Taking Solution Proton NMR to Its Extreme: Prediction and Detection of a Hydride Resonance in an Intermediate-Spin Iron Complex.
Ott, Jonas C.; Wadepohl, Hubert; Enders, Markus; Gade, Lutz H.; Journal of the American Chemical Society 140 (2018) 17413–17417; doi:10.1021/jacs.8b11330

data_4133576
_publ_section_title
;
 Taking Solution Proton NMR to Its Extreme: Prediction and Detection of a
 Hydride Resonance in an Intermediate-Spin Iron Complex.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17413
_journal_page_last               17417
_journal_paper_doi               10.1021/jacs.8b11330
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C39.25 H66 Fe N P2'
_chemical_formula_weight         669.72
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_jo14
_audit_creation_date             2017-12-22
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_audit_update_record
'24.09.2018 16:26:14 CEST UTC+02:00  encif 1.84'
_cell_angle_alpha                90
_cell_angle_beta                 102.5436(13)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   25.6211(3)
_cell_length_b                   13.0431(2)
_cell_length_c                   47.8048(7)
_cell_measurement_reflns_used    45450
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      69.5280
_cell_measurement_theta_min      3.5070
_cell_volume                     15594.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-17); encifer 1.5.2 (CCDC, 2016)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2014 (Giacovazzo et al., 2014)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_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 0.994
_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    -31.00  73.00   1.00    2.50    --    0.00  38.00 120.00  104
  2  \w    -33.00  72.00   1.00    2.50    --    0.00  77.00-150.00  105
  3  \w    -31.00  73.00   1.00    2.50    --    0.00  38.00 -30.00  104
  4  \w    -71.00  24.00   1.00    2.50    --    0.00 -57.00-180.00   95
  5  \w    -35.00  11.00   1.00    2.50    --   16.00 109.00  -0.16   46
  6  \w    -25.00   8.00   1.00    7.50    --   28.00 113.00  79.73   33
  7  \w    -10.00  18.00   1.00    7.50    --   36.00 101.00   8.24   28
  8  \w      3.00  29.00   1.00    7.50    --   44.00  91.00  82.20   26
  9  \w      6.00  34.00   1.00    7.50    --   44.00  87.00 -55.74   28
 10  \w      3.00  29.00   1.00    7.50    --   44.00  91.00-136.82   26
 11  \w     12.00  40.00   1.00    7.50    --   48.00  83.00 -48.67   28
 12  \w     11.00  38.00   1.00    7.50    --   48.00  84.00   9.77   27
 13  \w     12.00  40.00   1.00    7.50    --   48.00  83.00 173.90   28
 14  \w     16.00  45.00   1.00    7.50    --   52.00  82.00  98.20   29
 15  \w     16.00  45.00   1.00    7.50    --   52.00  82.00  -5.38   29
 16  \w     17.00  46.00   1.00    7.50    --   52.00  80.00 127.61   29
 17  \w     16.00  45.00   1.00    7.50    --   52.00  82.00 -14.17   29
 18  \w    -17.00  78.00   1.00    7.50    --   54.00 -57.00  30.00   95
 19  \w    -17.00  78.00   1.00    7.50    --   54.00 -57.00 -90.00   95
 20  \w     21.00 126.00   1.00    7.50    --   54.00  77.00  60.00  105
 21  \w     21.00 126.00   1.00    7.50    --   54.00  77.00 120.00  105
 22  \w     23.00 114.00   1.00    7.50    --   54.00-125.00  60.00   91
 23  \w      1.00  99.00   1.00    7.50    --   54.00 -99.00-150.00   98
 24  \w     23.00 114.00   1.00    7.50    --   54.00-125.00-180.00   91
 25  \w     21.00 126.00   1.00    7.50    --   54.00  77.00  30.00  105
 26  \w     22.00  49.00   1.00    7.50    --   56.00  78.00  99.76   27
 27  \w     23.00 128.00   1.00    7.50    --   56.00  76.00  -7.40  105
 28  \w     22.00  49.00   1.00    7.50    --   56.00  78.00 -51.67   27
 29  \w     22.00  49.00   1.00    7.50    --   56.00  78.00  10.41   27
 30  \w     22.00  49.00   1.00    7.50    --   56.00  78.00-102.81   27
 31  \w     23.00 128.00   1.00    7.50    --   56.00  76.00-150.48  105
 32  \w     22.00  49.00   1.00    7.50    --   56.00  78.00-134.67   27
 33  \w     27.00 132.00   1.00    7.50    --   60.00  76.00 157.89  105
 34  \w     32.00 131.00   1.00    7.50    --   60.00  67.00  16.82   99
 35  \w     27.00 132.00   1.00    7.50    --   60.00  77.00 -78.42  105
 36  \w     28.00 132.00   1.00    7.50    --   60.00  75.00-117.67  104
 37  \w     27.00 132.00   1.00    7.50    --   60.00  76.00-100.73  105
 38  \w     30.00 132.00   1.00    7.50    --   60.00  72.00 114.90  102
 39  \w     31.00 136.00   1.00    7.50    --   64.00  77.00 -34.80  105
 40  \w     33.00 136.00   1.00    7.50    --   64.00  73.00 -82.12  103
 41  \w     34.00 136.00   1.00    7.50    --   64.00  72.00 -63.53  102
 42  \w     31.00 136.00   1.00    7.50    --   64.00  76.00 176.51  105
 43  \w     33.00 136.00   1.00    7.50    --   64.00  73.00-161.09  103
 44  \w     35.00 135.00   1.00    7.50    --   64.00  69.00  20.72  100
 45  \w     35.00 140.00   1.00    7.50    --   68.00  76.00  47.79  105
 46  \w     42.00 138.00   1.00    7.50    --   68.00  63.00 -75.36   96
 47  \w     35.00 129.00   1.00    7.50    --   68.00  76.00 101.47   94
 48  \w     42.00  68.00   1.00    7.50    --   68.00  64.00-167.32   26
 49  \w     47.00  95.00   1.00    7.50    --   68.00  74.00-142.52   48
 50  \w     45.00 115.00   1.00    7.50    --   72.00  71.00  52.17   70
 51  \w     46.00  98.00   1.00    7.50    --   72.00  72.00  94.81   52
 52  \w     53.00  79.00   1.00    7.50    --   72.00  69.00   1.58   26
 53  \w     44.00  70.00   1.00    7.50    --   72.00  67.00-112.20   26
 54  \w     51.00  96.00   1.00    7.50    --   76.00  64.00 126.55   45
 55  \w     43.00  84.00   1.00    7.50    --   76.00  77.00  62.19   41
 56  \w     48.00  74.00   1.00    7.50    --   76.00  67.00  -1.75   26
 57  \w     51.00 103.00   1.00    7.50    --   76.00  63.00 161.51   52
 58  \w     51.00 103.00   1.00    7.50    --   76.00  47.00-149.92   52
 59  \w     92.00 133.00   1.00    7.50    --   76.00  76.00 -50.99   41
 60  \w     43.00  89.00   1.00    7.50    --   76.00  76.00 -50.99   46
 61  \w     57.00  88.00   1.00    7.50    --   80.00  65.00  50.61   31
 62  \w     52.00 114.00   1.00    7.50    --   80.00  69.00 -16.14   62
 63  \w     47.00  78.00   1.00    7.50    --   80.00  77.00 -97.90   31
 64  \w     56.00 109.00   1.00    7.50    --   80.00  61.00-113.63   53
 65  \w     56.00  81.00   1.00    7.50    --   80.00  56.00 114.23   25
 66  \w     55.00 150.00   1.00    7.50    --   80.00  67.00   9.43   95
 67  \w     48.00  74.00   1.00    7.50    --   80.00  75.00  20.82   26
 68  \w     53.00  79.00   1.00   15.00    --   84.00  74.00 -15.13   26
 69  \w     53.00  95.00   1.00   15.00    --   84.00  73.00 -95.25   42
 70  \w     57.00  83.00   1.00   15.00    --   84.00  65.00-172.49   26
 71  \w     56.00  89.00   1.00   15.00    --   88.00  75.00 -52.44   33
 72  \w     58.00 137.00   1.00   15.00    --   88.00  72.00  43.73   79
 73  \w     55.00  81.00   1.00   15.00    --   88.00  77.00 -62.05   26
 74  \w     56.00 119.00   1.00   15.00    --   88.00  75.00 117.94   63
 75  \w     62.00 155.00   1.00   15.00    --   88.00  63.00 158.13   93
 76  \w     58.00  96.00   1.00   15.00    --   88.00  72.00   8.70   38
 77  \w     63.00  88.00   1.00   15.00    --   88.00  49.00 106.96   25
 78  \w     58.00 160.00   1.00   15.00    --   88.00  72.00 -89.27  102
 79  \w     68.00 111.00   1.00   15.00    --   92.00  60.00-169.84   43
 80  \w     61.00  88.00   1.00   15.00    --   92.00  74.00  49.08   27
 81  \w     59.00  92.00   1.00   15.00    --   92.00  76.00 -20.66   33
 82  \w     71.00 127.00   1.00   15.00    --   96.00  53.00  51.40   56
 83  \w     66.00  91.00   1.00   15.00    --   96.00  72.00  84.87   25
 84  \w     71.00 113.00   1.00   15.00    --   96.00  61.00  -6.77   42
 85  \w     67.00  93.00   1.00   15.00    --  100.00  76.00-138.30   26
 86  \w     74.00 127.00   1.00   15.00    --  100.00  50.00  35.03   53
 87  \w     78.00 123.00   1.00   15.00    --  100.00  59.00-106.12   45
 88  \w     75.00 169.00   1.00   15.00    --  104.00  70.00-134.54   94
 89  \w     78.00 104.00   1.00   15.00    --  108.00  77.00-150.00   26
 90  \w     38.00 133.00   1.00   15.00    --  108.00 -64.00   0.00   95
 91  \w     84.00 178.00   1.00   15.00    --  108.00  64.00  90.00   94
 92  \w     82.00 177.00   1.00   15.00    --  108.00  64.00  30.00   95
 93  \w     82.00 162.00   1.00   15.00    --  108.00  64.00   0.00   80
 94  \w     82.00 178.00   1.00   15.00    --  108.00  64.00 -30.00   96
 95  \w    136.00 174.00   1.00   15.00    --  108.00  64.00-150.00   38
 96  \w     82.00 107.00   1.00   15.00    --  108.00  64.00-150.00   25
 97  \w     76.00 102.00   1.00   15.00    --  108.00  77.00  60.00   26
 98  \w     82.00 108.00   1.00   15.00    --  108.00  64.00 150.00   26
 99  \w     82.00 178.00   1.00   15.00    --  108.00  64.00-180.00   96
100  \w     85.00 178.00   1.00   15.00    --  108.00  64.00  60.00   93
101  \w    101.00 140.00   1.00   15.00    --  108.00 -77.00  60.00   39
102  \w     37.00  78.00   1.00   15.00    --  108.00 -77.00  60.00   41
103  \w    152.00 178.00   1.00   15.00    --  108.00  77.00 -90.00   26
104  \w     75.00 101.00   1.00   15.00    --  108.00  77.00 -90.00   26
105  \w     76.00 102.00   1.00   15.00    --  108.00  77.00  30.00   26
106  \w     82.00 108.00   1.00   15.00    --  108.00  64.00 -60.00   26
107  \w     74.00 115.00   1.00   15.00    --  108.00-111.00 -60.00   41
108  \w     75.00 101.00   1.00   15.00    --  108.00  77.00   0.00   26
109  \w     75.00 101.00   1.00   15.00    --  108.00  77.00 -30.00   26
110  \w    129.00 162.00   1.00   15.00    --  108.00  77.00-120.00   33
111  \w     75.00 101.00   1.00   15.00    --  108.00  77.00-120.00   26
112  \w     75.00 101.00   1.00   15.00    --  108.00  77.00  90.00   26
113  \w     75.00 160.00   1.00   15.00    --  108.00  77.00 150.00   85
114  \w     82.00 124.00   1.00   15.00    --  108.00  64.00 120.00   42
115  \w     75.00 100.00   1.00   15.00    --  108.00  77.00-180.00   25
116  \w     75.00 169.00   1.00   15.00    --  108.00  77.00 -60.00   94
117  \w     82.00 164.00   1.00   15.00    --  108.00  64.00 -90.00   82
118  \w     53.00 108.00   1.00   15.00    --  108.00 -77.00 -60.00   55
119  \w     69.00 109.00   1.00   15.00    --  108.00-103.00 120.00   40
120  \w     37.00 134.00   1.00   15.00    --  108.00 -50.00-180.00   97
121  \w    113.00 178.00   1.00   15.00    --  108.00  77.00 120.00   65
122  \w     75.00 101.00   1.00   15.00    --  108.00  77.00 120.00   26
123  \w     41.00 148.00   1.00   15.00    --  108.00 -92.00-150.00  107
124  \w     84.00 114.00   1.00   15.00    --  108.00-111.00  60.00   30
125  \w     80.00 106.00   1.00   15.00    --  108.00  70.00-147.77   26
126  \w     78.00 145.00   1.00   15.00    --  108.00  38.00-120.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, 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      -0.0502207000
_diffrn_orient_matrix_UB_12      0.0351424000
_diffrn_orient_matrix_UB_13      -0.0188901000
_diffrn_orient_matrix_UB_21      -0.0523814000
_diffrn_orient_matrix_UB_22      0.0139535000
_diffrn_orient_matrix_UB_23      -0.0571370000
_diffrn_orient_matrix_UB_31      -0.0223171000
_diffrn_orient_matrix_UB_32      -0.1118278000
_diffrn_orient_matrix_UB_33      -0.0130606000
_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  0.1039
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            460540
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.046
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.053
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             5832
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.074
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1601
_refine_ls_number_reflns         29398
_refine_ls_number_restraints     3819
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+15.5862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22763
_reflns_number_total             29398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11330_si_002.cif
_cod_data_source_block           ga_jo14_sq
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               4133576
_audit_block_refno               3005
_audit_block_usercomment         'JO135, block, yellow'
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.687
_reflns_odcompleteness_completeness 59.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C16-C17 \\sim C16-C18 \\sim C16-C19
 with sigma of 0.02
 C17-C18 \\sim C17-C19 \\sim C18-C19
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30,
 C31, C32, C33, C34, C35, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, C57, C58, C59, C60, C61, C62, C63, C64, C65, C66, C67, C68, C69, C70,
 C71, C72, C73, C74, C75, C76, C77, C78, C79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C96, C97, C98, C99, C100, C101, C102, C103, C104, C105, C106, C107, C108,
 C109, C110, C111, C112, C113, C114, C115, C116, C117, C118, C119
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C136, C137, C138, C139, C140, C141, C142, C143, C144, C145, C146, C147, C148,
 C149, C150, C151, C152, C153, C154, C155, C156, C157, C158, C159
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C20, C21, C22, C23}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C24, C25, C26, C27}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C28, C29, C30, C31}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C32, C33, C34, C35}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C36, C37, C38, C39}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C56, C57, C58, C59}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C60, C61, C62, C63}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C64, C65, C66, C67}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C68, C69, C70, C71}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C72, C73, C74, C75}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C76, C77, C78, C79}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C96, C97, C98, C99}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C100, C101, C102, C103}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C104, C105, C106, C107}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C108, C109, C110, C111}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C112, C113, C114, C115}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C116, C117, C118, C119}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C136, C137, C138, C139}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C140, C141, C142, C143}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C144, C145, C146, C147}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C148, C149, C150, C151}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C152, C153, C154, C155}
{C16, C17, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04
as
{C156, C157, C158, C159}
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C54(H54A,H54B), C55(H55A,H55B), C94(H94A,
 H94B), C95(H95A,H95B), C134(H13A,H13B), C135(H13C,H13D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C9(H9), C11(H11), C44(H44), C46(H46), C49(H49), C51(H51),
 C84(H84), C86(H86), C89(H89), C91(H91), C124(H124), C126(H126), C129(H129),
 C131(H131)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C97(H97A,H97B,
 H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C), C101(H10A,H10B,H10C),
 C102(H10D,H10E,H10F), C103(H10G,H10H,H10I), C105(H10J,H10K,H10L), C106(H10M,
 H10N,H10O), C107(H10P,H10Q,H10R), C109(H10S,H10T,H10U), C110(H11A,H11B,H11C),
 C111(H11D,H11E,H11F), C113(H11G,H11H,H11I), C114(H11J,H11K,H11L), C115(H11M,
 H11N,H11O), C117(H11P,H11Q,H11R), C118(H11S,H11T,H11U), C119(H11V,H11W,H11X),
 C137(H13E,H13F,H13G), C138(H13H,H13I,H13J), C139(H13K,H13L,H13M), C141(H14C,
 H14D,H14E), C142(H14F,H14G,H14H), C143(H14I,H14J,H14K), C145(H14L,H14M,H14N),
 C146(H14O,H14P,H14Q), C147(H14R,H14S,H14T), C149(H14U,H14V,H14W), C150(H15C,
 H15D,H15E), C151(H15F,H15G,H15H), C153(H15I,H15J,H15K), C154(H15L,H15M,H15N),
 C155(H15O,H15P,H15Q), C157(H15R,H15S,H15T), C158(H15U,H15V,H15W), C159(H15X,
 H15Y,HD)
;
_shelx_hkl_checksum              7072
_shelx_fab_checksum              88453
_platon_squeeze_void_probe_radius 1.20
_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
;
_shelx_res_checksum              67322
_cell_oxdiff_length_a            31.0293441(6)
_cell_oxdiff_length_b            8.4712
_cell_oxdiff_length_c            38.2557566(8)
_cell_oxdiff_angle_alpha         90.0
_cell_oxdiff_angle_beta          102.4597
_cell_oxdiff_angle_gamma         89.6113
_cell_oxdiff_volume              2.00e-004
_cell_oxdiff_measurement_reflns_used 47892