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_1571871
_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, 0.787(C15 H16 O3), 0.258(C6 H12)'
_chemical_formula_sum            'C85.35 H63.69 I12 N24 O2.36 Zn6'
_chemical_formula_weight         3378.30
_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             2024-01-22
_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                 101.732(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.4790(8)
_cell_length_b                   15.0233(3)
_cell_length_c                   34.2503(6)
_cell_measurement_reflns_used    27841
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.4040
_cell_measurement_theta_min      2.9210
_cell_volume                     15859.2(6)
_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      100.00(10)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix Arc-100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     70.00  96.00   0.50    3.00    --   83.36-171.00-101.00   52
  2  \w     30.00  90.00   0.50    3.00    --   83.36-114.00  40.00  120
  3  \w     93.00 118.00   0.50    3.00    --   83.36 114.00 130.00   50
  4  \w    109.00 143.00   0.50    3.00    --   83.36 171.00 -87.00   68
  5  \w     12.00  37.00   0.50    3.00    --   83.36 -37.00-120.00   50
  6  \w     12.00  37.00   0.50    3.00    --   83.36 -37.00 -90.00   50
  7  \w     23.00  59.00   0.50    3.00    --   83.36 -57.00  60.00   72
  8  \w     17.00  42.00   0.50    3.00    --   83.36 -37.00 -60.00   50
  9  \w     15.00  41.00   0.50    3.00    --   83.36 -37.00  30.00   52
 10  \w     12.00  37.00   0.50    3.00    --   83.36 -37.00 -30.00   50
 11  \w     48.00  93.00   0.50    3.00    --   83.36 -77.00  30.00   90
 12  \w     17.00  62.00   0.50    3.00    --   83.36 -57.00 120.00   90
 13  \w     67.00 110.00   0.50    3.00    --   83.36-125.00 150.00   86
 14  \w     17.00  58.00   0.50    3.00    --   83.36 -57.00  90.00   82
 15  \w     32.00  58.00   0.50    3.00    --   83.36-125.00 150.00   52
 16  \w     22.00  67.00   0.50    3.00    --   83.36 -57.00  30.00   90
 17  \w     75.00 102.00   0.50    3.00    --   83.36-125.00-120.00   54
 18  \w     75.00 105.00   0.50    3.00    --   83.36  57.00 -60.00   60
 19  \w    116.00 150.00   0.50    3.00    --   83.36  57.00 -60.00   68
 20  \w     27.00  76.00   0.50    3.00    --   83.36-125.00  30.00   98
 21  \w     32.00  59.00   0.50    3.00    --   83.36-125.00-120.00   54
 22  \w     94.00 121.00   0.50    3.00    --   83.36  77.00-150.00   54
 23  \w     17.00  42.00   0.50    3.00    --   83.36 -37.00-180.00   50
 24  \w     67.00 105.00   0.50    3.00    --   83.36-125.00  90.00   76
 25  \w     16.00  41.00   0.50    3.00    --   83.36 -57.00 150.00   50
 26  \w     16.00  43.00   0.50    3.00    --   83.36 -37.00-150.00   54
 27  \w   -108.00 -48.00   0.50    3.00    --  -79.36 114.00 130.00  120
 28  \w   -118.00 -93.00   0.50    3.00    --  -79.36-171.00-101.00   50
 29  \w   -140.00 -95.00   0.50    3.00    --  -79.36-114.00  40.00   90
 30  \w    -39.00  -9.00   0.50    3.00    --  -79.36  37.00  60.00   60
 31  \w    -40.00 -11.00   0.50    3.00    --  -79.36  37.00 120.00   58
 32  \w    -35.00 -10.00   0.50    3.00    --  -79.36  37.00  90.00   50
 33  \w   -114.00 -47.00   0.50    0.75    --  -55.06-171.00-101.00  134
 34  \w    -76.00 -51.00   0.50    0.75    --  -55.06 114.00 130.00   50
 35  \w     47.00  74.00   0.50    0.75    --   51.56-114.00  40.00   54
 36  \w     58.00  83.00   0.50    0.75    --   51.56 171.00 -87.00   50
 37  \w    -17.00  26.00   0.50    0.75    --   51.56 -19.00-180.00   86
 38  \w    -16.00  27.00   0.50    0.75    --   51.56 -19.00  90.00   86
 39  \w    -11.00  23.00   0.50    0.75    --   51.56 -19.00  60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
; Rigaku 007HF diffractometer equipped with Arc)Sec VHF Varimax confocal
 mirrors and a UG2 goniometer and HyPix Arc-100 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      0.0497218000
_diffrn_orient_matrix_UB_12      -0.0080520000
_diffrn_orient_matrix_UB_13      0.0062526000
_diffrn_orient_matrix_UB_21      -0.0044698000
_diffrn_orient_matrix_UB_22      -0.1008164000
_diffrn_orient_matrix_UB_23      -0.0080042000
_diffrn_orient_matrix_UB_31      -0.0027307000
_diffrn_orient_matrix_UB_32      0.0168520000
_diffrn_orient_matrix_UB_33      -0.0448052000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Arc)Sec VHF Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            157903
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.135
_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    19.641
_exptl_absorpt_correction_T_max  0.366
_exptl_absorpt_correction_T_min  0.032
_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    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             6315
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.329
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1576
_refine_ls_number_reflns         28931
_refine_ls_number_restraints     669
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.1149
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1938P)^2^+161.8441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3535
_refine_ls_wR_factor_ref         0.3774
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20059
_reflns_number_total             28931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_10_24b
_cod_database_code               1571871
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     9300-04
_shelx_estimated_absorpt_t_max   0.385
_shelx_estimated_absorpt_t_min   0.055
_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
 O2A-C14A = O1A-C13A = O3A-C15A
 1.43 with sigma of 0.02
 O1B-C13B = O3B-C15B = O2B-C14B
 1.43 with sigma of 0.02
 C803-C804 = C803-C802 = C804-C805 = C805-C806 = C806-C801 = C801-C802
 1.54 with sigma of 0.02
 C8B-C7B = C8B-C9B = C10B-C9B = C10B-C11B = C12B-C11B = C12B-C7B
 1.39 with sigma of 0.02
 C5B-C13B
 1.51 with sigma of 0.02
 C4B-C7B
 1.5 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 O2B-C8B = O3B-C12B
 1.37 with sigma of 0.02
 C5B-O1B
 2.4 with sigma of 0.04
 C12A-C15A
 2.4 with sigma of 0.04
 C8B-C14B = C12B-C15B
 2.4 with sigma of 0.04
 C803-C805 = C803-C801 = C804-C806 = C805-C801 = C806-C802
 2.54 with sigma of 0.04
 C7B-C9B = C8B-C10B = C9B-C11B = C10B-C12B = C11B-C7B = C12B-C8B
 2.4 with sigma of 0.04
 C4B-C13B = C13B-C6B
 2.5 with sigma of 0.04
 C7B-O2B = C7B-O3B
 2.35 with sigma of 0.04
 C2A-C1A \\sim C2A-C3A \\sim C4A-C3A \\sim C5A-C4A \\sim C6A-C5A \\sim C6A-C1A
 with sigma of 0.02
 C803-C804 \\sim C804-C805 \\sim C805-C806 \\sim C806-C801 \\sim C801-C802
\\sim C802-C803
 with sigma of 0.02
 C8A-C7A \\sim C9A-C8A \\sim C10A-C9A \\sim C11A-C10A \\sim C11A-C12A \\sim
C12A-C7A
 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
 C7A-C9A \\sim C8A-C10A \\sim C11A-C7A \\sim C12A-C8A
 with sigma of 0.04
 C803-C801 \\sim C805-C801 \\sim C804-C802 \\sim C804-C806 \\sim C806-C802
\\sim C803-C805
 with sigma of 0.04
 C12B-C4B \\sim C4B-C8B
 with sigma of 0.04
 C1A-C4A \\sim C2A-C5A \\sim C3A-C6A
 with sigma of 0.04
 C3B-C7B \\sim C7B-C5B
 with sigma of 0.04
 O2A-C8A \\sim O3A-C12A
 with sigma of 0.02
 I410-Zn45 \\sim I310-Zn35
 with sigma of 0.02
 I409-Zn45 \\sim I309-Zn35
 with sigma of 0.02
 Zn45-N319 \\sim Zn35-N319
 with sigma of 0.02
 Zn45-N318 \\sim Zn35-N318
 with sigma of 0.02
 I410-I409 \\sim I310-I309
 with sigma of 0.04
 I410-N319 \\sim I310-N319
 with sigma of 0.04
 I410-N318 \\sim I310-N318
 with sigma of 0.04
 I409-N319 \\sim I309-N319
 with sigma of 0.04
 I409-N318 \\sim I309-N318
 with sigma of 0.04
 I404-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 Zn42-N305 \\sim Zn32-N305
 with sigma of 0.02
 I404-I403 \\sim I304-I303
 with sigma of 0.04
 I404-N305 \\sim I304-N305
 with sigma of 0.04
 I403-N305 \\sim I303-N305
 with sigma of 0.04
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 Zn43-N307 \\sim Zn33-N307
 with sigma of 0.02
 Zn43-N306 \\sim Zn33-N306
 with sigma of 0.02
 I405-I406 \\sim I305-I306
 with sigma of 0.04
 I405-N307 \\sim I305-N307
 with sigma of 0.04
 I405-N306 \\sim I305-N306
 with sigma of 0.04
 I406-N307 \\sim I306-N307
 with sigma of 0.04
 I406-N306 \\sim I306-N306
 with sigma of 0.04
 I307-Zn34 \\sim I407-Zn44
 with sigma of 0.02
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 Zn34-N312 \\sim Zn44-N312
 with sigma of 0.02
 Zn34-N313 \\sim Zn44-N313
 with sigma of 0.02
 I307-I308 \\sim I407-I408
 with sigma of 0.04
 I307-N312 \\sim I407-N312
 with sigma of 0.04
 I307-N313 \\sim I407-N313
 with sigma of 0.04
 I308-N312 \\sim I408-N312
 with sigma of 0.04
 I308-N313 \\sim I408-N313
 with sigma of 0.04
 I401-Zn41 \\sim I301-Zn31
 with sigma of 0.02
 I402-Zn41 \\sim I302-Zn31
 with sigma of 0.02
 Zn41-N301 \\sim Zn31-N301
 with sigma of 0.02
 I401-I402 \\sim I301-I302
 with sigma of 0.04
 I401-N301 \\sim I301-N301
 with sigma of 0.04
 I402-N301 \\sim I302-N301
 with sigma of 0.04
 I510-Zn55 \\sim I410-Zn45
 with sigma of 0.02
 I509-Zn55 \\sim I309-Zn35
 with sigma of 0.02
 I506-Zn53 \\sim I505-Zn53
 with sigma of 0.02
 Zn55-N319 \\sim Zn55-N318
 with sigma of 0.02
3. Restrained planarity
 C9B, C11B, C7B, C12B, C8B, C10B
 with sigma of 0.1
 O2B, C8B, C7B, C12B, O3B
 with sigma of 0.1
 C6A, C5A, C4A, C13A
 with sigma of 0.1
 C4B, C5B, C6B, C13B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4A \\sim O2A \\sim C8A \\sim C14A \\sim C7A \\sim C9A \\sim C12A \\sim C10A
\\sim C3A \\sim C5A \\sim O3A \\sim C11A \\sim C2A \\sim C6A \\sim C13A \\sim
C15A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C803 \\sim C804 \\sim C805 \\sim C806 \\sim C801 \\sim C802: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C4B \\sim C3B \\sim C5B \\sim C7B \\sim C2B \\sim C6B \\sim C13B \\sim C12B
\\sim C8B \\sim C1B \\sim O1B \\sim O3B \\sim C11B \\sim C9B \\sim O2B \\sim
C15B \\sim C10B \\sim C14B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N317 \\sim C345 \\sim C349 \\sim C348 \\sim C347 \\sim C346: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I311 \\sim Zn36 \\sim I312 \\sim I411 \\sim Zn46 \\sim I412: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C803, C804, C805, C806, C801, C802
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4B, C3B, C5B, C7B, C2B, C6B, C13B, C12B, C8B, C1B, O1B, O3B, C11B, C9B, O2B,
 C15B, C10B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(I410)+Sof(I409)+Sof(Zn45)]+1*[Sof(I309)+Sof(Zn35)+Sof(I310)]+1*
 [Sof(I510)+Sof(I509)+Sof(Zn55)]=1 with esd of 0.00001
 Sof(I410)=Sof(I409)=Sof(Zn45)=FVAR(1)
 Sof(I309)=Sof(Zn35)=Sof(I310)=FVAR(2)
 Sof(I510)=Sof(I509)=Sof(Zn55)=FVAR(3)
 Fixed Sof: I405(0.46846) I404(0.21682) I401(0.48034) I402(0.48034)
 I307(0.53522) I406(0.46846) I403(0.21682) I308(0.53522) Zn43(0.46846)
 Zn42(0.21682) Zn41(0.48034) Zn34(0.53522) O2A(0.60767) O3A(0.60767)
 O1A(0.60767) H1A(0.60767) C7A(0.60767) C3A(0.60767) H3A(0.60767) C8A(0.60767)
 C9A(0.60767) H9A(0.60767) C4A(0.60767) C1A(0.60767) H1AA(0.60767) C2A(0.60767)
 H2A(0.60767) C10A(0.60767) H10A(0.60767) C12A(0.60767) C11A(0.60767)
 H11A(0.60767) C5A(0.60767) C6A(0.60767) H6A(0.60767) C13A(0.60767)
 H13A(0.60767) H13B(0.60767) C15A(0.60767) H15A(0.60767) H15B(0.60767)
 H15C(0.60767) C14A(0.60767) H14A(0.60767) H14B(0.60767) H14C(0.60767)
 I304(0.78318) Zn32(0.78318) I303(0.78318) I305(0.4949) Zn33(0.4949)
 I306(0.4949) I407(0.46478) Zn44(0.46478) I408(0.46478) I311(0.63535)
 Zn36(0.63535) I312(0.63535) I301(0.51966) Zn31(0.51966) I302(0.51966)
 I411(0.36464) Zn46(0.36464) I412(0.36464) I505(0.03665) Zn53(0.03665)
 I506(0.03665) C4B(0.17927) C3B(0.17927) H3B(0.17927) C2B(0.17927) H2B(0.17927)
 C1B(0.17927) H1B(0.17927) C6B(0.17927) H6B(0.17927) C5B(0.17927) C9B(0.17927)
 H9B(0.17927) O3B(0.17927) C11B(0.17927) H11B(0.17927) C7B(0.17927)
 O2B(0.17927) C12B(0.17927) C8B(0.17927) C10B(0.17927) H10B(0.17927)
 C803(0.25825) H80A(0.25825) H80B(0.25825) C804(0.25825) H80C(0.25825)
 H80D(0.25825) C805(0.25825) H80E(0.25825) H80F(0.25825) C806(0.25825)
 H80G(0.25825) H80H(0.25825) C801(0.25825) H80I(0.25825) H80J(0.25825)
 C802(0.25825) H80K(0.25825) H80L(0.25825) C14B(0.17927) H14D(0.17927)
 H14E(0.17927) H14F(0.17927) C15B(0.17927) H15D(0.17927) H15E(0.17927)
 H15F(0.17927) O1B(0.17927) H1BA(0.17927) C13B(0.17927) H13C(0.17927)
 H13D(0.17927)
 Fixed Uiso: I510(0.08) I509(0.08) Zn55(0.08) I505(0.08) Zn53(0.08) I506(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C803(H80A,H80B), C804(H80C,H80D), C805(H80E,H80F), C806(H80G,
 H80H), C801(H80I,H80J), C802(H80K,H80L), C13B(H13C,H13D)
7.b Aromatic/amide H refined with riding coordinates:
 C353(H353), C312(H312), C369(H369), C364(H364), C314(H314), C328(H328),
 C368(H368), C313(H313), C365(H365), C354(H354), C356(H356), C366(H366),
 C358(H358), C359(H359), C317(H317), C367(H367), C371(H371), C315(H315),
 C341(H341), C329(H329), C336(H336), C355(H355), C320(H320), C305(H305),
 C301(H301), C349(H349), C351(H351), C333(H333), C332(H332), C331(H331),
 C335(H335), C323(H323), C304(H304), C322(H322), C318(H318), C372(H372),
 C302(H302), C350(H350), C319(H319), C340(H340), C3A(H3A), C330(H330), C9A(H9A),
  C348(H348), C311(H311), C1A(H1AA), C338(H338), C310(H310), C2A(H2A),
 C10A(H10A), C11A(H11A), C6A(H6A), C337(H337), C347(H347), C346(H346), C3B(H3B),
  C2B(H2B), C1B(H1B), C6B(H6B), C9B(H9B), C11B(H11B), C10B(H10B)
7.c Fitted hexagon refined as free rotating group:
 C4B(C3B,C2B,C1B,C6B,C5B)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1B(H1BA)
7.e Idealised Me refined with everything fixed:
 C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C), C14B(H14D,H14E,H14F), C15B(H15D,
 H15E,H15F)
;
_shelx_res_checksum              60860
_shelx_hkl_checksum              7762
_olex2_date_sample_data_collection 2023-10-20
_olex2_date_sample_submission    2023-10-20
_olex2_submission_original_sample_id 50_10_24b
_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 3.121
_oxdiff_exptl_absorpt_empirical_full_min 0.299