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_4320275
_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            'C44 H90 Cl8 N2 O12 W6'
_chemical_formula_weight         2225.93
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
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_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                 94.220(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4369(13)
_cell_length_b                   14.182(2)
_cell_length_c                   21.891(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     3231.4(8)
_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
;

SIR92 (Altomare, et. al. 1993)

;
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device       'Rigaku CCD'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
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_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  0.05557
_diffrn_reflns_av_sigmaI/netI    0.054
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29822
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
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_exptl_absorpt_coefficient_mu    11.030
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.287
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'cut needle'
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_refine_diff_density_min         -1.39
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_refine_ls_goodness_of_fit_ref   1.330
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5601
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0484
_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         0.0650
_reflns_number_gt                5601
_reflns_number_total             7995
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic001480y_1.cif
_cod_data_source_block           '_Template_texray.inf'
_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        3231.5(6)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C44 H90 Cl8 N2 O12 W6 '
_cod_database_code               4320275