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_4104631
_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 H81 N3 Nb P Si'
_chemical_formula_weight         852.13
_chemical_name_common            iPr3SiPNb[Np]Ar)3
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.970(2)
_cell_angle_beta                 84.260(2)
_cell_angle_gamma                84.825(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9212(14)
_cell_length_b                   13.8989(16)
_cell_length_c                   15.3715(18)
_cell_measurement_reflns_used    9197
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.35
_cell_measurement_theta_min      2.17
_cell_volume                     2521.4(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0697
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49198
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.9744
_exptl_absorpt_correction_T_min  0.8944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       shard
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         12981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.6003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1046
_reflns_number_gt                9672
_reflns_number_total             12981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903860k_si_001_1.cif
_cod_data_source_block           NbPSi
_cod_database_code               4104631