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_4003479
_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_moiety         'C10 F16 Fe2 O10'
_chemical_formula_sum            'C10 F16 Fe2 O10'
_chemical_formula_weight         695.80
_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_primary     dual
_audit_creation_date             2018-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                106.748(16)
_cell_angle_beta                 92.231(18)
_cell_angle_gamma                90.877(17)
_cell_formula_units_Z            2
_cell_length_a                   8.483(2)
_cell_length_b                   8.5123(15)
_cell_length_c                   14.559(3)
_cell_measurement_reflns_used    894
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      50.4870
_cell_measurement_theta_min      5.1790
_cell_volume                     1005.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -20.00   7.00   0.50    5.00    --  -57.07  77.00   0.00   54
  2  \w    -32.00   0.00   0.50    5.00    --  -57.07  77.00 -90.00   64
  3  \w    -49.00  14.00   0.50    5.00    --  -57.07  57.00-150.00  126
  4  \w    -65.00 -35.00   0.50    5.00    --  -57.07  77.00   0.00   60
  5  \w    -80.00   3.00   0.50    5.00    --  -57.07  77.00 -30.00  166
  6  \w    -72.00 -37.00   0.50    5.00    --  -57.07  77.00 -90.00   70
  7  \w    -81.00 -46.00   0.50    5.00    --  -57.07  77.00-120.00   70
  8  \w   -132.00 -49.00   0.50    5.00    --  -57.07 -38.00  60.00  166
  9  \w   -118.00 -90.00   0.50    5.00    --  -57.07 -99.00   0.00   56
 10  \w   -115.00 -82.00   0.50    5.00    --  -57.07 -77.00 -60.00   66
 11  \w   -118.00 -78.00   0.50    5.00    --  -57.07 -77.00-180.00   80
 12  \w     -1.00  89.00   0.50    5.00    --   55.20 -99.00  60.00  180
 13  \w     55.00  89.00   0.50    5.00    --   55.20 -99.00 150.00   68
 14  \w     -5.00  32.00   0.50    5.00    --   55.20 -99.00 150.00   74
 15  \w     79.00 104.00   0.50    5.00    --   55.20  77.00  60.00   50
 16  \w     82.00 126.00   0.50    5.00    --   55.20 178.00-120.00   88
 17  \w     86.00 111.00   0.50    5.00    --   55.20  77.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0229166000
_diffrn_orient_matrix_UB_12      -0.1605899000
_diffrn_orient_matrix_UB_13      -0.0800927000
_diffrn_orient_matrix_UB_21      0.1605855000
_diffrn_orient_matrix_UB_22      0.0667676000
_diffrn_orient_matrix_UB_23      -0.0204793000
_diffrn_orient_matrix_UB_31      0.0821056000
_diffrn_orient_matrix_UB_32      -0.0741621000
_diffrn_orient_matrix_UB_33      0.0734947000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1199
_diffrn_reflns_av_unetI/netI     0.1754
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5103
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        50.435
_diffrn_reflns_theta_max         50.435
_diffrn_reflns_theta_min         5.220
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.506
_exptl_absorpt_correction_T_max  0.70941
_exptl_absorpt_correction_T_min  0.69535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.23a (Rigaku Oxford Diffraction, 2015) Spherical absorption correction using equivalent radius and absorption coefficient. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.298
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2086
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.0996
_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^)+(0.1404P)^2^+13.1967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2745
_refine_ls_wR_factor_ref         0.3125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1127
_reflns_number_total             2086
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm9b05004_si_002.cif
_cod_data_source_block           sm300118_3_1
_cod_database_code               4003479
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         Fe2C10O10F16
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.267
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_olex2_refinement_description
;
1. Restrained distances
 C10-C9 \\sim C9-C0
 with sigma of 0.001
 F15-C10 \\sim F14-C10 \\sim F13-C10 \\sim F15A-C0 \\sim F14A-C0 \\sim F13A-C0
 with sigma of 0.001
 F15-F13 \\sim F15-F14 \\sim F15A-F13A \\sim F13A-F14A \\sim F13-F14 \\sim
F15A-F14A
 with sigma of 0.02
 C7-O8 \\sim C7-O7 \\sim C7-C8
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uiso(C0) = Uiso(C10)
Uiso(F15A) = Uiso(F14) = Uiso(F14A) = Uiso(F13) = Uiso(F13A) = Uiso(F15)
Uiso(F10) = Uiso(F10A) = Uiso(F11) = Uiso(F11A) = Uiso(F12) = Uiso(F12A)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F13A)=Sof(F14A)=Sof(F15A)=Sof(C0)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(C10)=FVAR(1)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2)
;
_shelx_res_checksum              60840
_shelx_hkl_checksum              72895
_olex2_exptl_crystal_mounting_method tip-mounted
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.980
_oxdiff_exptl_absorpt_empirical_full_min 0.600