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_4071253
_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         'C30 H33 Mo3 O7 P1'
_chemical_formula_sum            'C30 H33 Mo3 O7 P'
_chemical_formula_weight         824.35
_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                 95.8950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0881(2)
_cell_length_b                   15.5800(3)
_cell_length_c                   19.2306(4)
_cell_measurement_reflns_used    8552
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.18
_cell_measurement_theta_min      2.41
_cell_measurement_wavelength     0.71073
_cell_volume                     3006.54(10)
_computing_cell_refinement       'BRUKER APEX'
_computing_data_collection       'BRUKER APEX'
_computing_data_reduction        'Bruker Smart'
_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    'DIRDIF (1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_radiation_monochromator  graphite
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40789
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.331
_exptl_absorpt_correction_T_max  0.9487
_exptl_absorpt_correction_T_min  0.8153
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER Sadabs'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       neddle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         9184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+1.7084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                7229
_reflns_number_total             9500
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800061z-file004.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_monochromador' tag replaced with
'_diffrn_radiation_monochromator'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_database_code               4071253