Tetra-<i>n</i>-butylammonium μ-fluorido-bis{tris[2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethanolato-κ<i>O</i>]aluminate(III)}
Krossing, Ingo; Raabe, Ines; Acta Crystallographica Section E 63 (2007) m2144–m2144; doi:10.1107/S1600536807033533

data_2214800
_publ_section_title
;Tetra-<i>n</i>-butylammonium
 \m-fluorido-bis{tris[2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethanolato-\k<i>O</i>]aluminate(III)}
;
_journal_coeditor_code           LX2013
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2144
_journal_page_last               m2144
_journal_paper_doi               10.1107/S1600536807033533
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C16 H36 N) '[Al2 (C4 F9 O)6 F]''
_chemical_formula_moiety         'C16 H36 N +, C24 Al2 F55 O6 -'
_chemical_formula_sum            'C40 H36 Al2 F55 N O6'
_chemical_formula_weight         1725.66
_chemical_name_common            '[NBu4]+[((CF3)3CO)3Al-F-Al(OC(CF3)3)3]-'
_chemical_name_systematic
;
Tetra-n-butylammonium
\m-fluorido-bis{tris[2,2,2-trifluoro-1,1-bis(trifluoromethyl)ethanolato-
\kO]aluminate(III)}
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.35(3)
_cell_angle_beta                 86.72(3)
_cell_angle_gamma                89.21(3)
_cell_formula_units_Z            4
_cell_length_a                   12.822(3)
_cell_length_b                   19.230(4)
_cell_length_c                   24.871(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.5
_cell_volume                     6119(2)
_computing_cell_refinement       '<i>CELL</i> (Stoe & Cie, 2003)'
_computing_data_collection       '<i>XPOSE</i> (Stoe & Cie, 2003)'
_computing_data_reduction        '<i>XRED</i> (Stoe & Cie, 2003)'
_computing_molecular_graphics    '<i>DIAMOND</i> (Crystal Impact, 2006)'
_computing_publication_material  <i>SHELXL97</i>
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 1997)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 1997)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \f
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            55213
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2215
_refine_ls_number_reflns         23694
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.105P)^2^+10.4575P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1959
_refine_ls_wR_factor_ref         0.2162
_reflns_number_gt                16301
_reflns_number_total             23694
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            lx2013.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -p_1
_cod_database_code               2214800
_cod_database_fobs_code          2214800