Nanocrystalline FeF3 and MF2 (M = Fe, Co, and Mn) from metal trifluoroacetates and their Li(Na)-ion storage properties
Guntlin, Christoph P.; Zünd, Tanja; Kravchyk, Kostiantyn V.; Wörle, Michael; Bodnarchuk, Maryna I.; Kovalenko, Maksym V.; Journal of Materials Chemistry A 5 (2017) 7383–; doi:10.1039/C7TA00862G

data_7236538
_publ_section_title
;
 Nanocrystalline FeF3 and MF2 (M = Fe, Co, and Mn) from metal
 trifluoroacetates and their Li(Na)-ion storage properties
;
_journal_issue                   16
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              7383
_journal_paper_doi               10.1039/C7TA00862G
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety         'C16 H4 F24 Mn2 O16'
_chemical_formula_sum            'C16 H4 F24 Mn2 O16'
_chemical_formula_weight         1018.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2015-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-10-07 deposited with the CCDC.
2017-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                105.172(2)
_cell_angle_beta                 111.289(2)
_cell_angle_gamma                107.081(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3229(17)
_cell_length_b                   13.518(2)
_cell_length_c                   13.940(2)
_cell_measurement_reflns_used    5640
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.448
_cell_measurement_theta_min      2.235
_cell_volume                     1577.4(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Apex I'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16256
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.479
_diffrn_reflns_theta_min         1.722
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.6929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0816 before and 0.0399 after correction.
The Ratio of minimum to maximum transmission is 0.8037.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_description       plate
_exptl_crystal_F_000             988
_exptl_crystal_recrystallization_method 'from trifluoroacetic acid'
_exptl_crystal_size_max          0.426
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         7786
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+1.8305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5807
_reflns_number_total             7786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta00862g2.cif
_cod_data_source_block           gunt18o05_new3
_cod_original_cell_volume        1577.4(5)
_cod_database_code               7236538
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O15) = Uanis(O15A)
Uanis(O7) = Uanis(O7A)
2. Rigid body (RIGU) restrains
 C3, C4, F4, F5, F6, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C13, C14, F19, F20, F21, F19A, F20A, F21A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9, C10, F13, F14, F15, F13A, F14A, F15A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(2)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(2)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(3)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(3)
 Sof(O15A)=1-FVAR(4)
 Sof(O15)=FVAR(4)
 Sof(O7)=1-FVAR(5)
 Sof(O7A)=FVAR(5)
;
_shelx_res_checksum              84093
_shelx_hkl_checksum              41701
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'