An Unusual P-P Double Bond Formed via Phospha-Wittig Transformation of a Terminal PO Complex
Nicholas A. Piro; Christopher C. Cummins; Journal of the American Chemical Society 131 (2009) 8764–8765; doi:10.1021/ja903860k

data_4104632
_publ_contact_author_address
;Massachusetts Institute of Technology
77 Massachusetts Avenue
Room 6-435
Cambridge, MA 02139
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_name        'Christopher C. Cummins'
_publ_contact_author_phone       617-253-5332
_publ_section_title
;
 An Unusual P-P Double Bond Formed via Phospha-Wittig Transformation of a
 Terminal PO Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8764
_journal_page_last               8765
_journal_paper_doi               10.1021/ja903860k
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C48 H82 Mo N3 P2 Si'
_chemical_formula_weight         887.14
_chemical_name_common            ' iPr3SiPPMo(N[tBu]Ar)3 '
_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                65.2370(10)
_cell_angle_beta                 72.983(2)
_cell_angle_gamma                75.312(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4081(10)
_cell_length_b                   15.4385(14)
_cell_length_c                   16.7680(15)
_cell_measurement_reflns_used    9638
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      0.00
_cell_measurement_theta_min      0.00
_cell_volume                     2534.9(4)
_computing_cell_refinement       'SAINT 7.4 (Bruker-AXS, 2008)'
_computing_data_collection       'APEX2 2.2 (Bruker-AXS, 2008)'
_computing_data_reduction        'SAINT 7.4 (Bruker-AXS, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_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  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62760
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.9813
_exptl_absorpt_correction_T_min  0.8483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       plate
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         13603
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+1.6021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                10776
_reflns_number_total             13603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903860k_si_001_2.cif
_cod_data_source_block           MoPP
_cod_database_code               4104632