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_4120359
_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 Mn Na O6'
_chemical_formula_sum            'C15 H3 F18 Mn Na O6'
_chemical_formula_weight         699.10
_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                   18.045(2)
_cell_length_b                   18.045(2)
_cell_length_c                   12.6335(14)
_cell_measurement_reflns_used    8094
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.8819
_cell_measurement_theta_min      2.2573
_cell_volume                     3562.6(7)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30\% \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29558
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.9566
_exptl_absorpt_correction_T_min  0.7445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2003)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.955
_exptl_crystal_description       needle
_exptl_crystal_F_000             2034
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0261P)^2^+12.5398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                2036
_reflns_number_total             2874
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja4069529_si_002_2.cif
_cod_data_source_block           NaMn(hfac)3
_cod_original_sg_symbol_Hall     '-P 3 2"c     '
_cod_original_sg_symbol_H-M      'P -3 c 1 '
_cod_database_code               4120359