Reactivity of the α-Agostic Methyl Bridge in the Unsaturated Complex [Mo2(η5-C5H5)2(μ-η1:η2-CH3)(μ-PCy2)(CO)2]: Migratory Behavior and Methylidyne Derivatives
Alvarez, M. Angeles; García-Vivó, Daniel; García, M. Esther; Martínez, M. Eugenia; Ramos, Alberto; Ruiz, Miguel A.; Organometallics 27 (2008) 1973–; doi:10.1021/om800061z

data_4071254
_publ_section_title
;
 Reactivity of the \a-Agostic Methyl Bridge in the Unsaturated Complex
 [Mo2(\h5-C5H5)2(\m-\h1:\h2-CH3)(\m-PCy2)(CO)2]: Migratory Behavior and
 Methylidyne Derivatives
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1973
_journal_paper_doi               10.1021/om800061z
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '2(C31 H33 Fe2 Mo2 O8 P), C7 H8'
_chemical_formula_sum            'C69 H74 Fe4 Mo4 O16 P2'
_chemical_formula_weight         1828.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 119.2620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3752(2)
_cell_length_b                   11.7509(2)
_cell_length_c                   25.3894(4)
_cell_measurement_reflns_used    6536
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.407
_cell_measurement_wavelength     0.71073
_cell_volume                     3481.26(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor, 1997) 
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '90 mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26616
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    1.617
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.7215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.353
_refine_diff_density_min         -2.155
_refine_diff_density_rms         0.412
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         6292
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.19
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+16.3131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                5368
_reflns_number_total             6292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800061z-file004.cif
_cod_data_source_block           compound7
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4071254