Phosphaalkynes from Acid Chlorides via P for O(Cl) Metathesis: A Recyclable Niobium Phosphide (P3-) Reagent that Effects C-P Triple-Bond Formation
Joshua S. Figueroa; Christopher C. Cummins; Journal of the American Chemical Society 126 (2004) 13916–13917; doi:10.1021/ja0461522

data_4113114
_publ_contact_author             'Christorpher C. Cummins'
_publ_contact_author_email       ccummins@mit.edu
_publ_section_title
;
 Phosphaalkynes from Acid Chlorides via P for O(Cl) Metathesis: A
 Recyclable Niobium Phosphide (P3-) Reagent that Effects C-P Triple-Bond
 Formation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13916
_journal_page_last               13917
_journal_paper_doi               10.1021/ja0461522
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C44 H63 N3 Nb O P'
_chemical_formula_weight         773.85
_chemical_name_common            (t-BuC(P)O)Nb(N[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                74.2510(10)
_cell_angle_beta                 72.9650(10)
_cell_angle_gamma                67.5820(10)
_cell_formula_units_Z            2
_cell_length_a                   11.9230(7)
_cell_length_b                   13.1067(8)
_cell_length_c                   16.6412(10)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      2.05
_cell_volume                     2260.7(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.648
_diffrn_measured_fraction_theta_max 0.648
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.1090
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6295
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.5468
_exptl_absorpt_correction_T_min  0.4136
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'Cherry Red'
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       Block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         4232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.099
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                3306
_reflns_number_total             4232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0461522si20040629_120747_1.cif
_cod_data_source_block           4-t-Bu
_cod_database_code               4113114