Edge-Bridged Octahedral Tungsten-Oxygen-Chlorine Clusters: Synthesis and Characterization of Two D3d-Symmetric [W6O6Cl12]2- Isomers and [W6O7Cl11]3-
Nathan R. M. Crawford; Jeffrey R. Long; Inorganic Chemistry 40 (2001) 3456–3462; doi:10.1021/ic0013734

data_4319935
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 642-8369'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 Edge-Bridged Octahedral Tungsten-Oxygen-Chlorine Clusters: Synthesis and
 Characterization of Two D3d-Symmetric [W6O6Cl12]2- Isomers and
 [W6O7Cl11]3-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3456
_journal_page_last               3462
_journal_paper_doi               10.1021/ic0013734
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        synthetic
_chemical_formula_structural     (Et4N)2[W6O6Cl12]
_chemical_formula_sum            'C16 H40 Cl12 N2 O6 W6'
_chemical_formula_weight         1885.00
_chemical_name_common            'alpha isomer'
_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
_cell_angle_alpha                118.684(4)
_cell_angle_beta                 90.7100(10)
_cell_angle_gamma                91.511(4)
_cell_formula_units_Z            4
_cell_length_a                   8.4643(10)
_cell_length_b                   22.526(2)
_cell_length_c                   22.743(2)
_cell_measurement_temperature    155(2)
_cell_volume                     3801.3(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      155(2)
_diffrn_measurement_device       'Bruker SMART'
_diffrn_measurement_method       'CCD area detector'
_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  0.0742
_diffrn_reflns_av_sigmaI/netI    0.1730
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19261
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    18.960
_exptl_absorpt_correction_T_max  0.490287
_exptl_absorpt_correction_T_min  0.385783
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.294
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.495
_refine_diff_density_min         -2.501
_refine_diff_density_rms         0.521
_refine_ls_extinction_coef       0.00008(2)
_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_all   1.067
_refine_ls_goodness_of_fit_obs   1.258
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         12104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.258
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_obs          0.0763
_refine_ls_shift/esd_max         -3.269
_refine_ls_shift/esd_mean        0.094
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+155.8119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2005
_refine_ls_wR_factor_obs         0.1746
_reflns_number_observed          6758
_reflns_number_total             12105
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0013734_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'not measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+155.8119P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+155.8119P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319935