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_7236539
_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 F24 Fe3 O17'
_chemical_formula_sum            'C16 H F24 Fe3 O17'
_chemical_formula_weight         1088.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-07-07
_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                90
_cell_angle_beta                 91.358(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7505(11)
_cell_length_b                   21.236(2)
_cell_length_c                   16.0879(18)
_cell_measurement_reflns_used    5103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.856
_cell_measurement_theta_min      2.299
_cell_volume                     3330.3(6)
_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  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Apex I'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type
'Bruker SMART Platform with a Apex I-detector'
_diffrn_measurement_method       '\f and \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  0.0652
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32972
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         1.588
_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    1.495
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0677 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.9241.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.171
_exptl_crystal_description       plate
_exptl_crystal_F_000             2108
_exptl_crystal_recrystallization_method
'crystallized from trifluoroacetic acid'
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.0025
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         7688
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+12.5704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6265
_reflns_number_total             7688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta00862g2.cif
_cod_data_source_block           gunt21o05
_cod_original_cell_volume        3330.2(6)
_cod_database_code               7236539
_olex2_refinement_description
;
1. Restrained distances
 O51-C52 \\sim C52A-O51A
 with sigma of 0.001
2. Uiso/Uaniso restraints and constraints
Uiso(O50A) = Uiso(O50)
Uiso(C53A) = Uiso(C53)
Uiso(C52A) = Uiso(C52)
Uanis(C11) = Uanis(C11A)
Uanis(C10A) = Uanis(C10)
Uiso(F55A) = Uiso(F55) = Uiso(F54) = Uiso(F54A) = Uiso(F56A) = Uiso(F56)
Uiso(O51A) = Uiso(O51)
3. Rigid body (RIGU) restrains
 C3, C4, F5, F6, F7, F5A, F6A, F7A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O8, O9, F12, F13, F14, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8, O9, F12A, F13A, F14A, C10A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F54, F55, F56, O50, O51, C52, C53, F54A, F55A, F56A, O50A, O51A, C52A, C53A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F5A)=Sof(F6A)=Sof(F7A)=1-FVAR(1)
 Sof(F5)=Sof(F6)=Sof(F7)=FVAR(1)
 Sof(F54A)=Sof(F55A)=Sof(F56A)=Sof(O50A)=Sof(O51A)=Sof(C52A)=Sof(C53A)=1-FVAR(2)
 Sof(F54)=Sof(F55)=Sof(F56)=Sof(O50)=Sof(O51)=Sof(C52)=Sof(C53)=FVAR(2)
 Sof(F12A)=Sof(F13A)=Sof(F14A)=Sof(C10A)=Sof(C11A)=1-FVAR(3)
 Sof(F12)=Sof(F13)=Sof(F14)=Sof(C10)=Sof(C11)=FVAR(3)
;
_shelx_res_checksum              30223
_shelx_hkl_checksum              88664
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'