Porous organic crystals crosslinked by free-radical reactions.
Samanta, Krishanu; Mi, Jiashan; Chen, Albert D.; Li, Fangzhou; Staples, Richard J.; Rossini, Aaron J.; Ke, Chenfeng; Chemical communications (Cambridge, England) 60 (2024) 7311–7314; doi:10.1039/d4cc02454k

data_7133246
_publ_section_title
;
 Porous organic crystals crosslinked by free-radical reactions.
;
_journal_issue                   57
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7311
_journal_page_last               7314
_journal_paper_doi               10.1039/d4cc02454k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C108 H103 N6 O18, 3[C6H14]'
_chemical_formula_sum            'C107 H98.1 N6 O18'
_chemical_formula_weight         1756.00
_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_block_doi                 10.5517/ccdc.csd.cc2jsk2z
_audit_creation_date             2023-08-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-04-10 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                60.357(3)
_cell_angle_beta                 83.564(3)
_cell_angle_gamma                74.230(4)
_cell_formula_units_Z            2
_cell_length_a                   14.4122(8)
_cell_length_b                   21.9201(8)
_cell_length_c                   22.0159(5)
_cell_measurement_reflns_used    5865
_cell_measurement_temperature    99.98(11)
_cell_measurement_theta_max      52.6740
_cell_measurement_theta_min      2.3920
_cell_volume                     5815.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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   -106.00 -28.00   0.50   10.00    --  -48.74 -72.00 147.00  156
  2  \w    -68.00  12.00   0.50   10.00    --  -48.74  72.00 -83.00  160
  3  \w    -20.00  70.00   0.50   10.00    --   48.74 -72.00 147.00  180
  4  \w     28.00 112.00   0.50   10.00    --   48.74  72.00 -83.00  168
  5  \w    -91.00 -19.00   0.50   40.00    --  -86.25  72.00 -83.00  144
  6  \w   -150.00 -65.00   0.50   40.00    --  -86.25 -72.00 147.00  170
  7  \w     87.00 164.00   0.50   40.00    --  107.75  72.00 -83.00  154
  8  \w     35.00  91.00   0.50   40.00    --  107.75 -72.00 147.00  112
  9  \w    -26.00  27.00   0.50   10.00    --   48.74 -19.00 150.00  106
 10  \w    -51.00 -14.00   0.50   40.00    --  -86.25  45.00 120.00   74
 11  \w    -71.00 -13.00   0.50   40.00    --  -86.25  61.00  90.00  116
 12  \w     94.00 178.00   0.50   40.00    --  107.75  15.00-150.00  168
 13  \w     36.00 106.00   0.50   40.00    --  107.75 -94.00 120.00  140
 14  \w     46.00 112.00   0.50   40.00    --  107.75-125.00 -60.00  132
 15  \w     95.00 178.00   0.50   40.00    --  107.75  30.00-120.00  166
 16  \w    116.00 178.00   0.50   40.00    --  107.75  45.00 150.00  124
 17  \w     35.00  70.00   0.50   40.00    --  107.75 -61.00 -30.00   70
 18  \w     39.00 112.00   0.50   40.00    --  107.75-125.00   0.00  146
 19  \w     40.00 112.00   0.50   40.00    --  107.75-125.00  90.00  144
 20  \w     95.00 178.00   0.50   40.00    --  107.75 125.00  90.00  166
 21  \w     36.00 104.00   0.50   40.00    --  107.75 -94.00  90.00  136
 22  \w     38.00 112.00   0.50   40.00    --  107.75-125.00  60.00  148
;
_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      -0.0306261000
_diffrn_orient_matrix_UB_12      -0.0687476000
_diffrn_orient_matrix_UB_13      0.0552516000
_diffrn_orient_matrix_UB_21      0.1015076000
_diffrn_orient_matrix_UB_22      -0.0322572000
_diffrn_orient_matrix_UB_23      0.0345258000
_diffrn_orient_matrix_UB_31      -0.0332326000
_diffrn_orient_matrix_UB_32      0.0347852000
_diffrn_orient_matrix_UB_33      0.0473499000
_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  0.0752
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            50666
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        58.934
_diffrn_reflns_theta_max         58.934
_diffrn_reflns_theta_min         4.780
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.003
_exptl_crystal_description       needle
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1384
_refine_ls_number_reflns         16236
_refine_ls_number_restraints     1089
_refine_ls_restrained_S_all      1.320
_refine_ls_R_factor_all          0.1991
_refine_ls_R_factor_gt           0.1490
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3708
_refine_ls_wR_factor_ref         0.4088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8388
_reflns_number_total             16236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02454k2.cif
_cod_data_source_block           ck1222b_1
_cod_depositor_comments
'Adding full bibliography for 7133244--7133247.cif.'
_cod_original_formula_sum        'C107 H98.10 N6 O18'
_cod_database_code               7133246
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C56H53N3O9
_chemical_oxdiff_usercomment     S1-BTAallyl-Isoprene
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.946
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C77B-C76B = C76B-C75 = C77B_$3-C85 = C84-C85 = C88-C85 = C86-C85 = C89B-C90B =
  C87-C89B = C87-C86 = C86-C105 = C1B-C105 = C88-C85 = C1B-C105 = C86-C105
 1.54 with sigma of 0.02
 C84-C88
 2.6 with sigma of 0.02
 C74-C73
 1.3 with sigma of 0.02
 C73-C72
 1.5 with sigma of 0.02
 C104-C103 = C1B-C1D
 1.5 with sigma of 0.02
 N6A-C103 = N6B-C1D = N6A-C102 = N6B-C102
 1.45 with sigma of 0.02
 C104-N6A
 2.4 with sigma of 0.02
 C104-C1
 1.35 with sigma of 0.02
 C103-C1
 2.5 with sigma of 0.02
 C87-C90B
 2.6 with sigma of 0.02
 C1D-C105
 2.6 with sigma of 0.02
 C47-C101
 2.6 with sigma of 0.02
 C84-C86
 2.6 with sigma of 0.02
 C1-C80B_$2
 1.54 with sigma of 0.02
 C1_$1-C80B
 1.54 with sigma of 0.02
 C79B-C1_$1
 2.66 with sigma of 0.02
 C78B-C80B
 2.66 with sigma of 0.02
 C1-C1D
 2.66 with sigma of 0.02
 C75-C77B
 2.66 with sigma of 0.02
 C105-C103
 2.66 with sigma of 0.02
 C105-C85
 2.66 with sigma of 0.02
 C1B-C86
 2.6 with sigma of 0.02
 C83-C82
 1.54 with sigma of 0.02
 C103-C1B
 1.54 with sigma of 0.02
 C86-C85
 1.54 with sigma of 0.02
 N2-C78A = N2-C78B
 1.47 with sigma of 0.02
 C105-C87
 2.6 with sigma of 0.02
 C85-C87
 2.6 with sigma of 0.02
 C103-C102
 2.6 with sigma of 0.02
 C103-C1G
 2.6 with sigma of 0.02
 O19A-N6A
 2.3 with sigma of 0.02
 C57-N6A
 2.5 with sigma of 0.02
 C77-C92
 2.5 with sigma of 0.02
 C75-C77A
 2.6 with sigma of 0.02
 C80B_$2-C104
 2.6 with sigma of 0.02
 C79B_$2-C1
 2.6 with sigma of 0.02
 C77A_$3-C85 = C77B_$3-C85
 1.54 with sigma of 0.02
 C84-C77A_$3
 2.6 with sigma of 0.02
 C84-C83
 1.54 with sigma of 0.02
 C90A-C91A
 1.5 with sigma of 0.02
 H4A-H84B
 1.8 with sigma of 0.02
 H87A-H16
 1.8 with sigma of 0.02
 H84B-H4A
 2 with sigma of 0.02
 H16-H87A
 2 with sigma of 0.02
 C85-C83
 2.5 with sigma of 0.02
 C86-C88 \\sim C88-C77B_$3
 with sigma of 0.02
 C87-C89B \\sim C87-C86 \\sim C86-C85 \\sim C88-C85 \\sim C84-C85 \\sim
C86-C105 \\sim C1B-C105
 with sigma of 0.02
 C76A-C77A \\sim C76B-C77B
 with sigma of 0.02
 C86-C88 \\sim C88-C84
 with sigma of 0.02
 C90B-C91B \\sim C87-C86 \\sim C86-C85 \\sim C84-C85
 with sigma of 0.02
 C86-C105 \\sim C1B-C105
 with sigma of 0.02
 C89B-C90B \\sim C87-C89B \\sim C87-C86
 with sigma of 0.02
 C1E-C47 \\sim C100-C47
 with sigma of 0.02
 C100-C1F \\sim C1E-C101
 with sigma of 0.02
 C96A-C97 \\sim C96B-C97
 with sigma of 0.02
 C93A-C43 \\sim C43-C93B
 with sigma of 0.02
 C79A-C78A \\sim C79B-C78B
 with sigma of 0.02
 N2-C78A \\sim N2-C78B
 with sigma of 0.02
 N6B-C1D \\sim N6A-C103
 with sigma of 0.02
 N6B-C102 \\sim N6A-C102
 with sigma of 0.02
 C104-C103 \\sim C1D-C1B
 with sigma of 0.02
 C4B-C77 \\sim C4A-C1A
 with sigma of 0.02
 C104-C1D \\sim C104-C1 \\sim C1_$1-C80B \\sim C79B-C80B \\sim C79B-C78B
 with sigma of 0.02
 C102-C57 \\sim C1G-C57
 with sigma of 0.02
 N6A-C1G \\sim N6B-C102
 with sigma of 0.02
 O18A-C102 \\sim O19A-C1G
 with sigma of 0.02
 C80A-C79A \\sim C80A-C82
 with sigma of 0.02
 C4B-N4 \\sim N4-C4A
 with sigma of 0.02
 O19A-C1G \\sim O18A-C102
 with sigma of 0.02
 N6B-C1G \\sim N6A-C102
 with sigma of 0.02
 C1G-C57 \\sim C102-C57
 with sigma of 0.02
 C4B-C92 \\sim C4A-C92
 with sigma of 0.02
 C4A-C1A \\sim C4B-C77
 with sigma of 0.02
 C83-C82 \\sim C84-C83 \\sim C84-C85 \\sim C86-C85 \\sim C87-C86
 with sigma of 0.02
 C99-C98 \\sim C90A-C98 \\sim C89A-C90A \\sim C89A-C99
 with sigma of 0.02
3. Restrained planarity
 C57, C102, O18A, N6A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N1 \\sim C76B \\sim C77B \\sim C75 \\sim C71 \\sim O5 \\sim C76A \\sim C77A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C83 \\sim C84 \\sim C85 \\sim C88 \\sim C86: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C88 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C89B: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C87 \\sim C85 \\sim C84 \\sim C86 \\sim C90B: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C89A \\sim C92A \\sim C91A \\sim C90A \\sim C96A \\sim C95A \\sim C94A \\sim
C93A \\sim C92B \\sim C93B \\sim C96B \\sim C94B \\sim C91B \\sim C90B \\sim
C95B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
C101 \\sim C100: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C101 \\sim C100 \\sim C1E \\sim C1F: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C72 \\sim C73: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C79A \\sim C80A \\sim C78A \\sim C78B \\sim C79B \\sim C80B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C103 \\sim N6B \\sim C1B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
N6A \\sim C103 \\sim C104 \\sim N6B \\sim C1B \\sim C1D: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C104: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
C105 \\sim C1B \\sim C1D: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C72 \\sim C73 \\sim C74: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C1 \\sim C103 \\sim C104 \\sim C1B \\sim C1D: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C92 \\sim C1A \\sim C4A \\sim C77 \\sim C4B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C78B \\sim C79B \\sim C80B \\sim C1 \\sim C104 \\sim C1D: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C83 \\sim C82: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C102 \\sim C1G: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O18A \\sim O19A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
N6B \\sim N6A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C1G \\sim C102: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C78A) \\sim Ueq, Uanis(C78B) \\sim Ueq, Uanis(C79B) \\sim Ueq,
Uanis(C80B) \\sim Ueq, Uanis(C79A) \\sim Ueq, Uanis(C80A) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C88) \\sim Ueq,
Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C89B)
\\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C101) \\sim Ueq,
Uanis(C1F) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C4B) \\sim Ueq,
Uanis(C92) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C1D)
\\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 N1, C76B, C77B, C75, C71, O5, C76A, C77A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C84, C85, C88, C86, C87
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C87, C85, C84, C86, C90B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C101, C100, C72, C73
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C101, C100, C1E, C1F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C97, C89A, C92A, C91A, C90A, C96A, C95A, C94A, C93A, C92B, C93B, C96B, C94B,
 C91B, C90B, C95B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C79A, C80A, C78A, C78B, C79B, C80B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C103, N6B, C1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N6A, C103, C104, N6B, C1B, C1D
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C105, C1B, C1D
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C72, C73, C74
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C103, C104, C1B, C1D
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C92, C1A, C4A, C77, C4B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, C104, C79B, C80B, C1D, C78B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C77B, C76B, C75
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C83
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(H98)=Sof(C89B)=Sof(H89A)=Sof(H89B)=Sof(C92B)=Sof(H92F)=Sof(C93B)=
 Sof(C96B)=Sof(C94B)=Sof(H94B)=Sof(C91B)=Sof(C90B)=Sof(H90B)=Sof(H90C)=
 Sof(C95B)=Sof(H95B)=1-FVAR(1)
 Sof(C89A)=Sof(H89C)=Sof(H89D)=Sof(C92A)=Sof(H92E)=Sof(C91A)=Sof(C96A)=
 Sof(C95A)=Sof(H95A)=Sof(C94A)=Sof(H94A)=Sof(C93A)=Sof(C90A)=Sof(H90A)=FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C104)=Sof(H10E)=Sof(H10F)=Sof(N6B)=Sof(H6B)=
 Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(C1G)=Sof(O19A)=1-FVAR(2)
 Sof(O18A)=Sof(C105)=Sof(H10A)=Sof(H10B)=Sof(C102)=Sof(N6A)=Sof(H6A)=Sof(C103)=
 Sof(H10C)=Sof(H10D)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=FVAR(2)
 Sof(H2B)=Sof(C78B)=Sof(H78C)=Sof(H78D)=Sof(C79B)=Sof(H79C)=Sof(H79D)=
 Sof(C80B)=Sof(H80C)=Sof(H80D)=1-FVAR(3)
 Sof(H2A)=Sof(C79A)=Sof(H79A)=Sof(H79B)=Sof(C80A)=Sof(H80A)=Sof(H80B)=
 Sof(C78A)=Sof(H78A)=Sof(H78B)=FVAR(3)
 Sof(H92C)=Sof(H92D)=Sof(C77)=Sof(H77C)=Sof(H77D)=Sof(C4B)=Sof(H4B)=1-FVAR(4)
 Sof(H92A)=Sof(H92B)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C4A)=Sof(H4AA)=FVAR(4)
 Sof(C101)=Sof(H10G)=Sof(H10H)=Sof(C1E)=Sof(H1E)=1-FVAR(5)
 Sof(C100)=Sof(H100)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=FVAR(5)
 Sof(C76B)=Sof(H76A)=Sof(H76B)=Sof(C77B)=Sof(H77A)=Sof(H77B)=Sof(H75C)=
 Sof(H75D)=1-FVAR(6)
 Sof(H75A)=Sof(H75B)=Sof(C76A)=Sof(H76C)=Sof(H76D)=Sof(C77A)=Sof(H77E)=
 Sof(H77F)=FVAR(6)
7.a Ternary CH refined with riding coordinates:
 C86(H86), C82(H82), C90A(H90A)
7.b Secondary CH2 refined with riding coordinates:
 C99(H99A,H99B), C87(H87A,H87B), C105(H10A,H10B), C89B(H89A,H89B), C76B(H76A,
 H76B), C77B(H77A,H77B), C84(H84A,H84B), C1(H1A,H1B), C60(H60A,H60B), C75(H75C,
 H75D), C75(H75A,H75B), C89A(H89C,H89D), C92(H92A,H92B), C92(H92C,H92D),
 C103(H10C,H10D), C79A(H79A,H79B), C104(H10E,H10F), C80A(H80A,H80B), C78A(H78A,
 H78B), C1B(H1BA,H1BB), C78B(H78C,H78D), C79B(H79C,H79D), C72(H72A,H72B),
 C90B(H90B,H90C), C80B(H80C,H80D), C1D(H1DA,H1DB), C76A(H76C,H76D), C77A(H77E,
 H77F), C83(H83A,H83B)
7.c Me refined with riding coordinates:
 C88(H88A,H88B,H88C)
7.d Aromatic/amide H refined with riding coordinates:
 N5(H5), N3(H3), N1(H1), N2(H2A), N2(H2B), N4(H4), C98(H98), C46(H46),
 C40(H40), C61(H61), C9(H9), C50(H50), C34(H34), C35(H35), C6(H6), C69(H69),
 C49(H49), C52(H52), C42(H42), C5(H5A), C67(H67), C19(H19), C54(H54), C32(H32),
 C15(H15A), C13(H13), C28(H28), C37(H37), C4(H4A), C11(H11A), C16(H16),
 C22(H22), C65(H65), C56(H56), C25(H25), C44(H44), N6A(H6A), C92A(H92E),
 C95A(H95A), C94A(H94A), C4A(H4AA), N6B(H6B), C92B(H92F), C94B(H94B),
 C95B(H95B), C73(H73), C100(H100), C4B(H4B), C1E(H1E), C26(H26)
7.e Fitted hexagon refined as free rotating group:
 C92A(C91A,C96A,C95A,C94A,C93A)
7.f X=CH2 refined with riding coordinates:
 C38(H38A,H38B), C62(H62A,H62B), C29(H29A,H29B), C1A(H1AA,H1AB), C101(H10G,
 H10H), C77(H77C,H77D), C74(H74A,H74B), C1F(H1FA,H1FB)
7.g Idealised tetrahedral OH refined as rotating group:
 O8(H8), O15(H15), O11(H11)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 268 electrons were 
found in a volume of 1636\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[C6H12] per Asymmetric Unit 
which account for 288 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6739
_shelx_hkl_checksum              1694
_shelx_fab_checksum              62780
_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 1.386
_oxdiff_exptl_absorpt_empirical_full_min 0.613