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_7236537
_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         'C4 H8 Co F6 O8'
_chemical_formula_sum            'C4 H8 Co F6 O8'
_chemical_formula_weight         357.03
_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     iterative
_audit_creation_date             2015-04-06
_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                75.139(6)
_cell_angle_beta                 64.574(6)
_cell_angle_gamma                71.426(6)
_cell_formula_units_Z            2
_cell_length_a                   8.1360(4)
_cell_length_b                   9.0331(7)
_cell_length_c                   9.2695(5)
_cell_measurement_reflns_used    5674
_cell_measurement_temperature    103(5)
_cell_measurement_theta_max      31.8010
_cell_measurement_theta_min      2.9940
_cell_volume                     577.48(7)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      103(5)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega  -31.00   -5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -57.0000 -150.0000 26

  2 omega  -91.00    3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -77.0000  120.0000 94

  3 omega  -64.00   -5.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -57.0000    0.0000 59

  4 omega  -56.00  -10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865   77.0000   60.0000 46

  5 omega  -35.00   41.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865   66.0000  -30.0000 76

  6 omega  -95.00    3.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -77.0000  -30.0000 98

  7 omega  -94.00   -6.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -66.0000 -165.0000 88

  8 omega  -31.00   64.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -19.0000    0.0000 95

  9 omega   19.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -99.0000  -60.0000 50

 10 omega  -17.00    9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -99.0000  -60.0000 26

 11 omega  -24.00   69.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -99.0000 -180.0000 93

 12 omega  -24.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -19.0000  150.0000 95
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0759819000
_diffrn_orient_matrix_UB_12      -0.0121997000
_diffrn_orient_matrix_UB_13      0.0236698000
_diffrn_orient_matrix_UB_21      -0.0204254000
_diffrn_orient_matrix_UB_22      0.0821346000
_diffrn_orient_matrix_UB_23      0.0015292000
_diffrn_orient_matrix_UB_31      -0.0607527000
_diffrn_orient_matrix_UB_32      -0.0101911000
_diffrn_orient_matrix_UB_33      0.0822138000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7011
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.576
_diffrn_reflns_theta_min         2.977
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. The HKLF 5-file with two components contains 7015 reflections unique reflections, merged from 20573 measured reflections.
R-int. for all components is 0.033, Rsigma 0.049.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_description       block
_exptl_crystal_F_000             354
_exptl_crystal_recrystallization_method
'crystallized from toluene/ethanole-mixture'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         7011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0367P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5604
_reflns_number_total             7011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta00862g2.cif
_cod_data_source_block           gunt05o04_100k
_cod_original_cell_volume        577.49(7)
_cod_database_code               7236537
_chemical_oxdiff_formula         'Co1 C4 O8 F6 H8 '
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.620
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5106(6) 0.4894(6)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H) groups
;
_shelx_res_checksum              82921
_shelx_hkl_checksum              75819
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'