Crystal structure of tributylmethylammonium tetrachloro(1,4-dioxane)oxotungstate(V) 1,4-dioxane hemisolvate, [N(CH3)(C4H9)3][WOCl4(C4H8O2)] · 0.5C4H8O2
Alexander Okrut; Claus Feldmann; Zeitschrift für Kristallographie - New Crystal Structures 223 (2008) 21–; doi:

data_8102200
_publ_section_title
;
 Crystal structure of tributylmethylammonium
 tetrachloro(1,4-dioxane)oxotungstate(V) 1,4-dioxane hemisolvate,
 [N(CH3)(C4H9)3][WOCl4(C4H8O2)] &#x00B7; 0.5C4H8O2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              21
_journal_volume                  223
_journal_year                    2008
_chemical_formula_structural
'[N(CH3)(C4H9)3][WOCl4(C4H8O2)] &#x00B7; 0.5C4H8O2'
_chemical_formula_sum            'C19 H42 Cl4 N O4 W'
_chemical_formula_weight         179.78
_chemical_name_systematic
; 
tributylmethylammonium tetrachloro(1,4-dioxane)oxotungstate(V) 1,4-dioxane 
hemisolvate
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.30(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.760(5)
_cell_length_b                   11.078(2)
_cell_length_c                   22.663(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5483(3)
_computing_cell_refinement       'CELL (STOE)'
_computing_data_collection       'EXPOSE (STOE)'
_computing_data_reduction        'INTEGRATE (STOE)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS I'
_diffrn_measurement_method       phi
_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  0.0577
_diffrn_reflns_av_sigmaI/netI    0.1057
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9574
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    4.626
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'bluish transparent'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.254
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.824
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                2631
_reflns_number_total             5269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2127.cff
_cod_data_source_block           '[NMeBu3]2[(WOCl4)*C4H8O2]2(C4H8O2)'
_cod_original_cell_volume        5483.2(19)
_cod_original_sg_symbol_H-M      C12/c1
_cod_original_formula_sum        'C19 H42 Cl4 N1 O4 W1'
_cod_database_code               8102200