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_1571860
_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
'C72 H48 I12 N24 Zn6, 0.697(C15 H16 O3), 0.431(C6 H12)'
_chemical_formula_sum            'C85.04 H63.33 I12 N24 O2.09 Zn6'
_chemical_formula_weight         3369.96
_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           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-07
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.01.24 svn.r2f8d729c for OlexSys, GUI svn.r6923)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.931(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.5355(9)
_cell_length_b                   14.9866(4)
_cell_length_c                   34.4588(11)
_cell_measurement_reflns_used    13421
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.9660
_cell_measurement_theta_min      2.6090
_cell_volume                     15933.8(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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_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 0.993
_diffrn_measured_fraction_theta_max 0.992
_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   -133.00 -75.00   0.50    6.00    -- -103.00-129.00  56.00  116
  2  \w   -133.00 -87.00   0.50    6.00    -- -103.00 -61.00-120.00   92
  3  \w   -173.00-140.00   0.50    6.00    -- -103.00 -61.00-120.00   66
  4  \w   -172.00 -94.00   0.50    6.00    -- -103.00 -77.00 -30.00  156
  5  \w    -66.00 -36.00   0.50    6.00    -- -103.00  61.00   0.00   60
  6  \w   -119.00 -92.00   0.50    6.00    -- -103.00 -30.00-120.00   54
  7  \w    -98.00 -73.00   0.50    6.00    -- -103.00 129.00 129.00   50
  8  \w   -100.00 -75.00   0.50    6.00    -- -103.00 139.00 -57.00   50
  9  \w     75.00 120.00   0.50    6.00    --  101.75-139.00-116.00   90
 10  \w     36.00  61.00   0.50    6.00    --  101.75-129.00  56.00   50
 11  \w    102.00 127.00   0.50    6.00    --  101.75 129.00 129.00   50
 12  \w     63.00 115.00   0.50    6.00    --  101.75-129.00  56.00  104
 13  \w    112.00 174.00   0.50    6.00    --  101.75  45.00 -60.00  124
 14  \w     30.00  72.00   0.50    6.00    --  101.75 -61.00-180.00   84
 15  \w     47.00 107.00   0.50    6.00    --  101.75-104.00 122.36  120
 16  \w     32.00  57.00   0.50    6.00    --  101.75 -61.00-150.00   50
 17  \w     32.00 109.00   0.50    6.00    --  101.75-125.00 120.00  154
 18  \w     29.00  69.00   0.50    6.00    --  101.75 -77.00-150.00   80
 19  \w     73.00 105.00   0.50    6.00    --  101.75 -94.00  30.00   64
 20  \w     30.00  80.00   0.50    6.00    --  101.75 -77.00  30.00  100
 21  \w   -117.00 -90.00   0.50    1.25    --  -46.26-139.00-116.00   54
 22  \w    -63.00 -27.00   0.50    1.25    --  -46.26 129.00 129.00   72
 23  \w    -92.00 -67.00   0.50    1.25    --  -46.26 129.00 129.00   50
 24  \w     27.00  95.00   0.50    1.25    --   46.26-129.00  56.00  136
 25  \w    -24.00  28.00   0.50    1.25    --  -46.26  19.00-150.00  104
 26  \w    -21.00  10.00   0.50    1.25    --  -46.26  19.00-180.00   62
 27  \w    -12.00  21.00   0.50    1.25    --  -46.26  19.00-120.00   66
 28  \w     25.00 117.00   0.50    1.25    --   46.26  77.00 120.00  184
;
_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      -0.0201589000
_diffrn_orient_matrix_UB_12      0.0056290000
_diffrn_orient_matrix_UB_13      0.0370293000
_diffrn_orient_matrix_UB_21      0.0005841000
_diffrn_orient_matrix_UB_22      -0.1025708000
_diffrn_orient_matrix_UB_23      0.0030323000
_diffrn_orient_matrix_UB_31      0.0456678000
_diffrn_orient_matrix_UB_32      0.0038250000
_diffrn_orient_matrix_UB_33      0.0266125000
_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  0.0565
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            114741
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         2.132
_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    19.546
_exptl_absorpt_correction_T_max  0.345
_exptl_absorpt_correction_T_min  0.061
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             6297
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1473
_refine_ls_number_reflns         28949
_refine_ls_number_restraints     350
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.1220
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1333P)^2^+267.6933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3350
_refine_ls_wR_factor_ref         0.3509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21213
_reflns_number_total             28949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_1_24c
_cod_database_code               1571860
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)3'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.272
_shelx_estimated_absorpt_t_min   0.094
_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
 C4B-C7B
 1.51 with sigma of 0.02
 O2B-C8B = O3B-C12B
 1.37 with sigma of 0.02
 O2A-C8A = O3A-C12A
 1.37 with sigma of 0.02
 O1B-C13B = O2B-C14B = O3B-C15B
 1.43 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 O1A-C13A = O2A-C14A = O3A-C15A
 1.43 with sigma of 0.02
 C13B-C5B
 1.51 with sigma of 0.02
 C807-C808 = C807-C812 = C808-C809 = C809-C810 = C810-C811 = C811-C812
 1.54 with sigma of 0.02
 C805-C806 = C805-C804 = C806-C801 = C801-C802 = C802-C803 = C803-C804
 1.54 with sigma of 0.02
 C5B-O1B
 2.4 with sigma of 0.04
 C8B-C14B
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.02
 C4A-C13A
 2.5 with sigma of 0.04
 C4B-C13B = C13B-C6B
 2.5 with sigma of 0.04
 C7B-O3B = C11B-O3B
 2.4 with sigma of 0.04
 C807-C809 = C807-C811 = C808-C810 = C809-C811 = C810-C812
 2.54 with sigma of 0.04
 C805-C801 = C805-C803 = C806-C802 = C801-C803 = C802-C804
 2.54 with sigma of 0.04
 C7A-C8A \\sim C9A-C8A \\sim C10A-C9A \\sim C10A-C11A \\sim C12A-C11A \\sim
C12A-C7A
 with sigma of 0.02
 C5A-C4A \\sim C4A-C3A \\sim C2A-C3A \\sim C2A-C1A \\sim C6A-C1A \\sim C6A-C5A
 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
 C10A-C12A \\sim C11A-C7A \\sim C12A-C8A
 with sigma of 0.04
 C12B-C4B \\sim C4B-C8B
 with sigma of 0.04
 C5B-C7B \\sim C7B-C3B
 with sigma of 0.04
 C807-C808 \\sim C808-C809 \\sim C809-C810 \\sim C810-C811 \\sim C811-C812
\\sim C812-C807
 with sigma of 0.02
 C807-C811 \\sim C809-C811 \\sim C808-C812 \\sim C808-C810 \\sim C810-C812
\\sim C807-C809
 with sigma of 0.04
 Zn46-N324 \\sim Zn36-N324
 with sigma of 0.02
 I412-Zn46 \\sim I312-Zn36
 with sigma of 0.02
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I411-Zn46 \\sim I311-Zn36
 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
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I301-I302 \\sim I401-I402
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I306-N311 \\sim I406-N311
 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I305-N311 \\sim I405-N311
 with sigma of 0.04
 Zn33-N311 \\sim Zn43-N311
 with sigma of 0.02
 I408-I407 \\sim I308-I307
 with sigma of 0.04
 I407-N313 \\sim I307-N313
 with sigma of 0.04
 I408-N313 \\sim I308-N313
 with sigma of 0.04
 I408-Zn44 \\sim I308-Zn34
 with sigma of 0.02
 I408-N312 \\sim I308-N312
 with sigma of 0.04
 I407-Zn44 \\sim I307-Zn34
 with sigma of 0.02
 I407-N312 \\sim I307-N312
 with sigma of 0.04
 Zn44-N312 \\sim Zn34-N312
 with sigma of 0.02
 Zn44-N313 \\sim Zn34-N313
 with sigma of 0.02
 I411-N324 \\sim I311-N324
 with sigma of 0.04
 I412-I411 \\sim I312-I311
 with sigma of 0.04
 I412-N324 \\sim I312-N324
 with sigma of 0.04
 I309-N318 \\sim I409-N318
 with sigma of 0.04
 I310-N318 \\sim I410-N318
 with sigma of 0.04
 I310-I309 \\sim I410-I409
 with sigma of 0.04
 Zn35-N318 \\sim Zn45-N318
 with sigma of 0.02
 I310-C355 \\sim I410-C355
 with sigma of 0.04
 Zn35-C355 \\sim Zn45-C355
 with sigma of 0.02
 I309-C355 \\sim I409-C355
 with sigma of 0.04
 I310-Zn35 \\sim I410-Zn45
 with sigma of 0.02
 I309-Zn35 \\sim I409-Zn45
 with sigma of 0.02
 I01-N307 \\sim I303-N307
 with sigma of 0.04
 I08-N306 \\sim I304-N306
 with sigma of 0.04
 I01-I08 \\sim I303-I304
 with sigma of 0.04
 I08-Zn52 \\sim I304-Zn32
 with sigma of 0.02
 I01-N306 \\sim I303-N306
 with sigma of 0.04
 Zn52-N306 \\sim Zn32-N306
 with sigma of 0.02
 Zn52-N307 \\sim Zn32-N307
 with sigma of 0.02
 I08-N307 \\sim I304-N307
 with sigma of 0.04
 I01-Zn52 \\sim I303-Zn32
 with sigma of 0.02
 Zn53-N311 \\sim Zn43-N311
 with sigma of 0.02
 I31-Zn53 \\sim I406-Zn43
 with sigma of 0.02
 N311-C429 \\sim N311-C329
 with sigma of 0.02
 C327-C428 \\sim C327-C328
 with sigma of 0.02
 C428-C429 \\sim C328-C329
 with sigma of 0.02
 N311-C428 \\sim N311-C328
 with sigma of 0.04
 C327-C429 \\sim C327-C329
 with sigma of 0.04
 N323-C365 \\sim N323-C464
 with sigma of 0.02
 C363-C364 \\sim C363-C465
 with sigma of 0.02
 C365-C364 \\sim C464-C465
 with sigma of 0.02
 N323-C364 \\sim N323-C465
 with sigma of 0.04
 C363-C365 \\sim C363-C464
 with sigma of 0.04
 I306-Zn33 \\sim I31-Zn53
 with sigma of 0.02
 I3-Zn53 \\sim I405-Zn43
 with sigma of 0.02
 C805-C806 \\sim C806-C801 \\sim C801-C802 \\sim C802-C803 \\sim C803-C804
\\sim C804-C805
 with sigma of 0.02
 C805-C803 \\sim C801-C803 \\sim C806-C804 \\sim C806-C802 \\sim C802-C804
\\sim C805-C801
 with sigma of 0.04
3. Restrained planarity
 C7B, C8B, C9B, O2B
 with sigma of 0.1
 C4B, C5B, C6B, C13B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7A \\sim O2A \\sim C8A \\sim C14A \\sim C9A \\sim C12A \\sim C4A \\sim C10A
\\sim O3A \\sim C11A \\sim C3A \\sim C5A \\sim C15A \\sim C2A \\sim C6A \\sim
C13A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C807 \\sim C808 \\sim C809 \\sim C810 \\sim C811 \\sim C812: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C805 \\sim C806 \\sim C801 \\sim C802 \\sim C803 \\sim C804: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Zn33 \\sim Zn43: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C365) = Uanis(C464) = Uanis(C465) = Uanis(C364)
Uanis(C428) = Uanis(C429) = Uanis(C329) = Uanis(C328)
5. Rigid body (RIGU) restrains
 C807, C808, C809, C810, C811, C812
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C805, C806, C801, C802, C803, C804
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(I305)+Sof(I306)+Sof(Zn33)]+1*[Sof(I405)+Sof(Zn43)+Sof(I406)]+1*
 [Sof(I3)+Sof(I31)+Sof(Zn53)]=1 with esd of 0.00001
 Sof(I401)=Sof(Zn41)=Sof(I402)=1-FVAR(1)
 Sof(I301)=Sof(I302)=Sof(Zn31)=FVAR(1)
 Sof(I311)=Sof(Zn36)=Sof(I312)=1-FVAR(2)
 Sof(I412)=Sof(I411)=Sof(Zn46)=FVAR(2)
 Sof(I410)=Sof(Zn45)=Sof(I409)=1-FVAR(3)
 Sof(I310)=Sof(I309)=Sof(Zn35)=FVAR(3)
 Sof(I305)=Sof(I306)=Sof(Zn33)=FVAR(4)
 Sof(I405)=Sof(Zn43)=Sof(I406)=FVAR(5)
 Sof(I3)=Sof(I31)=Sof(Zn53)=FVAR(6)
 Sof(C328)=Sof(H328)=Sof(C329)=Sof(H329)=1-FVAR(7)
 Sof(C428)=Sof(H428)=Sof(C429)=Sof(H429)=FVAR(7)
 Sof(C464)=Sof(H464)=Sof(C465)=Sof(H465)=1-FVAR(8)
 Sof(C365)=Sof(H365)=Sof(C364)=Sof(H364)=FVAR(8)
 Fixed Sof: I01(0.21006) I408(0.39494) I407(0.39494) I08(0.21006)
 Zn44(0.39494) Zn52(0.21006) O2A(0.54192) O3A(0.54192) O1A(0.54192)
 H1AA(0.54192) C7A(0.54192) C8A(0.54192) C9A(0.54192) H9A(0.54192)
 C10A(0.54192) H10A(0.54192) C11A(0.54192) H11A(0.54192) C12A(0.54192)
 C4A(0.54192) C3A(0.54192) H3A(0.54192) C2A(0.54192) H2A(0.54192) C1A(0.54192)
 H1A(0.54192) C6A(0.54192) H6A(0.54192) C5A(0.54192) C14A(0.54192)
 H14A(0.54192) H14B(0.54192) H14C(0.54192) C13A(0.54192) H13A(0.54192)
 H13B(0.54192) C15A(0.54192) H15A(0.54192) H15B(0.54192) H15C(0.54192)
 I307(0.55174) Zn34(0.55174) I308(0.55174) I303(0.51025) Zn32(0.51025)
 I304(0.51025) I404(0.27969) I403(0.27969) Zn42(0.27969) I4(0.05333)
 I10(0.05333) Zn54(0.05333) C4B(0.15535) C3B(0.15535) H3B(0.15535) C2B(0.15535)
 H2B(0.15535) C1B(0.15535) H1B(0.15535) C6B(0.15535) H6B(0.15535) C5B(0.15535)
 C7B(0.15535) C12B(0.15535) C11B(0.15535) H11B(0.15535) C10B(0.15535)
 H10B(0.15535) C9B(0.15535) H9B(0.15535) C8B(0.15535) O3B(0.15535) O1B(0.15535)
 H1BA(0.15535) C13B(0.15535) H13C(0.15535) H13D(0.15535) C805(0.19835)
 H80A(0.19835) H80B(0.19835) C806(0.19835) H80C(0.19835) H80D(0.19835)
 C801(0.19835) H80E(0.19835) H80F(0.19835) C802(0.19835) H80G(0.19835)
 H80H(0.19835) C803(0.19835) H80I(0.19835) H80J(0.19835) C804(0.19835)
 H80K(0.19835) H80L(0.19835) C807(0.23249) H80N(0.23249) H80M(0.23249)
 C808(0.23249) H80O(0.23249) H80P(0.23249) C809(0.23249) H80Q(0.23249)
 H80R(0.23249) C810(0.23249) H81A(0.23249) H81B(0.23249) C811(0.23249)
 H81C(0.23249) H81D(0.23249) C812(0.23249) H81E(0.23249) H81F(0.23249)
 C14B(0.15535) H14D(0.15535) H14E(0.15535) H14F(0.15535) C15B(0.15535)
 H15D(0.15535) H15E(0.15535) H15F(0.15535) O2B(0.15535)
 Fixed Uiso: I3(0.08) I31(0.08) Zn53(0.08) I4(0.08) I10(0.08) Zn54(0.08)
 C4B(0.08) C3B(0.08) C2B(0.08) C1B(0.08) C6B(0.08) C5B(0.08) C7B(0.08)
 C12B(0.08) C11B(0.08) C10B(0.08) C9B(0.08) C8B(0.08) O3B(0.08) O1B(0.08)
 C13B(0.08) C805(0.08) C806(0.08) C801(0.08) C802(0.08) C803(0.08) C804(0.08)
 C807(0.08) C808(0.08) C809(0.08) C810(0.08) C811(0.08) C812(0.08) C14B(0.08)
 C15B(0.08) O2B(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13B(H13C,H13D), C805(H80A,H80B), C806(H80C,H80D), C801(H80E,
 H80F), C802(H80G,H80H), C803(H80I,H80J), C804(H80K,H80L), C807(H80N,H80M),
 C808(H80O,H80P), C809(H80Q,H80R), C810(H81A,H81B), C811(H81C,H81D), C812(H81E,
 H81F)
7.b Aromatic/amide H refined with riding coordinates:
 C355(H355), C338(H338), C301(H301), C346(H346), C310(H310), C335(H335),
 C347(H347), C354(H354), C371(H371), C353(H353), C304(H304), C331(H331),
 C312(H312), C367(H367), C337(H337), C302(H302), C314(H314), C305(H305),
 C336(H336), C356(H356), C350(H350), C372(H372), C318(H318), C349(H349),
 C340(H340), C348(H348), C323(H323), C332(H332), C341(H341), C322(H322),
 C333(H333), C351(H351), C317(H317), C366(H366), C365(H365), C364(H364),
 C315(H315), C330(H330), C313(H313), C359(H359), C311(H311), C368(H368),
 C358(H358), C319(H319), C9A(H9A), C10A(H10A), C11A(H11A), C369(H369),
 C320(H320), C3A(H3A), C2A(H2A), C1A(H1A), C6A(H6A), C428(H428), C429(H429),
 C328(H328), C329(H329), C464(H464), C465(H465), C3B(H3B), C2B(H2B), C1B(H1B),
 C6B(H6B), C11B(H11B), C10B(H10B), C9B(H9B)
7.c Fitted hexagon refined as free rotating group:
 C4B(C3B,C2B,C1B,C6B,C5B), C7B(C12B,C11B,C10B,C9B,C8B)
7.d Tetrahedral OH refined with riding coordinates:
 O1B(H1BA)
7.e Idealised Me refined with everything fixed:
 C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F)
7.f Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C)
7.g Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA)
;
_shelx_res_checksum              57123
_shelx_hkl_checksum              97533
_olex2_date_sample_data_collection 2023-02-02
_olex2_date_sample_submission    2023-02-02
_olex2_submission_original_sample_id 50_1_24c
_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 2.621
_oxdiff_exptl_absorpt_empirical_full_min 0.440