Synthesis and Catalytic Application of Octahedral Lewis Base Adducts of Dichloro and Dialkyl Dioxotungsten(VI)
Fritz E. Kühn; Wen-Mei Xue; Ahmad Al-Ajlouni; Ana M. Santos; Shuliang Zang; Carlos C. Romão; Georg Eickerling; Eberhardt Herdtweck; Inorganic Chemistry 41 (2002) 4468–4477; doi:10.1021/ic0200085

data_4318376
_publ_contact_author
;
         Georg Eickerling
         Anorganisch-chemisches Institut der
         Technischen Universit\"at M\"unchen
         Lichtenbergstrasse 4
         D-85747 Garching bei M\"unchen
;
_publ_contact_author_email       georg.eickerling@ch.tum.de
_publ_contact_author_fax         '+49(0)89 289 13473'
_publ_contact_author_phone       '+49(0)89 289 14378'
_publ_section_title
;
 Synthesis and Catalytic Application of Octahedral Lewis Base Adducts of
 Dichloro and Dialkyl Dioxotungsten(VI)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4468
_journal_page_last               4477
_journal_paper_doi               10.1021/ic0200085
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C18 H24 Cl2 N2 O2 W'
_chemical_formula_sum            'C18 H24 Cl2 N2 O2 W'
_chemical_formula_weight         555.13
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             1-June-01
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
   11-Jun-01  Updated by the Author E.H.
   14-Dec-01  Updated by the Author G.E.
   28-March-02  Updated by the Author G.E.
   27-May-02 Updated by the Author G.E.
              Textwriting by G.E.
   28-May-02  Updated by the Author E.H.
              Checkcif    OK
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3198(1)
_cell_length_b                   13.3224(2)
_cell_length_c                   18.0415(2)
_cell_measurement_reflns_used    2089
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      1.90
_cell_volume                     1999.71(4)
_computing_cell_refinement       'Denzo and HKL (Nonius, 1998)'
_computing_data_collection       'Kappa CCD (Nonius, 1998)'
_computing_data_reduction        'Denzo and HKL (Nonius,1998)'
_computing_molecular_graphics    'PLATON (Spek, 2000)'
_computing_publication_material  'PLATON (Spek, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Kappa CCD (Nonius)'
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31495
_diffrn_reflns_theta_full        25.23
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    6.057
_exptl_absorpt_correction_T_max  0.4635
_exptl_absorpt_correction_T_min  0.1325
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.771
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+12.6271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                3558
_reflns_number_total             3586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0200085.cif
_cod_data_source_block           MEIX_E001-173
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'multi scan'
changed to 'multi-scan' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4318376