Statistical optimization of guest uptake in crystalline sponges: grading structural outcomes.
Carroll, Robert C.; Coles, Simon J.; IUCrJ 11 (2024) –; doi:10.1107/S2052252524004871

data_1571837
_publ_section_title
;
 Statistical optimization of guest uptake in crystalline sponges: grading
 structural outcomes.
;
_journal_coeditor_code           LT5068
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524004871
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety
'C108 H72 I18 N36 Zn9, 0.715(C15 H16 O3), 0.61(C6 H12)'
_chemical_formula_sum            'C122.39 H90.76 I18 N36 O2.14 Zn9'
_chemical_formula_weight         4972.58
_chemical_name_systematic
; (2',6'-dimethoxy-[1,1'-biphenyl]-2-yl)methanol
 (absorbed in crystalline sponge)
;
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.702(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   78.142(4)
_cell_length_b                   14.9754(2)
_cell_length_c                   41.6691(13)
_cell_measurement_reflns_used    12474
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.8710
_cell_measurement_theta_min      2.2730
_cell_volume                     48064(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.956
_diffrn_measured_fraction_theta_max 0.954
_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    -99.00 -73.80   0.15    0.20    --  -46.11 159.00-122.00  168
  2  \w    -76.00 -50.95   0.15    0.20    --  -46.11 118.00  85.00  167
  3  \w     41.00  75.95   0.15    0.20    --   46.11-118.00  -1.00  233
  4  \w     60.00 115.05   0.15    0.20    --   46.11 159.00-122.00  367
  5  \w     66.00 108.00   0.15    1.00    --  101.75-118.00  -1.00  280
  6  \w     45.00  88.05   0.15    1.00    --  101.75-159.00-154.00  287
  7  \w   -151.00-106.00   0.15    1.00    -- -103.00-118.00  -1.00  300
  8  \w    -99.00 -60.00   0.15    1.00    -- -103.00 159.00-122.00  260
  9  \w   -135.00-105.00   0.15    1.00    -- -103.00 159.00-122.00  200
 10  \w    -92.00 -66.95   0.15    1.00    -- -103.00 118.00  85.00  167
 11  \w    -19.00   8.00   0.15    0.20    --  -46.11  19.00  90.00  180
 12  \w     -4.00  24.05   0.15    0.20    --  -46.11  19.00-180.00  187
 13  \w    -14.00  27.10   0.15    0.20    --  -46.11  19.00 -90.00  274
 14  \w    -19.00  15.05   0.15    0.20    --  -46.11  19.00-120.00  227
 15  \w    -19.00  26.00   0.15    0.20    --   46.11 -19.00  90.00  300
 16  \w     80.00 105.05   0.15    0.20    --   46.11-159.00-154.00  167
 17  \w     44.00  73.10   0.15    1.00    --  101.75 -61.00 -30.00  194
 18  \w    144.00 172.95   0.15    1.00    --  101.75  45.00   0.00  193
 19  \w     32.00  73.25   0.15    1.00    --  101.75 -61.00-150.00  275
 20  \w     51.00 104.10   0.15    1.00    --  101.75 -94.00-180.00  354
 21  \w     89.00 129.20   0.15    1.00    --  101.75  45.00   0.00  268
 22  \w     29.00  86.00   0.15    1.00    --  101.75 -94.00   0.00  380
 23  \w    -63.00 -37.95   0.15    1.00    -- -103.00  61.00 -90.00  167
 24  \w   -171.00 -90.00   0.15    1.00    -- -103.00 -15.00  60.00  540
 25  \w   -154.00 -92.95   0.15    1.00    -- -103.00 -30.00 -90.00  407
 26  \w   -108.00 -54.90   0.15    1.00    -- -103.00 125.00-120.00  354
 27  \w    -62.00 -32.90   0.15    1.00    -- -103.00  61.00  90.00  194
 28  \w    -67.00 -35.95   0.15    1.00    -- -103.00  61.00  60.00  207
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details
'Rigaku Oxford Difffraction, UG2 \k goniometer'
_diffrn_measurement_device_type
; Rigaku 007HF equipped with Varimax confocal mirrors and a 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      0.0133427000
_diffrn_orient_matrix_UB_12      0.0058263000
_diffrn_orient_matrix_UB_13      -0.0232667000
_diffrn_orient_matrix_UB_21      -0.0148902000
_diffrn_orient_matrix_UB_22      0.0098312000
_diffrn_orient_matrix_UB_23      -0.0291407000
_diffrn_orient_matrix_UB_31      0.0006615000
_diffrn_orient_matrix_UB_32      0.1021996000
_diffrn_orient_matrix_UB_33      0.0041368000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       93
_diffrn_reflns_limit_h_min       -94
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            158843
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         2.261
_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    19.427
_exptl_absorpt_correction_T_max  0.389
_exptl_absorpt_correction_T_min  0.080
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             18546
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.504
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2102
_refine_ls_number_reflns         41978
_refine_ls_number_restraints     569
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1697
_refine_ls_R_factor_gt           0.1401
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1165P)^2^+2897.3889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3562
_refine_ls_wR_factor_ref         0.3743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28784
_reflns_number_total             41978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_1_24a
_cod_database_code               1571837
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.389
_shelx_estimated_absorpt_t_min   0.071
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C8A-C7A = C9A-C8A = C9A-C10A = C11A-C10A = C12A-C11A = C7A-C12A
 1.39 with sigma of 0.02
 O2A-C8A = O3A-C12A
 1.37 with sigma of 0.02
 O3A-C15A = O2A-C14A = O1A-C13A
 1.43 with sigma of 0.02
 C808-C807 = C808-C809 = C807-C812 = C812-C811 = C811-C810 = C810-C809
 1.54 with sigma of 0.02
 C806-C805 = C806-C801 = C805-C804 = C804-C803 = C803-C802 = C802-C801
 1.54 with sigma of 0.02
 C8A-C10A = C9A-C11A
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.02
 C808-C812 = C808-C810 = C807-C811 = C812-C810 = C811-C809
 2.54 with sigma of 0.04
 C806-C804 = C806-C802 = C805-C803 = C804-C802 = C803-C801
 2.54 with sigma of 0.04
 I315-Zn38 \\sim I415-Zn48
 with sigma of 0.02
 C2A-C1A \\sim C3A-C2A \\sim C4A-C3A \\sim C5A-C4A \\sim C6A-C5A \\sim C6A-C1A
 with sigma of 0.02
 I316-Zn38 \\sim I416-Zn48
 with sigma of 0.02
 C1A-C3A \\sim C2A-C4A \\sim C3A-C5A \\sim C4A-C6A \\sim C5A-C1A \\sim C6A-C2A
 with sigma of 0.04
 Zn38-N329 \\sim Zn48-N329
 with sigma of 0.02
 I315-I316 \\sim I415-I416
 with sigma of 0.04
 I315-N329 \\sim I415-N329
 with sigma of 0.04
 I316-N329 \\sim I416-N329
 with sigma of 0.04
 C7A-C4A \\sim C5A-C13A
 with sigma of 0.02
 I312-Zn36 \\sim I412-Zn46
 with sigma of 0.02
 I311-Zn36 \\sim I411-Zn46
 with sigma of 0.02
 Zn36-N323 \\sim Zn46-N323
 with sigma of 0.02
 I312-I311 \\sim I412-I411
 with sigma of 0.04
 I312-N323 \\sim I412-N323
 with sigma of 0.04
 I311-N323 \\sim I411-N323
 with sigma of 0.04
 I318-Zn39 \\sim I418-Zn49
 with sigma of 0.02
 I317-Zn39 \\sim I417-Zn49
 with sigma of 0.02
 Zn39-N331 \\sim Zn49-N331
 with sigma of 0.02
 Zn39-N330 \\sim Zn49-N330
 with sigma of 0.02
 I318-I317 \\sim I418-I417
 with sigma of 0.04
 I318-N331 \\sim I418-N331
 with sigma of 0.04
 I318-N330 \\sim I418-N330
 with sigma of 0.04
 I317-N331 \\sim I417-N331
 with sigma of 0.04
 I317-N330 \\sim I417-N330
 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 Zn33-N307 \\sim Zn43-N307
 with sigma of 0.02
 Zn33-N306 \\sim Zn43-N306
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N307 \\sim I406-N307
 with sigma of 0.04
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 I305-N307 \\sim I405-N307
 with sigma of 0.04
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I309-Zn35 \\sim I409-Zn45
 with sigma of 0.02
 I310-Zn35 \\sim I410-Zn45
 with sigma of 0.02
 Zn35-N319 \\sim Zn45-N319
 with sigma of 0.02
 Zn35-N318 \\sim Zn45-N318
 with sigma of 0.02
 I309-I310 \\sim I409-I410
 with sigma of 0.04
 I309-N319 \\sim I409-N319
 with sigma of 0.04
 I309-N318 \\sim I409-N318
 with sigma of 0.04
 I310-N319 \\sim I410-N319
 with sigma of 0.04
 I310-N318 \\sim I410-N318
 with sigma of 0.04
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 Zn32-N305 \\sim Zn42-N305
 with sigma of 0.02
 I304-I303 \\sim I404-I403
 with sigma of 0.04
 I304-N305 \\sim I404-N305
 with sigma of 0.04
 I303-N305 \\sim I403-N305
 with sigma of 0.04
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I301-I302 \\sim I401-I402
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 I307-Zn34 \\sim I407-Zn44
 with sigma of 0.02
 Zn34-N313 \\sim Zn44-N313
 with sigma of 0.02
 Zn34-N312 \\sim Zn44-N312
 with sigma of 0.02
 I308-I307 \\sim I408-I407
 with sigma of 0.04
 I308-N313 \\sim I408-N313
 with sigma of 0.04
 I308-N312 \\sim I408-N312
 with sigma of 0.04
 I307-N313 \\sim I407-N313
 with sigma of 0.04
 I307-N312 \\sim I407-N312
 with sigma of 0.04
 I314-Zn37 \\sim I414-Zn47
 with sigma of 0.02
 I313-Zn37 \\sim I413-Zn47
 with sigma of 0.02
 Zn37-N325 \\sim Zn47-N325
 with sigma of 0.02
 Zn37-N324 \\sim Zn47-N324
 with sigma of 0.02
 I314-I313 \\sim I414-I413
 with sigma of 0.04
 I314-N325 \\sim I414-N325
 with sigma of 0.04
 I314-N324 \\sim I414-N324
 with sigma of 0.04
 I313-N325 \\sim I413-N325
 with sigma of 0.04
 I313-N324 \\sim I413-N324
 with sigma of 0.04
 I514-Zn57 \\sim I513-Zn57
 with sigma of 0.02
 C808-C807 \\sim C807-C812 \\sim C812-C811 \\sim C811-C810 \\sim C810-C809
\\sim C809-C808
 with sigma of 0.02
 C808-C810 \\sim C812-C810 \\sim C807-C809 \\sim C807-C811 \\sim C811-C809
\\sim C808-C812
 with sigma of 0.04
 C806-C805 \\sim C805-C804 \\sim C804-C803 \\sim C803-C802 \\sim C802-C801
\\sim C801-C806
 with sigma of 0.02
 C806-C802 \\sim C804-C802 \\sim C805-C801 \\sim C805-C803 \\sim C803-C801
\\sim C806-C804
 with sigma of 0.04
3. Restrained planarity
 O2A, C8A, C7A, C12A, O3A
 with sigma of 0.1
 C8A, C12A, C11A, C9A, C7A, C10A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7A \\sim O3A \\sim C12A \\sim C15A \\sim C11A \\sim C10A \\sim C4A \\sim C8A
\\sim C9A \\sim C5A \\sim C3A \\sim O2A \\sim C6A \\sim C13A \\sim C2A \\sim
C14A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
I318 \\sim I317 \\sim Zn39 \\sim I418 \\sim Zn49 \\sim I417: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C808 \\sim C807 \\sim C812 \\sim C811 \\sim C810 \\sim C809: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C806 \\sim C805 \\sim C804 \\sim C803 \\sim C802 \\sim C801: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N335 \\sim C399 \\sim C403 \\sim C402 \\sim C401 \\sim C400: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn34) = Uanis(Zn44)
Uanis(Zn48) = Uanis(Zn38)
5. Rigid body (RIGU) restrains
 I318, I317, Zn39, I418, Zn49, I417
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N335, C399, C403, C402, C401, C400
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C808, C807, C812, C811, C810, C809
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C806, C805, C804, C803, C802, C801
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(I301)+Sof(I302)+Sof(Zn31)]+1*[Sof(I401)+Sof(Zn41)+Sof(I402)]+1*
 [Sof(I502)+Sof(I501)+Sof(Zn51)]+1*[Sof(I601)+Sof(I602)+Sof(Zn61)]=1 with esd
 of 0.00001
 Sof(I404)=Sof(Zn42)=Sof(I403)=1-FVAR(1)
 Sof(I304)=Sof(I303)=Sof(Zn32)=FVAR(1)
 Sof(I407)=Sof(I408)=Sof(Zn44)=1-FVAR(2)
 Sof(I308)=Sof(I307)=Sof(Zn34)=FVAR(2)
 Sof(I301)=Sof(I302)=Sof(Zn31)=FVAR(3)
 Sof(I401)=Sof(Zn41)=Sof(I402)=FVAR(4)
 Sof(I502)=Sof(I501)=Sof(Zn51)=FVAR(5)
 Sof(I416)=Sof(Zn48)=Sof(I415)=1-FVAR(6)
 Sof(I315)=Sof(I316)=Sof(Zn38)=FVAR(6)
 Sof(I601)=Sof(I602)=Sof(Zn61)=FVAR(7)
 Fixed Sof: I312(0.5005) I309(0.47055) I310(0.47055) I314(0.62239)
 I311(0.5005) I313(0.62239) I306(0.57758) I318(0.59) I317(0.59) I305(0.57758)
 Zn39(0.59) Zn36(0.5005) Zn35(0.47055) Zn33(0.57758) Zn37(0.62239) O3A(0.71518)
 O1A(0.71518) H1A(0.71518) O2A(0.71518) C3A(0.71518) H3A(0.71518) C2A(0.71518)
 H2A(0.71518) C4A(0.71518) C6A(0.71518) H6A(0.71518) C1A(0.71518) H1AA(0.71518)
 C12A(0.71518) C11A(0.71518) H11A(0.71518) C5A(0.71518) C14A(0.71518)
 H14A(0.71518) H14B(0.71518) H14C(0.71518) C7A(0.71518) C9A(0.71518)
 H9A(0.71518) C8A(0.71518) C13A(0.71518) H13A(0.71518) H13B(0.71518)
 I412(0.44535) Zn46(0.44535) I411(0.44535) I418(0.41) Zn49(0.41) I417(0.41)
 I406(0.39283) Zn43(0.39283) I405(0.39283) I410(0.48376) Zn45(0.48376)
 I409(0.48376) I512(0.05416) Zn56(0.05416) I511(0.05416) I20(0.02961)
 Zn26(0.02961) I36(0.02961) I509(0.04569) I510(0.04569) Zn55(0.04569)
 C10A(0.71518) H10A(0.71518) I413(0.31585) Zn47(0.31585) I414(0.31585)
 I513(0.06176) I514(0.06176) Zn57(0.06176) C15A(0.71518) H15A(0.71518)
 H15B(0.71518) H15C(0.71518) C808(0.26168) H80A(0.26168) H80B(0.26168)
 C807(0.26168) H80C(0.26168) H80D(0.26168) C812(0.26168) H81A(0.26168)
 H81B(0.26168) C811(0.26168) H81C(0.26168) H81D(0.26168) C810(0.26168)
 H81E(0.26168) H81F(0.26168) C809(0.26168) H80E(0.26168) H80F(0.26168)
 C806(0.34842) H80G(0.34842) H80H(0.34842) C805(0.34842) H80I(0.34842)
 H80J(0.34842) C804(0.34842) H80K(0.34842) H80L(0.34842) C803(0.34842)
 H80M(0.34842) H80N(0.34842) C802(0.34842) H80O(0.34842) H80P(0.34842)
 C801(0.34842) H80Q(0.34842) H80R(0.34842)
 Fixed Uiso: I512(0.08) Zn56(0.08) I511(0.08) I502(0.08) I501(0.08) Zn51(0.08)
 I20(0.08) Zn26(0.08) I36(0.08) I509(0.08) I510(0.08) Zn55(0.08) I513(0.08)
 I514(0.08) Zn57(0.08) I601(0.08) I602(0.08) Zn61(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C808(H80A,H80B), C807(H80C,H80D), C812(H81A,H81B), C811(H81C,
 H81D), C810(H81E,H81F), C809(H80E,H80F), C806(H80G,H80H), C805(H80I,H80J),
 C804(H80K,H80L), C803(H80M,H80N), C802(H80O,H80P), C801(H80Q,H80R)
7.b Aromatic/amide H refined with riding coordinates:
 C405(H405), C385(H385), C390(H390), C404(H404), C395(H395), C384(H384),
 C347(H347), C394(H394), C373(H373), C349(H349), C304(H304), C340(H340),
 C348(H348), C355(H355), C365(H365), C317(H317), C356(H356), C305(H305),
 C354(H354), C376(H376), C328(H328), C302(H302), C341(H341), C366(H366),
 C314(H314), C320(H320), C319(H319), C346(H346), C374(H374), C367(H367),
 C377(H377), C337(H337), C389(H389), C312(H312), C351(H351), C383(H383),
 C353(H353), C364(H364), C315(H315), C311(H311), C318(H318), C3A(H3A),
 C301(H301), C338(H338), C382(H382), C310(H310), C408(H408), C350(H350),
 C407(H407), C387(H387), C329(H329), C386(H386), C372(H372), C2A(H2A),
 C369(H369), C313(H313), C403(H403), C391(H391), C359(H359), C392(H392),
 C358(H358), C335(H335), C6A(H6A), C1A(H1AA), C330(H330), C402(H402),
 C401(H401), C371(H371), C368(H368), C333(H333), C336(H336), C400(H400),
 C331(H331), C11A(H11A), C332(H332), C323(H323), C9A(H9A), C322(H322),
 C10A(H10A)
7.c Tetrahedral OH refined with riding coordinates:
 O1A(H1A)
7.d Idealised Me refined with everything fixed:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C)
;
_shelx_res_checksum              52685
_shelx_hkl_checksum              35036
_olex2_date_sample_data_collection 2022-02-01
_olex2_date_sample_submission    2022-02-01
_olex2_submission_original_sample_id 25_1_24a
_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 2.299
_oxdiff_exptl_absorpt_empirical_full_min 0.409