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_4305791
_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         'C22 H29 N O4 W'
_chemical_formula_sum            'C22 H29 N O4 W'
_chemical_formula_weight         555.31
_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                99.903(6)
_cell_angle_beta                 97.032(7)
_cell_angle_gamma                92.263(6)
_cell_formula_units_Z            2
_cell_length_a                   8.4166(11)
_cell_length_b                   10.2419(13)
_cell_length_c                   13.3165(19)
_cell_measurement_reflns_used    9344
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.00
_cell_volume                     1120.1(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX-II 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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41685
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    5.182
_exptl_absorpt_correction_T_max  0.6253
_exptl_absorpt_correction_T_min  0.3574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.072
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         6522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.2909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                6209
_reflns_number_total             6522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800738a_si_002_3.cif
_cod_data_source_block           c07228
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4305791