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_4319936
_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            'beta isomer'
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 113.1200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6748(3)
_cell_length_b                   24.8097(8)
_cell_length_c                   14.5093(4)
_cell_measurement_temperature    163(2)
_cell_volume                     3865.06(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Briker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17251
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    18.647
_exptl_absorpt_correction_T_max  0.148680
_exptl_absorpt_correction_T_min  0.058263
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.053
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.878
_refine_ls_goodness_of_fit_obs   0.976
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.878
_refine_ls_restrained_S_obs      0.976
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_obs          0.0226
_refine_ls_shift/esd_max         0.385
_refine_ls_shift/esd_mean        0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0405
_refine_ls_wR_factor_obs         0.0384
_reflns_number_observed          4848
_reflns_number_total             6515
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0013734_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+0.0000P] 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^)+(0.0099P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3865.1(2)
_cod_database_code               4319936