Design and synthesis of macrocycles with tuneable diameters and helical foldamers with customizable peripheral side chains.
Farooq, Saquib; Crochet, Aurelien; Kilbinger, Andreas F. M.; Chemical science 16 (2025) 20570–20579; doi:10.1039/d5sc04138d

data_1575958
_publ_section_title
;
 Design and synthesis of macrocycles with tuneable diameters and helical
 foldamers with customizable peripheral side chains.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              20570
_journal_page_last               20579
_journal_paper_doi               10.1039/d5sc04138d
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C115 H138 N10 O30, 7.3[CH3OH]'
_chemical_formula_sum            'C122.3 H167.2 N10 O37.3'
_chemical_formula_weight         2374.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-01-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-02-17 deposited with the CCDC.	2025-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1706(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.0174(5)
_cell_length_b                   27.1277(7)
_cell_length_c                   33.8432(6)
_cell_measurement_reflns_used    23381
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      50.6340
_cell_measurement_theta_min      2.2640
_cell_volume                     25654.3(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -15.00  10.00   0.50   40.00    --   29.63 -14.00 151.00   50
  2  \w     14.00  40.00   0.50   40.00    --   29.63  14.00 -37.00   52
  3  \w      6.00  32.00   0.50   40.00    --   30.71  14.00 -37.00   52
  4  \w     49.00  75.00   0.50   40.00    --   30.71  14.00 -37.00   52
  5  \w    -76.00   0.00   0.50   40.00    --  -31.27 -14.00 151.00  152
  6  \w    -19.00   7.00   0.50   40.00    --   -6.00 103.00 155.88   52
  7  \w      1.00  26.00   0.50   40.00    --   10.00  97.00-142.73   50
  8  \w    -19.00  27.00   0.50   40.00    --  -10.00  98.00 100.45   92
  9  \w     16.00  41.00   0.50   40.00    --   18.00  85.00  13.05   50
 10  \w    -58.00 -33.00   0.50   40.00    --  -22.00 -75.00  17.61   50
 11  \w     17.00  42.00   0.50   40.00    --   22.00  90.00  74.40   50
 12  \w    -16.00  18.00   0.50   40.00    --   29.63 -19.00 -90.00   68
 13  \w    -15.00  16.00   0.50   40.00    --   29.63 -19.00  60.00   62
 14  \w     41.00  67.00   0.50   40.00    --   30.17  74.00-103.49   52
 15  \w     34.00  60.00   0.50   40.00    --   30.17  76.00  15.08   52
 16  \w     34.00  59.00   0.50   40.00    --   30.17  76.00 112.70   50
 17  \w     35.00  60.00   0.50   40.00    --   30.17  75.00  42.11   50
 18  \w     38.00  63.00   0.50   40.00    --   30.17  70.00-120.54   50
 19  \w     35.00  60.00   0.50   40.00    --   30.17  75.00  83.88   50
 20  \w     38.00  63.00   0.50   40.00    --   30.17  68.00  96.55   50
 21  \w     47.00  72.00   0.50   40.00    --   30.17  58.00 105.65   50
 22  \w     37.00  62.00   0.50   40.00    --   30.17  75.00  47.04   50
 23  \w    -14.00  22.00   0.50   40.00    --   30.71 -19.00 -60.00   72
 24  \w     -8.00  17.00   0.50   40.00    --   30.71 -14.00 151.00   50
 25  \w    -73.00 -48.00   0.50   40.00    --  -31.27 -58.00  -4.83   50
 26  \w    -72.00 -47.00   0.50   40.00    --  -31.27 -58.00  68.25   50
 27  \w    -18.00  10.00   0.50   40.00    --  -31.27  59.00  -5.02   56
 28  \w    -75.00 -50.00   0.50   40.00    --  -31.27 -53.00  94.82   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0445384000
_diffrn_orient_matrix_UB_12      -0.0060725000
_diffrn_orient_matrix_UB_13      0.0237222000
_diffrn_orient_matrix_UB_21      -0.0310313000
_diffrn_orient_matrix_UB_22      -0.0086410000
_diffrn_orient_matrix_UB_23      -0.0388322000
_diffrn_orient_matrix_UB_31      0.0096466000
_diffrn_orient_matrix_UB_32      -0.0558050000
_diffrn_orient_matrix_UB_33      0.0034353000
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67912
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        50.429
_diffrn_reflns_theta_max         50.429
_diffrn_reflns_theta_min         2.270
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale colourless'
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       plate
_exptl_crystal_F_000             10155
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.608
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1607
_refine_ls_number_reflns         13355
_refine_ls_number_restraints     2464
_refine_ls_restrained_S_all      1.628
_refine_ls_R_factor_all          0.1810
_refine_ls_R_factor_gt           0.1400
_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          0.3976
_refine_ls_wR_factor_ref         0.4299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7473
_reflns_number_total             13355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04138d2.cif
_cod_data_source_block           sl-754-pentamer-d
_cod_depositor_comments
'Adding full bibliography for 1575958--1575961.cif.'
_cod_original_formula_sum        'C122.30 H167.20 N10 O37.30'
_cod_database_code               1575958
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C115 H140 N10 O30'
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.845
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C105-C102 = C106-C102
 1.54 with sigma of 0.02
 O1-C3 = O8-C22
 1.43 with sigma of 0.02
 C79-C82
 1.54 with sigma of 0.02
 C130-C135
 1.54 with sigma of 0.02
 C104-C117
 1.54 with sigma of 0.02
 C98-C104 = C117-C104 = C118-C117 = C91-C90 = C98-C91
 1.54 with sigma of 0.02
 C107-C112
 1.54 with sigma of 0.02
 C112-C127
 1.54 with sigma of 0.02
 C127-C139
 1.54 with sigma of 0.02
 C107-C103
 1.54 with sigma of 0.02
 C133-C130
 2.5 with sigma of 0.02
 C97-C140
 1.54 with sigma of 0.02
 C97-C96 = C149-C148
 1.54 with sigma of 0.02
 C93-C92 = C93-C120 = C125-C120 = C125-C121 = C128-C121
 1.54 with sigma of 0.02
 C125-C128
 2.5 with sigma of 0.02
 C121-C120
 2.5 with sigma of 0.02
 C125-C93
 2.5 with sigma of 0.02
 C92-C120
 2.5 with sigma of 0.02
 C109-C101 = C145-C109 = C145-C126 = C129-C126
 1.54 with sigma of 0.02
 C129-C144
 1.54 with sigma of 0.02
 C145-C101
 2.5 with sigma of 0.02
 C109-C126
 2.5 with sigma of 0.02
 C145-C129
 2.5 with sigma of 0.02
 C126-C144
 2.5 with sigma of 0.02
 C140-C105
 1.54 with sigma of 0.02
 C97-C105
 2.5 with sigma of 0.02
 C105-C106
 2.5 with sigma of 0.02
 C140-C102
 2.5 with sigma of 0.02
 C91-C90
 1.54 with sigma of 0.02
 C91-C90 = C90-C103
 1.54 with sigma of 0.02
 O19-C90
 1.43 with sigma of 0.02
 C89-C88 = C89-C116 = C116-C111 = C113-C111 = C113-C110
 1.54 with sigma of 0.02
 C88-C116
 2.5 with sigma of 0.02
 C89-C111
 2.5 with sigma of 0.02
 C116-C113
 2.5 with sigma of 0.02
 C111-C110
 2.5 with sigma of 0.02
 C113-C116
 2.5 with sigma of 0.02
 C111-C89
 2.5 with sigma of 0.02
 C116-C88
 2.5 with sigma of 0.02
 C75-C71
 1.5 with sigma of 0.02
 O26-C73 \\sim O19-C54 \\sim O14-C37 \\sim O8-C22 \\sim O1-C3
 with sigma of 0.02
 O5-C16 \\sim O4-C15 \\sim O2-C7 \\sim O29-C83 \\sim O29-C84 \\sim O28-C86
\\sim O28-C85 \\sim O7-C32 ~
 O10-C31 \\sim O11-C33 \\sim O13-C41 \\sim O16-C49 \\sim O17-C50 \\sim O20-C58
\\sim O22-C66 \\sim O23-C67
 \\sim O25-C87
 with sigma of 0.02
 C95-C94 \\sim C138-C137 \\sim C95-C100 \\sim C137-C134 \\sim C119-C100 \\sim
C134-C133 \\sim C132-
 C119 \\sim C135-C133 \\sim C132-C131
 with sigma of 0.02
 O1-C138 \\sim O1-C94
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C144 \\sim C129 \\sim C126 \\sim C145 \\sim C109 \\sim C101 \\sim C92 \\sim C93
\\sim C120 \\sim C125 \\sim C121 \\sim C128 \\sim C103 \\sim C107 \\sim C112
\\sim C127 \\sim C139 \\sim C118 \\sim C117 \\sim C104 \\sim C98 \\sim C91
\\sim C90 \\sim C138 \\sim O1 \\sim C94 \\sim C95 \\sim C137 \\sim C100 \\sim
C134 \\sim C119 \\sim C132 \\sim C133 \\sim C131 \\sim C130 \\sim C135 \\sim
C96 \\sim C97 \\sim C148 \\sim C149 \\sim C140 \\sim C105 \\sim C102 \\sim
C106: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O14 \\sim C88 \\sim C89 \\sim C116 \\sim C111 \\sim C113 \\sim C110: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(O12) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=
 1-FVAR(1)
 Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(H86C)=
 FVAR(1)
 Sof(C130)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C133)=Sof(H13I)=Sof(H13J)=
 Sof(C134)=Sof(H13K)=Sof(H13L)=Sof(C135)=Sof(H13M)=Sof(H13N)=Sof(C137)=
 Sof(H13O)=Sof(H13P)=Sof(C138)=Sof(H13Q)=Sof(H13R)=1-FVAR(2)
 Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(C100)=Sof(H10A)=
 Sof(H10B)=Sof(C119)=Sof(H11Q)=Sof(H11R)=Sof(C131)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C132)=Sof(H13G)=Sof(H13H)=FVAR(2)
 Sof(H90C)=Sof(H90D)=Sof(C103)=Sof(H10E)=Sof(H10F)=Sof(C107)=Sof(H10I)=
 Sof(H10J)=Sof(C112)=Sof(H11F)=Sof(H11G)=Sof(C127)=Sof(H12I)=Sof(H12J)=
 Sof(C139)=Sof(H13S)=Sof(H13T)=Sof(H13U)=1-FVAR(3)
 Sof(H90A)=Sof(H90B)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(C98)=Sof(H98A)=Sof(H98B)=
 Sof(C104)=Sof(H10G)=Sof(H10H)=Sof(C117)=Sof(H11L)=Sof(H11M)=Sof(C118)=
 Sof(H11N)=Sof(H11O)=Sof(H11P)=FVAR(3)
 Sof(C148)=Sof(H14F)=Sof(H14G)=Sof(C149)=Sof(H14H)=Sof(H14I)=1-FVAR(4)
 Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(C97)=Sof(H97A)=Sof(H97B)=FVAR(4)
 Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C120)=Sof(H12A)=
 Sof(H12B)=Sof(C121)=Sof(H12C)=Sof(H12D)=Sof(C125)=Sof(H12E)=Sof(H12F)=
 Sof(C128)=Sof(H12K)=Sof(H12L)=Sof(H12M)=1-FVAR(5)
 Sof(C101)=Sof(H10C)=Sof(H10D)=Sof(C109)=Sof(H10K)=Sof(H10L)=Sof(C126)=
 Sof(H12G)=Sof(H12H)=Sof(C129)=Sof(H12N)=Sof(H12O)=Sof(C144)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C145)=Sof(H14D)=Sof(H14E)=FVAR(5)
6.a Secondary CH2 refined with riding coordinates:
 C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C90(H90C,H90D), C91(H91A,
 H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
 C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C100(H10A,H10B), C101(H10C,
 H10D), C103(H10E,H10F), C104(H10G,H10H), C107(H10I,H10J), C109(H10K,H10L),
 C111(H11D,H11E), C112(H11F,H11G), C113(H11H,H11I), C116(H11J,H11K), C117(H11L,
 H11M), C119(H11Q,H11R), C120(H12A,H12B), C121(H12C,H12D), C125(H12E,H12F),
 C126(H12G,H12H), C127(H12I,H12J), C129(H12N,H12O), C132(H13G,H13H), C133(H13I,
 H13J), C134(H13K,H13L), C135(H13M,H13N), C137(H13O,H13P), C138(H13Q,H13R),
 C145(H14D,H14E), C148(H14F,H14G), C149(H14H,H14I), C102(H10M,H10N), C105(H10R,
 H10S)
6.b Me refined with riding coordinates:
 C110(H11A,H11B,H11C), C118(H11N,H11O,H11P), C128(H12K,H12L,H12M), C130(H13A,
 H13B,H13C), C131(H13D,H13E,H13F), C139(H13S,H13T,H13U), C144(H14A,H14B,H14C),
 C106(H10O,H10P,H10Q)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), N9(H9),
 N10(H10), C2(H2A), C4(H4A), C13(H13), C14(H14), C21(H21), C23(H23), C29(H29),
 C30(H30), C36(H36), C38(H38), C44(H44), C45(H45), C53(H53), C55(H55), C64(H64),
  C65(H65), C72(H72), C74(H74), C77(H77), C78(H78)
6.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C58(H58A,H58B,H58C), C66(H66A,H66B,H66C),
 C67(H67A,H67B,H67C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,
 H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 1036 electrons were 
found in a volume of 4860\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
7.3[CH3OH] per Asymmetric Unit 
which account for 1051 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2889
_shelx_fab_checksum              2021
_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 2.017
_oxdiff_exptl_absorpt_empirical_full_min 0.583