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_1571865
_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, 1.026(C15 H16 O3), 1.222(C6 H12)'
_chemical_formula_sum            'C94.73 H79.09 I12 N24 O3.08 Zn6'
_chemical_formula_weight         3517.93
_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                 101.939(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.6098(9)
_cell_length_b                   15.0289(2)
_cell_length_c                   34.3656(8)
_cell_measurement_reflns_used    19887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2730
_cell_measurement_theta_min      2.5940
_cell_volume                     15972.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.994
_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   -164.00 -58.00   0.50    4.00    -- -103.00  -4.00 119.00  212
  2  \w   -110.00 -45.00   0.50    4.00    -- -103.00 125.00 -60.00  130
  3  \w   -137.00 -90.00   0.50    4.00    -- -103.00 -15.00  60.00   94
  4  \w    -96.00 -71.00   0.50    4.00    -- -103.00  77.00 -30.00   50
  5  \w   -174.00-145.00   0.50    4.00    -- -103.00 -15.00  60.00   58
  6  \w    -65.00 -40.00   0.50    4.00    -- -103.00  61.00 -90.00   50
  7  \w    -96.00 -47.00   0.50    4.00    -- -103.00 125.00  90.00   98
  8  \w    -60.00 -35.00   0.50    4.00    -- -103.00  77.00 -30.00   50
  9  \w     63.00 117.00   0.50    4.00    --  101.75   4.00 -63.00  108
 10  \w     30.00  72.00   0.50    4.00    --  101.75 -61.00  30.00   84
 11  \w     42.00  73.00   0.50    4.00    --  101.75 -61.00-120.00   62
 12  \w     34.00  70.00   0.50    4.00    --  101.75 -77.00  30.00   72
 13  \w     74.00 101.00   0.50    4.00    --  101.75 -77.00  30.00   54
 14  \w     32.00  63.00   0.50    4.00    --  101.75 -94.00 -30.00   62
 15  \w     29.00  68.00   0.50    4.00    --  101.75 -61.00 -30.00   78
 16  \w     33.00  69.00   0.50    4.00    --  101.75 -94.00-150.00   72
 17  \w     81.00 106.00   0.50    4.00    --  101.75 -94.00-150.00   50
 18  \w     75.00 106.00   0.50    4.00    --  101.75 -94.00 -30.00   62
 19  \w   -119.00 -49.00   0.50    0.50    --  -46.36  -4.00 119.00  140
 20  \w    -32.00  -7.00   0.50    0.50    --  -46.36   4.00 -63.00   50
 21  \w      8.00 116.00   0.50    0.50    --   46.36   4.00 -63.00  216
 22  \w    -14.00  11.00   0.50    0.50    --   46.36  -4.00 119.00   50
 23  \w    -23.00  27.00   0.50    0.50    --   46.36 -19.00 -60.00  100
 24  \w     26.00  90.00   0.50    0.50    --   46.36-125.00  30.00  128
;
_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      0.0497238000
_diffrn_orient_matrix_UB_12      -0.0051421000
_diffrn_orient_matrix_UB_13      0.0096832000
_diffrn_orient_matrix_UB_21      -0.0002959000
_diffrn_orient_matrix_UB_22      -0.0025891000
_diffrn_orient_matrix_UB_23      0.0447838000
_diffrn_orient_matrix_UB_31      -0.0024873000
_diffrn_orient_matrix_UB_32      -0.1023407000
_diffrn_orient_matrix_UB_33      -0.0016346000
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            102894
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.249
_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    19.528
_exptl_absorpt_correction_T_max  0.442
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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    1.463
_exptl_crystal_description       block
_exptl_crystal_F_000             6624
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1652
_refine_ls_number_reflns         29074
_refine_ls_number_restraints     824
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0957
_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^)+(0.1101P)^2^+171.8980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2742
_refine_ls_wR_factor_ref         0.2871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21866
_reflns_number_total             29074
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_5_48b
_cod_database_code               1571865
_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   0.442
_shelx_estimated_absorpt_t_min   0.089
_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
 1.5 with sigma of 0.02
 C5B-C13B
 1.51 with sigma of 0.02
 C8A-C7A = C9A-C8A = C9A-C10A = C11A-C10A = C12A-C11A = C7A-C12A
 1.39 with sigma of 0.02
 O1B-C13B = O3B-C15B = O2B-C14B
 1.43 with sigma of 0.02
 C5A-C13A = C7A-C4A
 1.51 with sigma of 0.02
 O3A-C12A = O2A-C8A
 1.37 with sigma of 0.02
 O2B-C8B = O3B-C12B
 1.37 with sigma of 0.02
 O1A-C13A
 1.43 with sigma of 0.02
 C804-C803 = C804-C805 = C803-C802 = C802-C801 = C801-C806 = C806-C805
 1.54 with sigma of 0.02
 C809-C810 = C809-C808 = C810-C811 = C811-C812 = C812-C807 = C807-C808
 1.54 with sigma of 0.02
 C817-C818 = C817-C816 = C818-C813 = C813-C814 = C814-C815 = C815-C816
 1.54 with sigma of 0.02
 C823-C822 = C823-C824 = C822-C821 = C821-C820 = C820-C819 = C819-C824
 1.54 with sigma of 0.02
 C7A-C9A = C8A-C10A = C9A-C11A = C10A-C12A = C11A-C7A = C12A-C8A
 2.4 with sigma of 0.04
 C5B-O1B
 2.4 with sigma of 0.04
 C8B-C14B = C12B-C15B
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.04
 C804-C802 = C804-C806 = C803-C801 = C802-C806 = C801-C805
 2.54 with sigma of 0.04
 C809-C811 = C809-C807 = C810-C812 = C811-C807 = C812-C808
 2.54 with sigma of 0.04
 C817-C813 = C817-C815 = C818-C814 = C813-C815 = C814-C816
 2.54 with sigma of 0.04
 C823-C821 = C823-C819 = C822-C820 = C821-C819 = C820-C824
 2.54 with sigma of 0.04
 O1A-C13A \\sim O2A-C14A \\sim O3A-C15A
 with sigma of 0.02
 C5B-C7B \\sim C7B-C3B
 with sigma of 0.04
 C12B-C4B \\sim C4B-C8B
 with sigma of 0.04
 C2A-C1A \\sim C3A-C2A \\sim C4A-C3A \\sim C5A-C4A \\sim C6A-C5A \\sim C6A-C1A
 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 0.02
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 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
 I305-N307 \\sim I405-N307
 with sigma of 0.04
 I306-N307 \\sim I406-N307
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 Zn33-N307 \\sim Zn43-N307
 with sigma of 0.02
 Zn33-N306 \\sim Zn43-N306
 with sigma of 0.02
 I411-N318 \\sim I311-N318
 with sigma of 0.04
 I411-I412 \\sim I311-I312
 with sigma of 0.04
 I412-N319 \\sim I312-N319
 with sigma of 0.04
 I411-N319 \\sim I311-N319
 with sigma of 0.04
 I411-Zn46 \\sim I311-Zn36
 with sigma of 0.02
 I412-N318 \\sim I312-N318
 with sigma of 0.04
 I412-Zn46 \\sim I312-Zn36
 with sigma of 0.02
 Zn46-N318 \\sim Zn36-N318
 with sigma of 0.02
 Zn46-N319 \\sim Zn36-N319
 with sigma of 0.02
 I307-I308 \\sim I407-I408
 with sigma of 0.04
 I307-N313 \\sim I407-N313
 with sigma of 0.04
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 I308-N312 \\sim I408-N312
 with sigma of 0.04
 I307-N312 \\sim I407-N312
 with sigma of 0.04
 Zn34-N312 \\sim Zn44-N312
 with sigma of 0.02
 Zn34-N313 \\sim Zn44-N313
 with sigma of 0.02
 I308-N313 \\sim I408-N313
 with sigma of 0.04
 I307-Zn34 \\sim I407-Zn44
 with sigma of 0.02
 C804-C803 \\sim C803-C802 \\sim C802-C801 \\sim C801-C806 \\sim C806-C805
\\sim C805-C804
 with sigma of 0.02
 C804-C806 \\sim C802-C806 \\sim C803-C805 \\sim C803-C801 \\sim C801-C805
\\sim C804-C802
 with sigma of 0.04
 C809-C810 \\sim C810-C811 \\sim C811-C812 \\sim C812-C807 \\sim C807-C808
\\sim C808-C809
 with sigma of 0.02
 C809-C807 \\sim C811-C807 \\sim C810-C808 \\sim C810-C812 \\sim C812-C808
\\sim C809-C811
 with sigma of 0.04
 C817-C818 \\sim C818-C813 \\sim C813-C814 \\sim C814-C815 \\sim C815-C816
\\sim C816-C817
 with sigma of 0.02
 C817-C815 \\sim C813-C815 \\sim C818-C816 \\sim C818-C814 \\sim C814-C816
\\sim C817-C813
 with sigma of 0.04
 C823-C822 \\sim C822-C821 \\sim C821-C820 \\sim C820-C819 \\sim C819-C824
\\sim C824-C823
 with sigma of 0.02
 C823-C819 \\sim C821-C819 \\sim C822-C824 \\sim C822-C820 \\sim C820-C824
\\sim C823-C821
 with sigma of 0.04
 N306-C414 \\sim N306-C314
 with sigma of 0.02
 C316-C415 \\sim C316-C315
 with sigma of 0.02
 C415-C414 \\sim C315-C314
 with sigma of 0.02
 N306-C415 \\sim N306-C315
 with sigma of 0.04
 C316-C414 \\sim C316-C314
 with sigma of 0.04
 C314-C318 \\sim C318-C414
 with sigma of 0.02
3. Restrained planarity
 C7A, C8A, C12A, C9A, C10A, C11A
 with sigma of 0.1
 C4B, C5B, C6B, C13B
 with sigma of 0.1
 O2B, C8B, C7B, C12B, O3B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C12A \\sim O2A \\sim C8A \\sim C14A \\sim C7A \\sim C9A \\sim C4A \\sim C10A
\\sim C5A \\sim C3A \\sim C11A \\sim O3A \\sim C6A \\sim C13A \\sim C2A \\sim
C15A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C4B \\sim C5B \\sim C3B \\sim C7B \\sim C6B \\sim C13B \\sim C2B \\sim C12B
\\sim C8B \\sim C1B \\sim O1B \\sim C11B \\sim O3B \\sim C9B \\sim O2B \\sim
C10B \\sim C15B \\sim C14B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C804 \\sim C803 \\sim C802 \\sim C801 \\sim C806 \\sim C805: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C809 \\sim C810 \\sim C811 \\sim C812 \\sim C807 \\sim C808: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C817 \\sim C818 \\sim C813 \\sim C814 \\sim C815 \\sim C816: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C823 \\sim C822 \\sim C821 \\sim C820 \\sim C819 \\sim C824: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C414 \\sim C415 \\sim C314 \\sim C315: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C415) = Uanis(C414)
5. Rigid body (RIGU) restrains
 C8B, C4B, C5B, C3B, C7B, C6B, C13B, C2B, C12B, C1B, O1B, C11B, O3B, C9B, O2B,
 C10B, C15B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C804, C803, C802, C801, C806, C805
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C809, C810, C811, C812, C807, C808
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C817, C818, C813, C814, C815, C816
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C823, C822, C821, C820, C819, C824
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I304)=Sof(Zn32)=Sof(I303)=1-FVAR(1)
 Sof(I404)=Sof(I403)=Sof(Zn42)=FVAR(1)
 Sof(I409)=Sof(Zn45)=Sof(I410)=1-FVAR(2)
 Sof(I310)=Sof(I309)=Sof(Zn35)=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(I305)=Sof(I306)=Sof(Zn33)=FVAR(4)
 Sof(I311)=Sof(Zn36)=Sof(I312)=1-FVAR(5)
 Sof(I411)=Sof(I412)=Sof(Zn46)=FVAR(5)
 Sof(I407)=Sof(Zn44)=Sof(I408)=1-FVAR(6)
 Sof(I307)=Sof(I308)=Sof(Zn34)=FVAR(6)
 Sof(C314)=Sof(H314)=Sof(C315)=Sof(H315)=1-FVAR(7)
 Sof(C415)=Sof(H415)=Sof(C414)=Sof(H414)=FVAR(7)
 Fixed Sof: O2A(0.72626) O3A(0.72626) O1A(0.72626) H1AA(0.72626) C7A(0.72626)
 C4A(0.72626) C5A(0.72626) C6A(0.72626) H6A(0.72626) C1A(0.72626) H1A(0.72626)
 C2A(0.72626) H2A(0.72626) C3A(0.72626) H3A(0.72626) C8A(0.72626) C12A(0.72626)
 C9A(0.72626) H9A(0.72626) C10A(0.72626) H10A(0.72626) C11A(0.72626)
 H11A(0.72626) C15A(0.72626) H15A(0.72626) H15B(0.72626) H15C(0.72626)
 C13A(0.72626) H13A(0.72626) H13B(0.72626) C14A(0.72626) H14A(0.72626)
 H14B(0.72626) H14C(0.72626) C804(0.3581) H80A(0.3581) H80B(0.3581)
 C803(0.3581) H80C(0.3581) H80D(0.3581) C802(0.3581) H80E(0.3581) H80F(0.3581)
 C801(0.3581) H80G(0.3581) H80H(0.3581) C806(0.3581) H80I(0.3581) H80J(0.3581)
 C805(0.3581) H80K(0.3581) H80L(0.3581) C4B(0.3) C5B(0.3) C6B(0.3) H6B(0.3)
 C1B(0.3) H1B(0.3) C2B(0.3) H2B(0.3) C3B(0.3) H3B(0.3) C7B(0.3) C12B(0.3)
 C11B(0.3) H11B(0.3) C10B(0.3) H10B(0.3) C9B(0.3) H9B(0.3) C8B(0.3)
 C809(0.31711) H80M(0.31711) H80N(0.31711) C810(0.31711) H81A(0.31711)
 H81B(0.31711) C811(0.31711) H81C(0.31711) H81D(0.31711) C812(0.31711)
 H81E(0.31711) H81F(0.31711) C807(0.31711) H80O(0.31711) H80P(0.31711)
 C808(0.31711) H80Q(0.31711) H80R(0.31711) C817(0.28958) H81G(0.28958)
 H81H(0.28958) C818(0.28958) H81I(0.28958) H81J(0.28958) C813(0.28958)
 H81K(0.28958) H81L(0.28958) C814(0.28958) H81M(0.28958) H81N(0.28958)
 C815(0.28958) H81O(0.28958) H81P(0.28958) C816(0.28958) H81Q(0.28958)
 H81R(0.28958) O2B(0.3) O3B(0.3) C823(0.25745) H82A(0.25745) H82B(0.25745)
 C822(0.25745) H82C(0.25745) H82D(0.25745) C821(0.25745) H82E(0.25745)
 H82F(0.25745) C820(0.25745) H82G(0.25745) H82H(0.25745) C819(0.25745)
 H81S(0.25745) H81T(0.25745) C824(0.25745) H82I(0.25745) H82J(0.25745)
 C15B(0.3) H15D(0.3) H15E(0.3) H15F(0.3) C14B(0.3) H14D(0.3) H14E(0.3)
 H14F(0.3) O1B(0.3) H1BA(0.3) C13B(0.3) H13C(0.3) H13D(0.3)
 Fixed Uiso: C809(0.08) C810(0.08) C811(0.08) C812(0.08) C807(0.08) C808(0.08)
 C823(0.08) C822(0.08) C821(0.08) C820(0.08) C819(0.08) C824(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C804(H80A,H80B), C803(H80C,H80D), C802(H80E,H80F), C801(H80G,
 H80H), C806(H80I,H80J), C805(H80K,H80L), C809(H80M,H80N), C810(H81A,H81B),
 C811(H81C,H81D), C812(H81E,H81F), C807(H80O,H80P), C808(H80Q,H80R), C817(H81G,
 H81H), C818(H81I,H81J), C813(H81K,H81L), C814(H81M,H81N), C815(H81O,H81P),
 C816(H81Q,H81R), C823(H82A,H82B), C822(H82C,H82D), C821(H82E,H82F), C820(H82G,
 H82H), C819(H81S,H81T), C824(H82I,H82J), C13B(H13C,H13D)
7.b Aromatic/amide H refined with riding coordinates:
 C335(H335), C336(H336), C349(H349), C331(H331), C350(H350), C351(H351),
 C312(H312), C313(H313), C328(H328), C320(H320), C319(H319), C369(H369),
 C329(H329), C322(H32A), C333(H333), C348(H348), C332(H332), C330(H330),
 C310(H310), C356(H356), C353(H353), C358(H358), C367(H367), C311(H311),
 C317(H317), C368(H368), C364(H364), C341(H341), C337(H337), C355(H355),
 C365(H365), C366(H366), C338(H338), C302(H302), C323(H323), C354(H354),
 C340(H340), C6A(H6A), C1A(H1A), C2A(H2A), C3A(H3A), C359(H359), C372(H372),
 C301(H301), C371(H371), C318(H318), C346(H346), C347(H347), C304(H30A),
 C9A(H9A), C10A(H10A), C305(H305), C11A(H11A), C415(H415), C414(H414), C6B(H6B),
  C1B(H1B), C2B(H2B), C3B(H3B), C11B(H11B), C10B(H10B), C9B(H9B), C314(H314),
 C315(H315)
7.c Fitted hexagon refined as free rotating group:
 C4B(C5B,C6B,C1B,C2B,C3B), C7B(C12B,C11B,C10B,C9B,C8B)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1AA), O1B(H1BA)
7.e Idealised Me refined with everything fixed:
 C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C), C15B(H15D,H15E,H15F), C14B(H14D,
 H14E,H14F)
;
_shelx_res_checksum              1377
_shelx_hkl_checksum              9293
_olex2_date_sample_data_collection 2022-07-28
_olex2_date_sample_submission    2022-07-28
_olex2_submission_original_sample_id 50_5_48b
_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 3.138
_oxdiff_exptl_absorpt_empirical_full_min 0.474