Reduction of (pddi)Cr reveals redox noninnocence <i>via</i> C-C bond formation amidst competing electrophilicity: [(cpta)CrMe<sub><i>n</i></sub>]<sup>-</sup> (<i>n</i> = 0, 1) and [(pta)Cr]<sup/>.
D'Arpino, Alexander A; Wolczanski, Peter T.; MacMillan, Samantha N.; Cundari, Thomas R.; Krumov, Mihail R.; Chemical communications (Cambridge, England) 60 (2024) 6785–6788; doi:10.1039/d4cc01690d

data_7133141
_publ_section_title
;
 Reduction of (pddi)Cr reveals redox noninnocence <i>via</i> C-C bond
 formation amidst competing electrophilicity:
 [(cpta)CrMe<sub><i>n</i></sub>]<sup>-</sup> (<i>n</i> = 0, 1) and
 [(pta)Cr]<sup/>.
;
_journal_issue                   53
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6785
_journal_page_last               6788
_journal_paper_doi               10.1039/d4cc01690d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C41 H50 Cr N4, C55 H64 Cr N4, 2(C20 H40 K O8), C4 H8 O'
_chemical_formula_sum            'C140 H202 Cr2 K2 N8 O17'
_chemical_formula_weight         2451.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-25
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-05-30 deposited with the CCDC.	2024-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                82.7670(10)
_cell_angle_beta                 81.4080(10)
_cell_angle_gamma                78.7040(10)
_cell_formula_units_Z            2
_cell_length_a                   12.11610(10)
_cell_length_b                   19.5547(2)
_cell_length_c                   29.7051(2)
_cell_measurement_reflns_used    88167
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      79.6600
_cell_measurement_theta_min      2.2640
_cell_volume                     6790.16(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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    -55.00  16.00   0.50    3.91    --  -48.20  55.00  37.00  142
  2  \w   -116.00 -35.00   0.50    3.91    --  -48.20 -55.00-105.00  162
  3  \w     -2.00  59.00   0.50    3.91    --   48.20 -55.00-105.00  122
  4  \w     44.00 117.00   0.50    3.91    --   48.20  55.00  37.00  146
  5  \w   -143.00-118.00   0.50   15.63    --  -90.00 -55.00-105.00   50
  6  \w    -63.00 -38.00   0.50   15.63    --  -90.00  55.00  37.00   50
  7  \w    113.00 154.00   0.50   15.63    --  111.50  55.00  37.00   82
  8  \w    -26.00  13.00   0.50    3.91    --  -48.20  19.00 150.00   78
  9  \w    -25.00  24.00   0.50    3.91    --  -48.20  19.00   0.00   98
 10  \w     43.00  86.00   0.50    3.91    --   48.20-125.00 120.00   86
 11  \w    -25.00  26.00   0.50    3.91    --   48.20 -19.00 150.00  102
 12  \w     57.00  92.00   0.50    3.91    --   48.20-125.00 -60.00   70
 13  \w    -15.00  11.00   0.50    3.91    --   48.20 -19.00  30.00   52
 14  \w    -67.00 -41.00   0.50   15.63    --  -90.00  61.00  60.00   52
 15  \w    -71.00 -19.00   0.50   15.63    --  -90.00  61.00-150.00  104
 16  \w     99.00 177.00   0.50   15.63    --  111.50 125.00 -30.00  156
 17  \w     44.00  69.00   0.50   15.63    --  111.50-116.00 -94.73   50
 18  \w     65.00 105.00   0.50   15.63    --  111.50 -94.00   0.00   80
 19  \w     76.00 109.00   0.50   15.63    --  111.50-116.00 -94.73   66
 20  \w     41.00  78.00   0.50   15.63    --  111.50 -94.00  60.00   74
 21  \w    102.00 130.00   0.50   15.63    --  111.50 -88.00 -85.13   56
 22  \w    116.00 159.00   0.50   15.63    --  111.50  45.00 -60.00   86
 23  \w    143.00 169.00   0.50   15.63    --  111.50 125.00 120.00   52
 24  \w     80.00 105.00   0.50   15.63    --  111.50 -94.00-120.00   50
 25  \w     45.00  71.00   0.50   15.63    --  111.50 -61.00 120.00   52
 26  \w     41.00  70.00   0.50   15.63    --  111.50 -61.00 150.00   58
 27  \w     47.00  72.00   0.50   15.63    --  111.50-125.00-120.00   50
 28  \w     77.00 111.00   0.50   15.63    --  111.50-125.00-120.00   68
 29  \w     42.00  68.00   0.50   15.63    --  111.50 -94.00 -30.00   52
 30  \w     80.00 105.00   0.50   15.63    --  111.50 -94.00 -30.00   50
 31  \w    115.00 141.00   0.50   15.63    --  111.50  30.00 150.00   52
 32  \w     43.00  69.00   0.50   15.63    --  111.50 -96.00 118.20   52
 33  \w     75.00 105.00   0.50   15.63    --  111.50 -96.00 118.20   60
 34  \w     43.00  71.00   0.50   15.63    --  111.50 -61.00 -30.00   56
 35  \w    147.00 173.00   0.50   15.63    --  111.50  15.00-150.00   52
 36  \w    101.00 178.00   0.50   15.63    --  111.50  45.00  60.00  154
 37  \w     45.00  70.00   0.50   15.63    --  111.50 -61.00-120.00   50
 38  \w    125.00 177.00   0.50   15.63    --  111.50  15.00   0.00  104
 39  \w    128.00 176.00   0.50   15.63    --  111.50  30.00  30.00   96
 40  \w     41.00  67.00   0.50   15.63    --  111.50 -94.00 -60.00   52
 41  \w    144.00 176.00   0.50   15.63    --  111.50  45.00 -90.00   64
 42  \w    133.00 159.00   0.50   15.63    --  111.50  45.00-120.00   52
 43  \w     80.00 105.00   0.50   15.63    --  111.50 -96.00  74.40   50
 44  \w     44.00  96.00   0.50   15.63    --  111.50-125.00 -60.00  104
 45  \w     40.00  65.00   0.50   15.63    --  111.50 -94.00 120.00   50
 46  \w     73.00 104.00   0.50   15.63    --  111.50-100.00  52.20   62
 47  \w     40.00  65.00   0.50   15.63    --  111.50 -61.00 -90.00   50
 48  \w    135.00 178.00   0.50   15.63    --  111.50  61.00  90.00   86
 49  \w     46.00  72.00   0.50   15.63    --  111.50 -77.00 -60.00   52
 50  \w     73.00 100.00   0.50   15.63    --  111.50 -77.00 -60.00   54
 51  \w     82.00 111.00   0.50   15.63    --  111.50-125.00  60.00   58
 52  \w     59.00  95.00   0.50   15.63    --  111.50 -77.00 150.00   72
 53  \w     70.00 105.00   0.50   15.63    --  111.50 -94.00  90.00   70
 54  \w    110.00 152.00   0.50   15.63    --  111.50  45.00 120.00   84
 55  \w     63.00  92.00   0.50   15.63    --  111.50 -77.00 -90.00   58
 56  \w     40.00  69.00   0.50   15.63    --  111.50 -61.00-180.00   58
 57  \w     40.00  70.00   0.50   15.63    --  111.50 -81.00  87.67   60
 58  \w     93.00 134.00   0.50   15.63    --  111.50 -81.00  87.67   82
 59  \w    115.00 150.00   0.50   15.63    --  111.50  45.00   0.00   70
 60  \w     95.00 120.00   0.50   15.63    --  111.50 125.00-180.00   50
 61  \w    152.00 177.00   0.50   15.63    --  111.50 125.00-180.00   50
 62  \w     41.00  96.00   0.50   15.63    --  111.50 -77.00   0.00  110
 63  \w     68.00  94.00   0.50   15.63    --  111.50 -77.00 120.00   52
 64  \w     94.00 177.00   0.50   15.63    --  111.50  77.00 -60.00  166
 65  \w     70.00  96.00   0.50   15.63    --  111.50 -88.00 -85.13   52
 66  \w     54.00  80.00   0.50   15.63    --  111.50-125.00-150.00   52
 67  \w     77.00 105.00   0.50   15.63    --  111.50 -94.00 150.00   56
 68  \w     55.00  81.00   0.50   15.63    --  111.50 -77.00-150.00   52
 69  \w    112.00 147.00   0.50   15.63    --  111.50  61.00 -30.00   70
 70  \w    100.00 126.00   0.50   15.63    --  111.50 -84.00-123.63   52
 71  \w     40.00  69.00   0.50   15.63    --  111.50 -84.00-123.63   58
 72  \w    153.00 178.00   0.50   15.63    --  111.50  61.00 -30.00   50
 73  \w     44.00  70.00   0.50   15.63    --  111.50 -61.00  90.00   52
 74  \w     49.00  75.00   0.50   15.63    --  111.50 -77.00  30.00   52
 75  \w     63.00  98.00   0.50   15.63    --  111.50 -77.00  60.00   70
 76  \w     52.00 102.00   0.50   15.63    --  111.50 -94.00-180.00  100
 77  \w     43.00  72.00   0.50   15.63    --  111.50 -63.00-140.67   58
 78  \w    102.00 167.00   0.50   15.63    --  111.50  30.00 -90.00  130
 79  \w    134.00 162.00   0.50   15.63    --  111.50  30.00  90.00   56
 80  \w    130.00 156.00   0.50   15.63    --  111.50 123.00  52.48   52
 81  \w    130.00 178.00   0.50   15.63    --  111.50 125.00-150.00   96
 82  \w     41.00  66.00   0.50   15.63    --  111.50 -81.00 -30.30   50
 83  \w     47.00  72.00   0.50   15.63    --  111.50 -94.00 150.00   50
 84  \w     44.00  71.00   0.50   15.63    --  111.50 -94.00-150.00   54
 85  \w     80.00 105.00   0.50   15.63    --  111.50 -94.00-150.00   50
 86  \w    104.00 133.00   0.50   15.63    --  111.50  45.00 -90.00   58
 87  \w     66.00 105.00   0.50   15.63    --  111.50 -94.00 -90.00   78
 88  \w     48.00  84.00   0.50   15.63    --  111.50-125.00-180.00   72
 89  \w     43.00  70.00   0.50   15.63    --  111.50-125.00 -30.00   54
 90  \w    104.00 158.00   0.50   15.63    --  111.50  45.00-180.00  108
 91  \w    120.00 145.00   0.50   15.63    --  111.50  45.00-150.00   50
 92  \w    120.00 146.00   0.50   15.63    --  111.50  45.00 150.00   52
 93  \w    102.00 136.00   0.50   15.63    --  111.50  30.00-180.00   68
 94  \w    120.00 155.00   0.50   15.63    --  111.50  30.00   0.00   70
 95  \w    123.00 149.00   0.50   15.63    --  111.50  15.00 -90.00   52
 96  \w    101.00 161.00   0.50   15.63    --  111.50  15.00  60.00  120
 97  \w    144.00 175.00   0.50   15.63    --  111.50  61.00-120.00   62
 98  \w    103.00 146.00   0.50   15.63    --  111.50  61.00  60.00   86
 99  \w    102.00 128.00   0.50   15.63    --  111.50  61.00 120.00   52
100  \w    108.00 134.00   0.50   15.63    --  111.50 125.00 -60.00   52
101  \w    130.00 170.00   0.50   15.63    --  111.50 125.00   0.00   80
102  \w    142.00 167.00   0.50   15.63    --  111.50 125.00  30.00   50
103  \w     40.00  81.00   0.50   15.63    --  111.50 -85.00  24.43   82
104  \w     96.00 122.00   0.50   15.63    --  111.50 -85.00  24.43   52
105  \w     43.00  68.00   0.50   15.63    --  111.50 -61.00  45.55   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1003373000
_diffrn_orient_matrix_UB_12      0.0424312000
_diffrn_orient_matrix_UB_13      0.0288480000
_diffrn_orient_matrix_UB_21      0.0433500000
_diffrn_orient_matrix_UB_22      0.0681751000
_diffrn_orient_matrix_UB_23      -0.0192811000
_diffrn_orient_matrix_UB_31      -0.0717385000
_diffrn_orient_matrix_UB_32      0.0084113000
_diffrn_orient_matrix_UB_33      -0.0396823000
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            181578
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.007
_diffrn_reflns_theta_min         2.316
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.376
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1809
_refine_ls_number_reflns         29216
_refine_ls_number_restraints     3159
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+4.6375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26948
_reflns_number_total             29216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01690d2.cif
_cod_data_source_block           raad18_abs
_cod_depositor_comments
'Adding full bibliography for 7133137--7133141.cif.'
_cod_original_cell_volume        6790.16(11)
_cod_database_code               7133141
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C136H200Cr2K2N8O16
_chemical_oxdiff_usercomment
'Recrystallized from hexanes diffusion into THF'
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.559
_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
 C1SA-C2SA = C3SA-C4SA
 1.53 with sigma of 0.02
 C2SA-C3SA
 1.54 with sigma of 0.02
 O1SA-C1SA = O1SA-C4SA
 1.44 with sigma of 0.02
 C1SB-C2SB = C3SB-C4SB
 1.53 with sigma of 0.02
 O1SB-C1SB = O1SB-C4SB
 1.44 with sigma of 0.02
 C2SB-C3SB
 1.54 with sigma of 0.02
 O1SA-C2SA = O1SA-C3SA = C1SA-C3SA = C2SA-C4SA
 2.38 with sigma of 0.04
 O1SB-C2SB = O1SB-C3SB = C1SB-C3SB = C2SB-C4SB
 2.38 with sigma of 0.04
 C203-C201 \\sim C301-C203 \\sim C302-C203 \\sim C203-C202
 with sigma of 0.02
 C1SA-C2SA \\sim C2SA-C3SA \\sim C3SA-C4SA
 with sigma of 0.02
 O1SA-C1SA \\sim O1SA-C4SA
 with sigma of 0.02
 O1SA-C2SA \\sim O1SA-C3SA
 with sigma of 0.04
 C2SA-C4SA \\sim C1SA-C3SA
 with sigma of 0.04
 O1SB-C2SB \\sim O1SB-C3SB
 with sigma of 0.04
 C2SB-C4SB \\sim C1SB-C3SB
 with sigma of 0.04
 O1SB-C1SB \\sim O1SB-C4SB
 with sigma of 0.02
 C1SB-C2SB \\sim C2SB-C3SB \\sim C3SB-C4SB
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C220 \\sim C221 \\sim C222 \\sim C223 \\sim C224 \\sim C225 \\sim C321 \\sim
C322 \\sim C324 \\sim C325: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
K1 \\sim O1 \\sim O1B \\sim O2 \\sim O2B \\sim O3 \\sim O3B \\sim O4 \\sim O4B
\\sim O5 \\sim O5B \\sim O6 \\sim O6B \\sim O7 \\sim O8 \\sim C1 \\sim H1A
\\sim H1B \\sim C1B \\sim H1BA \\sim H1BB \\sim C2 \\sim H2A \\sim H2B \\sim
C2B \\sim H2BA \\sim H2BB \\sim C3 \\sim H3A \\sim H3B \\sim C3B \\sim H3BA
\\sim H3BB \\sim C4 \\sim H4A \\sim H4B \\sim C4B \\sim H4BA \\sim H4BB \\sim
C5 \\sim H5A \\sim H5B \\sim C5B \\sim H5BA \\sim H5BB \\sim C6 \\sim H6A \\sim
H6B \\sim C6B \\sim H6BA \\sim H6BB \\sim C7 \\sim H7A \\sim H7B \\sim C7B
\\sim H7BA \\sim H7BB \\sim C8 \\sim H8A \\sim H8B \\sim C8B \\sim H8BA \\sim
H8BB \\sim C9 \\sim H9A \\sim H9B \\sim C9B \\sim H9BA \\sim H9BB \\sim C10
\\sim H10A \\sim H10B \\sim C10B \\sim H10C \\sim H10D \\sim C11 \\sim H11A
\\sim H11B \\sim C11B \\sim H11C \\sim H11D \\sim C12 \\sim H12A \\sim H12B
\\sim C12B \\sim H12C \\sim H12D \\sim C13 \\sim H13A \\sim H13B \\sim C14
\\sim H14A \\sim H14B \\sim C15 \\sim H15A \\sim H15B \\sim C16 \\sim H16A
\\sim H16B \\sim C17 \\sim H17A \\sim H17B \\sim C18 \\sim H18A \\sim H18B
\\sim C19 \\sim H19A \\sim H19B \\sim C20 \\sim H20H \\sim H20I: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C201 \\sim C202 \\sim C203 \\sim C301 \\sim C302: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1SA \\sim C1SA \\sim C2SA \\sim C3SA \\sim C4SA: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1SB \\sim C1SB \\sim C2SB \\sim C3SB \\sim C4SB: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O1SA \\sim C1SA \\sim C4SA \\sim C2SA \\sim C3SA \\sim C2SB \\sim C3SB \\sim
C4SB \\sim C1SB \\sim O1SB: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C220, C221, C222, C223, C224, C225, C321, C322, C324, C325
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 K1, O1, O1B, O2, O2B, O3, O3B, O4, O4B, O5, O5B, O6, O6B, O7, O8, C1, H1A,
 H1B, C1B, H1BA, H1BB, C2, H2A, H2B, C2B, H2BA, H2BB, C3, H3A, H3B, C3B, H3BA,
 H3BB, C4, H4A, H4B, C4B, H4BA, H4BB, C5, H5A, H5B, C5B, H5BA, H5BB, C6, H6A,
 H6B, C6B, H6BA, H6BB, C7, H7A, H7B, C7B, H7BA, H7BB, C8, H8A, H8B, C8B, H8BA,
 H8BB, C9, H9A, H9B, C9B, H9BA, H9BB, C10, H10A, H10B, C10B, H10C, H10D, C11,
 H11A, H11B, C11B, H11C, H11D, C12, H12A, H12B, C12B, H12C, H12D, C13, H13A,
 H13B, C14, H14A, H14B, C15, H15A, H15B, C16, H16A, H16B, C17, H17A, H17B, C18,
 H18A, H18B, C19, H19A, H19B, C20, H20H, H20I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C201, C202, C203, C301, C302
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1SA, C1SA, C2SA, C3SA, C4SA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1SB, C1SB, C2SB, C3SB, C4SB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1SA, C1SA, C4SA, C2SA, C3SA, C2SB, C3SB, C4SB, C1SB, O1SB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O1SB, C1SB, C2SB, C3SB, C4SB} sigma for 1-2: 0.02, 1-3: 0.02
as in
{O1SA, C1SA, C2SA, C3SA, C4SA}
6. Others
 Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C4B)=
 Sof(H4BA)=Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=
 Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=
 Sof(H9BB)=Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=
 Sof(C12B)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(C1)=Sof(H1A)=Sof(H1B)=
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=
 Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Sof(H20G)=Sof(C301)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C302)=Sof(H30D)=
 Sof(H30E)=Sof(H30F)=1-FVAR(2)
 Sof(C201)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C202)=Sof(H20D)=Sof(H20E)=
 Sof(H20F)=Sof(H203)=FVAR(2)
 Sof(H22A)=Sof(C321)=Sof(H321)=Sof(C322)=Sof(H322)=Sof(C324)=Sof(H324)=
 Sof(C325)=Sof(H325)=1-FVAR(3)
 Sof(C221)=Sof(H221)=Sof(C222)=Sof(H222)=Sof(H223)=Sof(C224)=Sof(H224)=
 Sof(C225)=Sof(H225)=FVAR(3)
 Sof(O1SB)=Sof(C1SB)=Sof(H1SC)=Sof(H1SD)=Sof(C2SB)=Sof(H2SC)=Sof(H2SD)=
 Sof(C3SB)=Sof(H3SC)=Sof(H3SD)=Sof(C4SB)=Sof(H4SC)=Sof(H4SD)=1-FVAR(4)
 Sof(O1SA)=Sof(C1SA)=Sof(H1SA)=Sof(H1SB)=Sof(C2SA)=Sof(H2SA)=Sof(H2SB)=
 Sof(C3SA)=Sof(H3SA)=Sof(H3SB)=Sof(C4SA)=Sof(H4SA)=Sof(H4SB)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C103(H103), C110(H110), C119(H119), C120(H120), C136(H136), C139(H139),
 C203(H203), C203(H20G), C210(H210), C219(H219), C227(H227), C249(H249),
 C252(H252)
7.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C230(H23A,H23B), C1(H1A,H1B), C1B(H1BA,H1BB), C2(H2A,H2B),
 C2B(H2BA,H2BB), C3(H3A,H3B), C3B(H3BA,H3BB), C4(H4A,H4B), C4B(H4BA,H4BB),
 C5(H5A,H5B), C5B(H5BA,H5BB), C6(H6A,H6B), C6B(H6BA,H6BB), C7(H7A,H7B),
 C7B(H7BA,H7BB), C8(H8A,H8B), C8B(H8BA,H8BB), C9(H9A,H9B), C9B(H9BA,H9BB),
 C10(H10A,H10B), C10B(H10C,H10D), C11(H11A,H11B), C11B(H11C,H11D), C12(H12A,
 H12B), C12B(H12C,H12D), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20H,H20I),
  C21(H21G,H21H), C22(H22H,H22I), C23(H23C,H23D), C24(H24A,H24B), C25(H25M,
 H25N), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30G,H30H), 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), C1SA(H1SA,H1SB), C2SA(H2SA,H2SB), C3SA(H3SA,H3SB),
 C4SA(H4SA,H4SB), C1SB(H1SC,H1SD), C2SB(H2SC,H2SD), C3SB(H3SC,H3SD), C4SB(H4SC,
 H4SD)
7.c Aromatic/amide H refined with riding coordinates:
 C105(H105), C106(H106), C107(H107), C114(H114), C115(H115), C116(H116),
 C117(H117), C125(H125), C126(H126), C127(H127), C128(H128), C132(H132),
 C133(H133), C134(H134), C205(H205), C206(H206), C207(H207), C214(H214),
 C215(H215), C216(H216), C217(H217), C221(H221), C222(H222), C223(H223),
 C223(H22A), C224(H224), C225(H225), C232(H232), C233(H233), C234(H234),
 C235(H235), C236(H236), C238(H238), C239(H239), C240(H240), C241(H241),
 C245(H245), C246(H246), C247(H247), C321(H321), C322(H322), C324(H324),
 C325(H325)
7.d Idealised Me refined as rotating group:
 C101(H10E,H10F,H10G), C102(H10H,H10I,H10J), C111(H11E,H11F,H11G), C112(H11H,
 H11I,H11J), C122(H12E,H12F,H12G), C123(H12H,H12I,H12J), C137(H13C,H13D,H13E),
 C138(H13F,H13G,H13H), C140(H14C,H14D,H14E), C141(H14F,H14G,H14H), C201(H20A,
 H20B,H20C), C202(H20D,H20E,H20F), C211(H21A,H21B,H21C), C212(H21D,H21E,H21F),
 C228(H22B,H22C,H22D), C229(H22E,H22F,H22G), C250(H25A,H25B,H25C), C251(H25D,
 H25E,H25F), C253(H25G,H25H,H25I), C254(H25J,H25K,H25L), C301(H30A,H30B,H30C),
 C302(H30D,H30E,H30F)
;
_shelx_res_checksum              11746
_shelx_hkl_checksum              99689
_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 1.768
_oxdiff_exptl_absorpt_empirical_full_min 0.583