Ring Expansion vs. Addition – Reactivity of a cyclo-P4 Complex Towards Pnictogenium Cations
Riesinger, Christoph; Erhard, Alexander; Scheer, Manfred; Chemical Communications  (2023) –; doi:10.1039/D3CC03369D

data_7131936
_publ_section_title
;
 Ring Expansion vs. Addition -- Reactivity of a cyclo-P4 Complex Towards
 Pnictogenium Cations
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03369D
_journal_year                    2023
_chemical_formula_moiety
'C31 H39 O2 P5 Ta, Al C14.88 F33.48 O4, 0.28(C4 F9)'
_chemical_formula_sum            'C47.01 H39 Al F36.01 O6 P5 Ta'
_chemical_formula_weight         1746.71
_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             2023-03-15
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-10 deposited with the CCDC.	2023-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                95.299(2)
_cell_angle_beta                 108.400(2)
_cell_angle_gamma                110.628(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9785(3)
_cell_length_b                   15.3177(3)
_cell_length_c                   15.6939(3)
_cell_measurement_reflns_used    23415
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.7300
_cell_measurement_theta_min      3.5830
_cell_volume                     3112.48(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.974
_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    -76.00  18.00   1.00    5.00    --  -40.72  77.00   0.00   94
  2  \w     10.00 117.00   1.00    5.00    --   40.72  57.00-120.00  107
  3  \w    -37.00  43.00   1.00    5.00    --   40.72 -38.00 120.00   80
  4  \w      6.00  93.00   1.00    5.00    --   40.72-133.00 107.00   87
  5  \w    -37.00  43.00   1.00    5.00    --   40.72 -38.00  90.00   80
  6  \w     83.00 178.00   1.00   20.00    --  104.78 111.00-120.00   95
  7  \w     20.00  80.00   1.00   20.00    --  104.78 -95.00-120.00   60
  8  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00-169.51  126
  9  \w     75.00 178.00   1.00   20.00    --  104.78  49.00 -26.14  103
 10  \w     76.00 178.00   1.00   20.00    --  104.78  45.00 120.00  102
 11  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00 -11.65  126
 12  \w     71.00 178.00   1.00   20.00    --  104.78  30.00  90.00  107
 13  \w     18.00 143.00   1.00   20.00    --  104.78 -87.00 -83.15  125
 14  \w     76.00 178.00   1.00   20.00    --  104.78  45.00  30.00  102
 15  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00  77.86  126
 16  \w     17.00 143.00   1.00   20.00    --  104.78 -88.00 158.24  126
 17  \w      6.00 121.00   1.00    5.00    --   40.72  75.00 -41.55  115
 18  \w      6.00 121.00   1.00    5.00    --   40.72  75.00 153.28  115
 19  \w      6.00 121.00   1.00    5.00    --   40.72  75.00  56.45  115
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0869125000
_diffrn_orient_matrix_UB_12      0.0032134000
_diffrn_orient_matrix_UB_13      -0.0827485000
_diffrn_orient_matrix_UB_21      -0.0358853000
_diffrn_orient_matrix_UB_22      0.0462833000
_diffrn_orient_matrix_UB_23      0.0666835000
_diffrn_orient_matrix_UB_31      0.0720787000
_diffrn_orient_matrix_UB_32      0.1001817000
_diffrn_orient_matrix_UB_33      -0.0013066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34318
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.881
_diffrn_reflns_theta_min         3.591
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.048
_exptl_absorpt_correction_T_max  0.789
_exptl_absorpt_correction_T_min  0.234
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.27a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'intense orange'
_exptl_crystal_density_diffrn    1.864
_exptl_crystal_description       plate
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.444
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.048
_refine_diff_density_max         1.695
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1478
_refine_ls_number_reflns         11896
_refine_ls_number_restraints     6336
_refine_ls_restrained_S_all      2.926
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+4.1262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11032
_reflns_number_total             11896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03369d2.cif
_cod_data_source_block           cr561_cua
_cod_original_cell_volume        3112.47(12)
_cod_database_code               7131936
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C47H39TaP5AlO6F36
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 O3-C4 = C5-F8 = O17-C18 = C23-F24 = C27-F29 = O31-C32
 1.35 with sigma of 0.02
 Al2-O3 = Al2-O17 = Al2-O45
 1.72 with sigma of 0.02
 C4-C5
 1.57 with sigma of 0.02
 C4-C9 = C18-C27
 1.56 with sigma of 0.02
 C4-C13 = C18-C19 = C18-C23 = C32-C33 = C32-C37 = C47-C51
 1.55 with sigma of 0.02
 Al2-O31
 1.73 with sigma of 0.02
 C5-F6 = C9-F10 = C23-F26 = C27-F30 = C46-F48 = C51-F52
 1.31 with sigma of 0.02
 C5-F7 = C13-F14 = C19-F21 = C33-F34 = C37-F38 = C41-F42 = C46-F50 = C51-F54 =
 C55-F57
 1.32 with sigma of 0.02
 C9-F11 = C13-F15 = C19-F20 = C23-F25 = C41-F43 = C46-F49 = C55-F58
 1.34 with sigma of 0.02
 C9-F12 = C13-F16 = C19-F22 = C27-F28 = C33-F35 = C33-F36 = C37-F39 = C37-F40 =
  C51-F53 = C55-F56
 1.33 with sigma of 0.02
 C32-C41 = C46-C47
 1.58 with sigma of 0.02
 C41-F44
 1.3 with sigma of 0.02
 O45-C47
 1.36 with sigma of 0.02
 C47-C55
 1.54 with sigma of 0.02
 F2-C2 = F3-C2 = F1-C2
 1.33 with sigma of 0.02
 C4B-C2
 1.53 with sigma of 0.02
 C4B-C3
 1.53 with sigma of 0.02
 F4-C3 = F5-C3 = F9-C3
 1.33 with sigma of 0.02
 O3-C5 = C4-F7 = C4-F16 = C18-F25
 2.41 with sigma of 0.04
 O3-C9 = C4-F14 = C18-F26 = O45-C55 = C47-F52
 2.36 with sigma of 0.04
 Al2-C4 = Al2-C18 = Al2-C32 = Al2-C47
 2.96 with sigma of 0.04
 O3-C13 = C18-F24 = O31-C37 = C32-F39 = O45-C51 = C47-F53 = C47-F56
 2.39 with sigma of 0.04
 C4-F6 = C4-F10 = C4-F12 = C18-F21 = C18-F22 = C18-F30 = C32-F34 = C32-F35 =
 C32-F44 = C47-F57 = C47-F58
 2.37 with sigma of 0.04
 C4-F8 = C4-F15 = O17-C23 = C18-F29 = C32-F43
 2.38 with sigma of 0.04
 C4-F11 = O17-C27 = C18-F20 = C32-F36 = C32-F40 = C47-F54
 2.4 with sigma of 0.04
 O17-C19 = O31-C33 = C32-F38
 2.35 with sigma of 0.04
 C18-F28 = O31-C41 = C32-F42
 2.42 with sigma of 0.04
 O45-C46
 2.43 with sigma of 0.04
 C46-C51
 2.53 with sigma of 0.04
 C46-C55
 2.55 with sigma of 0.04
 F2-F1
 2.2 with sigma of 0.04
 F1-F3
 2.2 with sigma of 0.04
 F3-F2
 2.2 with sigma of 0.04
 F4-F5
 2.2 with sigma of 0.04
 C4B-F1
 2.55 with sigma of 0.04
 C33-F35 \\sim C33A-F35A
 with sigma of 0.02
 C32-F35 \\sim C32-F35A
 with sigma of 0.04
 C5-F6 \\sim C4B-F1
 with sigma of 0.02
 F34-F35 \\sim F34A-F35A
 with sigma of 0.04
 F35-F36 \\sim F35A-F36A
 with sigma of 0.04
 C4-F6 \\sim C4B-F1
 with sigma of 0.04
 O3-C4 \\sim O17-C18 \\sim O31-C32 \\sim O45-C47
 with sigma of 0.03
 C4-F7 \\sim C4B-F1
 with sigma of 0.04
 O3-C4 \\sim O3-C4A
 with sigma of 0.02
 C4-F8 \\sim C4B-F1
 with sigma of 0.04
 C5-F7 \\sim C4B-F1
 with sigma of 0.02
 O3-C5 \\sim O3-C4B
 with sigma of 0.04
 C4-F10 \\sim C4B-F1
 with sigma of 0.04
 O3-C9 \\sim O3-C4B
 with sigma of 0.04
 O3-C13 \\sim O3-C4B
 with sigma of 0.04
 Al2-O3 \\sim Al2-O17 \\sim Al2-O31 \\sim Al2-O45
 with sigma of 0.02
 O3-O17 \\sim O3-O31 \\sim O3-O45 \\sim O17-O31 \\sim O17-O45 \\sim O31-O45
 with sigma of 0.04
 C4-F11 \\sim C4B-F1
 with sigma of 0.04
 C4-F12 \\sim C4B-F1
 with sigma of 0.04
 O3-C5 \\sim O3-C9 \\sim O3-C13 \\sim O17-C19 \\sim O17-C23 \\sim O17-C27 \\sim
O31-C33 \\sim O31-C37 ~
 O31-C41 \\sim O45-C46 \\sim O45-C51 \\sim O45-C55
 with sigma of 0.04
 C5-F8 \\sim C4B-F1
 with sigma of 0.02
 O3-C5 \\sim O3-C5A
 with sigma of 0.04
 O3-C9 \\sim O3-C9A
 with sigma of 0.04
 O3-C13 \\sim O3-C13A
 with sigma of 0.04
 C4-F14 \\sim C4B-F1
 with sigma of 0.04
 C4-F15 \\sim C4B-F1
 with sigma of 0.04
 C9-F10 \\sim C4B-F1
 with sigma of 0.02
 C4-F16 \\sim C4B-F1
 with sigma of 0.04
 Al2-C4 \\sim Al2-C18 \\sim Al2-C32 \\sim Al2-C47
 with sigma of 0.05
 C9-F11 \\sim C4B-F1
 with sigma of 0.02
 C4-C5 \\sim C4-C9 \\sim C4-C13 \\sim C18-C19 \\sim C18-C23 \\sim C18-C27 \\sim
C32-C33 \\sim C32-C37 ~
 C32-C41 \\sim C47-C46 \\sim C47-C51 \\sim C47-C55
 with sigma of 0.02
 C9-F12 \\sim C4B-F1
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C4-C9 \\sim C4A-C9A
 with sigma of 0.02
 C4-C13 \\sim C4A-C13A
 with sigma of 0.02
 C4-F6 \\sim C4A-F6A
 with sigma of 0.04
 C13-F14 \\sim C4B-F1
 with sigma of 0.02
 C4-F7 \\sim C4A-F7A
 with sigma of 0.04
 C4-F8 \\sim C4A-F8A
 with sigma of 0.04
 C13-F15 \\sim C4B-F1
 with sigma of 0.02
 C4-F10 \\sim C4A-F10A
 with sigma of 0.04
 C4-F11 \\sim C4A-F11A
 with sigma of 0.04
 C4-F12 \\sim C4A-F12A
 with sigma of 0.04
 C4-F14 \\sim C4A-F14A
 with sigma of 0.04
 C4-F15 \\sim C4A-F15A
 with sigma of 0.04
 C13-F16 \\sim C4B-F1
 with sigma of 0.02
 C4-F16 \\sim C4A-F16A
 with sigma of 0.04
 C5-C9 \\sim C5-C13 \\sim C9-C13 \\sim C19-C23 \\sim C19-C27 \\sim C23-C27
\\sim C33-C37 \\sim C33-C41 ~
 C37-C41 \\sim C46-C51 \\sim C46-C55 \\sim C51-C55
 with sigma of 0.04
 C5-F6 \\sim C5-F7 \\sim C5-F8 \\sim C9-F10 \\sim C9-F11 \\sim C9-F12 \\sim
C13-F14 \\sim C13-F15 \\sim C13-
 F16 \\sim C19-F20 \\sim C19-F21 \\sim C19-F22 \\sim C23-F24 \\sim C23-F25
\\sim C23-F26 \\sim C27-F28 ~
 C27-F29 \\sim C27-F30 \\sim C33-F34 \\sim C33-F35 \\sim C33-F36 \\sim C37-F38
\\sim C37-F39 \\sim C37-F40
 \\sim C41-F42 \\sim C41-F43 \\sim C41-F44 \\sim C46-F48 \\sim C46-F49 \\sim
C46-F50 \\sim C51-F52 \\sim C51-
 F53 \\sim C51-F54 \\sim C55-F56 \\sim C55-F57 \\sim C55-F58
 with sigma of 0.02
 F6-F7 \\sim F7-F8 \\sim F8-F6 \\sim F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim
F14-F15 \\sim F15-F16 \\sim F16-
 F14 \\sim F20-F21 \\sim F21-F22 \\sim F22-F20 \\sim F24-F25 \\sim F25-F26
\\sim F26-F24 \\sim F28-F29 ~
 F29-F30 \\sim F30-F28
 with sigma of 0.04
 C46-C47 \\sim C46A-C47
 with sigma of 0.02
 C46-F48 \\sim C46A-F48A
 with sigma of 0.02
 C46-F49 \\sim C46A-F49A
 with sigma of 0.02
 C46-F50 \\sim C46A-F50A
 with sigma of 0.02
 C47-C51 \\sim C47-C51A
 with sigma of 0.02
 C47-C55 \\sim C47-C55A
 with sigma of 0.02
 C51-F52 \\sim C51A-F52A
 with sigma of 0.02
 C51-F53 \\sim C51A-F53A
 with sigma of 0.02
 C51-F54 \\sim C51A-F54A
 with sigma of 0.02
 C55-F56 \\sim C55A-F56A
 with sigma of 0.02
 C55-F57 \\sim C55A-F57A
 with sigma of 0.02
 C55-F58 \\sim C55A-F58A
 with sigma of 0.02
 C47-F48 \\sim C47-F48A
 with sigma of 0.04
 C47-F49 \\sim C47-F49A
 with sigma of 0.04
 C47-F50 \\sim C47-F50A
 with sigma of 0.04
 C47-F52 \\sim C47-F52A
 with sigma of 0.04
 C47-F53 \\sim C47-F53A
 with sigma of 0.04
 C47-F54 \\sim C47-F54A
 with sigma of 0.04
 C47-F56 \\sim C47-F56A
 with sigma of 0.04
 C47-F57 \\sim C47-F57A
 with sigma of 0.04
 C47-F58 \\sim C47-F58A
 with sigma of 0.04
 F48-F49 \\sim F48A-F49A
 with sigma of 0.04
 F48-F50 \\sim F48A-F50A
 with sigma of 0.04
 F49-F50 \\sim F49A-F50A
 with sigma of 0.04
 F52-F53 \\sim F52A-F53A
 with sigma of 0.04
 F52-F54 \\sim F52A-F54A
 with sigma of 0.04
 F53-F54 \\sim F53A-F54A
 with sigma of 0.04
 F56-F57 \\sim F56A-F57A
 with sigma of 0.04
 F56-F58 \\sim F56A-F58A
 with sigma of 0.04
 F57-F58 \\sim F57A-F58A
 with sigma of 0.04
 C5-F6 \\sim C5A-F6A
 with sigma of 0.02
 C5-F7 \\sim C5A-F7A
 with sigma of 0.02
 C5-F8 \\sim C5A-F8A
 with sigma of 0.02
 C9-F10 \\sim C9A-F10A
 with sigma of 0.02
 C9-F11 \\sim C9A-F11A
 with sigma of 0.02
 C9-F12 \\sim C9A-F12A
 with sigma of 0.02
 C13-F14 \\sim C13A-F14A
 with sigma of 0.02
 C13-F15 \\sim C13A-F15A
 with sigma of 0.02
 C13-F16 \\sim C13A-F16A
 with sigma of 0.02
 C5-C9 \\sim C5A-C9A
 with sigma of 0.04
 C5-C13 \\sim C5A-C13A
 with sigma of 0.04
 F6-F7 \\sim F6A-F7A
 with sigma of 0.04
 F6-F8 \\sim F6A-F8A
 with sigma of 0.04
 F7-F8 \\sim F7A-F8A
 with sigma of 0.04
 C9-C13 \\sim C9A-C13A
 with sigma of 0.04
 F10-F11 \\sim F10A-F11A
 with sigma of 0.04
 F10-F12 \\sim F10A-F12A
 with sigma of 0.04
 F11-F12 \\sim F11A-F12A
 with sigma of 0.04
 F14-F15 \\sim F14A-F15A
 with sigma of 0.04
 F14-F16 \\sim F14A-F16A
 with sigma of 0.04
 F15-F16 \\sim F15A-F16A
 with sigma of 0.04
 C32-C33 \\sim C32-C33A
 with sigma of 0.02
 C32-C37 \\sim C32-C37A
 with sigma of 0.02
 C32-C41 \\sim C32-C41A
 with sigma of 0.02
 C33-F34 \\sim C33A-F34A
 with sigma of 0.02
 C33-F36 \\sim C33A-F36A
 with sigma of 0.02
 C37-F38 \\sim C37A-F38A
 with sigma of 0.02
 C37-F39 \\sim C37A-F39A
 with sigma of 0.02
 C37-F40 \\sim C37A-F40A
 with sigma of 0.02
 C41-F42 \\sim C41A-F42A
 with sigma of 0.02
 C41-F43 \\sim C41A-F43A
 with sigma of 0.02
 C41-F44 \\sim C41A-F44A
 with sigma of 0.02
 C32-F34 \\sim C32-F34A
 with sigma of 0.04
 C32-F36 \\sim C32-F36A
 with sigma of 0.04
 C32-F38 \\sim C32-F38A
 with sigma of 0.04
 C32-F39 \\sim C32-F39A
 with sigma of 0.04
 C32-F40 \\sim C32-F40A
 with sigma of 0.04
 C32-F42 \\sim C32-F42A
 with sigma of 0.04
 C32-F43 \\sim C32-F43A
 with sigma of 0.04
 C32-F44 \\sim C32-F44A
 with sigma of 0.04
 F34-F36 \\sim F34A-F36A
 with sigma of 0.04
 F38-F39 \\sim F38A-F39A
 with sigma of 0.04
 F38-F40 \\sim F38A-F40A
 with sigma of 0.04
 F39-F40 \\sim F39A-F40A
 with sigma of 0.04
 F42-F43 \\sim F42A-F43A
 with sigma of 0.04
 F42-F44 \\sim F42A-F44A
 with sigma of 0.04
 F43-F44 \\sim F43A-F44A
 with sigma of 0.04
 C18-C19 \\sim C18-C19A
 with sigma of 0.02
 C18-C23 \\sim C18-C23A
 with sigma of 0.02
 C18-C27 \\sim C18-C27A
 with sigma of 0.02
 C19-F20 \\sim C19A-F20A
 with sigma of 0.02
 C19-F21 \\sim C19A-F21A
 with sigma of 0.02
 C19-F22 \\sim C19A-F22A
 with sigma of 0.02
 C23-F24 \\sim C23A-F24A
 with sigma of 0.02
 C23-F25 \\sim C23A-F25A
 with sigma of 0.02
 C23-F26 \\sim C23A-F26A
 with sigma of 0.02
 C27-F28 \\sim C27A-F28A
 with sigma of 0.02
 C27-F29 \\sim C27A-F29A
 with sigma of 0.02
 C27-F30 \\sim C27A-F30A
 with sigma of 0.02
 C18-F20 \\sim C18-F20A
 with sigma of 0.04
 C18-F21 \\sim C18-F21A
 with sigma of 0.04
 C18-F22 \\sim C18-F22A
 with sigma of 0.04
 C18-F24 \\sim C18-F24A
 with sigma of 0.04
 C18-F25 \\sim C18-F25A
 with sigma of 0.04
 C18-F26 \\sim C18-F26A
 with sigma of 0.04
 C18-F28 \\sim C18-F28A
 with sigma of 0.04
 C18-F29 \\sim C18-F29A
 with sigma of 0.04
 C18-F30 \\sim C18-F30A
 with sigma of 0.04
 F20-F21 \\sim F20A-F21A
 with sigma of 0.04
 F20-F22 \\sim F20A-F22A
 with sigma of 0.04
 F21-F22 \\sim F21A-F22A
 with sigma of 0.04
 F24-F25 \\sim F24A-F25A
 with sigma of 0.04
 F24-F26 \\sim F24A-F26A
 with sigma of 0.04
 F25-F26 \\sim F25A-F26A
 with sigma of 0.04
 F28-F29 \\sim F28A-F29A
 with sigma of 0.04
 F28-F30 \\sim F28A-F30A
 with sigma of 0.04
 F29-F30 \\sim F29A-F30A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C32 \\sim C33 \\sim F34 \\sim F35 \\sim F36 \\sim C37 \\sim F38 \\sim F39 \\sim
F40 \\sim C41 \\sim F42 \\sim F43 \\sim F44 \\sim C33A \\sim F34A \\sim F35A
\\sim F36A \\sim C37A \\sim F38A \\sim F39A \\sim F40A \\sim C41A \\sim F42A
\\sim F43A \\sim F44A: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
Al2 \\sim O3 \\sim C4 \\sim C5 \\sim F6 \\sim F7 \\sim F8 \\sim C9 \\sim F10
\\sim F11 \\sim F12 \\sim C13 \\sim F14 \\sim F15 \\sim F16 \\sim O17 \\sim C18
\\sim C19 \\sim F20 \\sim F21 \\sim F22 \\sim C23 \\sim F24 \\sim F25 \\sim F26
\\sim C27 \\sim F28 \\sim F29 \\sim F30 \\sim O31 \\sim C32 \\sim C33 \\sim F34
\\sim F35 \\sim F36 \\sim C37 \\sim F38 \\sim F39 \\sim F40 \\sim C41 \\sim F42
\\sim F43 \\sim F44 \\sim O45 \\sim C46 \\sim C47 \\sim F48 \\sim F49 \\sim F50
\\sim C51 \\sim F52 \\sim F53 \\sim F54 \\sim C55 \\sim F56 \\sim F57 \\sim
F58: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
P002 \\sim P003 \\sim P005 \\sim P004 \\sim P006: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 1.7A
Ta \\sim Ta01: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
P0A \\sim P003: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
P1A \\sim P005: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
P4A \\sim P002: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
P2A \\sim P3A: within 2.5A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2.5A
P004 \\sim P2A: within 2.5A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2.5A
P3A \\sim P006: within 2.5A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2.5A
C4 \\sim C5 \\sim F6 \\sim F7 \\sim F8 \\sim C9 \\sim F10 \\sim F11 \\sim F12
\\sim C13 \\sim F14 \\sim F15 \\sim F16 \\sim C4A \\sim C5A \\sim F6A \\sim F7A
\\sim F8A \\sim C9A \\sim F10A \\sim F11A \\sim F12A \\sim C13A \\sim F14A
\\sim F15A \\sim F16A \\sim C4B \\sim C2 \\sim F1 \\sim F2 \\sim F3 \\sim C3
\\sim F4 \\sim F5 \\sim F9 \\sim C6 \\sim F13 \\sim F17 \\sim F18: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C46 \\sim C47 \\sim F48 \\sim F49 \\sim F50 \\sim C51 \\sim F52 \\sim F53 \\sim
F54 \\sim C55 \\sim F56 \\sim F57 \\sim F58 \\sim C46A \\sim F48A \\sim F49A
\\sim F50A \\sim C51A \\sim F52A \\sim F53A \\sim F54A \\sim C55A \\sim F56A
\\sim F57A \\sim F58A: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
C18 \\sim C19 \\sim F20 \\sim F21 \\sim F22 \\sim C23 \\sim F24 \\sim F25 \\sim
F26 \\sim C27 \\sim F28 \\sim F29 \\sim F30 \\sim C19A \\sim F20A \\sim F21A
\\sim F22A \\sim C23A \\sim F24A \\sim F25A \\sim F26A \\sim C27A \\sim F28A
\\sim F29A \\sim F30A: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
Uanis(O1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F35A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 Al2, O3, C4, C5, F6, F7, F8, C9, F10, F11, F12, C13, F14, F15, F16, O17, C18,
 C19, F20, F21, F22, C23, F24, F25, F26, C27, F28, F29, F30, O31, C32, C33, F34,
  F35, F36, C37, F38, F39, F40, C41, F42, F43, F44, O45, C46, C47, F48, F49,
 F50, C51, F52, F53, F54, C55, F56, F57, F58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Ta)=Sof(P2A)=Sof(P4A)=Sof(P0A)=Sof(P1A)=Sof(P3A)=1-FVAR(1)
 Sof(Ta01)=Sof(P002)=Sof(P003)=Sof(P004)=Sof(P005)=Sof(P006)=FVAR(1)
 Fixed Sof: O3(0.62) C4(0.38) C5(0.38) F6(0.38) F7(0.38) F8(0.38) C9(0.38)
 F10(0.38) F11(0.38) F12(0.38) C13(0.38) F14(0.38) F15(0.38) F16(0.38) C19(0.7)
 F20(0.7) F21(0.7) F22(0.7) C23(0.7) F24(0.7) F25(0.7) F26(0.7) C27(0.7)
 F28(0.7) F29(0.7) F30(0.7) O31(0.75) C33(0.75) F34(0.75) F35(0.75) F36(0.75)
 C37(0.75) F38(0.75) F39(0.75) F40(0.75) C41(0.75) F42(0.75) F43(0.75)
 F44(0.75) C46(0.29) F48(0.29) F49(0.29) F50(0.29) C51(0.29) F52(0.29)
 F53(0.29) F54(0.29) C55(0.29) F56(0.29) F57(0.29) F58(0.29) C46A(0.71)
 F48A(0.71) F49A(0.71) F50A(0.71) C51A(0.71) F52A(0.71) F53A(0.71) F54A(0.71)
 C55A(0.71) F56A(0.71) F57A(0.71) F58A(0.71) C4A(0.34) C5A(0.34) F6A(0.34)
 F7A(0.34) F8A(0.34) C9A(0.34) F10A(0.34) F11A(0.34) F12A(0.34) C13A(0.34)
 F14A(0.34) F15A(0.34) F16A(0.34) C33A(0.25) F34A(0.25) F35A(0.25) F36A(0.25)
 C37A(0.25) F38A(0.25) F39A(0.25) F40A(0.25) C41A(0.25) F42A(0.25) F43A(0.25)
 F44A(0.25) O1(0.38) O2(0.25) C19A(0.3) F20A(0.3) F21A(0.3) F22A(0.3) C23A(0.3)
 F24A(0.3) F25A(0.3) F26A(0.3) C27A(0.3) F28A(0.3) F29A(0.3) F30A(0.3)
 C4B(0.28) C2(0.28) F1(0.28) F2(0.28) F3(0.28) C3(0.28) F4(0.28) F5(0.28)
 F9(0.28) C6(0.28) F13(0.28) F17(0.28) F18(0.28)
 Fixed X: Ta(-0.818079) P2A(-0.841189) P4A(-0.710071) P0A(-0.654) P1A(-
 0.646719) P3A(-0.75922) O1(-0.263331) C4B(-0.26274) F1(-0.3195)
 Fixed Y: Ta(0.347589) P2A(0.445499) P4A(0.435679) P0A(0.373449) P1A(0.4733)
 P3A(0.52217) O1(0.26368) C4B(0.33795) F1(0.24894)
 Fixed Z: Ta(-0.489639) P2A(-0.3552) P4A(-0.253) P0A(-0.344739) P1A(-0.428619)
 P3A(-0.438709) O1(-0.09492) C4B(-0.026431) F1(0.06155)
5.a Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00N(H00N), C00Z(H00Z), C011(H011), C014(H014), C01H(H01J),
 C01J(H01N), C01R(H01R), C01W(H01W), C01Z(H01Z), C020(H020), C029(H029)
5.b Idealised Me refined as rotating group:
 C00V(H00A,H00B,H00C), C01A(H01A,H01B,H01C), C01B(H01D,H01E,H01F), C01F(H01G,
 H01H,H01I), C01I(H01K,H01L,H01M), C01S(H01O,H01P,H01Q), C01T(H01S,H01T,H01U),
 C01Y(H01V,H01X,H01Y), C022(H02A,H02B,H02C)
;
_shelx_res_checksum              89632
_shelx_hkl_checksum              44836
_olex2_date_sample_data_collection 2020-08-13
_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 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.720