Programmable synthesis of organic cages with reduced symmetry.
Andrews, Keith G.; Horton, Peter N.; Coles, Simon J.; Chemical science 15 (2024) 6536–6543; doi:10.1039/d4sc00889h

data_1571314
_publ_section_title
;
 Programmable synthesis of organic cages with reduced symmetry.
;
_journal_issue                   17
_journal_name_full               'Chemical science'
_journal_page_first              6536
_journal_page_last               6543
_journal_paper_doi               10.1039/d4sc00889h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '1(C126 H112 N6 O10), 4[C4H8O], 10[CH4O]'
_chemical_formula_sum            'C152 H184 N6 O24'
_chemical_formula_weight         2479.04
_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             2022-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-27 deposited with the CCDC.	2024-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                73.2304(5)
_cell_angle_beta                 71.3145(5)
_cell_angle_gamma                72.7778(5)
_cell_formula_units_Z            4
_cell_length_a                   21.54594(12)
_cell_length_b                   25.73674(14)
_cell_length_c                   29.44669(16)
_cell_measurement_reflns_used    134041
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.0830
_cell_measurement_theta_min      2.3860
_cell_volume                     14432.23(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_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(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.994
_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    -89.00  89.00   0.50    2.00    --    0.00   0.00-180.00  356
  2  \w    -84.00  94.00   0.50    2.00    --    5.00  49.00 -60.00  356
  3  \w   -179.00  -1.00   0.50   10.00    --  -90.00  56.00-178.38  356
  4  \w   -179.00  -1.00   0.50   10.00    --  -90.00  49.00 -47.77  356
  5  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00 -69.67  356
  6  \w   -179.00  -1.00   0.50   10.00    --  -90.00  30.00 150.00  356
  7  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00   6.14  356
  8  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00-133.17  356
  9  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00 129.47  356
 10  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00  39.81  356
 11  \w   -179.00  -1.00   0.50   10.00    --  -90.00  30.00 -90.00  356
 12  \w   -179.00  -1.00   0.50   10.00    --  -90.00  56.00-178.38  356
 13  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00 174.00  356
 14  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00 174.00  356
 15  \w   -179.00  -1.00   0.50   10.00    --  -90.00  39.00-150.00  356
 16  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00-171.04  356
 17  \w   -179.00  -1.00   0.50   10.00    --  -90.00  57.00  81.38  356
 18  \w    -89.00  89.00   0.50    2.00    --    0.00  30.00 150.00  356
 19  \w    -89.00  89.00   0.50    2.00    --    0.00  59.00   0.00  356
 20  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00  61.60  356
 21  \w   -179.00-154.00   0.50   10.00    --  -90.00  59.00 -13.74   50
 22  \w   -179.00  -1.00   0.50   10.00    --  -90.00  58.00 -99.46  356
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF diffractometer with HF Varimax confocal mirrors, an UG2 goniometer and HyPix 6000HE detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0167986000
_diffrn_orient_matrix_UB_12      -0.0128549000
_diffrn_orient_matrix_UB_13      0.0564697000
_diffrn_orient_matrix_UB_21      -0.0490010000
_diffrn_orient_matrix_UB_22      -0.0345394000
_diffrn_orient_matrix_UB_23      0.0026678000
_diffrn_orient_matrix_UB_31      0.0575876000
_diffrn_orient_matrix_UB_32      -0.0525134000
_diffrn_orient_matrix_UB_33      -0.0007937000
_diffrn_radiation_collimation    'HF Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            430498
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.244
_diffrn_reflns_theta_min         2.390
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             5320
_exptl_crystal_recrystallization_method
"'The material was crystallised by vapour diffusion of methanol into a solution of THF'"
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3255
_refine_ls_number_reflns         52471
_refine_ls_number_restraints     8190
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.1109
_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^)+(0.1991P)^2^+8.1795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3439
_refine_ls_wR_factor_ref         0.3530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                43495
_reflns_number_total             52471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00889h3.cif
_cod_data_source_block           2021ncs0528_2b
_cod_depositor_comments
'Adding full bibliography for 1571314--1571316.cif.'
_cod_original_cell_volume        14432.24(15)
_cod_database_code               1571314
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C126 H112 N6 O10'
_chemical_oxdiff_usercomment     k51_270
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.877
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{C425, C125, C525}
{C325, C725}
{C2, C2B}
{C202, C602}
3. Restrained distances
 O9B-C2E = O10B-C2E
 1.26 with sigma of 0.02
 C2E-C425
 1.5 with sigma of 0.02
 O10-C126 = O9-C126
 1.26 with sigma of 0.02
 C126-C125
 1.5 with sigma of 0.02
 O9C-C2I = O10C-C2I
 1.26 with sigma of 0.02
 C2I-C525
 1.5 with sigma of 0.02
 C267-C247 = C667-C647
 1.52 with sigma of 0.02
 O603-C644
 1.23 with sigma of 0.02
 C603-C602
 1.5 with sigma of 0.02
 O208-C203 = O207-C203
 1.26 with sigma of 0.02
 O7-C3 = O8-C3
 1.26 with sigma of 0.02
 O610-C726 = O609-C726
 1.26 with sigma of 0.02
 C726-C725
 1.5 with sigma of 0.02
 C3-C2
 1.5 with sigma of 0.02
 O8B-C131 = O7B-C131
 1.26 with sigma of 0.02
 C131-C2B
 1.5 with sigma of 0.02
 O209-C326 = O210-C326
 1.26 with sigma of 0.02
 C326-C325
 1.5 with sigma of 0.02
 C203-C202
 1.5 with sigma of 0.02
 O607-C603 = O608-C603
 1.26 with sigma of 0.02
 O9C-O10C
 2.19 with sigma of 0.04
 O10B-C425
 2.39 with sigma of 0.04
 O9B-O10B
 2.19 with sigma of 0.04
 O10-C125
 2.38 with sigma of 0.04
 O10C-C525
 2.39 with sigma of 0.04
 O9B-C425
 2.38 with sigma of 0.04
 O10-O9
 2.19 with sigma of 0.04
 O9-C125
 2.39 with sigma of 0.04
 O9C-C525
 2.38 with sigma of 0.04
 O7B-C2B
 2.39 with sigma of 0.04
 O209-O210
 2.19 with sigma of 0.04
 O609-C725
 2.39 with sigma of 0.04
 O607-C602
 2.38 with sigma of 0.04
 O210-C325
 2.39 with sigma of 0.04
 O610-O609
 2.19 with sigma of 0.04
 O208-C202
 2.38 with sigma of 0.04
 O209-C325
 2.38 with sigma of 0.04
 O610-C725
 2.38 with sigma of 0.04
 O208-O207
 2.19 with sigma of 0.04
 O207-C202
 2.39 with sigma of 0.04
 O607-O608
 2.19 with sigma of 0.04
 O608-C602
 2.39 with sigma of 0.04
 O7-O8
 2.19 with sigma of 0.04
 O7-C2
 2.38 with sigma of 0.04
 O8-C2
 2.39 with sigma of 0.04
 O8B-O7B
 2.19 with sigma of 0.04
 O8B-C2B
 2.38 with sigma of 0.04
 C2E-O9B \\sim C2E-O10B
 with sigma of 0.02
 O9B-C425 \\sim C425-O10B
 with sigma of 0.04
 C126-O10 \\sim C126-O9
 with sigma of 0.02
 O10-C125 \\sim C125-O9
 with sigma of 0.04
 C2I-O9C \\sim C2I-O10C
 with sigma of 0.02
 O9C-C525 \\sim C525-O10C
 with sigma of 0.04
 O203-C244 \\sim O603-C644
 with sigma of 0.02
 N203-O203 \\sim N603-O603
 with sigma of 0.04
 C51B-C49B \\sim C51B-C54B \\sim C51B-C52B \\sim C51B-C53B
 with sigma of 0.02
 C245-C244 \\sim C644-C645
 with sigma of 0.02
 C244-C219 \\sim C219-C644
 with sigma of 0.04
 C646-C644 \\sim C644-C650
 with sigma of 0.04
 C49B-C54B \\sim C49B-C52B \\sim C49B-C53B \\sim C54B-C52B \\sim C54B-C53B
\\sim C52B-C53B
 with sigma of 0.04
 C246-C244 \\sim C244-C250
 with sigma of 0.04
 N203-C219 \\sim N603-C219
 with sigma of 0.02
 N203-C244 \\sim N603-C644
 with sigma of 0.02
 C296-C317 \\sim C696-C717
 with sigma of 0.04
 C293-C670 \\sim C693-C670
 with sigma of 0.02
 C295-C296 \\sim C695-C696
 with sigma of 0.02
 C295-C317 \\sim C695-C717
 with sigma of 0.02
 C297-C302 \\sim C697-C702
 with sigma of 0.04
 C294-C295 \\sim C694-C695
 with sigma of 0.02
 C293-C270 \\sim C693-C270
 with sigma of 0.02
 C296-C298 \\sim C696-C698
 with sigma of 0.04
 C297-C300 \\sim C697-C700
 with sigma of 0.04
 C298-C270 \\sim C698-C270
 with sigma of 0.04
 C299-C300 \\sim C699-C700
 with sigma of 0.02
 C299-C301 \\sim C699-C701
 with sigma of 0.02
 C317-C318 \\sim C717-C318
 with sigma of 0.04
 C300-C302 \\sim C700-C702
 with sigma of 0.04
 N206-C317 \\sim N606-C717
 with sigma of 0.02
 N206-C318 \\sim N606-C318
 with sigma of 0.02
 C293-C294 \\sim C693-C694
 with sigma of 0.02
 C296-C297 \\sim C696-C697
 with sigma of 0.02
 C293-C298 \\sim C693-C698
 with sigma of 0.02
 C295-C297 \\sim C695-C697
 with sigma of 0.04
 C296-C299 \\sim C696-C699
 with sigma of 0.04
 C297-C301 \\sim C697-C701
 with sigma of 0.04
 C298-C299 \\sim C698-C699
 with sigma of 0.04
 C298-C670 \\sim C698-C670
 with sigma of 0.04
 O206-N206 \\sim O606-N606
 with sigma of 0.04
 O206-C295 \\sim O606-C695
 with sigma of 0.04
 N206-C295 \\sim N606-C695
 with sigma of 0.04
 C300-C301 \\sim C700-C701
 with sigma of 0.04
 C293-C295 \\sim C693-C695
 with sigma of 0.04
 C301-C302 \\sim C701-C702
 with sigma of 0.04
 C293-C297 \\sim C693-C697
 with sigma of 0.04
 C299-C302 \\sim C699-C702
 with sigma of 0.02
 C294-C296 \\sim C694-C696
 with sigma of 0.04
 C670-C693 \\sim C270-C293
 with sigma of 0.02
 C294-C298 \\sim C694-C698
 with sigma of 0.04
 C294-C317 \\sim C694-C717
 with sigma of 0.04
 C294-C270 \\sim C694-C270
 with sigma of 0.04
 C294-C670 \\sim C694-C670
 with sigma of 0.04
 O206-C317 \\sim O606-C717
 with sigma of 0.02
 C297-C298 \\sim C697-C698
 with sigma of 0.02
 C297-C299 \\sim C697-C699
 with sigma of 0.02
 O203-C245 \\sim O603-C645
 with sigma of 0.04
 C3-O7 \\sim C3-O8
 with sigma of 0.02
 O7-C2 \\sim C2-O8
 with sigma of 0.04
 C131-O8B \\sim C131-O7B
 with sigma of 0.02
 O8B-C2B \\sim C2B-O7B
 with sigma of 0.04
 C326-O209 \\sim C326-O210
 with sigma of 0.02
 O209-C325 \\sim C325-O210
 with sigma of 0.04
 C726-O610 \\sim C726-O609
 with sigma of 0.02
 O610-C725 \\sim C725-O609
 with sigma of 0.04
 C203-O208 \\sim C203-O207
 with sigma of 0.02
 O208-C202 \\sim C202-O207
 with sigma of 0.04
 C603-O607 \\sim C603-O608
 with sigma of 0.02
 O607-C602 \\sim C602-O608
 with sigma of 0.04
 C238-C243 \\sim C241-C242 \\sim C242-C243
 with sigma of 0.06
 C240-C238 \\sim C240-C241 \\sim C240-C242 \\sim C240-C243
 with sigma of 0.03
 C642-C641 \\sim C642-C643 \\sim C642-C638 \\sim C641-C638 \\sim C643-C638
 with sigma of 0.06
 C642-C641 \\sim C642-C643 \\sim C642-C638 \\sim C641-C643 \\sim C641-C638
\\sim C643-C638
 with sigma of 0.06
 C640-C642 \\sim C640-C641 \\sim C640-C643 \\sim C640-C638
 with sigma of 0.03
4. Restrained planarity
 O9, O10, C125, C126
 with sigma of 0.1
 O9B, O10B, C2E, C425
 with sigma of 0.1
 O9C, O10C, C2I, C525
 with sigma of 0.1
 O209, O210, C325, C326
 with sigma of 0.1
 O7B, O8B, C2B, C131
 with sigma of 0.1
 O609, O610, C725, C726
 with sigma of 0.1
 O7, O8, C2, C3
 with sigma of 0.1
 O207, O208, C202, C203
 with sigma of 0.1
 O607, O608, C602, C603
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C425) = Uanis(C125) = Uanis(C525)
Uanis(C325) = Uanis(C725)
Uanis(C2) = Uanis(C2B)
Uanis(C202) = Uanis(C602)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 1*[Sof(O9B)+Sof(O10B)+Sof(H10J)+Sof(C2E)+Sof(C425)]+1*[Sof(O9)+Sof(H9A)+
 Sof(O10)+Sof(C125)+Sof(C126)]+1*[Sof(O9C)+Sof(H9C)+Sof(O10C)+Sof(C2I)+
 Sof(C525)]=1 with esd of 0.000001
 1*[Sof(O7)+Sof(O8)+Sof(H8A)+Sof(C2)+Sof(C3)]+1*[Sof(O7B)+Sof(O8B)+Sof(H8B)+
 Sof(C2B)+Sof(C131)]=1 with esd of 0.000001
 1*[Sof(O209)+Sof(H20C)+Sof(O210)+Sof(C325)+Sof(C326)]+1*[Sof(O609)+Sof(H609)+
 Sof(O610)+Sof(C725)+Sof(C726)]=1 with esd of 0.000001
 1*[Sof(O207)+Sof(O208)+Sof(H20B)+Sof(C202)+Sof(C203)]+1*[Sof(O607)+Sof(O608)+
 Sof(H608)+Sof(C602)+Sof(C603)]=1 with esd of 0.000001
 Sof(O603)=Sof(O606)=Sof(N603)=Sof(H603)=Sof(N606)=Sof(H606)=Sof(C251)=
 Sof(C252)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C253)=Sof(H25D)=Sof(H25E)=
 Sof(H25F)=Sof(C254)=Sof(H25G)=Sof(H25H)=Sof(H25I)=Sof(C644)=Sof(C647)=
 Sof(C648)=Sof(H648)=Sof(C649)=Sof(C650)=Sof(H650)=Sof(C645)=Sof(C646)=
 Sof(H646)=Sof(C667)=Sof(C668)=Sof(H668)=Sof(C669)=Sof(H669)=Sof(C670)=
 Sof(C671)=Sof(H671)=Sof(C672)=Sof(H672)=Sof(C695)=Sof(C694)=Sof(H694)=
 Sof(C693)=Sof(C698)=Sof(H698)=Sof(C697)=Sof(C696)=Sof(H696)=Sof(C699)=
 Sof(C700)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C701)=Sof(H70D)=Sof(H70E)=
 Sof(H70F)=Sof(C702)=Sof(H70G)=Sof(H70H)=Sof(H70I)=Sof(C717)=1-FVAR(1)
 Sof(O203)=Sof(O206)=Sof(N203)=Sof(H203)=Sof(N206)=Sof(H20D)=Sof(C244)=
 Sof(C247)=Sof(C246)=Sof(H246)=Sof(C245)=Sof(C250)=Sof(H250)=Sof(C249)=
 Sof(C248)=Sof(H248)=Sof(C267)=Sof(C272)=Sof(H272)=Sof(C271)=Sof(H271)=
 Sof(C270)=Sof(C269)=Sof(H269)=Sof(C268)=Sof(H268)=Sof(C295)=Sof(C294)=
 Sof(H294)=Sof(C293)=Sof(C298)=Sof(H298)=Sof(C297)=Sof(C296)=Sof(H296)=
 Sof(C299)=Sof(C300)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C301)=Sof(H30D)=
 Sof(H30E)=Sof(H30F)=Sof(C302)=Sof(H30G)=Sof(H30H)=Sof(H30I)=Sof(C317)=
 Sof(C651)=Sof(C652)=Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C653)=Sof(H65D)=
 Sof(H65E)=Sof(H65F)=Sof(C654)=Sof(H65G)=Sof(H65H)=Sof(H65I)=FVAR(1)
 Sof(C47B)=Sof(C46B)=Sof(H46B)=Sof(C45B)=Sof(C50B)=Sof(H50B)=Sof(C49B)=
 Sof(C48B)=Sof(H48B)=Sof(C51B)=Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=
 Sof(C53B)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54B)=Sof(H54D)=Sof(H54E)=
 Sof(H54F)=Sof(C67)=Sof(C72)=Sof(H72)=Sof(C71)=Sof(H71)=Sof(C70)=Sof(C69)=
 Sof(H69)=Sof(C68)=Sof(H68)=1-FVAR(2)
 Sof(C47)=Sof(C46)=Sof(H46)=Sof(C45)=Sof(C50)=Sof(H50)=Sof(C49)=Sof(C48)=
 Sof(H48)=Sof(C51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=Sof(H53A)=
 Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C67B)=Sof(C68B)=
 Sof(H68B)=Sof(C69B)=Sof(H69B)=Sof(C70B)=Sof(C71B)=Sof(H71B)=Sof(C72B)=
 Sof(H72B)=FVAR(2)
 Sof(C64B)=Sof(C63B)=Sof(H63B)=Sof(C62B)=Sof(H62B)=Sof(C61B)=Sof(C66B)=
 Sof(H66B)=Sof(C65B)=Sof(H65J)=1-FVAR(3)
 Sof(C64)=Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66)=Sof(C61)=Sof(C62)=Sof(H62)=
 Sof(C63)=Sof(H63)=FVAR(3)
 Sof(C80B)=Sof(C81B)=Sof(H81D)=Sof(H81E)=Sof(H81F)=Sof(C82B)=Sof(H82D)=
 Sof(H82E)=Sof(H82F)=Sof(C83B)=Sof(H83D)=Sof(H83E)=Sof(H83F)=1-FVAR(4)
 Sof(C80)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C82)=Sof(H82A)=Sof(H82B)=
 Sof(H82C)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=FVAR(4)
 Sof(O602)=Sof(N602)=Sof(H602)=Sof(C633)=Sof(C636)=Sof(C637)=Sof(H637)=
 Sof(C638)=Sof(C639)=Sof(H639)=Sof(C634)=Sof(C635)=Sof(H635)=Sof(C640)=
 Sof(C641)=Sof(H64A)=Sof(H64B)=Sof(H64C)=Sof(C642)=Sof(H64D)=Sof(H64E)=
 Sof(H64F)=Sof(C643)=Sof(H64G)=Sof(H64H)=Sof(H64I)=Sof(C661)=Sof(C666)=
 Sof(H666)=Sof(C665)=Sof(H665)=Sof(C664)=Sof(C663)=Sof(H663)=Sof(C662)=
 Sof(H662)=1-FVAR(5)
 Sof(O202)=Sof(N202)=Sof(H202)=Sof(C233)=Sof(C236)=Sof(C235)=Sof(H235)=
 Sof(C234)=Sof(C239)=Sof(H239)=Sof(C238)=Sof(C237)=Sof(H237)=Sof(C240)=
 Sof(C241)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C242)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=Sof(C243)=Sof(H24G)=Sof(H24H)=Sof(H24I)=Sof(C261)=Sof(C266)=
 Sof(H266)=Sof(C265)=Sof(H265)=Sof(C264)=Sof(C263)=Sof(H263)=Sof(C262)=
 Sof(H262)=FVAR(5)
 Sof(O9B)=Sof(O10B)=Sof(H10J)=Sof(C2E)=Sof(C425)=FVAR(6)
 Sof(O9)=Sof(H9A)=Sof(O10)=Sof(C125)=Sof(C126)=FVAR(7)
 Sof(O9C)=Sof(H9C)=Sof(O10C)=Sof(C2I)=Sof(C525)=FVAR(8)
 Sof(O7)=Sof(O8)=Sof(H8A)=Sof(C2)=Sof(C3)=FVAR(9)
 Sof(O7B)=Sof(O8B)=Sof(H8B)=Sof(C2B)=Sof(C131)=FVAR(10)
 Sof(O209)=Sof(H20C)=Sof(O210)=Sof(C325)=Sof(C326)=FVAR(11)
 Sof(O609)=Sof(H609)=Sof(O610)=Sof(C725)=Sof(C726)=FVAR(12)
 Sof(O207)=Sof(O208)=Sof(H20B)=Sof(C202)=Sof(C203)=FVAR(13)
 Sof(O607)=Sof(O608)=Sof(H608)=Sof(C602)=Sof(C603)=FVAR(14)
8.a Ternary CH refined with riding coordinates:
 C1(H1A), C124(H124), C201(H20A), C324(H324)
8.b Me refined with riding coordinates:
 C700(H70A,H70B,H70C), C701(H70D,H70E,H70F), C702(H70G,H70H,H70I)
8.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), C6(H6A), C8(H8), C9(H9),
 C12(H12), C14(H14), C15(H15), C18(H18), C20(H20), C21(H21), C24(H24), C26(H26),
  C28(H28), C35(H35), C37(H37), C39(H39), C56(H56), C57(H57), C59(H59),
 C60(H60), C74(H74), C76(H76), C78(H78), C85(H85), C87(H87), C89(H89), C96(H96),
  C98(H98), C100(H100), C107(H107), C108(H108), C111(H111), C113(H113),
 C114(H114), C117(H117), C119(H119), C122(H122), C123(H123), C46(H46), C50(H50),
  C48(H48), C65(H65), C66(H66), C62(H62), C63(H63), C68B(H68B), C69B(H69B),
 C71B(H71B), C72B(H72B), C46B(H46B), C50B(H50B), C48B(H48B), C63B(H63B),
 C62B(H62B), C66B(H66B), C65B(H65J), C72(H72), C71(H71), C69(H69), C68(H68),
 N201(H201), N204(H204), N205(H205), C206(H206), C208(H208), C209(H209),
 C212(H212), C214(H214), C215(H215), C218(H218), C220(H220), C221(H221),
 C224(H224), C226(H226), C228(H228), C256(H256), C257(H257), C259(H259),
 C260(H260), C274(H274), C276(H276), C278(H278), C284(H284), C286(H286),
 C288(H288), C305(H305), C308(H308), C309(H309), C312(H312), C315(H315),
 C316(H316), C319(H319), C322(H322), C323(H323), N202(H202), N203(H203),
 N206(H20D), C235(H235), C239(H239), C237(H237), C246(H246), C250(H250),
 C248(H248), C266(H266), C265(H265), C263(H263), C262(H262), C272(H272),
 C271(H271), C269(H269), C268(H268), C294(H294), C298(H298), C296(H296),
 N602(H602), N603(H603), N606(H606), C637(H637), C639(H639), C635(H635),
 C648(H648), C650(H650), C646(H646), C666(H666), C665(H665), C663(H663),
 C662(H662), C668(H668), C669(H669), C671(H671), C672(H672), C694(H694),
 C698(H698), C696(H696)
8.d Fitted hexagon refined as free rotating group:
 C47(C46,C45,C50,C49,C48), C64(C65,C66,C61,C62,C63), C67B(C68B,C69B,C70B,C71B,
 C72B), C47B(C46B,C45B,C50B,C49B,C48B), C64B(C63B,C62B,C61B,C66B,C65B), C67(C72,
 C71,C70,C69,C68), C236(C235,C234,C239,C238,C237), C247(C246,C245,C250,C249,
 C248), C261(C266,C265,C264,C263,C262), C267(C272,C271,C270,C269,C268),
 C295(C294,C293,C298,C297,C296), C636(C637,C638,C639,C634,C635), C647(C648,C649,
 C650,C645,C646), C661(C666,C665,C664,C663,C662), C667(C668,C669,C670,C671,
 C672), C695(C694,C693,C698,C697,C696)
8.e Tetrahedral OH refined with riding coordinates:
 O8(H8A), O10B(H10J), O8B(H8B), O9(H9A), O9C(H9C), O208(H20B), O209(H20C),
 O608(H608), O609(H609)
8.f Idealised Me refined as rotating group:
 C30(H30J,H30K,H30L), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C92(H92A,H92B,H92C), C93(H93A,
 H93B,H93C), C94(H94A,H94B,H94C), C103(H10A,H10B,H10C), C104(H10D,H10E,H10F),
 C105(H10G,H10H,H10I), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C),
 C52B(H52D,H52E,H52F), C53B(H53D,H53E,H53F), C54B(H54D,H54E,H54F), C81B(H81D,
 H81E,H81F), C82B(H82D,H82E,H82F), C83B(H83D,H83E,H83F), C230(H23A,H23B,H23C),
 C231(H23D,H23E,H23F), C232(H23G,H23H,H23I), C280(H28A,H28B,H28C), C281(H28D,
 H28E,H28F), C282(H28G,H28H,H28I), C290(H29A,H29B,H29C), C291(H29D,H29E,H29F),
 C292(H29G,H29H,H29I), C241(H24A,H24B,H24C), C242(H24D,H24E,H24F), C243(H24G,
 H24H,H24I), C300(H30A,H30B,H30C), C301(H30D,H30E,H30F), C302(H30G,H30H,H30I),
 C652(H65A,H65B,H65C), C653(H65D,H65E,H65F), C654(H65G,H65H,H65I), C252(H25A,
 H25B,H25C), C253(H25D,H25E,H25F), C254(H25G,H25H,H25I), C641(H64A,H64B,H64C),
 C642(H64D,H64E,H64F), C643(H64G,H64H,H64I)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1387 electrons were 
found in a volume of 5311\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4[C4H8O], 10[CH4O] per Asymmetric Unit 
which account for 1360 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87162
_shelx_fab_checksum              26461
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in oil'
_olex2_submission_original_sample_id k51_270
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.868
_oxdiff_exptl_absorpt_empirical_full_min 0.728