Guest-triggered crystallization of π-conjugated pillar[5]arene: from amorphous aggregates to an ordered architecture <i>via</i> solid-state host-guest synergy.
Chen, Jin-Fa; Gao, Qing-Xiu; Wang, Yuxuan; Shi, Bingbing; Yao, Hong; Wei, Tai-Bao; Lin, Qi; Chemical communications (Cambridge, England) 61 (2025) 15882–15885; doi:10.1039/d5cc03945b

data_7134974
_publ_section_title
;
 Guest-triggered crystallization of &#x3c0;-conjugated pillar[5]arene:
 from amorphous aggregates to an ordered architecture <i>via</i>
 solid-state host-guest synergy.
;
_journal_issue                   81
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15882
_journal_page_last               15885
_journal_paper_doi               10.1039/d5cc03945b
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C87 H88 N2 O8, C5 H10 O, 0.203[C3H6O], 0.336[C3H6O]'
_chemical_formula_sum            'C93.62 H101.24 N2 O9.54'
_chemical_formula_weight         1407.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-08-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-08-29 deposited with the CCDC.	2025-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.4700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   43.0399(3)
_cell_length_b                   24.22730(10)
_cell_length_c                   61.0404(4)
_cell_measurement_reflns_used    119553
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.1450
_cell_measurement_theta_min      2.0720
_cell_volume                     62781.9(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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    -24.00  28.06   0.38    0.04    --  -46.79  19.00  30.00  137
  2  \w    -23.00  22.22   0.38    0.04    --  -46.79  19.00   0.00  119
  3  \w    -25.00  28.20   0.38    0.04    --  -46.79  19.00 -90.00  140
  4  \w     68.00  93.08   0.38    0.04    --   46.79 145.00-145.00   66
  5  \w     93.00 118.08   0.38    0.04    --  104.64 145.00-145.00   66
  6  \w     92.00 125.06   0.38    0.04    --  104.64 125.00  46.00   87
  7  \w     80.00 161.70   0.38    0.04    --  104.64 125.00  90.00  215
  8  \w     24.00 117.86   0.38    0.04    --   46.79  77.00  30.00  247
  9  \w     92.00 119.36   0.38    0.04    --  104.64  45.00-150.00   72
 10  \w    129.00 167.76   0.38    0.04    --  104.64  45.00-150.00  102
 11  \w    130.00 168.76   0.38    0.04    --  104.64  15.00-120.00  102
 12  \w    103.00 129.22   0.38    0.04    --  104.64  15.00-120.00   69
 13  \w    128.00 175.50   0.38    0.04    --  104.64  45.00 -30.00  125
 14  \w    139.00 168.64   0.38    0.04    --  104.64  30.00 150.00   78
 15  \w     92.00 117.08   0.38    0.04    --  104.64  30.00 150.00   66
 16  \w    -27.00  24.30   0.38    0.04    --   46.79 -19.00  60.00  135
 17  \w     32.00  62.02   0.38    0.04    --  104.64 -61.00 120.00   79
 18  \w     46.00  71.08   0.38    0.04    --  104.64 -61.00  30.00   66
 19  \w     42.00  67.08   0.38    0.04    --  104.64 -77.00 -60.00   66
 20  \w    -26.00  16.18   0.38    0.04    --   46.79 -19.00-180.00  111
 21  \w     32.00  57.08   0.38    0.04    --  104.64 -61.00-150.00   66
 22  \w     39.00 107.02   0.38    0.04    --  104.64 -77.00-120.00  179
 23  \w     34.00 103.16   0.38    0.04    --  104.64 -94.00-180.00  182
 24  \w     31.00  92.56   0.38    0.04    --   46.79-125.00 -30.00  162
 25  \w     37.00  71.20   0.38    0.04    --  104.64-125.00 -30.00   90
 26  \w     76.00 106.78   0.38    0.04    --  104.64-125.00 -30.00   81
 27  \w     55.00 102.50   0.38    0.04    --   46.79-145.00 161.00  125
 28  \w     32.00 120.16   0.38    0.04    --  104.64-145.00 161.00  232
 29  \w     52.00  96.08   0.38    0.04    --  104.64 -94.00 150.00  116
 30  \w    -91.00 -63.64   0.38    0.04    --  -46.79 145.00-145.00   72
 31  \w   -126.00 -84.20   0.38    0.04    -- -102.00 145.00-145.00  110
 32  \w    -87.00 -43.68   0.38    0.04    -- -102.00 142.00  14.71  114
 33  \w   -124.00 -92.08   0.38    0.04    -- -102.00 142.00  14.71   84
 34  \w   -126.00 -92.18   0.38    0.04    -- -102.00 144.00  27.42   89
 35  \w    -97.00 -69.64   0.38    0.04    -- -102.00 125.00  46.00   72
 36  \w   -105.00 -48.00   0.38    0.04    -- -102.00 125.00   0.00  150
 37  \w   -108.00 -60.88   0.38    0.04    -- -102.00 112.00 -11.84  124
 38  \w    -77.00 -50.78   0.38    0.04    --  -46.79 125.00  46.00   69
 39  \w   -107.00 -73.94   0.38    0.04    -- -102.00 107.00 119.43   87
 40  \w    -69.00 -31.00   0.38    0.04    -- -102.00  61.00  60.00  100
 41  \w    -68.00 -30.00   0.38    0.04    -- -102.00  61.00  30.00  100
 42  \w    -66.00 -31.80   0.38    0.04    -- -102.00  61.00   0.00   90
 43  \w    -59.00 -29.74   0.38    0.04    -- -102.00  61.00-120.00   77
 44  \w   -103.00 -29.66   0.38    0.04    -- -102.00  77.00 -90.00  193
 45  \w   -165.00 -89.00   0.38    0.04    -- -102.00 -30.00  30.00  200
 46  \w   -137.00 -74.68   0.38    0.04    -- -102.00-125.00 -30.00  164
 47  \w   -168.00 -74.14   0.38    0.04    -- -102.00-125.00   0.00  247
 48  \w   -109.00 -60.74   0.38    0.04    --  -46.79-145.00 161.00  127
 49  \w   -153.00 -93.72   0.38    0.04    -- -102.00-145.00 161.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0110654000
_diffrn_orient_matrix_UB_12      -0.0033796000
_diffrn_orient_matrix_UB_13      -0.0252852000
_diffrn_orient_matrix_UB_21      0.0343655500
_diffrn_orient_matrix_UB_22      -0.0081588500
_diffrn_orient_matrix_UB_23      -0.0034990000
_diffrn_orient_matrix_UB_31      -0.0038565000
_diffrn_orient_matrix_UB_32      -0.0629371000
_diffrn_orient_matrix_UB_33      0.0017896000
_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  0.0948
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       76
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            484053
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.520
_diffrn_reflns_theta_min         2.081
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
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    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             24105
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4660
_refine_ls_number_reflns         64455
_refine_ls_number_restraints     3588
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+26.3054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                42248
_reflns_number_total             64455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03945b2.cif
_cod_data_source_block           qxg_0722_auto
_cod_depositor_comments
'Adding full bibliography for 7134972--7134974.cif.'
_cod_database_code               7134974
_shelx_shelxl_version_number     2019/3
_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
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All C(H,H,H,H,H,H,H,H,H)
  groups
2. Restrained distances
 C362-C361 = C363-C362 = C409-C363 = C409-C408
 1.54 with sigma of 0.01
 C361-C360 = C360-C359
 1.51 with sigma of 0.01
 C363-C408
 2.515 with sigma of 0.02
 C361-C363
 2.515 with sigma of 0.02
 C361-C359
 2.615 with sigma of 0.02
 C325-C324 \\sim C399-C324
 with sigma of 0.01
3. Restrained planarity
 O35A, C406, C407, C408
 with sigma of 0.01
 O35, C359, C360, C361
 with sigma of 0.01
 C350, O33, C400, C401
 with sigma of 0.01
 C89, C94, N3A, C95A, C96A, C97A, C98A, C99A
 with sigma of 0.01
 N1, C13, C14, C15, C16, C17, C18
 with sigma of 0.01
 N3A, C369, C370, C371, C372, C373, C374
 with sigma of 0.01
 N5, C385, C386, C387, C388, C389, C390
 with sigma of 0.01
 N3, C100, C101, C102, C103, C104, C105
 with sigma of 0.01
 N1, C13A, C14A, C15A, C16A, C17A, C18A
 with sigma of 0.01
 N3A, C375, C376, C377, C378, C379, C380
 with sigma of 0.01
 N5, C187, C188, C189, C190, C191, C192
 with sigma of 0.01
 N1, C19A, C20A, C21A, C22A, C23A, C24A
 with sigma of 0.01
 N3, C106, C107, C108, C109, C110, C111
 with sigma of 0.01
 N1, C19, C20, C21, C22, C23, C24
 with sigma of 0.01
 N5, C193, C194, C195, C196, C197, C198
 with sigma of 0.01
 N5, C391, C392, C393, C394, C395, C396
 with sigma of 0.01
 C89, C94, N3, C95, C96, C97, C98, C99
 with sigma of 0.01
 C285, C281, C282, C284, C280, C283, N7
 with sigma of 0.01
 C279, C275, C276, C278, C274, C277, N7
 with sigma of 0.01
 C432, C428, C429, C431, C427, C430, N7A
 with sigma of 0.01
 C425, C423, C422, C426, C424, C268, C263, N7A
 with sigma of 0.01
 C272, C270, C269, C273, C271, C268, C263, N7
 with sigma of 0.01
 C438, C434, C435, C437, C433, C436, N7A
 with sigma of 0.01
 C271, C269, C268, C272, C270, C273, N7, C263
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O10 \\sim C137 \\sim C138 \\sim C381 \\sim C382 \\sim C439 \\sim C440: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C363 \\sim O35 \\sim C359 \\sim C360 \\sim C361 \\sim C362 \\sim O35A \\sim
C406 \\sim C407 \\sim C408 \\sim C409 \\sim O35B \\sim C416 \\sim C417 \\sim
C418 \\sim C419: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C268 \\sim N7 \\sim C269 \\sim C270 \\sim C271 \\sim C272 \\sim C273 \\sim C274
\\sim C275 \\sim C276 \\sim C277 \\sim C278 \\sim C279 \\sim C280 \\sim C281
\\sim C282 \\sim C283 \\sim C284 \\sim C285 \\sim N7A \\sim C422 \\sim C423
\\sim C424 \\sim C425 \\sim C426 \\sim C427 \\sim C428 \\sim C429 \\sim C430
\\sim C431 \\sim C432 \\sim C433 \\sim C434 \\sim C435 \\sim C436 \\sim C437
\\sim C438: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C355 \\sim C358 \\sim O34 \\sim C354 \\sim C356 \\sim C357 \\sim O34A \\sim
C403 \\sim C404 \\sim C405: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O6 \\sim C74 \\sim C75 \\sim C74A \\sim C75A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N5 \\sim C187 \\sim C188 \\sim C189 \\sim C190 \\sim C191 \\sim C192 \\sim C193
\\sim C194 \\sim C195 \\sim C196 \\sim C197 \\sim C198 \\sim C385 \\sim C386
\\sim C387 \\sim C388 \\sim C389 \\sim C390 \\sim C391 \\sim C392 \\sim C393
\\sim C394 \\sim C395 \\sim C396: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O16 \\sim C172 \\sim C173 \\sim C383 \\sim C384: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C94 \\sim N3 \\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim
C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim
C108 \\sim C109 \\sim C110 \\sim C111 \\sim N3A \\sim C95A \\sim C96A \\sim
C97A \\sim C98A \\sim C99A \\sim C369 \\sim C370 \\sim C371 \\sim C372 \\sim
C373 \\sim C374 \\sim C375 \\sim C376 \\sim C377 \\sim C378 \\sim C379 \\sim
C380: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
N1 \\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 C13A \\sim C14A \\sim C15A
\\sim C16A \\sim C17A \\sim C18A \\sim C19A \\sim C20A \\sim C21A \\sim C22A
\\sim C23A \\sim C24A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O22 \\sim C248 \\sim C249 \\sim C397 \\sim C398: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C324 \\sim C325 \\sim C399: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C350 \\sim C353 \\sim O33 \\sim C349 \\sim C351 \\sim C352 \\sim O33A \\sim
C400 \\sim C401 \\sim C402: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C368 \\sim O36 \\sim C364 \\sim C365 \\sim C366 \\sim C367 \\sim O36A \\sim
C410 \\sim C411 \\sim C412 \\sim C413: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
O21 \\sim C246 \\sim C247 \\sim C414 \\sim C415: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
O13 \\sim C159 \\sim C160 \\sim C420 \\sim C421: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
Uanis(C94) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C96)
\\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C99) \\sim Ueq,
Uanis(C100) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(N3A)
\\sim Ueq, Uanis(C95A) \\sim Ueq, Uanis(C96A) \\sim Ueq, Uanis(C97A) \\sim Ueq,
Uanis(C98A) \\sim Ueq, Uanis(C99A) \\sim Ueq, Uanis(C369) \\sim Ueq,
Uanis(C370) \\sim Ueq, Uanis(C371) \\sim Ueq, Uanis(C372) \\sim Ueq,
Uanis(C373) \\sim Ueq, Uanis(C374) \\sim Ueq, Uanis(C375) \\sim Ueq,
Uanis(C376) \\sim Ueq, Uanis(C377) \\sim Ueq, Uanis(C378) \\sim Ueq,
Uanis(C379) \\sim Ueq, Uanis(C380) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
5. Same fragment restrains
{O6, C74A, C75A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O6, C74, C75}
{N1, C13A, C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A}
sigma for 1-2: 0.01, 1-3: 0.01
as in
{N1, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24}
{O10, C381, C382} sigma for 1-2: 0.01, 1-3: 0.01
{O10, C439, C440} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O10, C137, C138}
{O13, C420, C421} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O13, C159, C160}
{O16, C383, C384} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O16, C172, C173}
{C94, N3A, C95A, C96A, C97A, C98A, C99A, C369, C370, C371, C372, C373, C374,
C375, C376, C377, C378, C379, C380} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C94, N3, C95, C96, C97, C98, C99, C100, C101, C102, C103, C104, C105, C106,
C107, C108, C109, C110, C111}
{O21, C414, C415} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O21, C246, C247}
{O22, C397, C398} sigma for 1-2: 0.01, 1-3: 0.01
as in
{O22, C248, C249}
{N5, C385, C386, C387, C388, C389, C390, C391, C392, C393, C394, C395, C396}
sigma for 1-2: 0.01, 1-3: 0.01
as in
{N5, C187, C188, C189, C190, C191, C192, C193, C194, C195, C196, C197, C198}
{C268, N7A, C422, C423, C424, C425, C426, C427, C428, C429, C430, C431, C432,
C433, C434, C435, C436, C437, C438} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C268, N7, C269, C270, C271, C272, C273, C274, C275, C276, C277, C278, C279,
C280, C281, C282, C283, C284, C285}
{C355, C358, O34A, C403, C404, C405} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C355, C358, O34, C354, C356, C357}
{C363, O35A, C406, C407, C408, C409} sigma for 1-2: 0.01, 1-3: 0.01
{C363, O35B, C416, C417, C418, C419} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C363, O35, C359, C360, C361, C362}
{C368, O36A, C410, C411, C412, C413} sigma for 1-2: 0.01, 1-3: 0.01
as in
{C368, O36, C364, C365, C366, C367}
6. Others
 1*[Sof(H36A)+Sof(H36B)+Sof(H36C)+Sof(O35)+Sof(C359)+Sof(H35A)+Sof(H35B)+
 Sof(H35C)+Sof(C360)+Sof(C361)+Sof(H36J)+Sof(H36K)+Sof(C362)+Sof(H36L)+
 Sof(H36M)]+1*[Sof(H36D)+Sof(H36E)+Sof(H36F)+Sof(O35A)+Sof(C406)+Sof(H40A)+
 Sof(H40B)+Sof(H40C)+Sof(C407)+Sof(C408)+Sof(H40D)+Sof(H40E)+Sof(C409)+
 Sof(H40F)+Sof(H40G)]+1*[Sof(H36G)+Sof(H36H)+Sof(H36I)+Sof(O35B)+Sof(C416)+
 Sof(H41F)+Sof(H41G)+Sof(H41H)+Sof(C417)+Sof(C418)+Sof(H41I)+Sof(H41J)+
 Sof(C419)+Sof(H41K)+Sof(H41L)]=1 with esd of 0
 1*[Sof(C137)+Sof(H13A)+Sof(H13B)+Sof(C138)+Sof(H13C)+Sof(H13D)+Sof(H13E)]+1*
 [Sof(C381)+Sof(H38A)+Sof(H38B)+Sof(C382)+Sof(H38C)+Sof(H38D)+Sof(H38E)]+1*
 [Sof(C439)+Sof(H43A)+Sof(H43B)+Sof(C440)+Sof(H44A)+Sof(H44B)+Sof(H44C)]=1 with
 esd of 0
 Sof(C74A)=Sof(H74C)=Sof(H74D)=Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=1-FVAR(1)
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=FVAR(1)
 Sof(C13A)=Sof(C14A)=Sof(H14K)=Sof(C15A)=Sof(H15J)=Sof(C16A)=Sof(H16K)=
 Sof(C17A)=Sof(H17M)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=
 Sof(C21A)=Sof(H21C)=Sof(C22A)=Sof(H22M)=Sof(C23A)=Sof(H23M)=Sof(C24A)=
 Sof(H24K)=1-FVAR(2)
 Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=
 Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=
 Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=FVAR(2)
 Sof(N3A)=Sof(C95A)=Sof(H95A)=Sof(C96A)=Sof(H96A)=Sof(C97A)=Sof(C98A)=
 Sof(H98A)=Sof(C99A)=Sof(H99A)=Sof(C369)=Sof(C370)=Sof(H370)=Sof(C371)=
 Sof(H371)=Sof(C372)=Sof(H372)=Sof(C373)=Sof(H373)=Sof(C374)=Sof(H374)=
 Sof(C375)=Sof(C376)=Sof(H376)=Sof(C377)=Sof(H377)=Sof(C378)=Sof(H378)=
 Sof(C379)=Sof(H379)=Sof(C380)=Sof(H380)=1-FVAR(3)
 Sof(N3)=Sof(C95)=Sof(H95)=Sof(C96)=Sof(H96)=Sof(C97)=Sof(C98)=Sof(H98)=
 Sof(C99)=Sof(H99)=Sof(C100)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C103)=
 Sof(H103)=Sof(C104)=Sof(H104)=Sof(C105)=Sof(H105)=Sof(C106)=Sof(C107)=
 Sof(H107)=Sof(C108)=Sof(H108)=Sof(C109)=Sof(H109)=Sof(C110)=Sof(H110)=
 Sof(C111)=Sof(H111)=FVAR(3)
 Sof(C137)=Sof(H13A)=Sof(H13B)=Sof(C138)=Sof(H13C)=Sof(H13D)=Sof(H13E)=FVAR(4)
 Sof(C383)=Sof(H38F)=Sof(H38G)=Sof(C384)=Sof(H38H)=Sof(H38I)=Sof(H38J)=1-FVAR(5)
 Sof(C172)=Sof(H17A)=Sof(H17B)=Sof(C173)=Sof(H17C)=Sof(H17D)=Sof(H17E)=FVAR(5)
 Sof(C385)=Sof(C386)=Sof(H386)=Sof(C387)=Sof(H387)=Sof(C388)=Sof(H388)=
 Sof(C389)=Sof(H389)=Sof(C390)=Sof(H390)=Sof(C391)=Sof(C392)=Sof(H392)=
 Sof(C393)=Sof(H393)=Sof(C394)=Sof(H394)=Sof(C395)=Sof(H395)=Sof(C396)=
 Sof(H396)=1-FVAR(6)
 Sof(C187)=Sof(C188)=Sof(H188)=Sof(C189)=Sof(H189)=Sof(C190)=Sof(H190)=
 Sof(C191)=Sof(H191)=Sof(C192)=Sof(H192)=Sof(C193)=Sof(C194)=Sof(H194)=
 Sof(C195)=Sof(H195)=Sof(C196)=Sof(H196)=Sof(C197)=Sof(H197)=Sof(C198)=
 Sof(H198)=FVAR(6)
 Sof(C397)=Sof(H39D)=Sof(H39E)=Sof(C398)=Sof(H39F)=Sof(H39G)=Sof(H39H)=1-FVAR(7)
 Sof(C248)=Sof(H24F)=Sof(H24G)=Sof(C249)=Sof(H24H)=Sof(H24I)=Sof(H24J)=FVAR(7)
 Sof(H32H)=Sof(H32I)=Sof(C399)=Sof(H39A)=Sof(H39B)=Sof(H39C)=1-FVAR(8)
 Sof(H32F)=Sof(H32G)=Sof(C325)=Sof(H32L)=Sof(H32M)=Sof(H32N)=FVAR(8)
 Sof(H35G)=Sof(H35H)=Sof(H35I)=Sof(O33A)=Sof(C400)=Sof(H40H)=Sof(H40I)=
 Sof(H40J)=Sof(C401)=Sof(H40K)=Sof(H40L)=Sof(C402)=Sof(H40M)=Sof(H40N)=1-FVAR(9)
 Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(O33)=Sof(C349)=Sof(H34M)=Sof(H34N)=
 Sof(H34O)=Sof(C351)=Sof(H35J)=Sof(H35K)=Sof(C352)=Sof(H35L)=Sof(H35M)=FVAR(9)
 Sof(H35Q)=Sof(H35R)=Sof(H35S)=Sof(O34A)=Sof(C403)=Sof(H40O)=Sof(H40P)=
 Sof(H40Q)=Sof(C404)=Sof(H40R)=Sof(H40S)=Sof(C405)=Sof(H40T)=Sof(H40U)=1-
 FVAR(10)
 Sof(H35N)=Sof(H35O)=Sof(H35P)=Sof(O34)=Sof(C354)=Sof(H35T)=Sof(H35U)=
 Sof(H35V)=Sof(C356)=Sof(H35W)=Sof(H35X)=Sof(C357)=Sof(H35Y)=Sof(H)=FVAR(10)
 Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(O35)=Sof(C359)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=Sof(C360)=Sof(C361)=Sof(H36J)=Sof(H36K)=Sof(C362)=Sof(H36L)=
 Sof(H36M)=FVAR(11)
 Sof(H36Q)=Sof(H36R)=Sof(H36S)=Sof(O36A)=Sof(C410)=Sof(H41M)=Sof(H41N)=
 Sof(H41O)=Sof(C411)=Sof(C412)=Sof(H41P)=Sof(H41Q)=Sof(C413)=Sof(H41R)=
 Sof(H41S)=1-FVAR(12)
 Sof(H36N)=Sof(H36O)=Sof(H36P)=Sof(O36)=Sof(C364)=Sof(H36T)=Sof(H36U)=
 Sof(H36V)=Sof(C365)=Sof(C366)=Sof(H36W)=Sof(H36X)=Sof(C367)=Sof(H36Y)=Sof(HA)=
 FVAR(12)
 Sof(C414)=Sof(H41A)=Sof(H41B)=Sof(C415)=Sof(H41C)=Sof(H41D)=Sof(H41E)=1-
 FVAR(13)
 Sof(C246)=Sof(H24A)=Sof(H24B)=Sof(C247)=Sof(H24C)=Sof(H24D)=Sof(H24E)=FVAR(13)
 Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(O35A)=Sof(C406)=Sof(H40A)=Sof(H40B)=
 Sof(H40C)=Sof(C407)=Sof(C408)=Sof(H40D)=Sof(H40E)=Sof(C409)=Sof(H40F)=
 Sof(H40G)=FVAR(14)
 Sof(H36G)=Sof(H36H)=Sof(H36I)=Sof(O35B)=Sof(C416)=Sof(H41F)=Sof(H41G)=
 Sof(H41H)=Sof(C417)=Sof(C418)=Sof(H41I)=Sof(H41J)=Sof(C419)=Sof(H41K)=
 Sof(H41L)=FVAR(15)
 Sof(C420)=Sof(H42A)=Sof(H42B)=Sof(C421)=Sof(H42C)=Sof(H42D)=Sof(H42E)=1-
 FVAR(16)
 Sof(C159)=Sof(H15A)=Sof(H15B)=Sof(C160)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(16)
 Sof(N7A)=Sof(C422)=Sof(H422)=Sof(C423)=Sof(H423)=Sof(C424)=Sof(C425)=
 Sof(H425)=Sof(C426)=Sof(H426)=Sof(C427)=Sof(C428)=Sof(H428)=Sof(C429)=
 Sof(H429)=Sof(C430)=Sof(H430)=Sof(C431)=Sof(H431)=Sof(C432)=Sof(H432)=
 Sof(C433)=Sof(C434)=Sof(H434)=Sof(C435)=Sof(H435)=Sof(C436)=Sof(H436)=
 Sof(C437)=Sof(H437)=Sof(C438)=Sof(H438)=1-FVAR(17)
 Sof(N7)=Sof(C269)=Sof(H269)=Sof(C270)=Sof(H270)=Sof(C271)=Sof(C272)=Sof(H272)=
 Sof(C273)=Sof(H273)=Sof(C274)=Sof(C275)=Sof(H275)=Sof(C276)=Sof(H276)=
 Sof(C277)=Sof(H277)=Sof(C278)=Sof(H278)=Sof(C279)=Sof(H279)=Sof(C280)=
 Sof(C281)=Sof(H281)=Sof(C282)=Sof(H282)=Sof(C283)=Sof(H283)=Sof(C284)=
 Sof(H284)=Sof(C285)=Sof(H285)=FVAR(17)
 Sof(C381)=Sof(H38A)=Sof(H38B)=Sof(C382)=Sof(H38C)=Sof(H38D)=Sof(H38E)=FVAR(18)
 Sof(C439)=Sof(H43A)=Sof(H43B)=Sof(C440)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(19)
7.a Riding coordinates:
 C358(H35N,H35O,H35P), C358(H35Q,H35R,H35S), C354(H35T,H35U,H35V), C403(H40O,
 H40P,H40Q)
7.b Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C43(H43C,H43D), C50(H50A,H50B), C52(H52A,H52B), C54(H54A,
 H54B), C61(H61A,H61B), C63(H63A,H63B), C65(H65A,H65B), C72(H72A,H72B),
 C76(H76A,H76B), C83(H83A,H83B), C85(H85A,H85B), C87(H87A,H87B), C137(H13A,
 H13B), C159(H15A,H15B), C172(H17A,H17B), C130(H13F,H13G), C139(H13H,H13I),
 C141(H14D,H14E), C148(H14F,H14G), C150(H15C,H15D), C152(H15H,H15I), C161(H16D,
 H16E), C163(H16I,H16J), C170(H17F,H17G), C174(H17K,H17L), C439(H43A,H43B),
 C246(H24A,H24B), C248(H24F,H24G), C217(H21A,H21B), C224(H22A,H22B), C226(H22F,
 H22G), C228(H22K,H22L), C235(H23A,H23B), C237(H23F,H23G), C239(H23K,H23L),
 C250(H25A,H25B), C257(H25C,H25D), C259(H25H,H25I), C261(H26D,H26E), C304(H30A,
 H30B), C311(H31A,H31B), C313(H31F,H31G), C315(H31K,H31L), C322(H32A,H32B),
 C324(H32F,H32G), C324(H32H,H32I), C326(H32J,H32K), C333(H33A,H33B), C335(H33F,
 H33G), C337(H33K,H33L), C344(H34A,H34B), C346(H34F,H34G), C348(H34K,H34L),
 C351(H35J,H35K), C352(H35L,H35M), C401(H40K,H40L), C402(H40M,H40N), C356(H35W,
 H35X), C357(H35Y,H), C361(H36J,H36K), C362(H36L,H36M), C366(H36W,H36X),
 C367(H36Y,HA), C74A(H74C,H74D), C381(H38A,H38B), C383(H38F,H38G), C420(H42A,
 H42B), C397(H39D,H39E), C414(H41A,H41B), C404(H40R,H40S), C405(H40T,H40U),
 C408(H40D,H40E), C409(H40F,H40G), C418(H41I,H41J), C419(H41K,H41L), C412(H41P,
 H41Q), C413(H41R,H41S)
7.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C3(H3), C6(H6), C8(H8), C9(H9), C11(H11),
 C12(H12), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
 C46(H46), C49(H49), C57(H57), C60(H60), C68(H68), C71(H71), C79(H79), C82(H82),
  C90(H90), C93(H93), C95(H95), C96(H96), C98(H98), C99(H99), C101(H101),
 C102(H102), C103(H103), C104(H104), C105(H105), C107(H107), C108(H108),
 C109(H109), C110(H110), C111(H111), C113(H113), C114(H114), C116(H116),
 C117(H117), C119(H119), C120(H120), C121(H121), C122(H122), C123(H123),
 C125(H125), C126(H126), C127(H127), C128(H128), C129(H129), C133(H133),
 C136(H136), C144(H144), C147(H147), C155(H155), C158(H158), C166(H166),
 C169(H169), C188(H188), C189(H189), C190(H190), C191(H191), C192(H192),
 C194(H194), C195(H195), C196(H196), C197(H197), C198(H198), C177(H177),
 C180(H180), C182(H182), C183(H183), C185(H185), C186(H186), C200(H200),
 C201(H201), C203(H203), C204(H204), C206(H206), C207(H207), C208(H208),
 C209(H209), C210(H210), C212(H212), C213(H213), C214(H214), C215(H215),
 C216(H216), C220(H220), C223(H223), C231(H231), C234(H234), C242(H242),
 C245(H245), C253(H253), C256(H256), C264(H264), C267(H267), C269(H269),
 C270(H270), C272(H272), C273(H273), C275(H275), C276(H276), C277(H277),
 C278(H278), C279(H279), C281(H281), C282(H282), C283(H283), C284(H284),
 C285(H285), C287(H287), C288(H288), C290(H290), C291(H291), C293(H293),
 C294(H294), C295(H295), C296(H296), C297(H297), C299(H299), C300(H300),
 C301(H301), C302(H302), C303(H303), C307(H307), C310(H310), C318(H318),
 C321(H321), C329(H329), C332(H332), C340(H340), C343(H343), C14A(H14K),
 C15A(H15J), C16A(H16K), C17A(H17M), C18A(H18A), C20A(H20A), C21A(H21C),
 C22A(H22M), C23A(H23M), C24A(H24K), C95A(H95A), C96A(H96A), C98A(H98A),
 C99A(H99A), C370(H370), C371(H371), C372(H372), C373(H373), C374(H374),
 C376(H376), C377(H377), C378(H378), C379(H379), C380(H380), C386(H386),
 C387(H387), C388(H388), C389(H389), C390(H390), C392(H392), C393(H393),
 C394(H394), C395(H395), C396(H396), C422(H422), C423(H423), C425(H425),
 C426(H426), C428(H428), C429(H429), C430(H430), C431(H431), C432(H432),
 C434(H434), C435(H435), C436(H436), C437(H437), C438(H438)
7.d Idealised Me refined as rotating group:
 C75(H75A,H75B,H75C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C62(H62A,H62B,
 H62C), C64(H64A,H64B,H64C), C73(H73A,H73B,H73C), C84(H84A,H84B,H84C), C86(H86A,
 H86B,H86C), C138(H13C,H13D,H13E), C160(H16A,H16B,H16C), C173(H17C,H17D,H17E),
 C140(H14A,H14B,H14C), C149(H14H,H14I,H14J), C151(H15E,H15F,H15G), C162(H16F,
 H16G,H16H), C171(H17H,H17I,H17J), C440(H44A,H44B,H44C), C247(H24C,H24D,H24E),
 C249(H24H,H24I,H24J), C225(H22C,H22D,H22E), C227(H22H,H22I,H22J), C236(H23C,
 H23D,H23E), C238(H23H,H23I,H23J), C258(H25E,H25F,H25G), C260(H26A,H26B,H26C),
 C312(H31C,H31D,H31E), C314(H31H,H31I,H31J), C323(H32C,H32D,H32E), C334(H33C,
 H33D,H33E), C336(H33H,H33I,H33J), C345(H34C,H34D,H34E), C347(H34H,H34I,H34J),
 C325(H32L,H32M,H32N), C399(H39A,H39B,H39C), C353(H35D,H35E,H35F), C353(H35G,
 H35H,H35I), C349(H34M,H34N,H34O), C400(H40H,H40I,H40J), C363(H36A,H36B,H36C),
 C363(H36D,H36E,H36F), C363(H36G,H36H,H36I), C359(H35A,H35B,H35C), C368(H36N,
 H36O,H36P), C368(H36Q,H36R,H36S), C364(H36T,H36U,H36V), C75A(H75D,H75E,H75F),
 C382(H38C,H38D,H38E), C384(H38H,H38I,H38J), C421(H42C,H42D,H42E), C398(H39F,
 H39G,H39H), C415(H41C,H41D,H41E), C406(H40A,H40B,H40C), C416(H41F,H41G,H41H),
 C410(H41M,H41N,H41O)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 560 electrons were 
found in a volume of 3412\%A^3^ in 5 voids per unit cell. 
This is consistent with the presence of 
0.203[C3H6O], 0.336[C3H6O] per Asymmetric Unit 
which account for 552 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82189
_shelx_hkl_checksum              2476
_shelx_fab_checksum              32762
_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 1.606
_oxdiff_exptl_absorpt_empirical_full_min 0.594