Metallation of sensitive fluoroarenes using a potassium TMP-zincate supported by a silyl(bis)amido ligand
Mastropierro, Pasquale; Kennedy, Alan R.; Hevia, Eva; Chemical Communications  (2022) –; doi:10.1039/D2CC00979J

data_7129963
_publ_section_title
;
 Metallation of sensitive fluoroarenes using a potassium TMP-zincate
 supported by a silyl(bis)amido ligand
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00979J
_journal_year                    2022
_chemical_formula_moiety         'C42 H47 F2 N2 Si Zn, C24 H48 K O6'
_chemical_formula_sum            'C66 H95 F2 K N2 O6 Si Zn'
_chemical_formula_weight         1182.99
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-03T16:39:47-00:00
_audit_update_record
;
2022-03-04 deposited with the CCDC.	2022-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.4963(14)
_cell_angle_beta                 93.1729(12)
_cell_angle_gamma                92.1929(12)
_cell_formula_units_Z            4
_cell_length_a                   18.6356(2)
_cell_length_b                   18.8587(3)
_cell_length_c                   18.8788(3)
_cell_measurement_reflns_used    42773
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      76.484
_cell_measurement_theta_min      2.296
_cell_volume                     6619.42(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15(10)
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -75.00 -17.00   0.50    2.00    --  -23.00 134.00  92.00  116
  2  \w    -76.00 -18.00   0.50    2.00    --  -23.00 136.00 -89.00  116
  3  \w    -94.00  -8.00   0.50    2.00    --  -23.00 -57.00 120.00  172
  4  \w    -95.00 -10.00   0.50    2.00    --  -23.00 -45.00-120.00  170
  5  \w    -38.00  50.00   0.50    2.00    --  -23.00  57.00  30.00  176
  6  \w     -7.00  27.00   0.50    2.00    --   26.00  98.00 -36.72   68
  7  \w      9.00  42.00   0.50    2.00    --   38.00  91.00 -63.06   66
  8  \w      8.00  34.00   0.50    2.00    --   38.00  93.00  67.06   52
  9  \w     17.00  43.00   0.50    2.00    --   46.00  90.00-173.96   52
 10  \w     25.00 121.00   0.50    2.00    --   47.92  77.00 150.00  192
 11  \w     25.00 121.00   0.50    2.00    --   47.92  77.00  90.00  192
 12  \w     -1.00  81.00   0.50    2.00    --   47.92 -99.00 120.00  164
 13  \w     -1.00  81.00   0.50    2.00    --   47.92 -99.00 -60.00  164
 14  \w     27.00 122.00   0.50    2.00    --   50.00  77.00 -43.73  190
 15  \w     31.00 126.00   0.50    2.00    --   54.00  77.00   0.72  190
 16  \w     36.00 131.00   0.50    2.00    --   58.00  75.00 -82.29  190
 17  \w     36.00 131.00   0.50    2.00    --   58.00  76.00-109.29  190
 18  \w     35.00 131.00   0.50    2.00    --   58.00  77.00  31.57  192
 19  \w     40.00 135.00   0.50    2.00    --   62.00  75.00  93.91  190
 20  \w     44.00 139.00   0.50    2.00    --   66.00  75.00 -25.22  190
 21  \w     44.00 139.00   0.50    2.00    --   66.00  76.00  -6.76  190
 22  \w     44.00 139.00   0.50    2.00    --   66.00  76.00 141.03  190
 23  \w     43.00 139.00   0.50    2.00    --   66.00  77.00 159.69  192
 24  \w     44.00 139.00   0.50    2.00    --   66.00  76.00 -47.00  190
 25  \w     48.00 143.00   0.50    2.00    --   70.00  76.00  50.77  190
 26  \w     48.00 143.00   0.50    2.00    --   70.00  76.00-154.03  190
 27  \w     47.00 143.00   0.50    2.00    --   70.00  77.00 -92.34  192
 28  \w     48.00 143.00   0.50    2.00    --   70.00  75.00 107.74  190
 29  \w     48.00 143.00   0.50    2.00    --   70.00  76.00  79.52  190
 30  \w     48.00 143.00   0.50    2.00    --   70.00  75.00-177.56  190
 31  \w     48.00 143.00   0.50    2.00    --   70.00  76.00-120.16  190
 32  \w     53.00 146.00   0.50    2.00    --   74.00  73.00  12.94  186
 33  \w     64.00 151.00   0.50    2.00    --   78.00  54.00  87.99  174
 34  \w     58.00 151.00   0.50    2.00    --   78.00  71.00 -21.58  186
 35  \w     67.00 159.00   0.50   12.00    --   86.00  68.00 130.62  184
 36  \w     68.00 159.00   0.50   12.00    --   86.00  66.00 119.74  182
 37  \w     69.00  95.00   0.50   12.00    --   86.00  62.00 172.31   52
 38  \w     68.00 109.00   0.50   12.00    --   86.00  65.00 -56.28   82
 39  \w     68.00 108.00   0.50   12.00    --  102.00-108.00   8.80   80
 40  \w     29.00  62.00   0.50   12.00    --  102.00-108.00   8.80   66
 41  \w     43.00 107.00   0.50   12.00    --  113.25-103.00 -36.29  128
 42  \w     62.00 106.00   0.50   12.00    --  113.25 -94.00 150.00   88
 43  \w     97.00 163.00   0.50   12.00    --  113.25  61.00 -60.00  132
 44  \w     97.00 155.00   0.50   12.00    --  113.25  61.00-180.00  116
 45  \w     97.00 157.00   0.50   12.00    --  113.25  61.00  90.00  120
 46  \w     97.00 162.00   0.50   12.00    --  113.25  61.00 -90.00  130
 47  \w     42.00 105.00   0.50   12.00    --  113.25 -94.00-120.00  126
 48  \w    127.00 174.00   0.50   12.00    --  113.25  77.00  90.00   94
 49  \w     91.00 117.00   0.50   12.00    --  113.25  77.00  90.00   52
 50  \w    128.00 176.00   0.50   12.00    --  113.25  77.00 -90.00   96
 51  \w     92.00 119.00   0.50   12.00    --  113.25  77.00 -90.00   54
 52  \w    132.00 177.00   0.50   12.00    --  113.25  77.00-180.00   90
 53  \w     97.00 123.00   0.50   12.00    --  113.25  61.00  60.00   52
 54  \w    127.00 163.00   0.50   12.00    --  113.25  61.00  60.00   72
 55  \w     97.00 167.00   0.50   12.00    --  113.25  61.00 150.00  140
 56  \w     43.00  95.00   0.50   12.00    --  113.25 -77.00   0.00  104
 57  \w     91.00 116.00   0.50   12.00    --  113.25  77.00-180.00   50
 58  \w     98.00 159.00   0.50   12.00    --  113.25  61.00 -30.00  122
 59  \w     43.00 106.00   0.50   12.00    --  113.25 -94.00   0.00  126
 60  \w    137.00 176.00   0.50   12.00    --  113.25  77.00-150.00   78
 61  \w     91.00 122.00   0.50   12.00    --  113.25  77.00-150.00   62
 62  \w     44.00  93.00   0.50   12.00    --  113.25 -77.00-180.00   98
 63  \w     42.00  79.00   0.50   12.00    --  113.25 -77.00  90.00   74
 64  \w     97.00 168.00   0.50   12.00    --  113.25  61.00   0.00  142
 65  \w    130.00 176.00   0.50   12.00    --  113.25  77.00  60.00   92
 66  \w     42.00 105.00   0.50   12.00    --  113.25 -94.00  90.00  126
 67  \w     77.00 102.00   0.50   12.00    --  113.25 -77.00 150.00   50
 68  \w    131.00 177.00   0.50   12.00    --  113.25  77.00-120.00   92
 69  \w     91.00 118.00   0.50   12.00    --  113.25  77.00  60.00   54
 70  \w     91.00 125.00   0.50   12.00    --  113.25  77.00-120.00   68
 71  \w    134.00 177.00   0.50   12.00    --  113.25  61.00 120.00   86
 72  \w     97.00 164.00   0.50   12.00    --  113.25  61.00-150.00  134
 73  \w     80.00 106.00   0.50   12.00    --  113.25 -94.00 -90.00   52
 74  \w    103.00 131.00   0.50   12.00    --  113.25  61.00 120.00   56
 75  \w     81.00 106.00   0.50   12.00    --  113.25 -94.00-150.00   50
 76  \w    137.00 174.00   0.50   12.00    --  113.25  77.00  30.00   74
 77  \w    128.00 177.00   0.50   12.00    --  113.25  77.00   0.00   98
 78  \w     44.00  70.00   0.50   12.00    --  113.25 -94.00-150.00   52
 79  \w     42.00  96.00   0.50   12.00    --  113.25 -77.00  30.00  108
 80  \w     42.00  81.00   0.50   12.00    --  113.25 -77.00 -90.00   78
 81  \w     42.00  70.00   0.50   12.00    --  113.25 -77.00 150.00   56
 82  \w     91.00 116.00   0.50   12.00    --  113.25  77.00  30.00   50
 83  \w     42.00 108.00   0.50   12.00    --  113.25-108.00 162.40  132
 84  \w     77.00 105.00   0.50   12.00    --  113.25 -94.00  60.00   56
 85  \w     91.00 122.00   0.50   12.00    --  113.25  77.00   0.00   62
 86  \w     43.00  76.00   0.50   12.00    --  113.25 -94.00 -90.00   66
 87  \w    127.00 175.00   0.50   12.00    --  113.25  77.00 -60.00   96
 88  \w     91.00 116.00   0.50   12.00    --  113.25  77.00 -60.00   50
 89  \w     43.00  69.00   0.50   12.00    --  113.25 -94.00  60.00   52
 90  \w    127.00 170.00   0.50   12.00    --  113.25  61.00  30.00   86
 91  \w     97.00 122.00   0.50   12.00    --  113.25  61.00  30.00   50
 92  \w    134.00 174.00   0.50   12.00    --  113.25  77.00 -30.00   80
 93  \w     91.00 176.00   0.50   12.00    --  113.25  77.00 150.00  170
 94  \w     91.00 130.00   0.50   12.00    --  113.25  77.00 -30.00   78
 95  \w     91.00 142.00   0.50   12.00    --  113.25  77.00 120.00  102
 96  \w     97.00 166.00   0.50   12.00    --  113.25  61.00-120.00  138
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            236341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.132
_diffrn_reflns_theta_min         2.344
_exptl_absorpt_coefficient_mu    1.681
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
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            colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.1
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1456
_refine_ls_number_reflns         24646
_refine_ls_number_restraints     520
_refine_ls_restrained_S_all      1.388
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.1143
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3376
_refine_ls_wR_factor_ref         0.3734
_reflns_Friedel_coverage         0
_reflns_number_gt                14948
_reflns_number_total             24646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00979j2.cif
_cod_data_source_block           22EH020_PM489
_cod_original_cell_volume        6619.39(18)
_cod_database_code               7129963
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.87
_oxdiff_exptl_absorpt_empirical_details
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
        1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
        2. Restrained distances
 C1A-C1B = C1C-C1D = C1B-C51 = C1C-C1E
 1.53 with sigma of 0.001
 O6A-C1E = O6A-C51
 1.44 with sigma of 0.001
 C1B-C1C
 1.54 with sigma of 0.001
 O6-C1A = O6-C1D
 1.44 with sigma of 0.001
 O6-C1B = O6-C1C = C1A-C1C = C1B-C1D
 2.38 with sigma of 0.001
 C102-C101 \\sim C104-C103
 with sigma of 0.002
 C1B-C1D \\sim C1A-C1C
 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D
 with sigma of 0.02
 O6-C1A \\sim O6-C1D
 with sigma of 0.02
 O6-C1B \\sim O6-C1C
 with sigma of 0.04
 O8-C101 \\sim O8-C104
 with sigma of 0.002
 C99-C98 \\sim C119-C118 \\sim C107-C106 \\sim C111-C110 \\sim C103-C102 \\sim
        C115-C114 \\sim C43-C44
 with sigma of 0.002
        3. Rigid bond restraints
 F2, C6, C1, C5, C4, C3, C2, F1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O4, C46, C45, C44, C43
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O12, C117, C118, C119, C120
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C116, C115, C114, C113, O11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C128, C127, C126, O2, C129
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, C122, C124, C123, C125
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C36, C38, C37, C31, C32, C33, C34, C35, C30, C39, C41, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C101, C102, C103, C104, O8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
        4. Uiso/Uaniso restraints and constraints
O6 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
        sigma for terminal atoms of 0.08 within 2A
Uanis(O6A) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C1E) \\sim Ueq: with sigma of
        0.02 and sigma for terminal atoms of 0.02
Uanis(C83) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C1D) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of
        0.01 and sigma for terminal atoms of 0.02
Uanis(C45) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C101) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C103) \\sim Ueq: with sigma
        of 0.01 and sigma for terminal atoms of 0.02
Uanis(C84) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for terminal
        atoms of 0.02
Uanis(F2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O11) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C99) \\sim Ueq,
Uanis(C49) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C111) \\sim Ueq: with sigma of 0.01 and
        sigma for terminal atoms of 0.02
Uanis(C44) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C129) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(C97) \\sim Ueq,
Uanis(C108) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C27)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C117) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C118) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma
        of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C38) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
Uanis(C119) \\sim Ueq, Uanis(C112) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
        5. Rigid body (RIGU) restrains
 O6, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
        6. Others
 Sof(H1BC)=Sof(H1BD)=Sof(H1CC)=Sof(H1CD)=Sof(O6A)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=
 Sof(C51)=Sof(H51B)=Sof(H51A)=1-FVAR(1)
 Sof(O6)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1BA)=Sof(H1BB)=Sof(H1CA)=Sof(H1CB)=
 Sof(C1D)=Sof(H1DA)=Sof(H1DB)=FVAR(1)
        7.a Ternary CH refined with riding coordinates:
 C94(H94), C82(H82), C39(H39), C79(H79), C28(H28), C91(H91), C36(H36), C25(H25)
        7.b Secondary CH2 refined with riding coordinates:
 C132(H13A,H13B), C130(H13C,H13D), C131(H13E,H13F), C111(H11A,H11B), C42(H42A,
 H42B), C113(H11C,H11D), C123(H12D,H12E), C112(H11E,H11F), C50(H50A,H50B),
 C122(H12G,H12F), C124(H12H,H12I), C110(H11G,H11H), C47(H47A,H47B), C125(H12J,
 H12K), C116(H11I,H11J), C99(H99A,H99B), C114(H11K,H11L), C48(H48A,H48B),
 C49(H49A,H49B), C100(H10A,H10B), C105(H10C,H10D), C106(H10E,H10F), C102(H10G,
 H10H), C129(H12L,H12M), C107(H10I,H10J), C109(H10L,H10K), C43(H43A,H43B),
 C118(H11M,H11N), C98(H98A,H98B), C101(H10M,H10N), C126(H12N,H12O), C97(H97A,
 H97B), C45(H45A,H45B), C117(H11O,H11P), C108(H10O,H10P), C103(H10Q,H10R),
 C127(H12P,H12Q), C44(H44A,H44B), C128(H12R,H12S), C119(H11Q,H11R), C46(H46A,
 H46B), C120(H12T,H12U), C115(H11S,H11T), C104(H10S,H10T), C1A(H1AA,H1AB),
 C1B(H1BA,H1BB), C1B(H1BC,H1BD), C1C(H1CA,H1CB), C1C(H1CC,H1CD), C1D(H1DA,H1DB),
  C1E(H1EA,H1EB), C51(H51B,H51A)
        7.c Aromatic/amide H refined with riding coordinates:
 C77(H77), C72(H72), C66(H66), C14(H14), C62(H62), C75(H75), C76(H76),
 C12(H12), C65(H65), C63(H63), C10(H10), C64(H64), C88(H88), C34(H34), C89(H89),
  C11(H11), C87(H87), C9(H9), C8(H8), C23(H23), C71(H71), C68(H68), C32(H32),
 C15(H15), C70(H70), C59(H59), C18(H18), C58(H58), C33(H33), C22(H22), C21(H21),
  C5(H5), C4(H4), C3(H3), C69(H69), C57(H57), C16(H16), C17(H17)
        7.d Fitted hexagon refined as free rotating group:
 C6(C5,C4,C3,C2,C1)
        7.e Idealised Me refined as rotating group:
 C96(H96A,H96B,H96C), C95(H95A,H95B,H95C), C41(H41A,H41B,H41C), C81(H81A,H81B,
 H81C), C80(H80A,H80B,H80C), C29(H29A,H29B,H29C), C40(H40A,H40B,H40C),
 C121(H12A,H12B,H12C), C93(H93A,H93B,H93C), C84(H84A,H84B,H84C), C38(H38A,H38B,
 H38C), C37(H37A,H37B,H37C), C83(H83A,H83B,H83C), C92(H92A,H92B,H92C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              10312
_shelx_hkl_checksum              14471