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_7236536
_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         '0.5(C16 H4 F24 Fe2 O16)'
_chemical_formula_sum            'C8 H2 F12 Fe O8'
_chemical_formula_weight         509.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-09
_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                 98.571(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.658(6)
_cell_length_b                   9.753(3)
_cell_length_c                   8.341(3)
_cell_measurement_reflns_used    2077
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      29.891
_cell_measurement_theta_min      2.337
_cell_volume                     1581.3(9)
_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      150.0
_diffrn_detector                 'Bruker Apex I'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type
'Bruker SMART Platform with a Apex I-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2370
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.547
_diffrn_reflns_theta_min         2.095
_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    1.129
_exptl_absorpt_correction_T_max  0.494737
_exptl_absorpt_correction_T_min  0.353389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1216 before and 0.0520 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1184 before and 0.0573 after correction.
 The Ratio of minimum to maximum transmission is 0.71.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 12369 reflections, Rint = 0.0552
 (7755 with I > 3sig(I), Rint = 0.0521)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_description       needle
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
'crystallized from trifluoroacetic acid'
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.228
_refine_diff_density_max         1.559
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2370
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0948P)^2^+0.7184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1408
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2111
_reflns_number_total             2370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ta00862g2.cif
_cod_data_source_block           gunt07o08_h
_cod_original_cell_volume        1581.3(8)
_cod_database_code               7236536
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.546(2) 0.454(2)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, F1, F2, F3, F4, F5, F6, F1A, F2A, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
5.a Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              85973
_shelx_hkl_checksum              1739
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'