Volatile Heterometallic Precursors for the Low-Temperature Synthesis of Prospective Sodium Ion Battery Cathode Materials
Zheng Wei; Alexander S. Filatov; Evgeny V. Dikarev; Journal of the American Chemical Society 135 (2013) 12216–12219; doi:10.1021/ja4069529

data_4120360
_publ_contact_author_address
;
Department of Chemistry
University at Albany
1400 Washington Avenue
Albany NY 12222
USA
;
_publ_contact_author_email       dikarev@albany.edu
_publ_contact_author_fax         518-442-3462
_publ_contact_author_name
;
Dikarev, Evgeny V. 
;
_publ_contact_author_phone       518-442-4401
_publ_section_title
;
 Volatile Heterometallic Precursors for the Low-Temperature Synthesis of
 Prospective Sodium Ion Battery Cathode Materials
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12216
_journal_page_last               12219
_journal_paper_doi               10.1021/ja4069529
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C15 H3 F18 Fe Na O6'
_chemical_formula_sum            'C15 H3 F18 Fe Na O6'
_chemical_formula_weight         700.01
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.0016(4)
_cell_length_b                   18.0016(4)
_cell_length_c                   12.3451(3)
_cell_measurement_reflns_used    1813
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      3.85
_cell_volume                     3464.55(14)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_source         'INCOATEC ImuS micro-focus source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34616
_diffrn_reflns_theta_full        66.77
_diffrn_reflns_theta_max         66.77
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    7.149
_exptl_absorpt_correction_T_max  0.8304
_exptl_absorpt_correction_T_min  0.1226
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_description       needle
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0205P)^2^+6.0020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0852
_reflns_number_gt                1664
_reflns_number_total             2054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4069529_si_002_3.cif
_cod_data_source_block           NaFe(hfac)3
_cod_database_code               4120360