Structural Evolution of Iron(III) Trifluoroacetate upon Thermal Decomposition: Chains, Layers, and Rings
Wörle, Michael; Guntlin, Christoph P.; Gyr, Luzia; Sougrati, Moulay T.; Lambert, Charles-Henri; Kravchyk, Kostiantyn V.; Zenobi, Renato; Kovalenko, Maksym V.; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.9b05004

data_4003476
_publ_section_title
;
 Structural Evolution of Iron(III) Trifluoroacetate upon Thermal
 Decomposition: Chains, Layers, and Rings
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.9b05004
_journal_year                    2020
_chemical_formula_sum            'C6 F9 Fe O6'
_chemical_formula_weight         394.89
_space_group_IT_number           158
_space_group_name_Hall           'P 3 -2"c'
_space_group_name_H-M_alt        'P 3 c 1'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'P 3 c 1'
_audit_creation_date             2018-01-15T14:31
_audit_creation_method           'created in GSAS-II'
_audit_update_record
'2018-01-15T14:31  Initial software-generated CIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   13.02830(25)
_cell_length_b                   13.02830(25)
_cell_length_c                   8.74990(16)
_cell_measurement_temperature    298
_cell_volume                     1286.20(4)
_computing_structure_refinement
'GSAS-II (Toby & Von Dreele, J. Appl. Cryst. 46, 544-549, 2013)'
_diffrn_ambient_pressure         100
_diffrn_ambient_temperature      298
_diffrn_detector                 'Silicon strip detector'
_diffrn_detector_type            'Dectris Mythen 1K'
_diffrn_measurement_device_type  'Stoe STADIP'
_diffrn_radiation_monochromator  'Focussing Ge'
_diffrn_radiation_polarisn_ratio 0.7000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Cu
_exptl_crystal_density_diffrn    2.039
_exptl_crystal_F_000             764
_pd_block_id
2018-01-15T14:31|FeTFA3_3529_new|WorleMichael|Stoe_STADIP
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  colourless
_pd_instr_location               ' ?'
_pd_meas_2theta_range_inc        0.01000
_pd_meas_2theta_range_max        99.99000
_pd_meas_2theta_range_min        4.00000
_pd_phase_name                   FeTFA3
_pd_proc_2theta_range_inc        0.01000
_pd_proc_2theta_range_max        99.94950
_pd_proc_2theta_range_min        3.95950
_pd_proc_info_datetime           2018-01-15T14:31
_pd_proc_info_excluded_regions   ' ?'
_pd_proc_ls_background_function
; Background function: "chebyschev" function with 21 terms:
    6547.653, -870.525, 13.049, -2854.326, 71093.432, 41887.126, 
    -1.119463214e6, -302652.369, 8.017100560e6, 547545.667, -3.0932894502e7, 
    1.294751764e6, 6.9919588290e7, -6.180329718e6, -9.5798550121e7, 
    9.064338538e6, 7.8545076355e7, -5.958721699e6, -3.5543665464e7, 
    1.496322122e6, 6.842000944e6, 
;
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function
; Finger-Cox-Jephcoat function parameters U, V, W, X, Y, SH/L:
  peak variance(Gauss) = Utan(Th)^2^+Vtan(Th)+W:
  peak HW(Lorentz) = X/cos(Th)+Ytan(Th); SH/L = S/L+H/L
  U, V, W in (centideg)^2^, X & Y in centideg
    192.711, -52.495, 22.312, 0.000, 0.000, 0.049, 
  Crystallite size model "isotropic" for FeTFA3 (microns)
  parameters: Size, G/L mix
    0.347, 1.000, 
  Mustrain model "isotropic" for FeTFA3 (10^6^)
    parameters: Mustrain, G/L mix
    1681.277, 1.000, 

;
_pd_proc_ls_prof_R_factor        0.01583
_pd_proc_ls_prof_wR_expected     0.01173
_pd_proc_ls_prof_wR_factor       0.02482
_pd_proc_number_of_points        9600
_pd_spec_mounting                ' ?'
_refine_diff_density_max         3.776
_refine_diff_density_min         -1.076
_refine_ls_goodness_of_fit_all   2.117
_refine_ls_matrix_type           full
_refine_ls_number_parameters     11
_refine_ls_R_Fsqd_factor         0.18385
_refine_ls_wR_factor_obs         0.02483
_reflns_d_resolution_high        1.007
_reflns_d_resolution_low         11.283
_reflns_limit_h_max              10
_reflns_limit_h_min              10
_reflns_limit_k_max              2
_reflns_limit_k_min              2
_reflns_limit_l_max              1
_reflns_limit_l_min              1
_reflns_number_total             449
_cod_data_source_file            cm9b05004_si_006.cif
_cod_data_source_block           FeTFA3_3529_new
_cod_original_cell_volume        1286.20(3)
_cod_database_code               4003476
_refine_ls_r_f_factor            0.11627
_gsas_proc_ls_prof_r_b_factor    0.03529
_gsas_proc_ls_prof_wr_b_factor   0.04876