Tungsten(VI) Complexes with Aminobis(phenolato) [O,N,O] Donor Ligands
Ari Lehtonen; Reijo Sillanpää; Inorganic Chemistry 43 (2004) 6501–6506; doi:10.1021/ic049448h

data_4311683
_publ_section_title
;
 Tungsten(VI) Complexes with Aminobis(phenolato) [O,N,O] Donor Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6501
_journal_page_last               6506
_journal_paper_doi               10.1021/ic049448h
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C25 H35 Cl2 N O3 W'
_chemical_formula_sum            'C25 H35 Cl2 N O3 W'
_chemical_formula_weight         652.29
_chemical_name_systematic
;
  cis-dichloro(methylamino-N,N-bis(2-methylene-4-methyl-6-t- 
butylphenolato)oxotungsten(VI)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.417(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4438(9)
_cell_length_b                   7.7968(2)
_cell_length_c                   19.9166(12)
_cell_measurement_reflns_used    5123
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      0.407
_cell_volume                     2598.3(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17457
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.43
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.677
_exptl_absorpt_correction_T_max  0.8348
_exptl_absorpt_correction_T_min  0.4855
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998)
I/sigma threshold for reflections     =   5.000
Delta(U)/lambda**2                    =   0.000
Highest even order spherical harmonic =       6
Highest odd  order spherical harmonic =       3
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.886
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.00091(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5441
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                3834
_reflns_number_total             5441
_reflns_threshold_expression     >2s(I)
_cod_data_source_file            ic049448hsi20040429_074507_4.cif
_cod_data_source_block           wbuabi=cis-5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4311683
_exptl_absorpt_factor_mur        0.327
_exptl_absorpt_rmerge_before     0.0497
_exptl_absorpt_rmerge_after      0.0395