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_4105494
_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            'C47 H47 F6 O1.5 P2 Ru'
_chemical_formula_weight         912.86
_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                85.489(2)
_cell_angle_beta                 75.201(2)
_cell_angle_gamma                82.549(2)
_cell_formula_units_Z            4
_cell_length_a                   13.9207(3)
_cell_length_b                   13.9477(4)
_cell_length_c                   22.7647(7)
_cell_measurement_reflns_used    14585
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.2210
_cell_measurement_theta_min      2.8159
_cell_volume                     4232.5(2)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) 
(compiled Feb 27 2009,15:38:38) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) 
(compiled Feb 27 2009,15:38:38) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) 
(compiled Feb 27 2009,15:38:38) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A'
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43601
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) 
(compiled Feb 27 2009,15:38:38) 
empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1036
_refine_ls_number_reflns         19377
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1219
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                10541
_reflns_number_total             19377
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906745j_si_003.cif
_cod_data_source_block           ic13727
_cod_original_formula_sum        'C47 H47 F6 O1.50 P2 Ru'
_cod_database_code               4105494