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_4003477
_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            'C2 F5 Fe O2'
_chemical_formula_weight         206.86
_space_group_IT_number           67
_space_group_name_Hall           '-C 2a 2'
_space_group_name_H-M_alt        'C m m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C m m a'
_audit_creation_date             2018-01-14T12:06
_audit_creation_method           'created in GSAS-II'
_audit_update_record
'2018-01-14T12:06  Initial software-generated CIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.13216(31)
_cell_length_b                   7.53768(25)
_cell_length_c                   11.25845(29)
_cell_measurement_temperature    298
_cell_volume                     605.25(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    2.270
_exptl_crystal_F_000             396
_pd_block_id
2018-01-14T12:06|FeFxTFAy|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        69.99000
_pd_meas_2theta_range_min        5.00000
_pd_phase_name                   FeF2TFA
_pd_proc_2theta_range_inc        0.01000
_pd_proc_2theta_range_max        69.94801
_pd_proc_2theta_range_min        4.95801
_pd_proc_info_datetime           2018-01-14T12:06
_pd_proc_info_excluded_regions   ' ?'
_pd_proc_ls_background_function
; Background function: "chebyschev" function with 21 terms:
    4885.975, -3628.767, 8454.814, -11555.358, -84053.551, 123323.979, 
    777795.347, -697687.533, -4.124958234e6, 2.419103606e6, 1.3252151136e7, 
    -5.343531555e6, -2.6767852718e7, 7.593673615e6, 3.4053469081e7, 
    -6.722681828e6, -2.6385903463e7, 3.359230938e6, 1.1345497415e7, 
    -719148.415, -2.072765732e6, 
;
_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
    382.477, 0.517, 29.082, 0.000, 0.000, 0.053, 
  Crystallite size model "isotropic" for FeF2TFA (microns)
  parameters: Size, G/L mix
    1.000, 1.000, 
  Mustrain model "isotropic" for FeF2TFA (10^6^)
    parameters: Mustrain, G/L mix
    1000.000, 1.000, 

;
_pd_proc_ls_prof_R_factor        0.01565
_pd_proc_ls_prof_wR_expected     0.01270
_pd_proc_ls_prof_wR_factor       0.02265
_pd_proc_number_of_points        6500
_pd_spec_mounting                ' ?'
_refine_diff_density_max         1.412
_refine_diff_density_min         -0.840
_refine_ls_goodness_of_fit_all   1.809
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_R_Fsqd_factor         0.13918
_refine_ls_wR_factor_obs         0.02295
_reflns_d_resolution_high        1.358
_reflns_d_resolution_low         11.258
_reflns_limit_h_max              1
_reflns_limit_h_min              1
_reflns_limit_k_max              1
_reflns_limit_k_min              1
_reflns_limit_l_max              8
_reflns_limit_l_min              8
_reflns_number_total             84
_cod_data_source_file            cm9b05004_si_003.cif
_cod_data_source_block           FeFxTFAy
_cod_original_cell_volume        605.253(31)
_cod_original_sg_symbol_H-M      Cmma
_cod_database_code               4003477
_refine_ls_r_f_factor            0.13189
_gsas_proc_ls_prof_r_b_factor    0.02783
_gsas_proc_ls_prof_wr_b_factor   0.04123