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_4319937
_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_formula_structural     (Et4N)3[W6O7Cl11]
_chemical_formula_sum            'C24 H60 Cl11 N3 O7 W6'
_chemical_formula_weight         1995.80
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 92.545(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.545(4)
_cell_length_b                   18.563(3)
_cell_length_c                   13.422(2)
_cell_measurement_temperature    147(2)
_cell_volume                     4864.9(15)
_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      147(2)
_diffrn_measurement_device       'Siemens 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  0.0841
_diffrn_reflns_av_sigmaI/netI    0.1922
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10769
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    14.772
_exptl_absorpt_correction_T_max  0.074434
_exptl_absorpt_correction_T_min  0.045121
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.768
_refine_ls_goodness_of_fit_obs   0.974
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         4105
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.768
_refine_ls_restrained_S_obs      0.974
_refine_ls_R_factor_all          0.1454
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/esd_max         0.131
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0779
_refine_ls_wR_factor_obs         0.0625
_reflns_number_observed          1766
_reflns_number_total             4105
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0013734_3.cif
_cod_data_source_block           3
_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^)+(0.0205P)^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^)+(0.0205P)^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        4865.0(15)
_cod_database_code               4319937