Four-Electron-Donor Hemilabile η3-PPh3Ligand that Binds through a CC Bond Rather than an Agostic C−H Interaction, and Displacement of the CC by Methyl Iodide or Water
Cheng, Tan-Yun; Szalda, David J.; Hanson, Jonathan C.; Muckerman, James T.; Bullock, R. Morris; Organometallics 27 (2008) 3785–; doi:10.1021/om800401d

data_4071809
_publ_section_title
;
 Four-Electron-Donor Hemilabile \h3-PPh3Ligand that Binds through a
 C&#xE5FB;C Bond Rather than an Agostic C&#x2212;H Interaction, and
 Displacement of the C&#xE5FB;C by Methyl Iodide or Water
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3785
_journal_paper_doi               10.1021/om800401d
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        CH3C6H5/CH2Cl2/C6H14
_chemical_formula_moiety
;
(C25 H22 O3 P1 Mo1 1+), (C32 H12 B1 F24 1-), (C7H8)
;
_chemical_formula_structural
;
(Mo (C5 H5) (CO)2 (H2O) (P (C6 H5)3))(B C32 H12 F24) (C6H5CH3)
;
_chemical_formula_sum            'C64 H42 B F24 Mo O3 P'
_chemical_formula_weight         1452.70
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                69.08(2)
_cell_angle_beta                 72.550(10)
_cell_angle_gamma                82.62(2)
_cell_formula_units_Z            2
_cell_length_a                   13.792(4)
_cell_length_b                   15.032(6)
_cell_length_c                   16.414(7)
_cell_measurement_temperature    95(2)
_cell_volume                     3031(2)
_computing_cell_refinement
;
average of cell contants determined on each image plate
;
_computing_data_collection
;
see M.J. Gray etal for a description of data collection at beamline x7b
;
_computing_data_reduction        'DENZO, SCALEPACK (Otwinowski)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELX76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      95(2)
_diffrn_measurement_device       Huber
_diffrn_measurement_method       'Fuji image plates'
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source
;
National Synchrotron Light Source beamline x7b
;
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.008
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17076
_diffrn_reflns_theta_max         38.43
_diffrn_reflns_theta_min         3.67
_exptl_absorpt_coefficient_mu    9.53
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0064(9)
_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_all   1.112
_refine_ls_goodness_of_fit_obs   1.174
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         6722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_restrained_S_obs      1.174
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_obs          0.0689
_refine_ls_shift/esd_max         -0.050
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1608P)^2^+1.1360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2409
_refine_ls_wR_factor_obs         0.2088
_reflns_number_observed          5253
_reflns_number_total             6736
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om800401d-file004.cif
_cod_data_source_block           mopbzig4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1608P)^2^+1.1360P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1608P)^2^+1.1360P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3031.5(20)
_cod_database_code               4071809