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_4071808
_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
;
(C26 H23 O2 P1 I1 Mo1 1+), (C32 H12 B1 F24 1-) 
;
_chemical_formula_structural
;
 (Mo (C5 H5) (CO)2 (I C H3) (P (C6 H5)3)) (B C32 H12 F24)
;
_chemical_formula_sum            'C58 H35 B F24 I Mo O2 P'
_chemical_formula_weight         1484.48
_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                96.53(2)
_cell_angle_beta                 96.34(2)
_cell_angle_gamma                90.11(2)
_cell_formula_units_Z            2
_cell_length_a                   12.421(2)
_cell_length_b                   13.151(2)
_cell_length_c                   18.319(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      10
_cell_volume                     2954.5(11)
_computing_cell_refinement       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_collection       'CAD-4 (Enraf-Nonius, 1977)'
_computing_data_reduction        'XCAD4VAX (Sheldrick, 1993)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELX76 (Sheldrick, 1976)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD-4'
_diffrn_measurement_method       \q/2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2054
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10322
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        <2.6%
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_T_max  0.9135
_exptl_absorpt_correction_T_min  0.7408
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.999
_refine_ls_goodness_of_fit_obs   1.181
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         10316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_restrained_S_obs      1.181
_refine_ls_R_factor_all          0.2345
_refine_ls_R_factor_obs          0.0609
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+5.4709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1981
_refine_ls_wR_factor_obs         0.1377
_reflns_number_observed          4148
_reflns_number_total             10322
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om800401d-file003.cif
_cod_data_source_block           momeicor
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+5.4709P] 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^)+(0.0775P)^2^+5.4709P] 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        2954.5(10)
_cod_database_code               4071808