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_1571825
_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, 0.633(C15 H16 O3)'
_chemical_formula_sum            'C117.5 H82.13 I18 N36 O1.9 Zn9'
_chemical_formula_weight         4901.17
_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                 99.853(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   78.3675(18)
_cell_length_b                   14.9505(2)
_cell_length_c                   41.6842(7)
_cell_measurement_reflns_used    15771
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.4770
_cell_measurement_theta_min      2.6130
_cell_volume                     48118.2(15)
_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 0.990
_diffrn_measured_fraction_theta_max 0.989
_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    -75.00 -48.90   0.15    1.30    -- -103.00  70.00-137.00  174
  2  \w   -132.00 -84.90   0.15    1.30    -- -103.00 -70.00  90.00  314
  3  \w    -60.00 -33.90   0.15    1.30    -- -103.00  61.00-150.00  174
  4  \w    -64.00 -38.95   0.15    1.30    -- -103.00  61.00  90.00  167
  5  \w   -174.00-102.00   0.15    1.30    -- -103.00 -61.00-180.00  480
  6  \w   -104.00 -38.00   0.15    1.30    -- -103.00  77.00 -30.00  440
  7  \w   -100.00 -55.90   0.15    1.30    -- -103.00 125.00-150.00  294
  8  \w    -58.00 -31.90   0.15    1.30    -- -103.00  61.00  60.00  174
  9  \w     35.00  60.05   0.15    1.30    --  101.75 -70.00  90.00  167
 10  \w     83.00 138.20   0.15    1.30    --  101.75  70.00-137.00  368
 11  \w     93.00 163.20   0.15    1.30    --  101.75  45.00  60.00  468
 12  \w     29.00  72.05   0.15    1.30    --  101.75 -61.00 -60.00  287
 13  \w     30.00  55.05   0.15    1.30    --  101.75-125.00  90.00  167
 14  \w     30.00  55.05   0.15    1.30    --  101.75 -61.00-120.00  167
 15  \w     89.00 172.10   0.15    1.30    --  101.75  61.00   0.00  554
 16  \w     68.00 107.00   0.15    1.30    --  101.75-125.00  90.00  260
 17  \w     29.00  59.00   0.15    1.30    --  101.75 -61.00 -90.00  200
 18  \w     43.00  69.10   0.15    1.30    --  101.75 -61.00-180.00  174
 19  \w    -23.00   2.05   0.15    0.30    --  -46.48  70.00-137.00  167
 20  \w    -23.00  52.00   0.15    0.30    --   46.48 -70.00  90.00  500
 21  \w     28.00 110.05   0.15    0.30    --   46.48  70.00-137.00  547
 22  \w    -71.00 -20.00   0.15    0.30    --  -46.48 125.00-120.00  340
 23  \w    -24.00  20.10   0.15    0.30    --  -46.48  19.00-120.00  294
 24  \w     -9.00  17.10   0.15    0.30    --  -46.48  37.00  30.00  174
 25  \w    -27.00   2.10   0.15    0.30    --   46.48 -19.00 -60.00  194
;
_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      0.0145281000
_diffrn_orient_matrix_UB_12      0.0033071000
_diffrn_orient_matrix_UB_13      -0.0206363000
_diffrn_orient_matrix_UB_21      -0.0062902000
_diffrn_orient_matrix_UB_22      0.0930353000
_diffrn_orient_matrix_UB_23      -0.0128368000
_diffrn_orient_matrix_UB_31      0.0121520000
_diffrn_orient_matrix_UB_32      0.0441254000
_diffrn_orient_matrix_UB_33      0.0285713000
_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_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       94
_diffrn_reflns_limit_h_min       -94
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            148464
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         2.152
_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    19.396
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.096
_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    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             18226
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.637
_refine_diff_density_min         -1.754
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1906
_refine_ls_number_reflns         43548
_refine_ls_number_restraints     1000
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1937
_refine_ls_R_factor_gt           0.1670
_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^)+(0.1569P)^2^+4146.2759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4218
_refine_ls_wR_factor_ref         0.4374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31204
_reflns_number_total             43548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_1_96a
_cod_original_formula_sum        'C117.50 H82.13 I18 N36 O1.90 Zn9'
_cod_database_code               1571825
_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   0.137
_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
 C2A-C1A = C3A-C2A = C4A-C3A = C5A-C4A = C6A-C5A = C6A-C1A
 1.39 with sigma of 0.02
 C8A-C7A = C9A-C8A = C9A-C10A = C11A-C10A = C12A-C11A = C7A-C12A
 1.39 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 O1A-C13A = O2A-C14A = O3A-C15A
 1.43 with sigma of 0.02
 C1A-C3A = C3A-C5A = C6A-C2A
 2.4 with sigma of 0.04
 C7A-C9A = C8A-C10A = C9A-C11A = C10A-C12A = C11A-C7A = C12A-C8A
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.04
 I408-Zn44 \\sim I308-Zn34
 with sigma of 0.02
 I407-Zn44 \\sim I307-Zn34
 with sigma of 0.02
 Zn33-N313 \\sim Zn43-N313
 with sigma of 0.02
 Zn44-N317 \\sim Zn34-N317
 with sigma of 0.02
 I408-I407 \\sim I308-I307
 with sigma of 0.04
 I408-N317 \\sim I308-N317
 with sigma of 0.04
 I407-N317 \\sim I307-N317
 with sigma of 0.04
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I306-N313 \\sim I406-N313
 with sigma of 0.04
 I305-N313 \\sim I405-N313
 with sigma of 0.04
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 Zn36-N325 \\sim Zn46-N325
 with sigma of 0.02
 I301-I302 \\sim I401-I402
 with sigma of 0.04
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I411-N325 \\sim I311-N325
 with sigma of 0.04
 I412-N325 \\sim I312-N325
 with sigma of 0.04
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 I304-I303 \\sim I404-I403
 with sigma of 0.04
 I304-N307 \\sim I404-N307
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I303-N307 \\sim I403-N307
 with sigma of 0.04
 I303-N306 \\sim I403-N306
 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-N329 \\sim Zn47-N329
 with sigma of 0.02
 I314-I313 \\sim I414-I413
 with sigma of 0.04
 I314-N329 \\sim I414-N329
 with sigma of 0.04
 I313-N329 \\sim I413-N329
 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-N312 \\sim Zn43-N312
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I315-Zn38 \\sim I415-Zn48
 with sigma of 0.02
 I316-Zn38 \\sim I416-Zn48
 with sigma of 0.02
 Zn38-N330 \\sim Zn48-N330
 with sigma of 0.02
 Zn38-N331 \\sim Zn48-N331
 with sigma of 0.02
 I315-I316 \\sim I415-I416
 with sigma of 0.04
 I315-N330 \\sim I415-N330
 with sigma of 0.04
 I315-N331 \\sim I415-N331
 with sigma of 0.04
 I316-N330 \\sim I416-N330
 with sigma of 0.04
 I316-N331 \\sim I416-N331
 with sigma of 0.04
 I411-Zn36 \\sim I311-Zn46
 with sigma of 0.02
 I412-Zn36 \\sim I312-Zn46
 with sigma of 0.02
 Zn36-N324 \\sim Zn46-N324
 with sigma of 0.02
 I411-I412 \\sim I311-I312
 with sigma of 0.04
 I411-N324 \\sim I311-N324
 with sigma of 0.04
 I412-N324 \\sim I312-N324
 with sigma of 0.04
 I507-Zn54 \\sim I508-Zn54
 with sigma of 0.02
 I516-Zn58 \\sim I515-Zn58
 with sigma of 0.02
 N335-C502 \\sim N335-C402
 with sigma of 0.02
 C399-C503 \\sim C399-C403
 with sigma of 0.02
 C502-C503 \\sim C402-C403
 with sigma of 0.02
 N335-C503 \\sim N335-C403
 with sigma of 0.04
 C399-C502 \\sim C399-C402
 with sigma of 0.04
 N323-C466 \\sim N323-C366
 with sigma of 0.02
 C363-C467 \\sim C363-C367
 with sigma of 0.02
 C467-C466 \\sim C367-C366
 with sigma of 0.02
 N323-C467 \\sim N323-C367
 with sigma of 0.04
 C363-C466 \\sim C363-C366
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C5A \\sim O1A \\sim C13A \\sim C4A \\sim C6A \\sim C7A \\sim C3A \\sim C1A
\\sim C8A \\sim C12A \\sim C2A \\sim O2A \\sim C9A \\sim O3A \\sim C11A \\sim
C14A \\sim C10A \\sim C15A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
I408 \\sim I308 \\sim I307 \\sim I407 \\sim Zn44 \\sim Zn34: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I301 \\sim I302 \\sim Zn31 \\sim I401 \\sim Zn41 \\sim I402: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N331 \\sim C393 \\sim C392 \\sim C391 \\sim C395 \\sim C394: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N306 \\sim C316 \\sim C315 \\sim C314 \\sim C318 \\sim C317: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N305 \\sim C309 \\sim C311 \\sim C310 \\sim C313 \\sim C312: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N311 \\sim C327 \\sim C329 \\sim C328 \\sim C331 \\sim C330: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C302 \\sim C301 \\sim N301 \\sim C305 \\sim C304 \\sim C303: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N303 \\sim C306 \\sim N302 \\sim C308 \\sim N304 \\sim C307: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N314 \\sim N315 \\sim N316 \\sim C342 \\sim C343 \\sim C344: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N310 \\sim N309 \\sim N308 \\sim C324 \\sim C325 \\sim C326: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N313 \\sim C338 \\sim C339 \\sim C341 \\sim C337 \\sim C340: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn44) = Uanis(Zn34)
Uanis(C403) = Uanis(C503) = Uanis(C502) = Uanis(C402)
Uanis(Zn41) = Uanis(Zn31)
Uanis(I308) = Uanis(I408)
Uanis(C467) = Uanis(C367)
Uanis(C466) = Uanis(C366)
4. Rigid body (RIGU) restrains
 I408, I308, I307, I407, Zn44, Zn34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I301, I302, Zn31, I401, Zn41, I402
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N331, C393, C392, C391, C395, C394
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N306, C316, C315, C314, C318, C317
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N305, C309, C311, C310, C313, C312
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N311, C327, C329, C328, C331, C330
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C302, C301, N301, C305, C304, C303
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N303, C306, N302, C308, N304, C307
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N310, N309, N308, C324, C325, C326
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N313, C338, C339, C341, C337, C340
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N326, N327, N328, C380, C378, C379
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N318, C352, C354, C351, C353, C350
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N314, N315, N316, C342, C343, C344
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(I315)+Sof(I316)+Sof(Zn38)]+1*[Sof(I416)+Sof(Zn48)+Sof(I415)]+1*
 [Sof(Zn58)+Sof(I515)+Sof(I516)]=1 with esd of 0.00001
 Sof(I404)=Sof(Zn42)=Sof(I403)=1-FVAR(1)
 Sof(I304)=Sof(I303)=Sof(Zn32)=FVAR(1)
 Sof(I414)=Sof(Zn47)=Sof(I413)=1-FVAR(2)
 Sof(I314)=Sof(I313)=Sof(Zn37)=FVAR(2)
 Sof(I401)=Sof(Zn41)=Sof(I402)=1-FVAR(3)
 Sof(I301)=Sof(I302)=Sof(Zn31)=FVAR(3)
 Sof(I405)=Sof(Zn43)=Sof(I406)=1-FVAR(4)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(4)
 Sof(I312)=Sof(Zn46)=Sof(I311)=1-FVAR(5)
 Sof(I411)=Sof(I412)=Sof(Zn36)=FVAR(5)
 Sof(I315)=Sof(I316)=Sof(Zn38)=FVAR(6)
 Sof(I416)=Sof(Zn48)=Sof(I415)=FVAR(7)
 Sof(Zn58)=Sof(I515)=Sof(I516)=FVAR(8)
 Sof(C403)=Sof(H403)=Sof(C402)=Sof(H402)=1-FVAR(9)
 Sof(C502)=Sof(H502)=Sof(C503)=Sof(H503)=FVAR(9)
 Fixed Sof: I408(0.40426) I407(0.40426) Zn44(0.40426) O1A(0.63301)
 H1A(0.63301) C7A(0.63301) O2A(0.63301) C4A(0.63301) C3A(0.63301) H3A(0.63301)
 C2A(0.63301) H2A(0.63301) C5A(0.63301) O3A(0.63301) C8A(0.63301) C467(0.16395)
 H467(0.16395) C11A(0.63301) H11A(0.63301) C466(0.16395) H466(0.16395)
 C1A(0.63301) H1AA(0.63301) C12A(0.63301) C9A(0.63301) H9A(0.63301)
 C14A(0.63301) H14A(0.63301) H14B(0.63301) H14C(0.63301) C10A(0.63301)
 H10A(0.63301) C13A(0.63301) H13A(0.63301) H13B(0.63301) C6A(0.63301)
 H6A(0.63301) C15A(0.63301) H15A(0.63301) H15B(0.63301) H15C(0.63301)
 I307(0.55596) Zn34(0.55596) I308(0.55596) I507(0.03978) I508(0.03978)
 Zn54(0.03978) C367(0.83605) H367(0.83605) C366(0.83605) H366(0.83605)
 Fixed Uiso: I507(0.08) I508(0.08) Zn54(0.08) Zn58(0.08) I515(0.08) I516(0.08)
6.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B)
6.b Aromatic/amide H refined with riding coordinates:
 C356(H356), C338(H338), C304(H304), C354(H354), C315(H315), C341(H341),
 C364(H364), C355(H355), C329(H329), C305(H305), C320(H320), C389(H389),
 C348(H348), C351(H351), C353(H353), C382(H382), C337(H337), C401(H401),
 C319(H319), C311(H311), C314(H314), C323(H323), C365(H365), C340(H340),
 C359(H359), C400(H400), C349(H349), C350(H350), C310(H310), C346(H346),
 C318(H318), C328(H328), C317(H317), C335(H335), C376(H376), C390(H390),
 C385(H385), C368(H368), C358(H358), C313(H313), C302(H302), C312(H312),
 C333(H333), C404(H404), C377(H377), C384(H384), C3A(H3A), C2A(H2A), C331(H331),
  C347(H347), C374(H374), C392(H392), C336(H336), C369(H369), C383(H383),
 C373(H373), C322(H322), C467(H467), C387(H387), C11A(H11A), C301(H301),
 C372(H372), C408(H408), C371(H371), C407(H407), C466(H466), C502(H502),
 C391(H391), C395(H395), C332(H332), C330(H330), C394(H394), C386(H386),
 C1A(H1AA), C405(H405), C503(H503), C9A(H9A), C10A(H10A), C6A(H6A), C403(H403),
 C402(H402), C367(H367), C366(H366)
6.c Tetrahedral OH refined with riding coordinates:
 O1A(H1A)
6.d Idealised Me refined with everything fixed:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C)
;
_shelx_res_checksum              56957
_shelx_hkl_checksum              21730
_olex2_date_sample_data_collection 2022-03-15
_olex2_date_sample_submission    2022-03-15
_olex2_submission_original_sample_id 4_1_96a
_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 4.011
_oxdiff_exptl_absorpt_empirical_full_min 0.328