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_1571869
_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, 0.858(C15 H16 O3), 0.514(C6 H12)'
_chemical_formula_sum            'C87.95 H67.9 I12 N24 O2.58 Zn6'
_chemical_formula_weight         3417.24
_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             2024-02-12
_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                 101.680(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.4491(6)
_cell_length_b                   15.0235(2)
_cell_length_c                   34.2150(5)
_cell_measurement_reflns_used    20990
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.2470
_cell_measurement_theta_min      2.6590
_cell_volume                     15831.0(4)
_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_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 Arc-100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -89.00 -55.00   0.50    3.00    -- -103.00  72.00 -30.00   68
  2  \w   -171.00 -87.00   0.50    3.00    -- -103.00 -72.00-160.00  168
  3  \w   -153.00-103.00   0.50    3.00    -- -103.00 -30.00 -90.00  100
  4  \w    -76.00 -40.00   0.50    3.00    -- -103.00  77.00 -90.00   72
  5  \w    -69.00 -36.00   0.50    3.00    -- -103.00  61.00-180.00   66
  6  \w    -99.00 -34.00   0.50    3.00    -- -103.00  77.00  60.00  130
  7  \w    -61.00 -30.00   0.50    3.00    -- -103.00  61.00 -30.00   62
  8  \w    -69.00 -44.00   0.50    3.00    -- -103.00  61.00 -60.00   50
  9  \w   -161.00 -91.00   0.50    3.00    -- -103.00 -30.00  60.00  140
 10  \w    104.00 129.00   0.50    3.00    --  101.75  72.00 -30.00   50
 11  \w     33.00  93.00   0.50    3.00    --  101.75 -72.00-160.00  120
 12  \w     30.00  72.00   0.50    3.00    --  101.75 -61.00  90.00   84
 13  \w     67.00  94.00   0.50    3.00    --  101.75 -94.00-180.00   54
 14  \w     31.00  72.00   0.50    3.00    --  101.75 -61.00 150.00   82
 15  \w     89.00 174.00   0.50    3.00    --  101.75  45.00 -60.00  170
 16  \w     29.00  68.00   0.50    3.00    --  101.75 -61.00   0.00   78
 17  \w     91.00 117.00   0.50    3.00    --  101.75  45.00 -90.00   52
 18  \w     45.00 110.00   0.50    3.00    --  101.75-125.00  90.00  130
 19  \w     45.00  72.00   0.50    3.00    --  101.75 -61.00 -30.00   54
 20  \w     97.00 158.00   0.50    3.00    --  101.75  45.00-120.00  122
 21  \w     30.00  55.00   0.50    3.00    --  101.75 -94.00-180.00   50
 22  \w    -96.00 -71.00   0.50    0.75    --  -46.26 -72.00-160.00   50
 23  \w    -65.00  26.00   0.50    0.75    --  -46.26  72.00 -30.00  182
 24  \w    -25.00  22.00   0.50    0.75    --   46.26 -72.00-160.00   94
 25  \w     45.00 107.00   0.50    0.75    --   46.26  72.00 -30.00  124
 26  \w    -23.00  28.00   0.50    0.75    --   46.26 -19.00  30.00  102
 27  \w      0.00  27.00   0.50    0.75    --   46.26 -19.00-180.00   54
;
_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      -0.0493698000
_diffrn_orient_matrix_UB_12      -0.0077434000
_diffrn_orient_matrix_UB_13      -0.0028737000
_diffrn_orient_matrix_UB_21      -0.0011676000
_diffrn_orient_matrix_UB_22      -0.0821736000
_diffrn_orient_matrix_UB_23      -0.0271351000
_diffrn_orient_matrix_UB_31      0.0078801000
_diffrn_orient_matrix_UB_32      -0.0608766000
_diffrn_orient_matrix_UB_33      0.0370101000
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            121588
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.136
_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    19.684
_exptl_absorpt_correction_T_max  0.244
_exptl_absorpt_correction_T_min  0.043
_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    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             6401
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.300
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1618
_refine_ls_number_reflns         28909
_refine_ls_number_restraints     719
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0803
_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^)+(0.1331P)^2^+80.7275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2470
_refine_ls_wR_factor_ref         0.2602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21863
_reflns_number_total             28909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_5_96c
_cod_original_formula_sum        'C87.95 H67.90 I12 N24 O2.58 Zn6'
_cod_database_code               1571869
_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   0.221
_shelx_estimated_absorpt_t_min   0.046
_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
 O1B-C13B = O2B-C14B = O3B-C15B
 1.43 with sigma of 0.02
 O3B-C12B = O2B-C8B
 1.37 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 C4A-C7A
 1.5 with sigma of 0.02
 O3A-C15A
 1.43 with sigma of 0.02
 C5B-C13B
 1.51 with sigma of 0.02
 C807-C812 = C807-C808 = C812-C811 = C811-C810 = C810-C809 = C809-C808
 1.54 with sigma of 0.02
 C804-C803 = C804-C805 = C803-C802 = C802-C801 = C801-C806 = C806-C805
 1.54 with sigma of 0.02
 C14B-C8B
 2.4 with sigma of 0.04
 C15B-C12B
 2.4 with sigma of 0.02
 C7B-O3B = C7B-O2B
 2.35 with sigma of 0.04
 O3B-C11B
 2.45 with sigma of 0.04
 C5B-O1B
 2.4 with sigma of 0.04
 C807-C811 = C807-C809 = C812-C810 = C811-C809 = C810-C808
 2.54 with sigma of 0.04
 C804-C802 = C804-C806 = C803-C801 = C802-C806 = C801-C805
 2.54 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 0.04
 C8A-C7A \\sim C9A-C8A \\sim C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim
C7A-C12A
 with sigma of 0.02
 C3B-C7B \\sim C7B-C5B
 with sigma of 0.04
 C7A-C9A \\sim C8A-C10A \\sim C9A-C11A \\sim C10A-C12A \\sim C11A-C7A \\sim
C12A-C8A
 with sigma of 0.04
 C8B-C4B \\sim C4B-C12B
 with sigma of 0.04
 C7A-C10A \\sim C8A-C11A \\sim C9A-C12A
 with sigma of 0.04
 O2A-C14A \\sim O1A-C13A
 with sigma of 0.02
 O3A-C12A \\sim O2A-C8A
 with sigma of 0.02
 C4B-C13B \\sim C13B-C6B
 with sigma of 0.04
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 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
 I304-N307 \\sim I404-N307
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 Zn43-N311 \\sim Zn33-N311
 with sigma of 0.02
 I406-I405 \\sim I306-I305
 with sigma of 0.04
 I406-N311 \\sim I306-N311
 with sigma of 0.04
 I405-N311 \\sim I305-N311
 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
 Zn35-N317 \\sim Zn45-N317
 with sigma of 0.02
 I310-I309 \\sim I410-I409
 with sigma of 0.04
 I310-N317 \\sim I410-N317
 with sigma of 0.04
 I309-N317 \\sim I409-N317
 with sigma of 0.04
 I411-Zn46 \\sim I311-Zn36
 with sigma of 0.02
 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
 I411-I412 \\sim I311-I312
 with sigma of 0.04
 I411-N318 \\sim I311-N318
 with sigma of 0.04
 I411-N319 \\sim I311-N319
 with sigma of 0.04
 I412-N318 \\sim I312-N318
 with sigma of 0.04
 I412-N319 \\sim I312-N319
 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
 Zn51-N301 \\sim Zn41-N301
 with sigma of 0.02
 I501-Zn51 \\sim I401-Zn41
 with sigma of 0.02
 I502-Zn51 \\sim I402-Zn41
 with sigma of 0.02
 Zn55-N317 \\sim Zn35-N317
 with sigma of 0.02
 I510-Zn55 \\sim I310-Zn35
 with sigma of 0.02
 I509-Zn55 \\sim I309-Zn35
 with sigma of 0.02
 N306-C314 \\sim N306-C414
 with sigma of 0.02
 C316-C315 \\sim C316-C415
 with sigma of 0.02
 C314-C315 \\sim C414-C415
 with sigma of 0.02
 N306-C315 \\sim N306-C415
 with sigma of 0.04
 C316-C314 \\sim C316-C414
 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-N312 \\sim Zn44-N312
 with sigma of 0.02
 Zn34-N313 \\sim Zn44-N313
 with sigma of 0.02
 I308-I307 \\sim I408-I407
 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
 I307-N312 \\sim I407-N312
 with sigma of 0.04
 I307-N313 \\sim I407-N313
 with sigma of 0.04
 Zn54-N312 \\sim Zn34-N312
 with sigma of 0.02
 I507-Zn54 \\sim I307-Zn34
 with sigma of 0.02
 I508-Zn54 \\sim I308-Zn34
 with sigma of 0.02
 C807-C812 \\sim C812-C811 \\sim C811-C810 \\sim C810-C809 \\sim C809-C808
\\sim C808-C807
 with sigma of 0.02
 C807-C809 \\sim C811-C809 \\sim C812-C808 \\sim C812-C810 \\sim C810-C808
\\sim C807-C811
 with sigma of 0.04
 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
 Zn54-N313 \\sim Zn34-N313
 with sigma of 0.02
3. Restrained planarity
 O2B, C8B, C7B, C12B, O3B
 with sigma of 0.1
 C6B, C5B, C4B, C13B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7B \\sim C3B \\sim C4B \\sim C2B \\sim C5B \\sim C1B \\sim C6B \\sim C13B
\\sim C8B \\sim C12B \\sim O1B \\sim C9B \\sim O2B \\sim O3B \\sim C11B \\sim
C10B \\sim C14B \\sim C15B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C13A \\sim O2A \\sim C8A \\sim C14A \\sim C7A \\sim C9A \\sim C4A \\sim C12A
\\sim C10A \\sim C3A \\sim C5A \\sim O3A \\sim C11A \\sim C2A \\sim C6A \\sim
C15A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C807 \\sim C812 \\sim C811 \\sim C810 \\sim C809 \\sim C808: 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
I407 \\sim I307 \\sim Zn44 \\sim Zn34 \\sim I308 \\sim I408: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C414) = Uanis(C314)
Uanis(C415) = Uanis(C315)
5. Rigid body (RIGU) restrains
 C7B, C3B, C4B, C2B, C5B, C1B, C6B, C13B, C8B, C12B, O1B, C9B, O2B, O3B, C11B,
 C10B, C14B, C15B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C314, C315, C414, C415
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C807, C812, C811, C810, C809, C808
 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
 I407, I307, Zn44, Zn34, I308, I408
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I305)=Sof(Zn33)=Sof(I306)=1-FVAR(1)
 Sof(I406)=Sof(I405)=Sof(Zn43)=FVAR(1)
 Sof(I311)=Sof(Zn36)=Sof(I312)=1-FVAR(2)
 Sof(I411)=Sof(I412)=Sof(Zn46)=FVAR(2)
 Sof(C414)=Sof(H414)=Sof(C415)=Sof(H415)=1-FVAR(3)
 Sof(C314)=Sof(H314)=Sof(C315)=Sof(H315)=FVAR(3)
 Fixed Sof: I310(0.56173) I301(0.38152) I303(0.55401) I308(0.64322)
 I307(0.64322) I309(0.56173) I304(0.55401) I302(0.38152) Zn32(0.55401)
 Zn35(0.56173) Zn34(0.64322) Zn31(0.38152) O3A(0.66291) O2A(0.66291)
 O1A(0.66291) H1A(0.66291) C4A(0.66291) C3A(0.66291) H3A(0.66291) C5A(0.66291)
 C2A(0.66291) H2A(0.66291) C7A(0.66291) C1A(0.66291) H1AA(0.66291) C6A(0.66291)
 H6A(0.66291) C8A(0.66291) C12A(0.66291) C11A(0.66291) H11A(0.66291)
 C10A(0.66291) H10A(0.66291) C9A(0.66291) H9A(0.66291) C13A(0.66291)
 H13A(0.66291) H13B(0.66291) C15A(0.66291) H15A(0.66291) H15B(0.66291)
 H15C(0.66291) C14A(0.66291) H14A(0.66291) H14B(0.66291) H14C(0.66291)
 I403(0.44599) Zn42(0.44599) I404(0.44599) I409(0.40127) Zn45(0.40127)
 I410(0.40127) I401(0.35445) Zn41(0.35445) I402(0.35445) I501(0.26403)
 I502(0.26403) Zn51(0.26403) I509(0.037) I510(0.037) Zn55(0.037) O3B(0.19505)
 C7B(0.19505) C12B(0.19505) C11B(0.19505) H11B(0.19505) C10B(0.19505)
 H10B(0.19505) C9B(0.19505) H9B(0.19505) C8B(0.19505) O2B(0.19505)
 C14B(0.19505) H14D(0.19505) H14E(0.19505) H14F(0.19505) Zn44(0.33231)
 I407(0.33231) I408(0.33231) I508(0.02447) I507(0.02447) Zn54(0.02447)
 O1B(0.19505) H1B(0.19505) C13B(0.19505) H13C(0.19505) H13D(0.19505)
 C1B(0.19505) H1BA(0.19505) C2B(0.19505) H2B(0.19505) C3B(0.19505) H3B(0.19505)
 C4B(0.19505) C5B(0.19505) C6B(0.19505) H6B(0.19505) C15B(0.19505)
 H15D(0.19505) H15E(0.19505) H15F(0.19505) C807(0.25589) H80A(0.25589)
 H80B(0.25589) C812(0.25589) H81A(0.25589) H81B(0.25589) C811(0.25589)
 H81C(0.25589) H81D(0.25589) C810(0.25589) H81E(0.25589) H81F(0.25589)
 C809(0.25589) H80C(0.25589) H80D(0.25589) C808(0.25589) H80E(0.25589)
 H80F(0.25589) C804(0.25828) H80G(0.25828) H80H(0.25828) C803(0.25828)
 H80I(0.25828) H80J(0.25828) C802(0.25828) H80K(0.25828) H80L(0.25828)
 C801(0.25828) H80M(0.25828) H80N(0.25828) C806(0.25828) H80O(0.25828)
 H80P(0.25828) C805(0.25828) H80Q(0.25828) H80R(0.25828)
 Fixed Uiso: I509(0.08) I510(0.08) Zn55(0.08) I508(0.08) I507(0.08) Zn54(0.08)
 C807(0.08) C812(0.08) C811(0.08) C810(0.08) C809(0.08) C808(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13B(H13C,H13D), C807(H80A,H80B), C812(H81A,H81B), C811(H81C,
 H81D), C810(H81E,H81F), C809(H80C,H80D), C808(H80E,H80F), C804(H80G,H80H),
 C803(H80I,H80J), C802(H80K,H80L), C801(H80M,H80N), C806(H80O,H80P), C805(H80Q,
 H80R)
7.b Aromatic/amide H refined with riding coordinates:
 C320(H320), C312(H312), C313(H313), C336(H336), C331(H331), C319(H319),
 C348(H348), C335(H335), C369(H369), C328(H328), C350(H350), C329(H329),
 C353(H353), C349(H349), C351(H351), C322(H322), C358(H358), C359(H359),
 C333(H333), C310(H310), C332(H332), C356(H356), C330(H330), C368(H368),
 C355(H355), C340(H340), C354(H354), C323(H323), C365(H365), C317(H317),
 C364(H364), C338(H338), C337(H337), C311(H311), C367(H367), C341(H341),
 C366(H366), C372(H372), C371(H371), C318(H318), C3A(H3A), C347(H347),
 C302(H302), C301(H301), C304(H304), C346(H346), C2A(H2A), C1A(H1AA), C6A(H6A),
 C305(H305), C11A(H11A), C10A(H10A), C9A(H9A), C314(H314), C315(H315),
 C11B(H11B), C10B(H10B), C9B(H9B), C414(H414), C415(H415), C1B(H1BA), C2B(H2B),
 C3B(H3B), C6B(H6B)
7.c Fitted hexagon refined as free rotating group:
 C7B(C12B,C11B,C10B,C9B,C8B), C1B(C2B,C3B,C4B,C5B,C6B)
7.d Tetrahedral OH refined with riding coordinates:
 O1B(H1B)
7.e Idealised Me refined with everything fixed:
 C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F)
7.f Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C)
7.g Idealised tetrahedral OH refined as rotating group:
 O1A(H1A)
;
_shelx_res_checksum              77020
_shelx_hkl_checksum              26481
_olex2_date_sample_data_collection 2023-04-03
_olex2_date_sample_submission    2023-04-03
_olex2_submission_original_sample_id 50_5_96c
_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 13.070
_oxdiff_exptl_absorpt_empirical_full_min 0.259