Defying strain in the synthesis of an electroactive bilayer helicene
Milton, Margarita; Schuster, Nathaniel J.; Paley, Daniel W.; Hernández Sánchez, Raúl; Ng, Fay; Steigerwald, Michael L.; Nuckolls, Colin; Chemical Science  (2019) –; doi:10.1039/C8SC04216K

data_1550264
_publ_section_title
;
 Defying strain in the synthesis of an electroactive bilayer helicene
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04216K
_journal_year                    2019
_chemical_formula_moiety         'C106 H110 N4 O8, C7 H8 O'
_chemical_formula_sum            'C113 H118 N4 O9'
_chemical_formula_weight         1676.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-28 deposited with the CCDC.
2018-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                75.736(3)
_cell_angle_beta                 74.285(3)
_cell_angle_gamma                76.470(3)
_cell_formula_units_Z            2
_cell_length_a                   15.2191(5)
_cell_length_b                   16.2207(6)
_cell_length_c                   19.6692(8)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.5700
_cell_measurement_theta_min      4.0300
_cell_volume                     4456.7(3)
_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  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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    -26.00   6.00   1.00    2.00    --   37.78 -37.00 120.00   32
  2  \w     51.00  76.00   1.00    2.00    --   37.78 -99.00 150.00   25
  3  \w     26.00  73.00   1.00    2.00    --   37.78 -99.00  30.00   47
  4  \w     45.00  71.00   1.00    2.00    --   37.78 -99.00 -60.00   26
  5  \w     47.00  73.00   1.00   10.00    --  111.00 -30.00  60.00   26
  6  \w     86.00 123.00   1.00   10.00    --  111.00 -45.00  90.00   37
  7  \w    114.00 140.00   1.00   10.00    --  111.00 -15.00 120.00   26
  8  \w     94.00 131.00   1.00   10.00    --  111.00 -30.00  60.00   37
  9  \w     97.00 138.00   1.00   10.00    --  111.00 -77.00  30.00   41
 10  \w    105.00 130.00   1.00   10.00    --  111.00 -30.00 -30.00   25
 11  \w    104.00 130.00   1.00   10.00    --  111.00 -15.00 -60.00   26
 12  \w    149.00 178.00   1.00   10.00    --  111.00   0.00 -90.00   29
 13  \w    150.00 177.00   1.00   10.00    --  111.00  45.00 -60.00   27
 14  \w    151.00 177.00   1.00   10.00    --  111.00 111.00-150.00   26
 15  \w    134.00 160.00   1.00   10.00    --  111.00  77.00 -60.00   26
 16  \w    126.00 168.00   1.00   10.00    --  111.00 111.00   0.00   42
 17  \w    125.00 150.00   1.00   10.00    --  111.00 178.00 -90.00   25
 18  \w    102.00 128.00   1.00   10.00    --  111.00 111.00 -30.00   26
 19  \w     97.00 175.00   1.00   10.00    --  111.00  61.00 -90.00   78
 20  \w    118.00 144.00   1.00   10.00    --  111.00  45.00-180.00   26
 21  \w    115.00 148.00   1.00   10.00    --  111.00 -15.00-120.00   33
 22  \w    102.00 141.00   1.00   10.00    --  111.00  45.00 -60.00   39
 23  \w    106.00 150.00   1.00   10.00    --  111.00  30.00   0.00   44
 24  \w    107.00 132.00   1.00   10.00    --  111.00  61.00  60.00   25
 25  \w    119.00 144.00   1.00   10.00    --  111.00  45.00 120.00   25
 26  \w    104.00 129.00   1.00   10.00    --  111.00  61.00 150.00   25
 27  \w    106.00 160.00   1.00   10.00    --  111.00 111.00  90.00   54
 28  \w     95.00 155.00   1.00   10.00    --  111.00  45.00 -30.00   60
 29  \w    102.00 127.00   1.00   10.00    --  111.00 -17.00 -25.87   25
 30  \w     95.00 124.00   1.00   10.00    --  111.00   0.00 -90.00   29
 31  \w     98.00 123.00   1.00   10.00    --  111.00  30.00 -30.00   25
 32  \w     94.00 119.00   1.00   10.00    --  111.00  61.00   0.00   25
 33  \w     95.00 132.00   1.00   10.00    --  111.00  45.00 -90.00   37
 34  \w     89.00 171.00   1.00   10.00    --  111.00  77.00-150.00   82
 35  \w     72.00 127.00   1.00   10.00    --  111.00 -61.00-180.00   55
 36  \w     97.00 128.00   1.00   10.00    --  111.00 -61.00-120.00   31
 37  \w     89.00 114.00   1.00   10.00    --  111.00-111.00 -30.00   25
 38  \w    102.00 137.00   1.00   10.00    --  111.00 -86.00   0.57   35
 39  \w    101.00 126.00   1.00   10.00    --  111.00 -61.00 -30.00   25
 40  \w     82.00 116.00   1.00   10.00    --  111.00-111.00  30.00   34
 41  \w     73.00 106.00   1.00   10.00    --  111.00 -94.00 -60.00   33
 42  \w     78.00 111.00   1.00   10.00    --  111.00 -99.00 -93.78   33
 43  \w     82.00 108.00   1.00   10.00    --  111.00 -77.00-150.00   26
 44  \w     78.00 116.00   1.00   10.00    --  111.00-111.00 -60.00   38
 45  \w     58.00  93.00   1.00   10.00    --  111.00 -77.00 -60.00   35
 46  \w     55.00 105.00   1.00   10.00    --  111.00 -38.00 -79.93   50
 47  \w     60.00  85.00   1.00   10.00    --  111.00 -45.00-150.00   25
 48  \w     47.00  72.00   1.00   10.00    --  111.00 -99.00 -93.78   25
 49  \w     50.00  84.00   1.00   10.00    --  111.00-111.00-150.00   34
 50  \w     45.00  73.00   1.00   10.00    --  111.00 -94.00-180.00   28
 51  \w     42.00 108.00   1.00   10.00    --  111.00 -94.00-150.00   66
 52  \w     57.00  82.00   1.00   10.00    --  111.00 -45.00 -60.00   25
 53  \w     47.00  83.00   1.00   10.00    --  111.00 -45.00   0.00   36
 54  \w     53.00  79.00   1.00   10.00    --  111.00 -94.00 -30.00   26
 55  \w     55.00 100.00   1.00   10.00    --  111.00 -94.00  30.00   45
 56  \w     54.00 116.00   1.00   10.00    --  111.00-111.00  90.00   62
 57  \w     87.00 112.00   1.00   10.00    --  111.00-111.00 150.00   25
 58  \w     79.00 120.00   1.00   10.00    --  111.00 -86.00 120.02   41
 59  \w     67.00  93.00   1.00   10.00    --  111.00 -15.00 120.00   26
 60  \w     73.00  98.00   1.00   10.00    --  111.00 -61.00 150.00   25
 61  \w     44.00  75.00   1.00   10.00    --  111.00 -45.00  90.00   31
 62  \w     42.00  91.00   1.00   10.00    --  111.00 -28.00 149.42   49
 63  \w     46.00  93.00   1.00   10.00    --  111.00 -61.00  90.00   47
 64  \w     44.00  93.00   1.00   10.00    --  111.00-113.00 131.00   49
 65  \w     45.00  70.00   1.00   10.00    --  111.00 -77.00  30.00   25
 66  \w     50.00  87.00   1.00   10.00    --  111.00 -86.00   0.57   37
 67  \w     49.00  77.00   1.00   10.00    --  111.00-111.00 -30.00   28
 68  \w     41.00  78.00   1.00   10.00    --  111.00 -30.00 -30.00   37
 69  \w     48.00  73.00   1.00   10.00    --  111.00   0.00 -90.00   25
 70  \w     47.00  80.00   1.00   10.00    --  111.00 -17.00 -25.87   33
 71  \w     41.00  66.00   1.00   10.00    --  111.00 -15.00 -60.00   25
 72  \w    -61.00  27.00   1.00    2.00    --  -37.78  77.00-180.00   88
 73  \w   -106.00 -30.00   1.00    2.00    --  -37.78 -37.00 -30.00   76
 74  \w   -105.00 -21.00   1.00    2.00    --  -37.78 -57.00  60.00   84
 75  \w   -105.00 -30.00   1.00    2.00    --  -37.78 -77.00 -60.00   75
 76  \w   -109.00 -38.00   1.00    2.00    --  -37.78-178.00 150.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0420418000
_diffrn_orient_matrix_UB_12      0.0171935000
_diffrn_orient_matrix_UB_13      -0.0816653000
_diffrn_orient_matrix_UB_21      0.0322096000
_diffrn_orient_matrix_UB_22      -0.0979520000
_diffrn_orient_matrix_UB_23      0.0029896000
_diffrn_orient_matrix_UB_31      -0.0928437000
_diffrn_orient_matrix_UB_32      -0.0056413000
_diffrn_orient_matrix_UB_33      -0.0143296000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65476
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.350
_diffrn_reflns_theta_min         3.342
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       prism
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         17715
_refine_ls_number_restraints     730
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0947
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1647P)^2^+2.3525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2589
_refine_ls_wR_factor_ref         0.3043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11204
_reflns_number_total             17715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04216k2.cif
_cod_data_source_block           heli7
_cod_database_code               1550264
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'c113 h118 N4 O9'
_reflns_odcompleteness_completeness 97.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
 N15_1-C16_1
 N15_2-C16_2
 N15_3-C16_3
 N15_4-C16_4
 1.5 with sigma of 0.02
 C16_1-C17_1 = C17_1-C18_1 = C18_1-C19_1 = C19_1-C20_1 = C20_1-C21_1 = C16_1-
 C22_1 = C22_1-C23_1 = C23_1-C24_1 = C24_1-C25_1 = C25_1-C26_1
 C16_2-C17_2 = C17_2-C18_2 = C18_2-C19_2 = C19_2-C20_2 = C20_2-C21_2 = C16_2-
 C22_2 = C22_2-C23_2 = C23_2-C24_2 = C24_2-C25_2 = C25_2-C26_2
 C16_3-C17_3 = C17_3-C18_3 = C18_3-C19_3 = C19_3-C20_3 = C20_3-C21_3 = C16_3-
 C22_3 = C22_3-C23_3 = C23_3-C24_3 = C24_3-C25_3 = C25_3-C26_3
 C16_4-C17_4 = C17_4-C18_4 = C18_4-C19_4 = C19_4-C20_4 = C20_4-C21_4 = C16_4-
 C22_4 = C22_4-C23_4 = C23_4-C24_4 = C24_4-C25_4 = C25_4-C26_4
 1.54 with sigma of 0.02
 N15_1-C17_1 = N15_1-C22_1
 N15_2-C17_2 = N15_2-C22_2
 N15_3-C17_3 = N15_3-C22_3
 N15_4-C17_4 = N15_4-C22_4
 2.5 with sigma of 0.04
 C16_1-C18_1 = C17_1-C19_1 = C18_1-C20_1 = C19_1-C21_1 = C16_1-C23_1 = C22_1-
 C24_1 = C23_1-C25_1 = C24_1-C26_1 = C17_1-C22_1
 C16_2-C18_2 = C17_2-C19_2 = C18_2-C20_2 = C19_2-C21_2 = C16_2-C23_2 = C22_2-
 C24_2 = C23_2-C25_2 = C24_2-C26_2 = C17_2-C22_2
 C16_3-C18_3 = C17_3-C19_3 = C18_3-C20_3 = C19_3-C21_3 = C16_3-C23_3 = C22_3-
 C24_3 = C23_3-C25_3 = C24_3-C26_3 = C17_3-C22_3
 C16_4-C18_4 = C17_4-C19_4 = C18_4-C20_4 = C19_4-C21_4 = C16_4-C23_4 = C22_4-
 C24_4 = C23_4-C25_4 = C24_4-C26_4 = C17_4-C22_4
 2.55 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02
N15_1 \\sim C16_1 \\sim C17_1 \\sim C18_1 \\sim C19_1 \\sim C20_1 \\sim C21_1
\\sim C22_1 \\sim C23_1 \\sim C24_1 \\sim C25_1 \\sim C26_1 \\sim C16B_1 \\sim
C17B_1 \\sim C18B_1 \\sim C19B_1 \\sim C20B_1 \\sim C21B_1 \\sim C22B_1 \\sim
C23B_1 \\sim C24B_1 \\sim C25B_1 \\sim C26B_1 \\sim N15_2 \\sim C16_2 \\sim
C17_2 \\sim C18_2 \\sim C19_2 \\sim C20_2 \\sim C21_2 \\sim C22_2 \\sim C23_2
\\sim C24_2 \\sim C25_2 \\sim C26_2 \\sim C24B_2 \\sim C25B_2 \\sim C26B_2
\\sim N15_3 \\sim C16_3 \\sim C17_3 \\sim C18_3 \\sim C19_3 \\sim C20_3 \\sim
C21_3 \\sim C22_3 \\sim C23_3 \\sim C24_3 \\sim C25_3 \\sim C26_3 \\sim C19B_3
\\sim C20B_3 \\sim C21B_3 \\sim N15_4 \\sim C16_4 \\sim C17_4 \\sim C18_4 \\sim
C19_4 \\sim C20_4 \\sim C21_4 \\sim C22_4 \\sim C23_4 \\sim C24_4 \\sim C25_4
\\sim C26_4 \\sim C20B_4 \\sim C21B_4 \\sim C23B_4 \\sim C24B_4 \\sim C25B_4
\\sim C26B_4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C25_2 \\sim C26_2: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C20_4) = Uanis(C20B_4)
Uanis(C25_4) = Uanis(C25B_4)
Uanis(C26_4) = Uanis(C26B_4)
4. Rigid body (RIGU) restrains
 N15_1, C16_1, C17_1, C18_1, C19_1, C20_1, C21_1, C22_1, C23_1, C24_1, C25_1,
 C26_1, C16B_1, C17B_1, C18B_1, C19B_1, C20B_1, C21B_1, C22B_1, C23B_1, C24B_1,
 C25B_1, C26B_1
 N15_2, C16_2, C17_2, C18_2, C19_2, C20_2, C21_2, C22_2, C23_2, C24_2, C25_2,
 C26_2, C24B_2, C25B_2, C26B_2
 N15_3, C16_3, C17_3, C18_3, C19_3, C20_3, C21_3, C22_3, C23_3, C24_3, C25_3,
 C26_3, C19B_3, C20B_3, C21B_3
 N15_4, C16_4, C17_4, C18_4, C19_4, C20_4, C21_4, C22_4, C23_4, C24_4, C25_4,
 C26_4, C20B_4, C21B_4, C23B_4, C24B_4, C25B_4, C26B_4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N15_1, C16_1, C17_1, C18_1, C19_1, C20_1, C21_1, C22_1, C23_1, C24_1, C25_1,
 C26_1, C16B_1, C17B_1, C18B_1, C19B_1, C20B_1, C21B_1, C22B_1, C23B_1, C24B_1,
 C25B_1, C26B_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23_2, C24_2, C25_2, C26_2, C24B_2, C25B_2, C26B_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18_3, C19_3, C20_3, C21_3, C19B_3, C20B_3, C21B_3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19_4, C20_4, C21_4, C20B_4, C21B_4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22_4, C23_4, C24_4, C25_4, C26_4, C23B_4, C24B_4, C25B_4, C26B_4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{N15_1, C16B_1, C17B_1, C18B_1, C19B_1, C20B_1, C21B_1, C22B_1, C23B_1, C24B_1,
C25B_1, C26B_1} sigma for 1-2: 0.02, 1-3: 0.04
as
{N15_1, C16_1, C17_1, C18_1, C19_1, C20_1, C21_1, C22_1, C23_1, C24_1, C25_1,
C26_1}
{C23_2, C24B_2, C25B_2, C26B_2} sigma for 1-2: 0.02, 1-3: 0.04
as
{C23_2, C24_2, C25_2, C26_2}
{C18_3, C19B_3, C20B_3, C21B_3} sigma for 1-2: 0.02, 1-3: 0.04
as
{C18_3, C19_3, C20_3, C21_3}
{C19_4, C20B_4, C21B_4} sigma for 1-2: 0.02, 1-3: 0.04
as
{C19_4, C20_4, C21_4}
{C22_4, C23B_4, C24B_4, C25B_4, C26B_4} sigma for 1-2: 0.02, 1-3: 0.04
as
{C22_4, C23_4, C24_4, C25_4, C26_4}
6. Others
 Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25C)=Sof(H25D)=Sof(C26B)=
 Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=FVAR(1)
 Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=
 Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(2)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(2)
 Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(H18C)=
 Sof(H18D)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=
 Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22C)=Sof(H22D)=
 Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=
 Sof(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(3)
 Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=FVAR(3)
 Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(4)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(4)
 Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C20B)=Sof(H20C)=Sof(H20D)=Sof(C21B)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(5)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=FVAR(5)
7.a Ternary CH refined with riding coordinates:
 C16(H16), C16B(H16B), C16(H16), C16(H16), C16(H16)
7.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C17B(H17C,H17D),
 C18B(H18C,H18D), C19B(H19C,H19D), C20B(H20C,H20D), C22B(H22C,H22D), C23B(H23C,
 H23D), C24B(H24C,H24D), C25B(H25C,H25D), C17(H17A,H17B), C18(H18A,H18B),
 C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
  C25(H25A,H25B), C24B(H24C,H24D), C25B(H25C,H25D), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C20(H20A,H20B), C19B(H19C,H19D), C20B(H20C,H20D),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C17(H17A,H17B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C20B(H20C,H20D), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C23B(H23C,H23D),
 C24B(H24C,H24D), C25B(H25C,H25D)
7.c Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C26(H26A,H26B,
 H26C), C26B(H26D,H26E,H26F), C21(H21A,H21B,H21C), C21B(H21D,H21E,H21F),
 C21(H21A,H21B,H21C), C21B(H21D,H21E,H21F), C26(H26A,H26B,H26C), C26B(H26D,H26E,
 H26F)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C3(H3), C8(H8), C9(H9), C3(H3), C8(H8), C9(H9),
 C3(H3), C8(H8), C9(H9), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
7.e Idealised Me refined as rotating group:
 C21B(H21D,H21E,H21F), C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              24949
_shelx_hkl_checksum              20683
_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 1.752
_oxdiff_exptl_absorpt_empirical_full_min 0.750