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_7133244
_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         'C106 H92.03 N6 O18'
_chemical_formula_sum            'C106 H92.03 N6 O18'
_chemical_formula_weight         1737.88
_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.cc2jsk30
_audit_creation_date             2023-11-14
_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                60.305(3)
_cell_angle_beta                 83.030(3)
_cell_angle_gamma                74.276(4)
_cell_formula_units_Z            2
_cell_length_a                   14.4561(7)
_cell_length_b                   21.9459(8)
_cell_length_c                   22.0092(6)
_cell_measurement_reflns_used    5500
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      52.7870
_cell_measurement_theta_min      3.4650
_cell_volume                     5837.8(4)
_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      100.0(2)
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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   -123.00 -35.00   0.50   15.00    --  -47.40 -19.00 -30.00  176
  2  \w    -69.00  13.00   0.50   15.00    --  -47.40  77.00 -60.00  164
  3  \w    -51.00  10.00   0.50   15.00    --  -47.40  77.00-180.00  122
  4  \w    -31.00  21.00   0.50   15.00    --  -47.40  37.00-120.00  104
  5  \w    -62.00  17.00   0.50   15.00    --  -47.40  57.00 150.00  158
  6  \w    -47.00  16.00   0.50   15.00    --  -47.40  37.00 120.00  126
  7  \w     -7.00  70.00   0.50   15.00    --   47.40 -77.00 -30.00  154
  8  \w   -155.00-119.00   0.50   45.00    --  -91.75 -45.00 -90.00   72
  9  \w    -46.00 -20.00   0.50   45.00    --  -91.75  45.00  60.00   52
 10  \w    -47.00 -22.00   0.50   45.00    --  -91.75  45.00 -90.00   50
 11  \w    109.00 145.00   0.50   45.00    --  113.25  30.00  30.00   72
 12  \w     42.00  69.00   0.50   45.00    --  113.25 -61.00 120.00   54
 13  \w    133.00 173.00   0.50   45.00    --  113.25  77.00 120.00   80
 14  \w     42.00  67.00   0.50   45.00    --  113.25 -61.00-120.00   50
 15  \w     47.00  73.00   0.50   45.00    --  113.25 -94.00-120.00   52
 16  \w    107.00 177.00   0.50   45.00    --  113.25  15.00 -90.00  140
 17  \w     42.00  75.00   0.50   45.00    --  113.25 -85.00-164.52   66
 18  \w    145.00 178.00   0.50   45.00    --  113.25  45.00  90.00   66
 19  \w    101.00 177.00   0.50   45.00    --  113.25  15.00-150.00  152
 20  \w     73.00 104.00   0.50   45.00    --  113.25 -94.00 -60.00   62
 21  \w     57.00  85.00   0.50   45.00    --  113.25-125.00   0.00   56
 22  \w     42.00  67.00   0.50   45.00    --  113.25 -61.00  30.00   50
 23  \w     76.00 103.00   0.50   45.00    --  113.25 -94.00-120.00   54
 24  \w    108.00 144.00   0.50   45.00    --  113.25  15.00-180.00   72
 25  \w     43.00  78.00   0.50   45.00    --  113.25 -77.00 120.00   70
 26  \w     45.00  88.00   0.50   45.00    --  113.25-125.00 -30.00   86
 27  \w     49.00 100.00   0.50   45.00    --  113.25 -94.00  30.00  102
 28  \w     43.00 104.00   0.50   45.00    --  113.25 -94.00 120.00  122
 29  \w     66.00  93.00   0.50   45.00    --  113.25 -77.00-150.00   54
 30  \w    104.00 177.00   0.50   45.00    --  113.25  30.00  60.00  146
 31  \w     77.00 104.00   0.50   45.00    --  113.25 -94.00   0.00   54
 32  \w    116.00 142.00   0.50   45.00    --  113.25  45.00  90.00   52
 33  \w     79.00 104.00   0.50   45.00    --  113.25 -94.00-180.00   50
 34  \w     46.00  86.00   0.50   45.00    --  113.25 -94.00  60.00   80
 35  \w    101.00 173.00   0.50   45.00    --  113.25  45.00   0.00  144
 36  \w     42.00  68.00   0.50   45.00    --  113.25 -94.00-180.00   52
 37  \w     78.00 104.00   0.50   45.00    --  113.25 -94.00 150.00   52
 38  \w    101.00 168.00   0.50   45.00    --  113.25  30.00 -30.00  134
 39  \w     42.00  67.00   0.50   45.00    --  113.25 -61.00 150.00   50
 40  \w     47.00 104.00   0.50   45.00    --  113.25 -94.00 -90.00  114
 41  \w     44.00  69.00   0.50   45.00    --  113.25 -61.00-180.00   50
 42  \w    109.00 144.00   0.50   45.00    --  113.25  61.00-150.00   70
 43  \w    150.00 178.00   0.50   45.00    --  113.25  61.00-150.00   56
 44  \w     77.00 104.00   0.50   45.00    --  113.25 -94.00-150.00   54
 45  \w     75.00 104.00   0.50   45.00    --  113.25 -94.00  90.00   58
 46  \w     43.00  69.00   0.50   45.00    --  113.25 -61.00  60.00   52
 47  \w    102.00 151.00   0.50   45.00    --  113.25  15.00 150.00   98
 48  \w     42.00  67.00   0.50   45.00    --  113.25 -77.00   0.00   50
 49  \w     79.00 106.00   0.50   45.00    --  113.25 -85.00-164.52   54
 50  \w     43.00 104.00   0.50   45.00    --  113.25 -96.00 -17.80  122
 51  \w     79.00 104.00   0.50   45.00    --  113.25-125.00-150.00   50
 52  \w     47.00 105.00   0.50   45.00    --  113.25-105.00  89.49  116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0503847000
_diffrn_orient_matrix_UB_12      -0.0023831000
_diffrn_orient_matrix_UB_13      0.0666994000
_diffrn_orient_matrix_UB_21      -0.0697261000
_diffrn_orient_matrix_UB_22      -0.0393243000
_diffrn_orient_matrix_UB_23      -0.0052676000
_diffrn_orient_matrix_UB_31      0.0696968000
_diffrn_orient_matrix_UB_32      -0.0734412000
_diffrn_orient_matrix_UB_33      0.0449258000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66606
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        58.934
_diffrn_reflns_theta_max         58.934
_diffrn_reflns_theta_min         2.311
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77011
_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    0.989
_exptl_crystal_description       needle
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.326
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1381
_refine_ls_number_reflns         16687
_refine_ls_number_restraints     875
_refine_ls_restrained_S_all      1.334
_refine_ls_R_factor_all          0.1938
_refine_ls_R_factor_gt           0.1498
_refine_ls_shift/su_max          0.000
_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          0.3900
_refine_ls_wR_factor_ref         0.4230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8872
_reflns_number_total             16687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02454k2.cif
_cod_data_source_block           s1-btaallyl-butadiene
_cod_depositor_comments
'Adding full bibliography for 7133244--7133247.cif.'
_cod_database_code               7133244
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C35H51N3O9
_chemical_oxdiff_usercomment     S1-BTAallyl-Buta
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.947
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C0-C6
 2.6 with sigma of 0.02
 C2-C1
 2.6 with sigma of 0.02
 C033-C4
 2.6 with sigma of 0.02
 C6-C033
 1.54 with sigma of 0.02
 C2-C02V
 1.54 with sigma of 0.02
 C03A-C033 = C44-C03A = C44-C20 = C24-C20 = C24-C17 = C37-C17
 1.54 with sigma of 0.02
 C03A-C033
 1.54 with sigma of 0.02
 C37-C03C
 1.54 with sigma of 0.02
 C033-C44
 2.6 with sigma of 0.02
 C70B-C12
 1.5 with sigma of 0.02
 C44-C24
 2.6 with sigma of 0.02
 C24-C37
 2.6 with sigma of 0.02
 C17-C03C
 2.6 with sigma of 0.02
 C12-C11 = C15-C13
 1.54 with sigma of 0.02
 C70A-C15 = C70B-C12
 1.5 with sigma of 0.02
 C70B-C11
 2.6 with sigma of 0.02
 C13-C70A
 2.6 with sigma of 0.02
 C21-N00O
 2.6 with sigma of 0.02
 C41-C22
 2.6 with sigma of 0.02
 C28-C26 = C83-C77
 1.39 with sigma of 0.02
 C26-C1F = C83-C27
 1.5 with sigma of 0.02
 C28-C20
 1.5 with sigma of 0.02
 C28-C1F
 2.5 with sigma of 0.02
 C27-C77
 2.5 with sigma of 0.02
 C27-C02L
 2.4 with sigma of 0.02
 N01B-C83
 2.4 with sigma of 0.02
 C77-C1_$1
 1.5 with sigma of 0.02
 N00O-C7A
 2.45 with sigma of 0.02
 C70B-C12 \\sim C7B-C21
 with sigma of 0.02
 C03C-C8B \\sim C16-C02R
 with sigma of 0.02
 N00M-C0 \\sim N00M-C2
 with sigma of 0.02
 C5-C02A \\sim C10-C02A
 with sigma of 0.02
 C8-C01C \\sim C9-C01C
 with sigma of 0.02
 C035-C031 \\sim C3-C14
 with sigma of 0.02
 C3-C035 \\sim C14-C031
 with sigma of 0.02
 C70B-C12 \\sim C70A-C15
 with sigma of 0.02
 C15-C13 \\sim C12-C11
 with sigma of 0.02
 N00B-C13 \\sim N00B-C11
 with sigma of 0.02
 C7B-C21 \\sim C7A-C41
 with sigma of 0.02
 N00O-C22 \\sim N00O-C1B
 with sigma of 0.02
 C21-C1B \\sim C7A-C22
 with sigma of 0.02
 C7-C23 \\sim C1C-C1D
 with sigma of 0.02
 N00K-C7 \\sim N00K-C1C
 with sigma of 0.02
 C25-C23 \\sim C1E-C1D
 with sigma of 0.02
 C28-C26 \\sim C83-C77
 with sigma of 0.02
 C1F-C26 \\sim C83-C27
 with sigma of 0.02
 N01B-C1F \\sim N01B-C27
 with sigma of 0.02
 C28-C20 \\sim C28-C26 \\sim C26-C1F
 with sigma of 0.02
 C3-C035 \\sim C14-C031 \\sim C035-C031 \\sim C3-C14
 with sigma of 0.02
 C031-C021 \\sim C15A-C14
 with sigma of 0.02
 C1A-C19 \\sim C18-C16
 with sigma of 0.02
 C19-C02R \\sim C16-C02R
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C02V \\sim C0 \\sim C1 \\sim C4 \\sim C6 \\sim C2: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C03C \\sim C37 \\sim C17 \\sim C24 \\sim C20 \\sim C44 \\sim C03A: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C13B \\sim C15B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C13B \\sim C15B \\sim C5 \\sim C8B \\sim C5B \\sim C9 \\sim C8 \\sim C13A \\sim
C15A \\sim C10 \\sim C8A \\sim C5A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C44 \\sim C20 \\sim C03A \\sim C24 \\sim C17 \\sim C37 \\sim C03C: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C11 \\sim C12 \\sim C70B \\sim C13 \\sim C15 \\sim C70A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08 within 2A
C16 \\sim C18 \\sim C19 \\sim C1A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C22 \\sim C21 \\sim C7B \\sim C1B \\sim C7A \\sim C41: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O005 \\sim C7 \\sim C23 \\sim C25 \\sim C1C \\sim C1D \\sim C1E: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C14 \\sim C3 \\sim C035 \\sim C031: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C6 \\sim C4 \\sim C033: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C03A) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C03C) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C28) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C1F)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
4. Rigid body (RIGU) restrains
 C02C, C02Y, C51, C27, C83, C7, C23, C25, C22, C21, C7B, C11, C12, C70B, C02V,
 C0
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, C6, C0, C2, C02V, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C03A, C37, C44, C03A, C20, C24, C17, C37, C03C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C13B, C15B, C5, C8B, C5B, C8, C13A, C15A, C10, C8A, C5A, C14, C03C, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, C70B, C13, C15, C70A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C18, C19, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22, C21, C7B, C1B, C7A, C41
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C7, C23, C25, C1C, C1D, C1E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H00D)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=1-FVAR(1)
 Sof(H00M)=Sof(C02V)=Sof(H02V)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=FVAR(1)
 Sof(C03C)=Sof(H03I)=Sof(H03J)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C13B)=
 Sof(H13B)=Sof(C15B)=Sof(H15B)=Sof(C5)=Sof(C8B)=Sof(C5B)=Sof(H5B)=Sof(C9)=1-
 FVAR(2)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C14)=Sof(H14)=Sof(C8)=Sof(C13A)=Sof(H13A)=
 Sof(C15A)=Sof(C10)=Sof(C8A)=Sof(H8A)=Sof(C5A)=Sof(H5A)=FVAR(2)
 Sof(H00A)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C12)=
 Sof(H12)=Sof(C70B)=Sof(H70A)=Sof(H70B)=Sof(C7A)=Sof(H7AA)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=1-FVAR(3)
 Sof(H00B)=Sof(H00O)=Sof(C21)=Sof(H21)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C13)=
 Sof(H13C)=Sof(H13D)=Sof(C15)=Sof(H15)=Sof(C70A)=Sof(H70C)=Sof(H70D)=Sof(C1B)=
 Sof(H1BA)=Sof(H1BB)=FVAR(3)
 Sof(C16)=Sof(H16)=Sof(C18)=Sof(H18A)=Sof(H18B)=1-FVAR(4)
 Sof(C19)=Sof(H19)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=FVAR(4)
 Sof(H00K)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C23)=Sof(H23)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=1-FVAR(5)
 Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1D)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=
 FVAR(5)
 Sof(H01C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C83)=Sof(H83)=Sof(C77)=Sof(H77A)=
 Sof(H77B)=1-FVAR(6)
 Sof(H01B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C1F)=
 Sof(H1FA)=Sof(H1FB)=FVAR(6)
6.a Ternary CH refined with riding coordinates:
 C031(H031), C20(H20), C14(H14)
6.b Secondary CH2 refined with riding coordinates:
 C02C(H02A,H02C), C11(H11A,H11B), C22(H22A,H22B), C7(H7A,H7B), C0(H0A,H0B),
 C035(H03E,H03F), C27(H27A,H27B), C03A(H03G,H03H), C03C(H03I,H03J), C4(H4A,H4B),
  C6(H6A,H6B), C2(H2A,H2B), C37(H37A,H37B), C17(H17A,H17B), C24(H24A,H24B),
 C44(H44A,H44B), C3(H3A,H3B), C13(H13C,H13D), C1B(H1BA,H1BB), C1C(H1CA,H1CB),
 C26(H26A,H26B), C28(H28A,H28B), C1F(H1FA,H1FB)
6.c Aromatic/amide H refined with riding coordinates:
 N00B(H00A), N00B(H00B), N00K(H00K), N00M(H00D), N00M(H00M), N00O(H00O),
 C00Q(H00Q), C00U(H00U), C00W(H00W), C010(H010), C015(H015), C016(H016),
 C017(H017), C018(H018), C01A(H01A), N01B(H01C), N01B(H01B), C01G(H01G),
 C01H(H01H), C01I(H01I), C01M(H01M), C01N(H01N), C01O(H01O), C01T(H01T),
 C01V(H01V), C023(H023), C025(H025), C026(H026), C028(H028), C029(H029),
 C02B(H02B), C02D(H02D), C02E(H02E), C02G(H02G), C02P(H02P), C02T(H02T),
 C02V(H02V), C21(H21), C02X(H02X), C02Y(H02Y), C12(H12), C16(H16), C23(H23),
 C83(H83), C13B(H13B), C15B(H15B), C5B(H5B), C13A(H13A), C8A(H8A), C5A(H5A),
 C15(H15), C19(H19), C7A(H7AA), C1D(H1D)
6.d Fitted hexagon refined as free rotating group:
 C13B(C15B,C5,C8B,C5B,C9), C8(C13A,C15A,C10,C8A,C5A)
6.e X=CH2 refined with riding coordinates:
 C032(H03A,H03B), C034(H03C,H03D), C18(H18A,H18B), C70B(H70A,H70B), C7B(H7BA,
 H7BB), C51(H51A,H51B), C25(H25A,H25B), C1(H1A,H1B), C70A(H70C,H70D), C1A(H1AA,
 H1AB), C41(H41A,H41B), C1E(H1EA,H1EB), C77(H77A,H77B)
6.f Idealised tetrahedral OH refined as rotating group:
 O00C(H00C), O00E(H00E), O00H(H00H)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 417 electrons were 
found in a volume of 1603\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[C6H14] per Asymmetric Unit 
which account for 400 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              18321
_shelx_hkl_checksum              87714
_shelx_fab_checksum              75988
_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 1.570
_oxdiff_exptl_absorpt_empirical_full_min 0.370