,4-Disubstituted-1,6-Enynes: Effect of Methyl Substituents in the
 Olefinic Fraction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18366
_journal_page_last               18375
_journal_paper_doi               10.1021/ja906745j
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C62 H57 F6 P3 Ru'
_chemical_formula_weight         1110.06
_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                72.6340(10)
_cell_angle_beta                 81.477(2)
_cell_angle_gamma                74.8460(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0106(2)
_cell_length_b                   13.8053(3)
_cell_length_c                   20.7787(4)
_cell_measurement_reflns_used    99088
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2637.72(9)
_computing_cell_refinement       'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_data_collection       'COLLECT (Nonius BV)'
_computing_data_reduction        'HKL Denzo & Scalepack (Otwinowski & Minor)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0860
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51129
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.449
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995) 
;
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.0088(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         12039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+3.5107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1873
_reflns_number_gt                8452
_reflns_number_total             12039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906745j_si_005.cif
_cod_data_source_block           ic13887
_cod_database_code               4105496