Calix[4]pyrrole aluminate: a planar tetracoordinate aluminum(III) anion and its unusual Lewis acidity.
Ebner, Fabian; Wadepohl, Hubert; Greb, Lutz; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10628

data_4129070
_publ_section_title
;
 Calix[4]pyrrole aluminate: a planar tetracoordinate aluminum(III) anion
 and its unusual Lewis acidity.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10628
_journal_year                    2019
_chemical_formula_moiety
'C28 H32.94 Al N4, 3.5(C6 H4 F2), C16 H32 Li2 O8'
_chemical_formula_sum            'C65 H79 Al F7 Li2 N4 O8'
_chemical_formula_weight         1218.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                gr_fe6
_audit_creation_date             2019-05-10
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
'09.07.2019 17:05:45 CEST UTC+02:00  encif 1.93'
_cell_angle_alpha                90
_cell_angle_beta                 96.3437(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5499(2)
_cell_length_b                   18.1193(3)
_cell_length_c                   22.0710(3)
_cell_measurement_reflns_used    33754
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      70.5170
_cell_measurement_theta_min      3.1530
_cell_volume                     6180.50(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53a (Rigaku OD, 2019)'
_computing_publication_material
'encif (Wadepohl, 2009-19); encifer 1.7.x (CCDC, 2018)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2019 (Giacovazzo et al., 2019)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -67.00 -21.00   1.00    3.00    --    0.00 -38.00  90.00   46
  2  \w    -26.00  68.00   1.00    3.00    --    0.00  38.00 -90.00   94
  3  \w    -69.00 -13.00   1.00    3.00    --    0.00 -77.00 -90.00   56
  4  \w    -19.00  34.00   1.00    3.00    --    0.00  57.00 150.00   53
  5  \w    -29.00  65.00   1.00    3.00    --    0.00  77.00  30.00   94
  6  \w    -36.00 -10.00   1.00    3.00    --   18.00 121.00 169.78   26
  7  \w    -18.00   7.00   1.00   12.00    --   30.00 111.00 162.23   25
  8  \w      1.00  30.00   1.00   12.00    --   38.00  90.00   9.33   29
  9  \w      0.00  25.00   1.00   12.00    --   38.00  92.00 -84.48   25
 10  \w      5.00  30.00   1.00   12.00    --   42.00  90.00  64.38   25
 11  \w      6.00  31.00   1.00   12.00    --   42.00  90.00 179.98   25
 12  \w     12.00  37.00   1.00   12.00    --   46.00  84.00 -37.99   25
 13  \w     14.00  39.00   1.00   12.00    --   46.00  81.00  -5.35   25
 14  \w     13.00  38.00   1.00   12.00    --   46.00  83.00 154.76   25
 15  \w     12.00  37.00   1.00   12.00    --   46.00  84.00  82.26   25
 16  \w     18.00  43.00   1.00   12.00    --   50.00  81.00  66.03   25
 17  \w     18.00  43.00   1.00   12.00    --   50.00  81.00 119.78   25
 18  \w     17.00  42.00   1.00   12.00    --   50.00  82.00-126.41   25
 19  \w     17.00  42.00   1.00   12.00    --   50.00  82.00 -90.22   25
 20  \w     19.00  44.00   1.00   12.00    --   50.00  80.00  19.81   25
 21  \w     17.00  42.00   1.00   12.00    --   50.00  82.00  38.49   25
 22  \w     17.00  45.00   1.00   12.00    --   50.00  82.00-177.28   28
 23  \w     18.00  43.00   1.00   12.00    --   50.00  81.00 -56.63   25
 24  \w     27.00  53.00   1.00   12.00    --   54.00  77.00 105.16   26
 25  \w     84.00 118.00   1.00   12.00    --   54.00  77.00 -43.62   34
 26  \w     23.00 110.00   1.00   12.00    --   54.00-125.00-180.00   87
 27  \w     24.00  50.00   1.00   12.00    --   54.00  77.00 -43.62   26
 28  \w     25.00  51.00   1.00   12.00    --   54.00  77.00  78.14   26
 29  \w     26.00  52.00   1.00   12.00    --   54.00  77.00 150.00   26
 30  \w    -15.00  75.00   1.00   12.00    --   54.00 -57.00 -30.00   90
 31  \w     26.00  52.00   1.00   12.00    --   54.00  77.00 -30.00   26
 32  \w     25.00  51.00   1.00   12.00    --   54.00  77.00   0.00   26
 33  \w     44.00  69.00   1.00   12.00    --   54.00-125.00  30.00   25
 34  \w    -16.00  84.00   1.00   12.00    --   54.00 -77.00-150.00  100
 35  \w     24.00  50.00   1.00   12.00    --   54.00  77.00-154.05   26
 36  \w     91.00 117.00   1.00   12.00    --   58.00  77.00 -76.15   26
 37  \w     30.00  56.00   1.00   12.00    --   58.00  76.00-129.21   26
 38  \w     29.00  55.00   1.00   12.00    --   58.00  75.00 138.30   26
 39  \w     29.00  55.00   1.00   12.00    --   58.00  77.00 172.10   26
 40  \w     29.00  62.00   1.00   12.00    --   58.00  75.00 -21.30   33
 41  \w     28.00  61.00   1.00   12.00    --   58.00  77.00 -76.15   33
 42  \w     29.00  54.00   1.00   12.00    --   58.00  76.00-137.48   25
 43  \w     31.00  57.00   1.00   12.00    --   58.00  76.00-101.74   26
 44  \w     28.00  54.00   1.00   12.00    --   58.00  77.00  28.78   26
 45  \w     30.00  56.00   1.00   12.00    --   58.00  76.00-111.99   26
 46  \w     29.00  55.00   1.00   12.00    --   58.00  76.00 -47.92   26
 47  \w     28.00  54.00   1.00   12.00    --   58.00  77.00  55.67   26
 48  \w     34.00  60.00   1.00   12.00    --   62.00  76.00 107.43   26
 49  \w     32.00  62.00   1.00   12.00    --   62.00  77.00 -19.43   30
 50  \w     32.00  58.00   1.00   12.00    --   62.00  77.00-164.30   26
 51  \w     34.00  60.00   1.00   12.00    --   62.00  75.00-117.18   26
 52  \w     36.00  61.00   1.00   12.00    --   62.00  74.00  24.40   25
 53  \w     33.00  59.00   1.00   12.00    --   62.00  75.00 -90.97   26
 54  \w     77.00 106.00   1.00   12.00    --   62.00  75.00 136.38   29
 55  \w     39.00  72.00   1.00   12.00    --   62.00  75.00 136.38   33
 56  \w     43.00  69.00   1.00   12.00    --   62.00  71.00 176.68   26
 57  \w     34.00  66.00   1.00   12.00    --   62.00  77.00 -67.41   32
 58  \w     33.00  59.00   1.00   12.00    --   62.00  75.00 159.08   26
 59  \w     40.00  84.00   1.00   12.00    --   66.00  73.00 159.45   44
 60  \w     37.00  62.00   1.00   12.00    --   66.00  76.00  -8.64   25
 61  \w     38.00  77.00   1.00   12.00    --   66.00  75.00  77.75   39
 62  \w     37.00  63.00   1.00   12.00    --   66.00  77.00 -54.95   26
 63  \w     37.00  63.00   1.00   12.00    --   66.00  76.00  59.62   26
 64  \w     40.00  66.00   1.00   12.00    --   66.00  76.00-158.79   26
 65  \w     45.00  71.00   1.00   12.00    --   66.00  61.00-106.60   26
 66  \w     47.00  75.00   1.00   12.00    --   70.00  67.00  29.24   28
 67  \w     44.00  70.00   1.00   12.00    --   70.00  74.00-108.26   26
 68  \w     45.00  71.00   1.00   12.00    --   70.00  69.00 -64.19   26
 69  \w     42.00  68.00   1.00   12.00    --   70.00  76.00-153.03   26
 70  \w     47.00  84.00   1.00   12.00    --   70.00  66.00 -20.41   37
 71  \w     42.00  68.00   1.00   12.00    --   70.00  73.00-172.50   26
 72  \w     79.00 135.00   1.00   12.00    --   70.00  73.00 -91.37   56
 73  \w     46.00  74.00   1.00   12.00    --   70.00  73.00 -91.37   28
 74  \w     74.00 110.00   1.00   12.00    --   70.00  74.00-108.26   36
 75  \w     46.00  76.00   1.00   12.00    --   74.00  73.00 138.18   30
 76  \w     55.00 138.00   1.00   12.00    --   74.00  48.00 -60.21   83
 77  \w     49.00  75.00   1.00   12.00    --   74.00  72.00  41.25   26
 78  \w     51.00  82.00   1.00   12.00    --   74.00  64.00 172.00   31
 79  \w     46.00  72.00   1.00   12.00    --   74.00  74.00  57.96   26
 80  \w     48.00  83.00   1.00   12.00    --   74.00  70.00  31.59   35
 81  \w     46.00  72.00   1.00   12.00    --   74.00  74.00 -11.87   26
 82  \w     49.00  75.00   1.00   12.00    --   74.00  69.00  16.83   26
 83  \w     48.00  80.00   1.00   12.00    --   74.00  71.00 126.96   32
 84  \w     48.00  84.00   1.00   12.00    --   74.00  70.00  90.79   36
 85  \w     54.00 143.00   1.00   12.00    --   78.00  67.00  83.58   89
 86  \w     49.00  91.00   1.00   12.00    --   78.00  76.00-160.98   42
 87  \w     51.00  77.00   1.00   12.00    --   78.00  76.00 -11.98   26
 88  \w     51.00  77.00   1.00   12.00    --   78.00  72.00  96.68   26
 89  \w     59.00 121.00   1.00   12.00    --   78.00  60.00 -24.61   62
 90  \w     50.00  81.00   1.00   12.00    --   78.00  73.00 -55.49   31
 91  \w     51.00  88.00   1.00   12.00    --   78.00  72.00 102.74   37
 92  \w     55.00  91.00   1.00   15.00    --   82.00  71.00-119.11   36
 93  \w     55.00  80.00   1.00   15.00    --   82.00  75.00-152.15   25
 94  \w     55.00  83.00   1.00   15.00    --   82.00  73.00-140.10   28
 95  \w     61.00  91.00   1.00   15.00    --   82.00  60.00   8.35   30
 96  \w     57.00  83.00   1.00   15.00    --   82.00  69.00  33.17   26
 97  \w     56.00  82.00   1.00   15.00    --   86.00  77.00 158.55   26
 98  \w     57.00 125.00   1.00   15.00    --   86.00  76.00  47.01   68
 99  \w     59.00  95.00   1.00   15.00    --   86.00  76.00 166.14   36
100  \w     56.00  82.00   1.00   15.00    --   86.00  77.00 -34.81   26
101  \w     59.00 156.00   1.00   15.00    --   86.00  74.00-138.32   97
102  \w     64.00 147.00   1.00   15.00    --   86.00  63.00  98.43   83
103  \w     65.00 102.00   1.00   15.00    --   86.00  63.00  15.56   37
104  \w     61.00  88.00   1.00   15.00    --   90.00  76.00 -84.91   27
105  \w     69.00 127.00   1.00   15.00    --   90.00  55.00 -27.22   58
106  \w     68.00 102.00   1.00   15.00    --   90.00  50.00-135.81   34
107  \w     81.00 107.00   1.00   15.00    --   90.00  60.00 -55.12   26
108  \w     67.00  93.00   1.00   15.00    --   94.00  72.00 134.05   26
109  \w     64.00  90.00   1.00   15.00    --   94.00  77.00   4.49   26
110  \w     73.00 100.00   1.00   15.00    --   98.00  70.00 -75.38   27
111  \w    109.00 135.00   1.00   15.00    --   98.00  68.00 152.32   26
112  \w     74.00 105.00   1.00   15.00    --   98.00  68.00 152.32   31
113  \w     76.00 114.00   1.00   15.00    --  102.00  70.00 -25.27   38
114  \w     41.00 130.00   1.00   15.00    --  108.00 -64.00 120.00   89
115  \w     78.00 103.00   1.00   15.00    --  108.00  77.00 150.00   25
116  \w     79.00 174.00   1.00   15.00    --  108.00  77.00 -30.00   95
117  \w    140.00 166.00   1.00   15.00    --  108.00  64.00-120.00   26
118  \w     85.00 111.00   1.00   15.00    --  108.00  64.00-120.00   26
119  \w    152.00 178.00   1.00   15.00    --  108.00  77.00 120.00   26
120  \w     78.00 104.00   1.00   15.00    --  108.00  77.00 120.00   26
121  \w     78.00 115.00   1.00   15.00    --  108.00  77.00   0.00   37
122  \w     78.00 173.00   1.00   15.00    --  108.00  77.00 -60.00   95
123  \w     78.00 103.00   1.00   15.00    --  108.00  77.00  60.00   25
124  \w    122.00 177.00   1.00   15.00    --  108.00  77.00-150.00   55
125  \w     78.00 103.00   1.00   15.00    --  108.00  77.00-150.00   25
126  \w    119.00 177.00   1.00   15.00    --  108.00  77.00  90.00   58
127  \w     78.00 104.00   1.00   15.00    --  108.00  77.00  90.00   26
128  \w     78.00 104.00   1.00   15.00    --  108.00  77.00  30.00   26
129  \w    128.00 156.00   1.00   15.00    --  108.00  77.00-180.00   28
130  \w     79.00 105.00   1.00   15.00    --  108.00  77.00-180.00   26
131  \w     79.00 105.00   1.00   15.00    --  108.00  77.00 -90.00   26
132  \w     73.00 110.00   1.00   15.00    --  108.00-111.00-120.00   37
133  \w     85.00 174.00   1.00   15.00    --  108.00  64.00 120.00   89
134  \w    135.00 161.00   1.00   15.00    --  108.00  64.00  60.00   26
135  \w     85.00 120.00   1.00   15.00    --  108.00  64.00  60.00   35
136  \w     85.00 111.00   1.00   15.00    --  108.00  64.00 -60.00   26
137  \w     37.00 112.00   1.00   15.00    --  108.00-111.00  90.00   75
138  \w     79.00 105.00   1.00   15.00    --  108.00  77.00-120.00   26
139  \w    100.00 174.00   1.00   15.00    --  108.00 111.00  30.00   74
140  \w     85.00 150.00   1.00   15.00    --  108.00  64.00  90.00   65
141  \w     36.00  96.00   1.00   15.00    --  108.00 -92.00   0.00   60
142  \w     36.00 103.00   1.00   15.00    --  108.00 -92.00 120.00   67
143  \w     36.00 109.00   1.00   15.00    --  108.00-111.00 -30.00   73
144  \w     87.00 155.00   1.00   15.00    --  108.00  50.00 164.17   68
145  \w     86.00 169.00   1.00   15.00    --  108.00  71.00  11.24   83
146  \w     87.00 131.00   1.00   15.00    --  108.00  53.00-139.93   44
147  \w     80.00 178.00   1.00   15.00    --  108.00  74.00 162.09   98
148  \w     86.00 158.00   1.00   15.00    --  108.00  38.00 -90.00   72
149  \w     87.00 171.00   1.00   15.00    --  108.00  64.00 -90.00   84
150  \w     86.00 106.00   1.00   15.00    --  108.00  64.00-150.00   20
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0818030000
_diffrn_orient_matrix_UB_12      -0.0407623000
_diffrn_orient_matrix_UB_13      0.0280249000
_diffrn_orient_matrix_UB_21      0.0368259000
_diffrn_orient_matrix_UB_22      0.0026563000
_diffrn_orient_matrix_UB_23      -0.0619875000
_diffrn_orient_matrix_UB_31      0.0434712000
_diffrn_orient_matrix_UB_32      0.0745139000
_diffrn_orient_matrix_UB_33      0.0175912000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            161650
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.067
_diffrn_reflns_theta_min         2.859
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2572
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     879
_refine_ls_number_reflns         11875
_refine_ls_number_restraints     255
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0798P)^2^+5.2474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9529
_reflns_number_total             11875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10628_si_008.cif
_cod_data_source_block           gr_fe6
_cod_original_cell_volume        6180.53(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129070
_audit_block_refno               3339
_audit_block_usercomment         'FE_470, irregular, light yellow'
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.911
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.45
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C51-F51 \\sim C52-F52 \\sim C61-F61 \\sim C62-F62 \\sim C71A-F71A \\sim
C76A-F76A \\sim C71B-F71B ~
 C72B-F72B \\sim C81-F81 \\sim C82-F82
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55
\\sim C56 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim
C71A \\sim C72A \\sim C73A \\sim C74A \\sim C75A \\sim C76A \\sim C71B \\sim
C72B \\sim C73B \\sim C74B \\sim C75B \\sim C76B \\sim C81 \\sim C82 \\sim C83
\\sim C84 \\sim C85 \\sim C86 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35
\\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43
\\sim C44 \\sim C45 \\sim C46 \\sim F51 \\sim F52 \\sim F61 \\sim F62 \\sim
F71A \\sim F76A \\sim F71B \\sim F72B \\sim F81 \\sim F82: within 1A with sigma
of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 F71A, F76A, C71A, C72A, C73A, C74A, C75A, C76A, F71B, F72B, C71B, C72B, C73B,
 C74B, C75B, C76B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F81, F82, C81, C82, C83, C84, C85, C86
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Al1B)=1-FVAR(1)
 Sof(Al1A)=Sof(H)=FVAR(1)
 Sof(F71B)=Sof(F72B)=Sof(C71B)=Sof(C72B)=Sof(C73B)=Sof(H73B)=Sof(C74B)=
 Sof(H74B)=Sof(C75B)=Sof(H75B)=Sof(C76B)=Sof(H76B)=1-FVAR(2)
 Sof(F71A)=Sof(F76A)=Sof(C71A)=Sof(C72A)=Sof(H72A)=Sof(C73A)=Sof(H73A)=
 Sof(C74A)=Sof(H74A)=Sof(C75A)=Sof(H75A)=Sof(C76A)=FVAR(2)
 Fixed Sof: F81(0.5) F82(0.5) C81(0.5) C82(0.5) C83(0.5) H83(0.5) C84(0.5)
 H84(0.5) C85(0.5) H85(0.5) C86(0.5) H86(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18),
 C53(H53), C54(H54), C55(H55), C56(H56), C63(H63), C64(H64), C65(H65), C66(H66),
  C72A(H72A), C73A(H73A), C74A(H74A), C75A(H75A), C73B(H73B), C74B(H74B),
 C75B(H75B), C76B(H76B), C83(H83), C84(H84), C85(H85), C86(H86)
6.c Fitted hexagon refined as free rotating group:
 C71A(C72A,C73A,C74A,C75A,C76A), C71B(C72B,C73B,C74B,C75B,C76B), C81(C82,C83,
 C84,C85,C86)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.428
_oxdiff_exptl_absorpt_empirical_full_min 0.788
_shelx_res_checksum              16390
_cell_oxdiff_length_a            15.5492(3)
_cell_oxdiff_length_b            18.1293(4)
_cell_oxdiff_length_c            22.0600(4)
_cell_oxdiff_angle_alpha         90.0345(16)
_cell_oxdiff_angle_beta          96.3480(16)
_cell_oxdiff_angle_gamma         90.0134(16)
_cell_oxdiff_volume              6180.5(2)
_cell_oxdiff_measurement_reflns_used 33754