Synthesis of ternary transition metal fluorides Li3MF6via a sol–gel route as candidates for cathode materials in lithium-ion batteries
Kohl, Julia; Wiedemann, Dennis; Nakhal, Suliman; Bottke, Patrick; Ferro, Noel; Bredow, Thomas; Kemnitz, Erhard; Wilkening, Martin; Heitjans, Paul; Lerch, Martin; Journal of Materials Chemistry 22 (2012) 15819–; doi:10.1039/c2jm32133e

data_7208416
_publ_section_title
;
 Synthesis of ternary transition metal fluorides Li3MF6via a sol--gel
 route as candidates for cathode materials in lithium-ion batteries
;
_journal_issue                   31
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              15819
_journal_paper_doi               10.1039/c2jm32133e
_journal_volume                  22
_journal_year                    2012
_chemical_formula_moiety         'C14 H20 N2 O4 V 1+, B F4 1-'
_chemical_formula_sum            'C14 H20 B F4 N2 O4 V'
_chemical_formula_weight         418.07
_chemical_name_common
'bis(acetonitrile)bis(acetylacetonato)vanadium(III) tetrafluoroborate'
_chemical_name_systematic
'bis(acetonitrile)bis(acetylacetonato)vanadium(III) tetrafluoroborate'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 119.774(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9556(10)
_cell_length_b                   5.7003(4)
_cell_length_c                   15.8568(19)
_cell_measurement_reflns_used    1444
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5296
_cell_measurement_theta_min      3.4334
_cell_volume                     937.99(17)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0635
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3866
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.55
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             428
_exptl_crystal_recrystallization_method
'diffusion: acetonitrile, diethyl ether, r. t., six weeks'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                1372
_reflns_number_total             1832
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2jm32133e.txt
_cod_data_source_block           Vacac2(CH3CN)2BF4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7208416