Bis(tetrabutylammonium) μ-oxalato-bis[dibromidodioxidotungstate(VI)]
Clegg, William; Elsegood, Mark R. J.; Errington, R. John; Wingad, Richard L.; Acta Crystallographica Section E 63 (2007) m1269–m1270; doi:10.1107/S1600536807017102

data_2213538
_publ_section_title
;
 Bis(tetrabutylammonium) \m-oxalato-bis[dibromidodioxidotungstate(VI)]
;
_journal_coeditor_code           SG2155
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1269
_journal_page_last               m1270
_journal_paper_doi               10.1107/S1600536807017102
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C16 H36 N)2 [W2 Br4 (C2 O4) O4]'
_chemical_formula_moiety         '2(C16 H36 N +), C2 Br4 O8 W2 2-'
_chemical_formula_sum            'C34 H72 Br4 N2 O8 W2'
_chemical_formula_weight         1324.28
_chemical_name_systematic
;
Bis(tetrabutylammonium) \m-oxalato-bis[dibromidodioxidotungstate(VI)]
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.905(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8891(9)
_cell_length_b                   18.0806(15)
_cell_length_c                   13.2945(11)
_cell_measurement_reflns_used    10570
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      1.1
_cell_volume                     2376.8(4)
_computing_cell_refinement       'local programs'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2001)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       'thin-slice \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12764
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.241
_exptl_absorpt_correction_T_max  0.270
_exptl_absorpt_correction_T_min  0.075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(XPREP in SHELXTL; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.213
_refine_diff_density_min         -1.181
_refine_ls_extinction_coef       0.00108(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         4689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+4.8146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0627
_reflns_number_gt                4435
_reflns_number_total             4689
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg2155.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2213538
_cod_database_fobs_code          2213538