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_4113116
_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            'C50 H75 N3 Nb O P'
_chemical_formula_weight         858.01
_chemical_name_common            (1-AdC(P)O)Nb(N[Np]Ar)3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.9950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5441(10)
_cell_length_b                   34.834(3)
_cell_length_c                   12.2793(10)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.94
_cell_volume                     4822.8(7)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1356
_diffrn_reflns_av_sigmaI/netI    0.1256
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18407
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.320
_exptl_absorpt_correction_T_max  0.4767
_exptl_absorpt_correction_T_min  0.4169
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'cherry red'
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       needle
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.790
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         6285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.0906
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+13.5422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                4363
_reflns_number_total             6285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0461522si20040629_120747_3.cif
_cod_data_source_block           4-1-Ad
_cod_database_code               4113116