Redox mediated dimerisation of a cyclo-As8 complex
Riesinger, Christoph; Scheer, Manfred; Chemical Science 16 (2025) 8807–8811; doi:10.1039/D5SC01685A

data_1574360
_publ_section_title
;
 Redox mediated dimerisation of a cyclo-As8 complex
;
_journal_issue                   20
_journal_name_full               'Chemical Science'
_journal_page_first              8807
_journal_page_last               8811
_journal_paper_doi               10.1039/D5SC01685A
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C26 H42 As7.088 Ta2, Al C16 F36 O4, 1[C6H4F2], 0.5[C5H12]'
_chemical_formula_sum            'C50.5 H52 Al As7.09 F38 O4 Ta2'
_chemical_formula_weight         2364.83
_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_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.11.02 svn.r19aeb66f for OlexSys, GUI svn.r7078)
;
_audit_update_record
;
2025-02-06 deposited with the CCDC.	2025-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                63.108(2)
_cell_angle_beta                 88.564(2)
_cell_angle_gamma                76.688(2)
_cell_formula_units_Z            2
_cell_length_a                   11.4386(2)
_cell_length_b                   18.7072(4)
_cell_length_c                   19.1356(5)
_cell_measurement_reflns_used    22282
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      30.0630
_cell_measurement_theta_min      2.0890
_cell_volume                     3539.01(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.131a 64-bit (release 19-07-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -15.00  14.00   0.50   20.00    --    0.11 102.00 148.25   58
  2  \w    -10.00  29.00   0.50   20.00    --    0.11  96.00-102.30   78
  3  \w    -15.00  14.00   0.50   20.00    --    0.11 102.00-174.16   58
  4  \w    -15.00  14.00   0.50   20.00    --    0.11 102.00  56.24   58
  5  \w    -37.00  -1.00   0.50   20.00    --    4.00 -68.00  41.45   72
  6  \w    -41.00   1.00   0.50   20.00    --    8.00 -36.00-135.98   84
  7  \w    -42.00  11.00   0.50   20.00    --    8.00 -28.00 -32.61  106
  8  \w    -42.00  14.00   0.50   20.00    --    8.00 -27.00 100.41  112
  9  \w    -37.00  11.00   0.50   20.00    --   12.00 -30.00-103.12   96
 10  \w    -45.00  24.00   0.50   20.00    --    4.00 -22.00  12.90  138
 11  \w    -14.00  42.00   0.50   20.00    --   -8.00  27.00  87.36  112
 12  \w    -41.00   0.00   0.50   20.00    --    8.00 -25.00 141.37   82
 13  \w    -37.00  30.00   0.50   20.00    --   12.00 -23.00 -89.27  134
 14  \w    -37.00  10.00   0.50   20.00    --   12.00 -31.00 169.61   94
 15  \w    -37.00  11.00   0.50   20.00    --   12.00 -30.00  51.40   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0075924000
_diffrn_orient_matrix_UB_12      -0.0004437000
_diffrn_orient_matrix_UB_13      -0.0364647000
_diffrn_orient_matrix_UB_21      -0.0071543000
_diffrn_orient_matrix_UB_22      0.0434350000
_diffrn_orient_matrix_UB_23      -0.0201062000
_diffrn_orient_matrix_UB_31      0.0631315000
_diffrn_orient_matrix_UB_32      -0.0060459000
_diffrn_orient_matrix_UB_33      -0.0028090000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            116687
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.068
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.532
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    2.219
_exptl_crystal_description       plate
_exptl_crystal_F_000             2244
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.572
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1547
_refine_ls_number_reflns         21595
_refine_ls_number_restraints     2123
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+18.1535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12997
_reflns_number_total             21595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc01685a2.cif
_cod_data_source_block           cr447
_cod_depositor_comments
'Adding full bibliography for 1574358--1574360.cif.'
_cod_original_formula_sum        'C50.50 H52 Al As7.09 F38 O4 Ta2'
_cod_database_code               1574360
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C45H44O4F37AlTa2As8
_cell_oxdiff_angle_alpha         63.108(2)
_cell_oxdiff_angle_beta          88.5641(18)
_cell_oxdiff_angle_gamma         76.6877(17)
_cell_oxdiff_length_a            11.4386(2)
_cell_oxdiff_length_b            18.7072(4)
_cell_oxdiff_length_c            19.1356(5)
_cell_oxdiff_measurement_reflns_used 22282
_cell_oxdiff_volume              3539.00(13)
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.658
_olex2_refinement_description
;
1. Restrained distances
 C40-C11 = C29-C11 = C36-C11 = C24-C9 = C25-C9 = C41-C9 = C39-C22 = C32-C22 =
 C37-C22 = C42-C14 = C23-C14 = C26-C14
 1.53 with sigma of 0.02
 C33-C30 = C35-C30 = C30-C21 = C38-C15 = C17-C15 = C19-C15
 1.53 with sigma of 0.02
 F57-C52 = F61-C52 = F62-C52
 1.33 with sigma of 0.02
 F6-C24 = F20-C24 = F1-C24 = F32-C41 = F27-C41 = F22-C41 = F23-C25 = F10-C25 =
 F15-C25 = F30-C36 = F35-C36 = F3-C36 = F34-C29 = F29-C29 = F19-C29 = F31-C40 =
 F18-C40 = F36-C40 = F33-C42 = F24-C42 = F16-C42 = F21-C23 = F5-C23 = F26-C23 =
 F13-C26 = F2-C26 = F8-C26 = F11-C37 = F14-C37 = F12-C37 = F25-C32 = F17-C32 =
 F9-C32 = F4-C39 = F28-C39 = F7-C39
 1.33 with sigma of 0.02
 C44-C43 = C46-C43 = C45-C43
 1.53 with sigma of 0.02
 C52-C51 = C54-C51 = C53-C51
 1.53 with sigma of 0.02
 F68-C56 = F64-C56 = F65-C56
 1.33 with sigma of 0.02
 C19-C17
 2.55 with sigma of 0.04
 C17-C38
 2.55 with sigma of 0.04
 C38-C19
 2.55 with sigma of 0.04
 C18-C34
 2.55 with sigma of 0.04
 C33-C21
 2.55 with sigma of 0.04
 C34-C7
 2.55 with sigma of 0.04
 C7-C18
 2.55 with sigma of 0.04
 C40-C36
 2.55 with sigma of 0.04
 C21-C35
 2.55 with sigma of 0.04
 C35-C33
 2.55 with sigma of 0.04
 C36-C29
 2.55 with sigma of 0.04
 C29-C40
 2.55 with sigma of 0.04
 C26-C42
 2.55 with sigma of 0.04
 F57-F62
 2.2 with sigma of 0.04
 C42-C23
 2.55 with sigma of 0.04
 C23-C26
 2.55 with sigma of 0.04
 F62-F61
 2.2 with sigma of 0.04
 F62-C51
 2.4 with sigma of 0.04
 C32-C37
 2.55 with sigma of 0.04
 C37-C39
 2.55 with sigma of 0.04
 C39-C32
 2.55 with sigma of 0.04
 C41-C24
 2.55 with sigma of 0.04
 C24-C25
 2.55 with sigma of 0.04
 C25-C41
 2.55 with sigma of 0.04
 F4-F28
 2.2 with sigma of 0.04
 F4-F7
 2.2 with sigma of 0.04
 F7-F28
 2.2 with sigma of 0.04
 F14-F12
 2.2 with sigma of 0.04
 F12-F11
 2.2 with sigma of 0.04
 F11-F14
 2.2 with sigma of 0.04
 F25-F17
 2.2 with sigma of 0.04
 F17-F9
 2.2 with sigma of 0.04
 F9-F25
 2.2 with sigma of 0.04
 F30-F35
 2.2 with sigma of 0.04
 F35-F3
 2.2 with sigma of 0.04
 F3-F30
 2.2 with sigma of 0.04
 F34-F29
 2.2 with sigma of 0.04
 F29-F19
 2.2 with sigma of 0.04
 F19-F34
 2.2 with sigma of 0.04
 F18-F36
 2.2 with sigma of 0.04
 F36-F31
 2.2 with sigma of 0.04
 F31-F18
 2.2 with sigma of 0.04
 F24-F16
 2.2 with sigma of 0.04
 F16-F33
 2.2 with sigma of 0.04
 F33-F24
 2.2 with sigma of 0.04
 F26-F21
 2.2 with sigma of 0.04
 F21-F5
 2.2 with sigma of 0.04
 F5-F26
 2.2 with sigma of 0.04
 F8-F2
 2.2 with sigma of 0.04
 F2-F13
 2.2 with sigma of 0.04
 F13-F8
 2.2 with sigma of 0.04
 F32-F22
 2.2 with sigma of 0.04
 F27-F32
 2.2 with sigma of 0.04
 F6-F1
 2.2 with sigma of 0.04
 F1-F20
 2.2 with sigma of 0.04
 F20-F6
 2.2 with sigma of 0.04
 F10-F23
 2.2 with sigma of 0.04
 F23-F15
 2.2 with sigma of 0.04
 F15-F10
 2.2 with sigma of 0.04
 F22-F27
 2.2 with sigma of 0.04
 F42-F39
 2.2 with sigma of 0.04
 F39-F38
 2.2 with sigma of 0.04
 F38-F42
 2.2 with sigma of 0.04
 C46-C44
 2.55 with sigma of 0.04
 C44-C45
 2.55 with sigma of 0.04
 C45-C46
 2.55 with sigma of 0.04
 C52-C54
 2.55 with sigma of 0.04
 C54-C53
 2.55 with sigma of 0.04
 C53-C52
 2.55 with sigma of 0.04
 F61-F57
 2.2 with sigma of 0.04
 F61-C51
 2.4 with sigma of 0.04
 F57-C51
 2.4 with sigma of 0.04
 C52-C53
 2.55 with sigma of 0.04
 F65-F68
 2.2 with sigma of 0.04
 F68-F64
 2.2 with sigma of 0.04
 F64-F65
 2.2 with sigma of 0.04
 C2-C15 \\sim C2-C15A
 with sigma of 0.02
 C15-C17 \\sim C15A-C17A
 with sigma of 0.02
 C15-C19 \\sim C15A-C19A
 with sigma of 0.02
 C15-C38 \\sim C15A-C38A
 with sigma of 0.02
 C2-C17 \\sim C2-C17A
 with sigma of 0.04
 C2-C19 \\sim C2-C19A
 with sigma of 0.04
 C2-C38 \\sim C2-C38A
 with sigma of 0.04
 C5-C27 \\sim C5-C65
 with sigma of 0.02
 C17-C19 \\sim C17A-C19A
 with sigma of 0.04
 C17-C38 \\sim C17A-C38A
 with sigma of 0.04
 C19-C38 \\sim C19A-C38A
 with sigma of 0.04
 C5-C28 \\sim C5-C64
 with sigma of 0.02
 F25-C32 \\sim F62-C52
 with sigma of 0.02
 C5-C31 \\sim C5-C63
 with sigma of 0.02
 C1-C20 \\sim C1-C66
 with sigma of 0.02
 F9-F25 \\sim F57-F62
 with sigma of 0.04
 F17-F25 \\sim F61-F62
 with sigma of 0.04
 C7-C20 \\sim C68-C66
 with sigma of 0.02
 C16-C30 \\sim C16-C59
 with sigma of 0.02
 C18-C20 \\sim C67-C66
 with sigma of 0.02
 C21-C30 \\sim C61-C59
 with sigma of 0.02
 C30-C33 \\sim C59-C60
 with sigma of 0.02
 F25-C22 \\sim F62-C51
 with sigma of 0.04
 C20-C34 \\sim C66-C69
 with sigma of 0.02
 C30-C35 \\sim C59-C62
 with sigma of 0.02
 C1-C7 \\sim C1-C68
 with sigma of 0.04
 C16-C21 \\sim C16-C61
 with sigma of 0.04
 C1-C18 \\sim C1-C67
 with sigma of 0.04
 C1-C34 \\sim C1-C69
 with sigma of 0.04
 C16-C33 \\sim C16-C60
 with sigma of 0.04
 C7-C18 \\sim C68-C67
 with sigma of 0.04
 C16-C35 \\sim C16-C62
 with sigma of 0.04
 C7-C34 \\sim C68-C69
 with sigma of 0.04
 C21-C33 \\sim C61-C60
 with sigma of 0.04
 C18-C34 \\sim C67-C69
 with sigma of 0.04
 C21-C35 \\sim C61-C62
 with sigma of 0.04
 C33-C35 \\sim C60-C62
 with sigma of 0.04
 Al1-O1 \\sim Al1-O5
 with sigma of 0.02
 O1-C11 \\sim O5-C43
 with sigma of 0.02
 F3-C36 \\sim F45-C45
 with sigma of 0.02
 C11-C29 \\sim C43-C44
 with sigma of 0.02
 C11-C36 \\sim C43-C45
 with sigma of 0.02
 C11-C40 \\sim C43-C46
 with sigma of 0.02
 F18-C40 \\sim F37-C46
 with sigma of 0.02
 F19-C29 \\sim F38-C44
 with sigma of 0.02
 F29-C29 \\sim F39-C44
 with sigma of 0.02
 F30-C36 \\sim F40-C45
 with sigma of 0.02
 F31-C40 \\sim F41-C46
 with sigma of 0.02
 F34-C29 \\sim F42-C44
 with sigma of 0.02
 F35-C36 \\sim F43-C45
 with sigma of 0.02
 F36-C40 \\sim F44-C46
 with sigma of 0.02
 Al1-C11 \\sim Al1-C43
 with sigma of 0.04
 O1-C29 \\sim O5-C44
 with sigma of 0.04
 O1-C36 \\sim O5-C45
 with sigma of 0.04
 O1-C40 \\sim O5-C46
 with sigma of 0.04
 F3-C11 \\sim F45-C43
 with sigma of 0.04
 F3-F30 \\sim F45-F40
 with sigma of 0.04
 F3-F35 \\sim F45-F43
 with sigma of 0.04
 C11-F18 \\sim C43-F37
 with sigma of 0.04
 C11-F19 \\sim C43-F38
 with sigma of 0.04
 C11-F29 \\sim C43-F39
 with sigma of 0.04
 C11-F30 \\sim C43-F40
 with sigma of 0.04
 C11-F31 \\sim C43-F41
 with sigma of 0.04
 C11-F34 \\sim C43-F42
 with sigma of 0.04
 C11-F35 \\sim C43-F43
 with sigma of 0.04
 C11-F36 \\sim C43-F44
 with sigma of 0.04
 F18-F31 \\sim F37-F41
 with sigma of 0.04
 F18-F36 \\sim F37-F44
 with sigma of 0.04
 F19-F29 \\sim F38-F39
 with sigma of 0.04
 F19-F34 \\sim F38-F42
 with sigma of 0.04
 F29-F34 \\sim F39-F42
 with sigma of 0.04
 F30-F35 \\sim F40-F43
 with sigma of 0.04
 F31-F36 \\sim F41-F44
 with sigma of 0.04
 C29-C36 \\sim C44-C45
 with sigma of 0.04
 C29-C40 \\sim C44-C46
 with sigma of 0.04
 C36-C40 \\sim C45-C46
 with sigma of 0.04
 O2-C14 \\sim O2-C47
 with sigma of 0.02
 F2-C26 \\sim F46-C49
 with sigma of 0.02
 F5-C23 \\sim F47-C48
 with sigma of 0.02
 F8-C26 \\sim F48-C49
 with sigma of 0.02
 F13-C26 \\sim F49-C49
 with sigma of 0.02
 F16-C42 \\sim F50-C50
 with sigma of 0.02
 C14-C23 \\sim C47-C48
 with sigma of 0.02
 C14-C26 \\sim C47-C49
 with sigma of 0.02
 C14-C42 \\sim C47-C50
 with sigma of 0.02
 F21-C23 \\sim F51-C48
 with sigma of 0.02
 F24-C42 \\sim F52-C50
 with sigma of 0.02
 F26-C23 \\sim F53-C48
 with sigma of 0.02
 F33-C42 \\sim F54-C50
 with sigma of 0.02
 O2-C23 \\sim O2-C48
 with sigma of 0.04
 O2-C26 \\sim O2-C49
 with sigma of 0.04
 O2-C42 \\sim O2-C50
 with sigma of 0.04
 F2-F8 \\sim F46-F48
 with sigma of 0.04
 F2-F13 \\sim F46-F49
 with sigma of 0.04
 F2-C14 \\sim F46-C47
 with sigma of 0.04
 F5-C14 \\sim F47-C47
 with sigma of 0.04
 F5-F21 \\sim F47-F51
 with sigma of 0.04
 F5-F26 \\sim F47-F53
 with sigma of 0.04
 F8-F13 \\sim F48-F49
 with sigma of 0.04
 F8-C14 \\sim F48-C47
 with sigma of 0.04
 F13-C14 \\sim F49-C47
 with sigma of 0.04
 F16-C14 \\sim F50-C47
 with sigma of 0.04
 F16-F24 \\sim F50-F52
 with sigma of 0.04
 F16-F33 \\sim F50-F54
 with sigma of 0.04
 C14-F21 \\sim C47-F51
 with sigma of 0.04
 C14-F24 \\sim C47-F52
 with sigma of 0.04
 C14-F26 \\sim C47-F53
 with sigma of 0.04
 C14-F33 \\sim C47-F54
 with sigma of 0.04
 F21-F26 \\sim F51-F53
 with sigma of 0.04
 F24-F33 \\sim F52-F54
 with sigma of 0.04
 C23-C26 \\sim C48-C49
 with sigma of 0.04
 C23-C42 \\sim C48-C50
 with sigma of 0.04
 C26-C42 \\sim C49-C50
 with sigma of 0.04
 Al1-O4 \\sim Al1-O6
 with sigma of 0.02
 F4-C39 \\sim F55-C54
 with sigma of 0.02
 F7-C39 \\sim F56-C54
 with sigma of 0.02
 O4-C22 \\sim O6-C51
 with sigma of 0.02
 F9-C32 \\sim F57-C52
 with sigma of 0.02
 F11-C37 \\sim F58-C53
 with sigma of 0.02
 F12-C37 \\sim F59-C53
 with sigma of 0.02
 F14-C37 \\sim F60-C53
 with sigma of 0.02
 F17-C32 \\sim F61-C52
 with sigma of 0.02
 F28-C39 \\sim F63-C54
 with sigma of 0.02
 C22-C32 \\sim C51-C52
 with sigma of 0.02
 C22-C37 \\sim C51-C53
 with sigma of 0.02
 C22-C39 \\sim C51-C54
 with sigma of 0.02
 Al1-C22 \\sim Al1-C51
 with sigma of 0.04
 F4-F7 \\sim F55-F56
 with sigma of 0.04
 F4-F28 \\sim F55-F63
 with sigma of 0.04
 F4-C22 \\sim F55-C51
 with sigma of 0.04
 F7-F28 \\sim F56-F63
 with sigma of 0.04
 F7-C22 \\sim F56-C51
 with sigma of 0.04
 O4-C32 \\sim O6-C52
 with sigma of 0.04
 O4-C37 \\sim O6-C53
 with sigma of 0.04
 O4-C39 \\sim O6-C54
 with sigma of 0.04
 F9-F17 \\sim F57-F61
 with sigma of 0.04
 F9-C22 \\sim F57-C51
 with sigma of 0.04
 F11-F12 \\sim F58-F59
 with sigma of 0.04
 F11-F14 \\sim F58-F60
 with sigma of 0.04
 F11-C22 \\sim F58-C51
 with sigma of 0.04
 F12-F14 \\sim F59-F60
 with sigma of 0.04
 F12-C22 \\sim F59-C51
 with sigma of 0.04
 F14-C22 \\sim F60-C51
 with sigma of 0.04
 F17-C22 \\sim F61-C51
 with sigma of 0.04
 F28-C22 \\sim F63-C51
 with sigma of 0.04
 C32-C37 \\sim C52-C53
 with sigma of 0.04
 C32-C39 \\sim C52-C54
 with sigma of 0.04
 C37-C39 \\sim C53-C54
 with sigma of 0.04
 Al1-O3 \\sim Al1-O7
 with sigma of 0.02
 F1-C24 \\sim F64-C56
 with sigma of 0.02
 O3-C9 \\sim O7-C55
 with sigma of 0.02
 F6-C24 \\sim F65-C56
 with sigma of 0.02
 F10-C25 \\sim F66-C57
 with sigma of 0.02
 C9-C24 \\sim C55-C56
 with sigma of 0.02
 C9-C25 \\sim C55-C57
 with sigma of 0.02
 C9-C41 \\sim C55-C58
 with sigma of 0.02
 F15-C25 \\sim F67-C57
 with sigma of 0.02
 F20-C24 \\sim F68-C56
 with sigma of 0.02
 F22-C41 \\sim F69-C58
 with sigma of 0.02
 F23-C25 \\sim F70-C57
 with sigma of 0.02
 F27-C41 \\sim F71-C58
 with sigma of 0.02
 F32-C41 \\sim F72-C58
 with sigma of 0.02
 F32-F60 \\sim F72-F60
 with sigma of 0.02
 Al1-C9 \\sim Al1-C55
 with sigma of 0.04
 F1-F6 \\sim F64-F65
 with sigma of 0.04
 F1-C9 \\sim F64-C55
 with sigma of 0.04
 F1-F20 \\sim F64-F68
 with sigma of 0.04
 O3-C24 \\sim O7-C56
 with sigma of 0.04
 O3-C25 \\sim O7-C57
 with sigma of 0.04
 O3-C41 \\sim O7-C58
 with sigma of 0.04
 F6-C9 \\sim F65-C55
 with sigma of 0.04
 F6-F20 \\sim F65-F68
 with sigma of 0.04
 F10-C9 \\sim F66-C55
 with sigma of 0.04
 F10-F15 \\sim F66-F67
 with sigma of 0.04
 F10-F23 \\sim F66-F70
 with sigma of 0.04
 C9-F15 \\sim C55-F67
 with sigma of 0.04
 C9-F20 \\sim C55-F68
 with sigma of 0.04
 C9-F22 \\sim C55-F69
 with sigma of 0.04
 C9-F23 \\sim C55-F70
 with sigma of 0.04
 C9-F27 \\sim C55-F71
 with sigma of 0.04
 C9-F32 \\sim C55-F72
 with sigma of 0.04
 F15-F23 \\sim F67-F70
 with sigma of 0.04
 F22-F27 \\sim F69-F71
 with sigma of 0.04
 F22-F32 \\sim F69-F72
 with sigma of 0.04
 F27-F32 \\sim F71-F72
 with sigma of 0.04
 C24-C25 \\sim C56-C57
 with sigma of 0.04
 C24-C41 \\sim C56-C58
 with sigma of 0.04
 C25-C41 \\sim C57-C58
 with sigma of 0.04
 C41-F60 \\sim C58-F60
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
F1 \\sim O3 \\sim F6 \\sim F10 \\sim C9 \\sim F15 \\sim F20 \\sim F22 \\sim F23
\\sim F27 \\sim C24 \\sim F32 \\sim C25 \\sim C41 \\sim F64 \\sim O7 \\sim F65
\\sim F66 \\sim C55 \\sim F67 \\sim F68 \\sim F69 \\sim F70 \\sim F71 \\sim C56
\\sim F72 \\sim C57 \\sim C58: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F2 \\sim F5 \\sim F8 \\sim F13 \\sim F16 \\sim C14 \\sim F21 \\sim F24 \\sim
F26 \\sim C23 \\sim F33 \\sim C26 \\sim C42 \\sim F46 \\sim F47 \\sim F48 \\sim
F49 \\sim F50 \\sim C47 \\sim F51 \\sim F52 \\sim F53 \\sim C48 \\sim F54 \\sim
C49 \\sim C50 \\sim O2: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
O1 \\sim F3 \\sim C11 \\sim F18 \\sim F19 \\sim F29 \\sim F30 \\sim F31 \\sim
F34 \\sim C29 \\sim F35 \\sim F36 \\sim C36 \\sim C40 \\sim O5 \\sim C43 \\sim
F37 \\sim F38 \\sim F39 \\sim F40 \\sim F41 \\sim F42 \\sim C44 \\sim F43 \\sim
F44 \\sim C45 \\sim C46 \\sim F45: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F4 \\sim F7 \\sim O4 \\sim F9 \\sim F11 \\sim F12 \\sim F14 \\sim F17 \\sim F25
\\sim F28 \\sim C22 \\sim C32 \\sim C37 \\sim C39 \\sim F55 \\sim F56 \\sim O6
\\sim F57 \\sim F58 \\sim F59 \\sim F60 \\sim F61 \\sim F62 \\sim F63 \\sim C51
\\sim C52 \\sim C53 \\sim C54: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C21 \\sim C30 \\sim C33 \\sim C59 \\sim C60 \\sim C61 \\sim C35 \\sim C62:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C5 \\sim C27 \\sim C28 \\sim C31 \\sim C63 \\sim C64 \\sim C65: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C7 \\sim C18 \\sim C20 \\sim C34 \\sim C66 \\sim C67 \\sim C68 \\sim C69:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C17 \\sim C17A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Uanis(C15) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C17A) \\sim Ueq,
Uanis(C38A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(As9)=Sof(As10)=Sof(As11)=Sof(As12)=Sof(Ta3)=Sof(Ta8)=1-FVAR(1)
 Sof(Ta1)=Sof(Ta2)=Sof(As3)=Sof(As4)=Sof(As5)=Sof(As6)=Sof(As7)=Sof(As8)=FVAR(1)
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C15A)=Sof(C17A)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=1-FVAR(2)
 Sof(C15)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(2)
 Fixed Sof: O1(0.6) F1(0.72) F2(0.67) O3(0.72) F3(0.6) F4(0.67) F5(0.67)
 F6(0.72) C7(0.58) H7A(0.58) H7B(0.58) H7C(0.58) F7(0.67) O4(0.67) F8(0.67)
 F9(0.67) F10(0.72) F11(0.67) F12(0.67) F13(0.67) F14(0.67) C9(0.72) F15(0.72)
 F16(0.67) F17(0.67) C11(0.6) F18(0.6) C14(0.67) F19(0.6) F20(0.72) F21(0.67)
 F22(0.72) F23(0.72) C18(0.58) H18A(0.58) H18B(0.58) H18C(0.58) F24(0.67)
 C20(0.58) F25(0.67) F26(0.67) F27(0.72) F28(0.67) F29(0.6) C21(0.56)
 H21A(0.56) H21B(0.56) H21C(0.56) C22(0.67) F30(0.6) F31(0.6) C23(0.67)
 C24(0.72) F32(0.72) C25(0.72) F33(0.67) C26(0.67) C27(0.77) H27A(0.77)
 H27B(0.77) H27C(0.77) F34(0.6) C28(0.77) H28A(0.77) H28B(0.77) H28C(0.77)
 C29(0.6) F35(0.6) C30(0.56) C31(0.77) H31A(0.77) H31B(0.77) H31C(0.77)
 C32(0.67) C33(0.56) H33A(0.56) H33B(0.56) H33C(0.56) F36(0.6) C34(0.58)
 H34A(0.58) H34B(0.58) H34C(0.58) C35(0.56) H35A(0.56) H35B(0.56) H35C(0.56)
 C36(0.6) C37(0.67) C39(0.67) C40(0.6) C41(0.72) C42(0.67) O5(0.4) C43(0.4)
 F37(0.4) F38(0.4) F39(0.4) F40(0.4) F41(0.4) F42(0.4) C44(0.4) F43(0.4)
 F44(0.4) C45(0.4) C46(0.4) F45(0.4) F46(0.33) F47(0.33) F48(0.33) F49(0.33)
 F50(0.33) C47(0.33) F51(0.33) F52(0.33) F53(0.33) C48(0.33) F54(0.33)
 C49(0.33) C50(0.33) F55(0.33) F56(0.33) O6(0.33) F57(0.33) F58(0.33) F59(0.33)
 F60(0.33) F61(0.33) F62(0.33) F63(0.33) C51(0.33) C52(0.33) C53(0.33)
 C54(0.33) F64(0.28) O7(0.28) F65(0.28) F66(0.28) C55(0.28) F67(0.28) F68(0.28)
 F69(0.28) F70(0.28) F71(0.28) C56(0.28) F72(0.28) C57(0.28) C58(0.28)
 C59(0.44) C60(0.44) H60A(0.44) H60B(0.44) H60C(0.44) C61(0.44) H61A(0.44)
 H61B(0.44) H61C(0.44) C62(0.44) H62A(0.44) H62B(0.44) H62C(0.44) C63(0.23)
 H63A(0.23) H63B(0.23) H63C(0.23) C64(0.23) H64A(0.23) H64B(0.23) H64C(0.23)
 C65(0.23) H65A(0.23) H65B(0.23) H65C(0.23) C66(0.42) C67(0.42) H67A(0.42)
 H67B(0.42) H67C(0.42) C68(0.42) H68A(0.42) H68B(0.42) H68C(0.42) C69(0.42)
 H69A(0.42) H69B(0.42) H69C(0.42)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C10(H10), C12(H12), C13(H13)
4.b Idealised Me refined with riding coordinates:
 C17(H17A,H17B,H17C)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C38(H38A,H38B,H38C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C), C69(H69A,H69B,H69C), C19A(H19D,H19E,H19F), C17A(H17D,H17E,H17F),
 C38A(H38D,H38E,H38F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 158 electrons were 
found in a volume of 507\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C6H4F2], 0.5[C5H12] per Asymmetric Unit 
which account for 158 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.4
_smtbx_masks_void_truncation_radius 1.4
_shelx_res_checksum              67516
_shelx_fab_checksum              7072
_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 1.925
_oxdiff_exptl_absorpt_empirical_full_min 0.545