Preparation and Substitution Chemistry of [Bu4N]2[W6Cl8(p-OSO2C6H4CH3)6]. A Useful Precursor for Pseudohalide, Acetate, and Organometallic Complexes Containing the {W6Cl8}4+ Core
Charles S. Weinert; Nicholas Prokopuk; Stephanie M. Arendt; Charlotte L. Stern; Duward F. Shriver; Inorganic Chemistry 40 (2001) 5162–5168; doi:10.1021/ic001480y

data_4320277
_publ_contact_author_address
;
      Department of Chemistry
      Northwestern University
      2145 Sheridan Road
      Evanston, IL 60208
;
_publ_contact_author_email       ' shriver@chem.nwu.edu'
_publ_contact_author_fax         ' (847) 491-7713 '
_publ_contact_author_name        ' Duward F. Shriver'
_publ_contact_author_phone       ' (847) 491-5655 '
_publ_section_title
;
 Preparation and Substitution Chemistry of [Bu4N]2[W6Cl8(p-OSO2C6H4CH3)6].
 A Useful Precursor for Pseudohalide, Acetate, and Organometallic
 Complexes Containing the {W6Cl8}4+ Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5162
_journal_page_last               5168
_journal_paper_doi               10.1021/ic001480y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C42.5 H67 Cl9 N8 O Se6 W6'
_chemical_formula_weight         2601.99
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 95.625(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.2034(9)
_cell_length_b                   16.471(1)
_cell_length_c                   20.038(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     3679.8(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997)'
_computing_structure_solution
;

SHELX97 (Sheldrick, 1997)

;
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device       'Rigaku CCD'
_diffrn_measurement_method       \w-2\q
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_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.12139
_diffrn_reflns_av_sigmaI/netI    0.164
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34036
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.02
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.679
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
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_exptl_crystal_size_max          0.15
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_refine_diff_density_max         2.11
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_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_ref   1.360
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    6
_refine_ls_number_parameters     211
_refine_ls_number_reflns         2484
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1272
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1010
_reflns_number_gt                2484
_reflns_number_total             9144
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic001480y_3.cif
_cod_data_source_block           '_s27i([Bu4N]2[W6Cl8(NCSe)6](5)'
_cod_depositor_comments
;
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 
;
_cod_original_cell_volume        3680.0(5)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C42.50 H67 Cl9 N8 O Se6 W6 '
_cod_database_code               4320277