Organic Nitriles from Acid Chlorides: An Isovalent N for (O)Cl Exchange Reaction Mediated by a Tungsten Nitride Complex
Christopher R. Clough; Jane B. Greco; Joshua S. Figueroa; Paula L. Diaconescu; William M. Davis; Christopher C. Cummins; Journal of the American Chemical Society 126 (2004) 7742–7743; doi:10.1021/ja0492438

data_4112707
_publ_section_title
;
 Organic Nitriles from Acid Chlorides: An Isovalent N for (O)Cl Exchange
 Reaction Mediated by a Tungsten Nitride Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7742
_journal_page_last               7743
_journal_paper_doi               10.1021/ja0492438
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C37 H48 F6 N4 O3 W'
_chemical_formula_weight         894.64
_chemical_name_common            W(NC(O)CF3)(O2CCF3)(N[i-Pr]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                91.902(2)
_cell_angle_beta                 100.9770(10)
_cell_angle_gamma                90.6950(10)
_cell_formula_units_Z            4
_cell_length_a                   12.0919(10)
_cell_length_b                   16.4768(13)
_cell_length_c                   20.0774(16)
_cell_measurement_reflns_used    303
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      1.24
_cell_volume                     3924.1(5)
_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 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'APEX CCD'
_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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19973
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    3.011
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       rod
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.430
_refine_diff_density_min         -2.285
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         14559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0968P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                12181
_reflns_number_total             14559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0492438si20040505_012304_2.cif
_cod_data_source_block           2mc
_cod_database_code               4112707