Expanding the Boxmi Ligand Family: Synthesis and Application of New NON and NSN Ligands.
Blasius, Clemens; Ren, Bing-Tao; Bürgy, David; Liu, Yan-Kai; Li, Bin; Michalsky, Ina; Wadepohl, Hubert; Deng, Qing-Hai; Gade, Lutz H.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c00751

data_4038298
_publ_section_title
;
 Expanding the Boxmi Ligand Family: Synthesis and Application of New NON
 and NSN Ligands.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c00751
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H30 Co F6 N2 O9 S2, 0.25(C H2 Cl2)'
_chemical_formula_sum            'C26.25 H30.5 Cl0.5 Co F6 N2 O9 S2'
_chemical_formula_weight         772.80
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_cb20
_audit_creation_date             2019-02-28
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record             '01.03.2019 17:00:51 CET UTC+01:00  encif 1.90'
_cell_angle_alpha                90
_cell_angle_beta                 90.025(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   10.9879(3)
_cell_length_b                   56.5870(16)
_cell_length_c                   21.0107(5)
_cell_measurement_reflns_used    36376
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      60.7180
_cell_measurement_theta_min      2.5860
_cell_volume                     13063.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (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    'SHELXD (Sheldrick, 2000-2008)'
_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 0.962
_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    -14.00  13.00   1.00    3.00    --    0.00 -57.00 -60.00   27
  2  \w    -22.00   8.00   1.00    3.00    --    0.00 -57.00 -90.00   30
  3  \w     21.00  63.00   1.00    3.00    --    0.00  38.00-120.00   42
  4  \w    -71.00 -11.00   1.00    3.00    --    0.00 -38.00  60.00   60
  5  \w    -25.00  18.00   1.00    3.00    --    0.00  38.00-120.00   43
  6  \w     -4.00  26.00   1.00    3.00    --    0.00 -38.00  60.00   30
  7  \w    -12.00  68.00   1.00    3.00    --    0.00  57.00  90.00   80
  8  \w    -31.00  -1.00   1.00    3.00    --   14.00 107.00-101.88   30
  9  \w    -26.00  -1.00   1.00    3.00    --   26.00 117.00-139.44   25
 10  \w     -1.00  26.00   1.00   12.00    --   38.00  94.00   0.87   27
 11  \w     10.00  35.00   1.00   12.00    --   42.00  81.00-137.15   25
 12  \w      5.00  30.00   1.00   12.00    --   42.00  90.00-155.63   25
 13  \w     14.00  39.00   1.00   12.00    --   46.00  82.00 112.84   25
 14  \w     13.00  38.00   1.00   12.00    --   46.00  83.00  66.97   25
 15  \w     12.00  37.00   1.00   12.00    --   46.00  84.00 -46.14   25
 16  \w     19.00  44.00   1.00   12.00    --   50.00  80.00 -87.59   25
 17  \w     18.00  43.00   1.00   12.00    --   50.00  81.00 145.91   25
 18  \w     18.00  43.00   1.00   12.00    --   50.00  82.00  20.65   25
 19  \w     17.00  42.00   1.00   12.00    --   50.00  82.00-115.28   25
 20  \w     25.00  51.00   1.00   12.00    --   54.00  77.00-120.00   26
 21  \w     95.00 123.00   1.00   12.00    --   54.00  77.00-150.00   28
 22  \w     26.00  52.00   1.00   12.00    --   54.00  77.00-150.00   26
 23  \w     25.00  67.00   1.00   12.00    --   54.00-125.00-150.00   42
 24  \w     28.00  54.00   1.00   12.00    --   54.00  77.00-180.00   26
 25  \w    -16.00  46.00   1.00   12.00    --   54.00 -77.00-120.00   62
 26  \w     29.00  55.00   1.00   12.00    --   54.00  75.00-105.66   26
 27  \w    -15.00  75.00   1.00   12.00    --   54.00 -57.00 -90.00   90
 28  \w     24.00 112.00   1.00   12.00    --   54.00-126.00  96.00   88
 29  \w     26.00  59.00   1.00   12.00    --   54.00  77.00   0.00   33
 30  \w     27.00  53.00   1.00   12.00    --   54.00  77.00 166.95   26
 31  \w     24.00  52.00   1.00   12.00    --   54.00  77.00 -90.00   28
 32  \w     29.00  55.00   1.00   12.00    --   58.00  77.00  87.71   26
 33  \w     34.00  63.00   1.00   12.00    --   58.00  77.00  61.31   29
 34  \w     29.00  55.00   1.00   12.00    --   58.00  76.00 -67.20   26
 35  \w    103.00 128.00   1.00   12.00    --   58.00  76.00 -67.20   25
 36  \w     30.00  55.00   1.00   12.00    --   58.00  73.00   6.89   25
 37  \w     34.00  60.00   1.00   12.00    --   58.00  72.00 162.56   26
 38  \w     29.00  55.00   1.00   12.00    --   58.00  76.00-173.58   26
 39  \w     29.00  55.00   1.00   12.00    --   58.00  76.00 101.19   26
 40  \w     34.00  60.00   1.00   12.00    --   62.00  76.00 171.93   26
 41  \w     33.00  59.00   1.00   12.00    --   62.00  76.00-113.31   26
 42  \w     39.00  67.00   1.00   12.00    --   62.00  69.00   4.02   28
 43  \w    107.00 132.00   1.00   12.00    --   62.00  77.00 -93.29   25
 44  \w     32.00  58.00   1.00   12.00    --   62.00  77.00 -93.29   26
 45  \w     36.00  71.00   1.00   12.00    --   62.00  72.00-124.35   35
 46  \w     34.00  60.00   1.00   12.00    --   62.00  74.00 143.03   26
 47  \w     33.00  59.00   1.00   12.00    --   62.00  76.00  45.21   26
 48  \w     78.00 112.00   1.00   12.00    --   62.00  69.00   4.02   34
 49  \w     33.00  64.00   1.00   12.00    --   62.00  76.00 -60.11   31
 50  \w     33.00  69.00   1.00   12.00    --   62.00  76.00  50.03   36
 51  \w     46.00 135.00   1.00   12.00    --   66.00  58.00-108.78   89
 52  \w     43.00  82.00   1.00   12.00    --   66.00  70.00 103.70   39
 53  \w     43.00  68.00   1.00   12.00    --   66.00  65.00-158.90   25
 54  \w     36.00  61.00   1.00   12.00    --   66.00  77.00  29.01   25
 55  \w     38.00  64.00   1.00   12.00    --   66.00  73.00-108.30   26
 56  \w     41.00  67.00   1.00   12.00    --   66.00  76.00  16.13   26
 57  \w     46.00  72.00   1.00   12.00    --   66.00  68.00 167.69   26
 58  \w     48.00  74.00   1.00   12.00    --   66.00  56.00-113.86   26
 59  \w     37.00  62.00   1.00   12.00    --   66.00  76.00 -37.68   25
 60  \w     44.00 107.00   1.00   12.00    --   70.00  76.00-167.71   63
 61  \w     79.00 109.00   1.00   12.00    --   70.00  71.00  19.97   30
 62  \w     43.00  69.00   1.00   12.00    --   70.00  71.00  19.97   26
 63  \w     42.00  77.00   1.00   12.00    --   70.00  73.00 115.30   35
 64  \w     42.00  68.00   1.00   12.00    --   70.00  77.00 -77.81   26
 65  \w     40.00  66.00   1.00   12.00    --   70.00  77.00 119.56   26
 66  \w     40.00  66.00   1.00   12.00    --   70.00  77.00 -91.17   26
 67  \w     46.00  72.00   1.00   12.00    --   74.00  73.00 -15.41   26
 68  \w     51.00  77.00   1.00   12.00    --   74.00  76.00 120.16   26
 69  \w     49.00 142.00   1.00   12.00    --   74.00  69.00 -47.25   93
 70  \w     45.00  71.00   1.00   12.00    --   74.00  76.00 -38.30   26
 71  \w     46.00  76.00   1.00   12.00    --   74.00  74.00  68.31   30
 72  \w     53.00  79.00   1.00   12.00    --   78.00  69.00 144.19   26
 73  \w     54.00  80.00   1.00   12.00    --   78.00  69.00 153.41   26
 74  \w     48.00  75.00   1.00   12.00    --   78.00  77.00  10.34   27
 75  \w     56.00  90.00   1.00   12.00    --   78.00  64.00  57.12   34
 76  \w     48.00  74.00   1.00   12.00    --   78.00  77.00-113.01   26
 77  \w     56.00  89.00   1.00   18.00    --   82.00  76.00 148.71   33
 78  \w     53.00  83.00   1.00   18.00    --   82.00  76.00 -90.30   30
 79  \w     57.00  94.00   1.00   18.00    --   82.00  71.00 177.80   37
 80  \w     52.00  78.00   1.00   18.00    --   82.00  77.00-139.10   26
 81  \w     53.00  79.00   1.00   18.00    --   82.00  77.00  81.73   26
 82  \w     57.00  85.00   1.00   18.00    --   82.00  73.00-164.21   28
 83  \w     68.00  94.00   1.00   18.00    --   86.00  71.00 -98.83   26
 84  \w     64.00  90.00   1.00   18.00    --   86.00  61.00 102.29   26
 85  \w     56.00  84.00   1.00   18.00    --   86.00  77.00-123.34   28
 86  \w     57.00 156.00   1.00   18.00    --   86.00  75.00  -2.50   99
 87  \w     64.00  90.00   1.00   18.00    --   86.00  61.00 125.92   26
 88  \w     65.00 118.00   1.00   18.00    --   86.00  54.00  69.94   53
 89  \w     57.00  83.00   1.00   18.00    --   86.00  75.00  61.66   26
 90  \w     63.00  89.00   1.00   18.00    --   90.00  71.00 139.52   26
 91  \w     69.00 119.00   1.00   18.00    --   90.00  50.00 148.19   50
 92  \w     63.00 159.00   1.00   18.00    --   90.00  74.00-112.84   96
 93  \w     71.00  97.00   1.00   18.00    --   90.00  62.00-159.79   26
 94  \w    107.00 141.00   1.00   18.00    --   90.00  75.00 166.73   34
 95  \w     61.00 100.00   1.00   18.00    --   90.00  75.00 166.73   39
 96  \w     65.00  92.00   1.00   18.00    --   94.00  75.00 -47.78   27
 97  \w     77.00 103.00   1.00   18.00    --   98.00  57.00  46.16   26
 98  \w    118.00 144.00   1.00   18.00    --  102.00  71.00 173.99   26
 99  \w     79.00 104.00   1.00   18.00    --  102.00  65.00  -1.23   25
100  \w     75.00 108.00   1.00   18.00    --  102.00  71.00 173.99   33
101  \w     73.00 100.00   1.00   18.00    --  102.00  76.00 -41.57   27
102  \w    151.00 176.00   1.00   18.00    --  108.00  67.00  91.91   25
103  \w     84.00 116.00   1.00   18.00    --  108.00  67.00  91.91   32
104  \w     84.00 168.00   1.00   18.00    --  108.00  43.00 115.75   84
105  \w     84.00 113.00   1.00   18.00    --  108.00-111.00 -90.00   29
106  \w     87.00 161.00   1.00   18.00    --  108.00  64.00-150.00   74
107  \w    113.00 177.00   1.00   18.00    --  108.00  75.00  65.33   64
108  \w     78.00 104.00   1.00   18.00    --  108.00  77.00-180.00   26
109  \w     80.00 105.00   1.00   18.00    --  108.00  75.00  65.33   25
110  \w     85.00 119.00   1.00   18.00    --  108.00  64.00  90.00   34
111  \w     85.00 171.00   1.00   18.00    --  108.00  64.00 120.00   86
112  \w     78.00 177.00   1.00   18.00    --  108.00  77.00 150.00   99
113  \w     91.00 117.00   1.00   18.00    --  108.00  50.00  60.00   26
114  \w     79.00 156.00   1.00   18.00    --  108.00  77.00-171.10   77
115  \w     85.00 117.00   1.00   18.00    --  108.00  64.00 -90.00   32
116  \w     76.00 102.00   1.00   18.00    --  108.00-111.00  60.00   26
117  \w     78.00 104.00   1.00   18.00    --  108.00  77.00  90.00   26
118  \w    136.00 176.00   1.00   18.00    --  108.00  77.00   0.00   40
119  \w     78.00 133.00   1.00   18.00    --  108.00  77.00   0.00   55
120  \w     78.00 104.00   1.00   18.00    --  108.00  77.00-120.00   26
121  \w     78.00 104.00   1.00   18.00    --  108.00  77.00 -30.00   26
122  \w     79.00 105.00   1.00   18.00    --  108.00  77.00 120.00   26
123  \w    150.00 178.00   1.00   18.00    --  108.00  77.00-150.00   28
124  \w     78.00 103.00   1.00   18.00    --  108.00  77.00-150.00   25
125  \w     85.00 165.00   1.00   18.00    --  108.00  64.00 -60.00   80
126  \w     94.00 138.00   1.00   18.00    --  108.00 -77.00-150.00   44
127  \w     38.00  71.00   1.00   18.00    --  108.00 -77.00-150.00   33
128  \w     42.00 130.00   1.00   18.00    --  108.00 -64.00 -30.00   88
129  \w     85.00 165.00   1.00   18.00    --  108.00  64.00-120.00   80
130  \w     36.00 105.00   1.00   18.00    --  108.00 -92.00-180.00   69
131  \w     78.00 177.00   1.00   18.00    --  108.00  77.00 -90.00   99
132  \w     72.00  98.00   1.00   18.00    --  108.00 -92.00   0.00   26
133  \w     78.00 104.00   1.00   18.00    --  108.00  77.00  60.00   26
134  \w     36.00 108.00   1.00   18.00    --  108.00 -92.00 -90.00   72
135  \w     36.00 109.00   1.00   18.00    --  108.00-111.00 150.00   73
136  \w     86.00 112.00   1.00   18.00    --  108.00  38.00  90.00   26
137  \w     87.00 175.00   1.00   18.00    --  108.00  64.00 -30.00   88
138  \w     86.00 177.00   1.00   18.00    --  108.00  51.00  42.66   91
139  \w     88.00 107.00   1.00   18.00    --  108.00  64.00-180.00   19
;
_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      -0.0367006135
_diffrn_orient_matrix_UB_12      0.0192645582
_diffrn_orient_matrix_UB_13      -0.0481743101
_diffrn_orient_matrix_UB_21      -0.0524794682
_diffrn_orient_matrix_UB_22      -0.0190879374
_diffrn_orient_matrix_UB_23      -0.0444294617
_diffrn_orient_matrix_UB_31      -0.1246430681
_diffrn_orient_matrix_UB_32      0.0024141469
_diffrn_orient_matrix_UB_33      0.0329589862
_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  0.110
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       69
_diffrn_reflns_limit_k_min       -69
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            320140
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.903
_diffrn_reflns_theta_min         2.619
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.480
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.557
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6328
_exptl_crystal_size_max          0.151
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.606
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 13592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0184(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3395
_refine_ls_number_reflns         49628
_refine_ls_number_restraints     1288
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0905P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1747
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                38362
_reflns_number_total             49628
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c00751_si_002.cif
_cod_data_source_block           ga_cb20_5
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C26.25 H30.50 Cl0.50 Co F6 N2 O9 S2'
_cod_database_code               4038298
_audit_block_refno               3288
_audit_block_usercomment         'CBIM26, irregular, red'
_shelx_estimated_absorpt_t_max   0.563
_shelx_estimated_absorpt_t_min   0.563
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelxl_version_number           2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.3164(13)
 0.6836(13)
2. 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
3. Restrained distances
 C170-C171 \\sim C170-C17A \\sim C170-C17B
 with sigma of 0.01
 C17A-C171 \\sim C17B-C171
 with sigma of 0.01
4. Rigid bond restraints
 S1, S2, S31, S32, S61, S62, S91, S92, S121, S122, S151, S152, S181, S182,
 S211, S212, O1, O2, O3, O4, O5, O6, O7, O8, O9, O31, O32, O33, O34, O35, O36,
 O37, O38, O39, O61, O62, O63, O64, O65, O66, O67, O68, O69, O91, O92, O93, O94,
  O95, O96, O97, O98, O99, O121, O122, O123, O124, O125, O126, O127, O128, O129,
  O151, O152, O153, O154, O155, O156, O157, O158, O159, O181, O182, O183, O184,
 O185, O186, O187, O188, O189, O211, O212, O213, O214, O215, O216, O217, O218,
 O219, F1, F2, F3, F4, F5, F6, F31, F32, F33, F34, F35, F36, F61, F62, F63, F64,
  F65, F66, F91, F92, F93, F94, F95, F96, F121, F122, F123, F124, F125, F126,
 F151, F152, F153, F154, F155, F156, F181, F182, F183, F184, F185, F186, F211,
 F212, F213, F214, F215, F216, C25, C26, C55, C56, C85, C86, C115, C116, C145,
 C146, C175, C176, C205, C206, C235, C236
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C170, C171, C17A, C17B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Uiso/Uaniso restraints and constraints
Uanis(F65) \\sim Ueq, Uanis(F214) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.1
6. Rigid body (RIGU) restrains
 S1, S2, S31, S32, S61, S62, S91, S92, S121, S122, S151, S152, S181, S182,
 S211, S212, O1, O2, O3, O4, O5, O6, O7, O8, O9, O31, O32, O33, O34, O35, O36,
 O37, O38, O39, O61, O62, O63, O64, O65, O66, O67, O68, O69, O91, O92, O93, O94,
  O95, O96, O97, O98, O99, O121, O122, O123, O124, O125, O126, O127, O128, O129,
  O151, O152, O153, O154, O155, O156, O157, O158, O159, O181, O182, O183, O184,
 O185, O186, O187, O188, O189, O211, O212, O213, O214, O215, O216, O217, O218,
 O219, F1, F2, F3, F4, F5, F6, F31, F32, F33, F34, F35, F36, F61, F62, F63, F64,
  F65, F66, F91, F92, F93, F94, F95, F96, F121, F122, F123, F124, F125, F126,
 F151, F152, F153, F154, F155, F156, F181, F182, F183, F184, F185, F186, F211,
 F212, F213, F214, F215, F216, C25, C26, C55, C56, C85, C86, C115, C116, C145,
 C146, C175, C176, C205, C206, C235, C236
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C170, C171, C17A, C17B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Same fragment restrains
{C25, F2, F3, F1} sigma for 1-2: 0.02, 1-3: 0.04
as
{C25, F1, F2, F3}
{C26, F5, F6, F4} sigma for 1-2: 0.02, 1-3: 0.04
as
{C26, F4, F5, F6}
{C55, F32, F33, F31} sigma for 1-2: 0.02, 1-3: 0.04
as
{C55, F31, F32, F33}
{C56, F35, F36, F34} sigma for 1-2: 0.02, 1-3: 0.04
as
{C56, F34, F35, F36}
{C85, F62, F63, F61} sigma for 1-2: 0.02, 1-3: 0.04
as
{C85, F61, F62, F63}
{C86, F65, F66, F64} sigma for 1-2: 0.02, 1-3: 0.04
as
{C86, F64, F65, F66}
{C115, F92, F93, F91} sigma for 1-2: 0.02, 1-3: 0.04
as
{C115, F91, F92, F93}
{C116, F95, F96, F94} sigma for 1-2: 0.02, 1-3: 0.04
as
{C116, F94, F95, F96}
{C145, F122, F123, F121} sigma for 1-2: 0.02, 1-3: 0.04
as
{C145, F121, F122, F123}
{C146, F125, F126, F124} sigma for 1-2: 0.02, 1-3: 0.04
as
{C146, F124, F125, F126}
{C175, F152, F153, F151} sigma for 1-2: 0.02, 1-3: 0.04
as
{C175, F151, F152, F153}
{C176, F155, F156, F154} sigma for 1-2: 0.02, 1-3: 0.04
as
{C176, F154, F155, F156}
{C205, F182, F183, F181} sigma for 1-2: 0.02, 1-3: 0.04
as
{C205, F181, F182, F183}
{C206, F185, F186, F184} sigma for 1-2: 0.02, 1-3: 0.04
as
{C206, F184, F185, F186}
{C235, F212, F213, F211} sigma for 1-2: 0.02, 1-3: 0.04
as
{C235, F211, F212, F213}
{C236, F215, F216, F214} sigma for 1-2: 0.02, 1-3: 0.04
as
{C236, F214, F215, F216}
{Cl1, Cl2, C501} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl3, Cl4, C502}
8. Others
 Sof(H17A)=Sof(C17B)=Sof(H17H)=Sof(H17I)=Sof(H17J)=1-FVAR(1)
 Sof(H170)=Sof(C17A)=Sof(H17E)=Sof(H17F)=Sof(H17G)=FVAR(1)
9.a Ternary CH refined with riding coordinates:
 C1(H1), C16(H16), C17(H17), C20(H20), C31(H31), C46(H46), C47(H47), C50(H50),
 C61(H61), C76(H76), C77(H77), C80(H80), C91(H91), C106(H106), C107(H107),
 C110(H110), C121(H121), C136(H136), C137(H137), C140(H140), C151(H151),
 C166(H166), C167(H167), C170(H170), C170(H17A), C181(H181), C196(H196),
 C197(H197), C200(H200), C211(H211), C226(H226), C227(H227), C230(H230)
9.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C15(H15C,H15D), C32(H32A,H32B), C45(H45A,H45B), C62(H62A,H62B),
 C75(H75A,H75B), C92(H92A,H92B), C105(H10A,H10B), C122(H12A,H12B), C135(H13A,
 H13B), C152(H15A,H15B), C165(H16A,H16B), C182(H18D,H18E), C195(H19D,H19E),
 C212(H21D,H21E), C225(H22D,H22E), C501(H50A,H50B), C502(H50C,H50D)
9.c Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C82(H82A,H82B,
 H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C108(H10C,H10D,H10E),
 C109(H10F,H10G,H10H), C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,
 H11H,H11I), C138(H13C,H13D,H13E), C139(H13F,H13G,H13H), C141(H14A,H14B,H14C),
 C142(H14D,H14E,H14F), C168(H16C,H16D,H16E), C169(H16F,H16G,H16H), C171(H17B,
 H17C,H17D), C17A(H17E,H17F,H17G), C17B(H17H,H17I,H17J), C174(H17N,H17O,H17P)
9.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8), C9(H9), C13(H13), C34(H34), C38(H38), C39(H39), C43(H43),
 C64(H64), C68(H68), C69(H69), C73(H73), C94(H94), C98(H98), C99(H99),
 C103(H103), C124(H124), C128(H128), C129(H129), C133(H133), C154(H154),
 C158(H158), C159(H159), C163(H163), C184(H184), C188(H188), C189(H189),
 C193(H193), C214(H214), C218(H218), C219(H219), C223(H223)
9.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C114(H11J,H11K,H11L), C143(H14G,H14H,H14I), C144(H14J,
 H14K,H14L), C173(H17K,H17L,H17M), C198(H19F,H19G,H19H), C199(H19I,H19J,H19K),
 C201(H20A,H20B,H20C), C202(H20D,H20E,H20F), C203(H20G,H20H,H20I), C204(H20J,
 H20K,H20L), C228(H22F,H22G,H22H), C229(H22I,H22J,H22K), C231(H23D,H23E,H23F),
 C232(H23G,H23H,H23I), C233(H23J,H23K,H23L), C234(H23M,H23N,H23O)
;
_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 1.631
_oxdiff_exptl_absorpt_empirical_full_min 0.695
_shelx_res_checksum              55766
_cell_oxdiff_length_a            10.9937(4)
_cell_oxdiff_length_b            56.5826(10)
_cell_oxdiff_length_c            21.0013(5)
_cell_oxdiff_angle_alpha         89.9878(16)
_cell_oxdiff_angle_beta          89.953(2)
_cell_oxdiff_angle_gamma         89.907(2)
_cell_oxdiff_volume              13063.9(6)
_cell_oxdiff_measurement_reflns_used 36556