Reduction of an η2-Iminoacyl Ligand to η2-Iminium Enabled by Adjacent Carbon Monoxide Ligand Replacement with a Variable Electron Donor Alkyne Ligand in a Cationic Tungsten(II) Bis(acetylacetonate) Complex
Andrew B. Jackson; Chetna Khosla; Peter S. White; Joseph L. Templeton; Inorganic Chemistry 47 (2008) 8776–8787; doi:10.1021/ic800738a

data_4305792
_publ_contact_author_address
;
University of North Carolina-Chapel Hill, Chemistry
Kenan and Caudill Labs
CB#3290
Chapel Hill, NC, USA 27599
;
_publ_contact_author_email       joetemp@unc.edu
_publ_contact_author_name        'Joseph L. Templeton'
_publ_contact_author_phone       919-966-4575
_publ_section_title
;
Reduction of an \h2-Iminoacyl Ligand to \h2-Iminium Enabled by Adjacent
Carbon Monoxide Ligand Replacement with a Variable Electron Donor Alkyne
Ligand in a Cationic Tungsten(II) Bis(acetylacetonate) Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8776
_journal_page_last               8787
_journal_paper_doi               10.1021/ic800738a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C32 H12 B F24, C23 H32 N O4 W'
_chemical_formula_sum            'C55 H44 B F24 N O4 W'
_chemical_formula_weight         1433.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                87.162(1)
_cell_angle_beta                 80.333(1)
_cell_angle_gamma                79.078(1)
_cell_formula_units_Z            2
_cell_length_a                   12.4372(3)
_cell_length_b                   12.7720(3)
_cell_length_c                   18.6366(5)
_cell_measurement_reflns_used    9608
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.0
_cell_measurement_theta_min      2.4
_cell_volume                     2865.01(12)
_computing_cell_refinement       'Bruker-AXS  APEX2'
_computing_data_collection       'Bruker-AXS APEX2'
_computing_data_reduction        'Bruker-AXS  SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX-II CCD detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            50256
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    4.863
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         9953
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+9.4256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1411
_reflns_number_gt                9819
_reflns_number_total             9953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800738a_si_002_4.cif
_cod_data_source_block           c07290
_cod_database_code               4305792