Solid–State Molecular Organometallic Catalysis in Gas/Solid Flow (Flow-SMOM) as Demonstrated by Efficient Room Temperature and Pressure 1-Butene Isomerization
Martínez-Martínez, Antonio J.; Royle, Cameron G.; Furfari, Samantha K.; Suriye, Kongkiat; Weller, Andrew S.; ACS Catalysis  (2020) 1984–1992; doi:10.1021/acscatal.9b03727

data_4517331
_publ_section_title
;
 Solid--State Molecular Organometallic Catalysis in Gas/Solid Flow
 (Flow-SMOM) as Demonstrated by Efficient Room Temperature and Pressure
 1-Butene Isomerization
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              1984
_journal_page_last               1992
_journal_paper_doi               10.1021/acscatal.9b03727
_journal_year                    2020
_chemical_formula_moiety         'C22 H46 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C54 H58 B F24 P2 Rh'
_chemical_formula_weight         1338.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6093(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.59335(7)
_cell_length_b                   18.77356(10)
_cell_length_c                   35.33268(14)
_cell_measurement_reflns_used    99388
_cell_measurement_temperature    150.02(18)
_cell_measurement_theta_max      76.1840
_cell_measurement_theta_min      3.5830
_cell_volume                     11665.42(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.02(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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    -27.00  27.00   1.00    3.00    --  -42.66  38.00  90.00   54
  2  \w    -34.00   9.00   1.00    3.00    --  -42.66  38.00-120.00   43
  3  \w   -120.00 -20.00   1.00    3.00    --  -42.66 -19.00 -90.00  100
  4  \w     81.00 128.00   1.00    3.00    --   42.66 178.00  30.00   47
  5  \w     37.00 105.00   1.00    9.00    --  111.00 -95.00  30.00   68
  6  \w    101.00 178.00   1.00    9.00    --  111.00  30.00-150.00   77
  7  \w     68.00 100.00   1.00    9.00    --  111.00-125.00 150.00   32
  8  \w     46.00  92.00   1.00    9.00    --  111.00 -45.00   0.00   46
  9  \w     43.00 107.00   1.00    9.00    --  111.00-125.00  30.00   64
 10  \w     68.00 126.00   1.00    9.00    --  111.00  15.00 -30.00   58
 11  \w    146.00 177.00   1.00    9.00    --  111.00  15.00 -30.00   31
 12  \w     40.00  80.00   1.00    9.00    --  111.00 -45.00  90.00   40
 13  \w     41.00  87.00   1.00    9.00    --  111.00 -45.00 150.00   46
 14  \w    -74.00 -48.00   1.00    3.00    --  -42.66 -57.00 -30.00   26
 15  \w    -66.00 -17.00   1.00    3.00    --  -42.66 -57.00 -60.00   49
 16  \w    -71.00 -26.00   1.00    3.00    --  -42.66 -77.00  60.00   45
 17  \w    -71.00 -11.00   1.00    3.00    --  -42.66 -77.00-120.00   60
 18  \w    -76.00 -50.00   1.00    3.00    --  -42.66 -57.00-120.00   26
 19  \w    -82.00 -56.00   1.00    3.00    --  -42.66 -38.00 -30.00   26
 20  \w     58.00 117.00   1.00    3.00    --   42.66 178.00-120.00   59
 21  \w     27.00  52.00   1.00    3.00    --   42.66  38.00 -90.00   25
 22  \w     15.00  43.00   1.00    3.00    --   42.66  77.00 -30.00   28
 23  \w     81.00 107.00   1.00    9.00    --  111.00  71.00   4.02   26
 24  \w     83.00 109.00   1.00    9.00    --  111.00  61.00 -30.00   26
 25  \w    150.00 176.00   1.00    9.00    --  111.00  61.00 -90.00   26
 26  \w     83.00 109.00   1.00    9.00    --  111.00  61.00 -60.00   26
 27  \w     83.00 109.00   1.00    9.00    --  111.00  61.00   0.00   26
 28  \w     83.00 108.00   1.00    9.00    --  111.00  62.00 -15.89   25
 29  \w     86.00 129.00   1.00    9.00    --  111.00  52.00  44.16   43
 30  \w     84.00 109.00   1.00    9.00    --  111.00  61.00 -90.00   25
 31  \w     80.00 106.00   1.00    9.00    --  111.00  77.00  30.00   26
 32  \w    148.00 176.00   1.00    9.00    --  111.00  77.00-120.00   28
 33  \w    141.00 170.00   1.00    9.00    --  111.00  61.00  60.00   29
 34  \w     81.00 106.00   1.00    9.00    --  111.00  77.00 -30.00   25
 35  \w     80.00 106.00   1.00    9.00    --  111.00  77.00 -90.00   26
 36  \w     85.00 111.00   1.00    9.00    --  111.00  53.00 -64.20   26
 37  \w     87.00 113.00   1.00    9.00    --  111.00  45.00 -60.00   26
 38  \w     84.00 109.00   1.00    9.00    --  111.00  61.00  60.00   25
 39  \w     81.00 106.00   1.00    9.00    --  111.00  77.00   0.00   25
 40  \w     87.00 139.00   1.00    9.00    --  111.00  45.00 -30.00   52
 41  \w     83.00 109.00   1.00    9.00    --  111.00  61.00  30.00   26
 42  \w     87.00 114.00   1.00    9.00    --  111.00  45.00   0.00   27
 43  \w     87.00 113.00   1.00    9.00    --  111.00  45.00  60.00   26
 44  \w     86.00 112.00   1.00    9.00    --  111.00  50.00 -34.69   26
 45  \w     88.00 115.00   1.00    9.00    --  111.00  30.00   0.00   27
 46  \w     88.00 125.00   1.00    9.00    --  111.00  45.00  30.00   37
 47  \w    148.00 174.00   1.00    9.00    --  111.00  77.00 -60.00   26
 48  \w     89.00 114.00   1.00    9.00    --  111.00  30.00  30.00   25
 49  \w     90.00 115.00   1.00    9.00    --  111.00  45.00 -90.00   25
 50  \w     80.00 107.00   1.00    9.00    --  111.00  77.00 -60.00   27
 51  \w     81.00 108.00   1.00    9.00    --  111.00  77.00-120.00   27
 52  \w     82.00 109.00   1.00    9.00    --  111.00  67.00  36.14   27
 53  \w    140.00 166.00   1.00    9.00    --  111.00  52.00  44.16   26
 54  \w     88.00 113.00   1.00    9.00    --  111.00  46.00 -48.49   25
 55  \w     80.00 106.00   1.00    9.00    --  111.00  75.00  -6.57   26
 56  \w   -112.00 -83.00   1.00    3.00    --  -42.66 -38.00  30.00   29
 57  \w     98.00 129.00   1.00    3.00    --   42.66 178.00-180.00   31
 58  \w     80.00 118.00   1.00    9.00    --  111.00-125.00-180.00   38
 59  \w     60.00  98.00   1.00    9.00    --  111.00 -95.00 -90.00   38
 60  \w     41.00  67.00   1.00    9.00    --  111.00 -30.00   0.00   26
 61  \w    105.00 131.00   1.00    9.00    --  111.00 125.00 -60.00   26
 62  \w     90.00 118.00   1.00    9.00    --  111.00-125.00   0.00   28
 63  \w    143.00 168.00   1.00    9.00    --  111.00 125.00 -60.00   25
 64  \w     52.00  78.00   1.00    9.00    --  111.00 -45.00-180.00   26
 65  \w     91.00 117.00   1.00    9.00    --  111.00-125.00  60.00   26
 66  \w     43.00  75.00   1.00    9.00    --  111.00 -30.00  30.00   32
 67  \w     68.00 110.00   1.00    9.00    --  111.00 -95.00-150.00   42
 68  \w      1.00  26.00   1.00    3.00    --   38.00  92.00  65.18   25
 69  \w   -114.00 -21.00   1.00    3.00    --  -42.66 -38.00 120.00   93
 70  \w    -44.00  30.00   1.00    3.00    --  -42.66  38.00 -60.00   74
 71  \w     16.00  42.00   1.00    3.00    --   42.66  57.00   0.00   26
 72  \w     13.00  45.00   1.00    3.00    --   46.00  82.00-168.53   32
 73  \w     17.00  42.00   1.00    3.00    --   50.00  82.00  95.23   25
 74  \w     17.00  42.00   1.00    3.00    --   50.00  82.00  25.30   25
 75  \w     18.00  43.00   1.00    3.00    --   50.00  80.00-113.15   25
 76  \w     31.00  57.00   1.00    3.00    --   62.00  76.00 141.56   26
 77  \w     31.00  71.00   1.00    3.00    --   62.00  76.00 174.90   40
 78  \w    106.00 133.00   1.00    3.00    --   62.00  76.00 174.90   27
 79  \w     31.00  57.00   1.00    3.00    --   62.00  77.00 -79.50   26
 80  \w     31.00  57.00   1.00    3.00    --   62.00  76.00  88.24   26
 81  \w     32.00  58.00   1.00    3.00    --   62.00  76.00 -12.16   26
 82  \w     35.00  61.00   1.00    3.00    --   66.00  76.00 -51.92   26
 83  \w     36.00  62.00   1.00    3.00    --   66.00  77.00-109.28   26
 84  \w    121.00 146.00   1.00    3.00    --   74.00  76.00  93.10   25
 85  \w     43.00  69.00   1.00    3.00    --   74.00  76.00  93.10   26
 86  \w     43.00  69.00   1.00    3.00    --   74.00  77.00-140.41   26
 87  \w     44.00  69.00   1.00    3.00    --   74.00  75.00  14.24   25
 88  \w     43.00  69.00   1.00    3.00    --   74.00  77.00-171.61   26
 89  \w     46.00  72.00   1.00    3.00    --   74.00  72.00  67.56   26
 90  \w     43.00  80.00   1.00    3.00    --   74.00  76.00 158.61   37
 91  \w     43.00  69.00   1.00    3.00    --   74.00  74.00 123.31   26
 92  \w     43.00  69.00   1.00    3.00    --   74.00  77.00  26.84   26
 93  \w     43.00  69.00   1.00    3.00    --   74.00  76.00  -8.35   26
 94  \w     49.00  76.00   1.00    9.00    --   78.00  72.00  42.53   27
 95  \w     51.00  80.00   1.00    9.00    --   82.00  74.00 -61.67   29
 96  \w    133.00 159.00   1.00    9.00    --   86.00  76.00-124.13   26
 97  \w     55.00  81.00   1.00    9.00    --   86.00  76.00-124.13   26
 98  \w     56.00  84.00   1.00    9.00    --   86.00  70.00-170.27   28
 99  \w     56.00  81.00   1.00    9.00    --   86.00  70.00 -91.12   25
100  \w     58.00  84.00   1.00    9.00    --   86.00  64.00-127.77   26
101  \w     61.00  87.00   1.00    9.00    --   90.00  66.00  85.67   26
102  \w    113.00 164.00   1.00    9.00    --   98.00  71.00 138.68   51
103  \w     68.00  95.00   1.00    9.00    --   98.00  71.00 138.68   27
104  \w    129.00 155.00   1.00    9.00    --   98.00  71.00   3.53   26
105  \w     68.00  94.00   1.00    9.00    --   98.00  71.00   3.53   26
106  \w    134.00 160.00   1.00    9.00    --  102.00  77.00 -22.14   26
107  \w     71.00  97.00   1.00    9.00    --  102.00  77.00 -22.14   26
108  \w    131.00 164.00   1.00    9.00    --  106.00  67.00-137.82   33
109  \w     77.00 114.00   1.00    9.00    --  106.00  67.00-137.82   37
110  \w    129.00 155.00   1.00    9.00    --  111.00  77.00-180.00   26
111  \w     80.00 106.00   1.00    9.00    --  111.00  77.00-180.00   26
112  \w    128.00 154.00   1.00    9.00    --  111.00  64.00  32.06   26
113  \w     83.00 167.00   1.00    9.00    --  111.00  61.00 120.00   84
114  \w     83.00 109.00   1.00    9.00    --  111.00  64.00  32.06   26
115  \w     48.00  91.00   1.00    9.00    --  111.00 -45.00-120.00   43
116  \w     80.00 106.00   1.00    9.00    --  111.00  77.00  90.00   26
117  \w     84.00 163.00   1.00    9.00    --  111.00  61.00  90.00   79
118  \w     50.00  76.00   1.00    9.00    --  111.00 -45.00-150.00   26
119  \w    135.00 177.00   1.00    9.00    --  111.00  77.00 150.00   42
120  \w     80.00 124.00   1.00    9.00    --  111.00  77.00 150.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0053689000
_diffrn_orient_matrix_UB_12      0.0177260000
_diffrn_orient_matrix_UB_13      -0.0423953000
_diffrn_orient_matrix_UB_21      -0.0870361000
_diffrn_orient_matrix_UB_22      -0.0067340000
_diffrn_orient_matrix_UB_23      -0.0047335000
_diffrn_orient_matrix_UB_31      -0.0085738000
_diffrn_orient_matrix_UB_32      0.0798408000
_diffrn_orient_matrix_UB_33      0.0090434000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            301140
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.540
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.524
_exptl_crystal_description       plate
_exptl_crystal_F_000             5424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1827
_refine_ls_number_reflns         24335
_refine_ls_number_restraints     1473
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+9.3655P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21819
_reflns_number_total             24335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b03727_si_002.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 4517328--4517333.cif.'
_cod_database_code               4517331
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C54 H66 Rh1 P2 F24 B1'
_shelx_estimated_absorpt_t_max   0.574
_shelx_estimated_absorpt_t_min   0.509
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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
 F24-F23 \\sim F2AA-F1AA \\sim F3AA-F1AA \\sim F22-F23
 with sigma of 0.04
 C54-F24 \\sim C54-F2AA \\sim C54-F3AA \\sim C54-F22 \\sim C54-F1AA \\sim
C54-F23
 with sigma of 0.02
 F22A-F23A \\sim F22A-F24A \\sim F23A-F24A \\sim F22B-F23B \\sim F22B-F24B
\\sim F23B-F24B
 with sigma of 0.04
 C53A-F22A \\sim C53A-F23A \\sim C53A-F24A \\sim C53A-F22B \\sim C53A-F23B
\\sim C53A-F24B
 with sigma of 0.02
 F8B-F9B \\sim F8B-F7B \\sim F8A-F9A \\sim F8A-F7A \\sim F9B-F7B \\sim F9A-F7A
 with sigma of 0.04
 C37A-F8B \\sim C37A-F8A \\sim C37A-F9B \\sim C37A-F9A \\sim C37A-F7B \\sim
C37A-F7A
 with sigma of 0.02
 F16A-F17A \\sim F16A-F18A \\sim F17A-F18A \\sim F16B-F17B \\sim F16B-F18B
\\sim F17B-F18B
 with sigma of 0.04
 C46A-F16A \\sim C46A-F17A \\sim C46A-F18A \\sim C46A-F16B \\sim C46A-F17B
\\sim C46A-F18B
 with sigma of 0.02
 F20-F21 \\sim F20-F19 \\sim F4AA-F5AA \\sim F4AA-F0AA \\sim F21-F19 \\sim
F5AA-F0AA
 with sigma of 0.04
 C53-F20 \\sim C53-F4AA \\sim C53-F21 \\sim C53-F5AA \\sim C53-F19 \\sim
C53-F0AA
 with sigma of 0.02
 F7-F8 \\sim F7-F9 \\sim F6AA-F7AA \\sim F6AA-F8AA \\sim F8-F9 \\sim F7AA-F8AA
 with sigma of 0.04
 C37-F7 \\sim C37-F6AA \\sim C37-F8 \\sim C37-F7AA \\sim C37-F9 \\sim C37-F8AA
 with sigma of 0.02
 F18-F17 \\sim F18-F16 \\sim F1BA-F0BA \\sim F1BA-F9AA \\sim F0BA-F9AA \\sim
F17-F16
 with sigma of 0.04
 C46-F18 \\sim C46-F1BA \\sim C46-F0BA \\sim C46-F17 \\sim C46-F9AA \\sim
C46-F16
 with sigma of 0.02
 F4-F5 \\sim F4-F6 \\sim F5-F6 \\sim F5BA-F6BA \\sim F5BA-F4BA \\sim F6BA-F4BA
 with sigma of 0.04
 C30-F4 \\sim C30-F5 \\sim C30-F6 \\sim C30-F5BA \\sim C30-F6BA \\sim C30-F4BA
 with sigma of 0.02
 F13A-F14A \\sim F13A-F15A \\sim F14A-F15A \\sim F13B-F14B \\sim F13B-F15B
\\sim F14B-F15B
 with sigma of 0.04
 C45A-F13A \\sim C45A-F14A \\sim C45A-F15A \\sim C45A-F13B \\sim C45A-F14B
\\sim C45A-F15B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F22 \\sim F23 \\sim F24 \\sim C54 \\sim F3AA \\sim F1AA \\sim F2AA: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
F22A \\sim F23A \\sim F24A \\sim C53A \\sim F22B \\sim F23B \\sim F24B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
F7A \\sim F8A \\sim F9A \\sim C37A \\sim F7B \\sim F8B \\sim F9B: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
F16A \\sim F17A \\sim F18A \\sim C46A \\sim F16B \\sim F17B \\sim F18B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
F19 \\sim F20 \\sim F21 \\sim C53 \\sim F0AA \\sim F4AA \\sim F5AA: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
F7 \\sim F8 \\sim F9 \\sim C37 \\sim F6AA \\sim F7AA \\sim F8AA: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
F16 \\sim F17 \\sim F18 \\sim C46 \\sim F9AA \\sim F0BA \\sim F1BA: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.01
F4 \\sim F5 \\sim F6 \\sim C30 \\sim F5BA \\sim F6BA \\sim F4BA: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C4C \\sim C3C \\sim C2C \\sim C1C:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C1B \\sim C2B \\sim C3B \\sim C4B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
F13A \\sim F14A \\sim F15A \\sim C45A \\sim F13B \\sim F14B \\sim F15B: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 F22, F23, F24, C54, F3AA, F1AA, F2AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F22A, F23A, F24A, C53A, F22B, F23B, F24B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7A, F8A, F9A, C37A, F7B, F8B, F9B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16A, F17A, F18A, C46A, F16B, F17B, F18B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F19, F20, F21, C53, F0AA, F4AA, F5AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, F8, F9, C37, F6AA, F7AA, F8AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16, F17, F18, C46, F9AA, F0BA, F1BA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4, F5, F6, C30, F5BA, F6BA, F4BA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C2A, C3A, C4A, C4C, C3C, C2C, C1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C3, C4, C1B, C2B, C3B, C4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F13A, F14A, F15A, C45A, F13B, F14B, F15B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F3AA)=Sof(F1AA)=Sof(F2AA)=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
 Sof(F22B)=Sof(F23B)=Sof(F24B)=1-FVAR(2)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=FVAR(2)
 Sof(F7B)=Sof(F8B)=Sof(F9B)=1-FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=FVAR(3)
 Sof(F16B)=Sof(F17B)=Sof(F18B)=1-FVAR(4)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=FVAR(4)
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=
 Sof(H4BA)=Sof(H4BB)=1-FVAR(5)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=FVAR(5)
 Sof(C4C)=Sof(H4CA)=Sof(H4CB)=Sof(C3C)=Sof(H3C)=Sof(C2C)=Sof(H2C)=Sof(C1C)=
 Sof(H1CA)=Sof(H1CB)=1-FVAR(6)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=FVAR(6)
 Sof(F0AA)=Sof(F4AA)=Sof(F5AA)=1-FVAR(7)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(7)
 Sof(F6AA)=Sof(F7AA)=Sof(F8AA)=1-FVAR(8)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(8)
 Sof(F9AA)=Sof(F0BA)=Sof(F1BA)=1-FVAR(9)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(9)
 Sof(F5BA)=Sof(F6BA)=Sof(F4BA)=1-FVAR(10)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(10)
 Sof(F13B)=Sof(F14B)=Sof(F15B)=1-FVAR(11)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=FVAR(11)
6.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C2A(H2A), C3A(H3A), C3C(H3C), C2C(H2C)
6.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C5A(H5AA,H5AB), C6A(H6AA,H6AB)
6.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C26(H26), C28(H28), C32(H32), C34(H34), C36(H36), C40(H40),
 C42(H42), C44(H44), C48(H48), C50(H50), C52(H52), C24A(H24A), C26A(H26A),
 C28A(H28A), C32A(H32A), C34A(H34A), C36A(H36A), C40A(H40A), C42A(H42A),
 C44A(H44A), C48A(H48A), C50A(H50A), C52A(H52A), C2B(H2B), C3B(H3B)
6.d X=CH2 refined with riding coordinates:
 C1(H1A,H1B), C4(H4A,H4B), C1A(H1AA,H1AB), C4A(H4AA,H4AB), C1B(H1BA,H1BB),
 C4B(H4BA,H4BB), C4C(H4CA,H4CB), C1C(H1CA,H1CB)
6.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,
 H22B,H22C), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10D,H10E,H10F),
 C12A(H12D,H12E,H12F), C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C16A(H16D,
 H16E,H16F), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F), C20A(H20D,H20E,H20F),
 C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              55542
_shelx_hkl_checksum              8249
_olex2_date_sample_data_collection 2019-02-18
_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 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.825