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_1571827
_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, 0.719(C15 H16 O3), 0.862(C6 H12)'
_chemical_formula_sum            'C123.96 H93.85 I18 N36 O2.16 Zn9'
_chemical_formula_weight         4994.73
_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                 99.869(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   78.371(2)
_cell_length_b                   14.9291(4)
_cell_length_c                   41.6991(13)
_cell_measurement_reflns_used    9764
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.1740
_cell_measurement_theta_min      2.5870
_cell_volume                     48066(2)
_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 0.993
_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    -59.00 -33.00   0.50    3.00    -- -103.00  58.00  85.00   52
  2  \w   -125.00 -92.00   0.50    3.00    -- -103.00 -58.00 -55.00   66
  3  \w   -174.00-148.00   0.50    3.00    -- -103.00 -58.00 -55.00   52
  4  \w    -69.00 -36.00   0.50    3.00    -- -103.00  61.00 -90.00   66
  5  \w    -68.00 -31.00   0.50    3.00    -- -103.00  61.00 120.00   74
  6  \w    -69.00 -37.00   0.50    3.00    -- -103.00  61.00 -60.00   64
  7  \w    -67.00 -42.00   0.50    3.00    -- -103.00  61.00   0.00   50
  8  \w     39.00  68.00   0.50    3.00    --  101.75 -58.00 -55.00   58
  9  \w    137.00 168.00   0.50    3.00    --  101.75  45.00 -60.00   62
 10  \w     35.00  61.00   0.50    3.00    --  101.75 -61.00 120.00   52
 11  \w     41.00  67.00   0.50    3.00    --  101.75 -94.00-180.00   52
 12  \w     76.00 106.00   0.50    3.00    --  101.75 -94.00 -90.00   60
 13  \w     31.00  90.00   0.50    3.00    --  101.75 -94.00-120.00  118
 14  \w     90.00 173.00   0.50    3.00    --  101.75  45.00 120.00  166
 15  \w     82.00 158.00   0.50    3.00    --  101.75 125.00 -60.00  152
 16  \w     56.00 107.00   0.50    3.00    --  101.75 -77.00-120.00  102
 17  \w     29.00  68.00   0.50    3.00    --  101.75 -61.00  90.00   78
 18  \w     69.00  94.00   0.50    3.00    --  101.75 -94.00-180.00   50
 19  \w    144.00 171.00   0.50    3.00    --  101.75  58.00  85.00   54
 20  \w     95.00 122.00   0.50    3.00    --  101.75  45.00 -60.00   54
 21  \w    -88.00 -31.00   0.50    0.75    --  -46.45 -58.00 -55.00  114
 22  \w     46.00 118.00   0.50    0.75    --   46.45  58.00  85.00  144
 23  \w    -25.00  17.00   0.50    0.75    --   46.45 -58.00 -55.00   84
 24  \w    -24.00  21.00   0.50    0.75    --  -46.45  19.00-150.00   90
 25  \w     28.00  91.00   0.50    0.75    --   46.45-125.00-180.00  126
;
_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      0.0132673000
_diffrn_orient_matrix_UB_12      -0.0080968000
_diffrn_orient_matrix_UB_13      -0.0231863000
_diffrn_orient_matrix_UB_21      0.0036078000
_diffrn_orient_matrix_UB_22      -0.0978019000
_diffrn_orient_matrix_UB_23      0.0108448000
_diffrn_orient_matrix_UB_31      -0.0144572000
_diffrn_orient_matrix_UB_32      -0.0318670000
_diffrn_orient_matrix_UB_33      -0.0274029000
_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  0.0872
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -94
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            150110
_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         68.248
_diffrn_reflns_theta_min         2.151
_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    19.428
_exptl_absorpt_correction_T_max  0.371
_exptl_absorpt_correction_T_min  0.017
_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    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             18647
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.649
_refine_diff_density_min         -2.608
_refine_diff_density_rms         0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2252
_refine_ls_number_reflns         43655
_refine_ls_number_restraints     790
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1677
_refine_ls_R_factor_gt           0.1320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1582P)^2^+2249.6082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3720
_refine_ls_wR_factor_ref         0.3966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28281
_reflns_number_total             43655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_1_96c
_cod_original_cell_volume        48066(3)
_cod_database_code               1571827
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)3'
_chemical_oxdiff_usercomment     9300-04
_shelx_estimated_absorpt_t_max   0.306
_shelx_estimated_absorpt_t_min   0.068
_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
 C1A-C2A = C2A-C3A = C4A-C3A = C5A-C4A = C6A-C5A = C6A-C1A
 1.39 with sigma of 0.02
 C1B-C2B = C3B-C2B = C3B-C4B = C5B-C4B = C5B-C6B = C6B-C1B
 1.39 with sigma of 0.02
 C7B-C8B = C9B-C8B = C9B-C10B = C11B-C10B = C11B-C12B = C12B-C7B
 1.39 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 O2A-C14A = O3A-C15A = O1A-C13A
 1.43 with sigma of 0.02
 C5B-C13B
 1.51 with sigma of 0.02
 O1B-C13B = O2B-C14B = O3B-C15B
 1.43 with sigma of 0.02
 O2B-C8B = O3B-C12B
 1.37 with sigma of 0.02
 C802-C803 = C802-C801 = C803-C804 = C804-C805 = C805-C806 = C806-C801
 1.54 with sigma of 0.02
 C810-C811 = C810-C809 = C811-C812 = C812-C807 = C807-C808 = C808-C809
 1.54 with sigma of 0.02
 C814-C813 = C814-C815 = C813-C818 = C818-C817 = C817-C816 = C816-C815
 1.54 with sigma of 0.02
 C4A-C6A = C5A-C1A
 2.4 with sigma of 0.04
 C1B-C3B = C2B-C4B = C3B-C5B = C4B-C6B = C5B-C1B = C6B-C2B
 2.4 with sigma of 0.04
 C7B-C9B = C8B-C10B = C9B-C11B = C10B-C12B = C11B-C7B = C12B-C8B
 2.4 with sigma of 0.04
 C8A-C14A
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.04
 C6B-C13B
 2.5 with sigma of 0.04
 C5B-O1B
 2.4 with sigma of 0.04
 C11B-O3B
 2.4 with sigma of 0.04
 C7B-O3B
 2.35 with sigma of 0.04
 C802-C804 = C802-C806 = C803-C805 = C804-C806 = C805-C801
 2.54 with sigma of 0.04
 C810-C812 = C810-C808 = C811-C807 = C812-C808 = C807-C809
 2.54 with sigma of 0.04
 C814-C818 = C814-C816 = C813-C817 = C818-C816 = C817-C815
 2.54 with sigma of 0.04
 C8A-C7A \\sim C9A-C8A \\sim C9A-C10A \\sim C10A-C11A \\sim C11A-C12A \\sim
C12A-C7A
 with sigma of 0.02
 C7A-C9A \\sim C8A-C10A \\sim C9A-C11A \\sim C10A-C12A \\sim C11A-C7A
 with sigma of 0.04
 O3A-C12A \\sim O2A-C8A
 with sigma of 0.02
 C1B-C4B \\sim C2B-C5B \\sim C3B-C6B
 with sigma of 0.04
 C8B-C4B \\sim C4B-C12B
 with sigma of 0.04
 C3B-C7B \\sim C7B-C5B
 with sigma of 0.04
 I318-Zn39 \\sim I418-Zn49
 with sigma of 0.02
 Zn39-I317 \\sim Zn49-I417
 with sigma of 0.02
 I318-I317 \\sim I418-I417
 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-N318 \\sim Zn45-N318
 with sigma of 0.02
 Zn35-N319 \\sim Zn45-N319
 with sigma of 0.02
 I310-I309 \\sim I410-I409
 with sigma of 0.04
 I310-N318 \\sim I410-N318
 with sigma of 0.04
 I310-N319 \\sim I410-N319
 with sigma of 0.04
 I309-N318 \\sim I409-N318
 with sigma of 0.04
 I309-N319 \\sim I409-N319
 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-N317 \\sim Zn44-N317
 with sigma of 0.02
 I307-I308 \\sim I407-I408
 with sigma of 0.04
 I307-N317 \\sim I407-N317
 with sigma of 0.04
 I308-N317 \\sim I408-N317
 with sigma of 0.04
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 I304-I303 \\sim I404-I403
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I304-N307 \\sim I404-N307
 with sigma of 0.04
 I303-N306 \\sim I403-N306
 with sigma of 0.04
 I303-N307 \\sim I403-N307
 with sigma of 0.04
 I313-Zn37 \\sim I413-Zn47
 with sigma of 0.02
 I314-Zn37 \\sim I414-Zn47
 with sigma of 0.02
 Zn37-N329 \\sim Zn47-N329
 with sigma of 0.02
 I313-I314 \\sim I413-I414
 with sigma of 0.04
 I313-N329 \\sim I413-N329
 with sigma of 0.04
 I314-N329 \\sim I414-N329
 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
 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
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 Zn33-N313 \\sim Zn43-N313
 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-N313 \\sim I406-N313
 with sigma of 0.04
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 I305-N313 \\sim I405-N313
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I504-Zn52 \\sim I404-Zn42
 with sigma of 0.02
 I303-Zn32 \\sim I503-Zn52
 with sigma of 0.02
 N307-Zn52 \\sim Zn52-N306
 with sigma of 0.02
 Zn55-N319 \\sim Zn55-N318
 with sigma of 0.02
 I312-Zn36 \\sim I412-Zn36
 with sigma of 0.02
 Zn36-I311 \\sim Zn36-I411
 with sigma of 0.02
 N331-C395 \\sim N331-C495
 with sigma of 0.02
 C393-C394 \\sim C393-C494
 with sigma of 0.02
 C394-C395 \\sim C494-C495
 with sigma of 0.02
 N331-C394 \\sim N331-C494
 with sigma of 0.04
 C393-C395 \\sim C393-C495
 with sigma of 0.04
 C802-C803 \\sim C803-C804 \\sim C804-C805 \\sim C805-C806 \\sim C806-C801
\\sim C801-C802
 with sigma of 0.02
 C802-C806 \\sim C804-C806 \\sim C803-C801 \\sim C803-C805 \\sim C805-C801
\\sim C802-C804
 with sigma of 0.04
 C810-C811 \\sim C811-C812 \\sim C812-C807 \\sim C807-C808 \\sim C808-C809
\\sim C809-C810
 with sigma of 0.02
 C810-C808 \\sim C812-C808 \\sim C811-C809 \\sim C811-C807 \\sim C807-C809
\\sim C810-C812
 with sigma of 0.04
 C814-C813 \\sim C813-C818 \\sim C818-C817 \\sim C817-C816 \\sim C816-C815
\\sim C815-C814
 with sigma of 0.02
 C814-C816 \\sim C818-C816 \\sim C813-C815 \\sim C813-C817 \\sim C817-C815
\\sim C814-C818
 with sigma of 0.04
3. Restrained planarity
 C7B, C12B, C10B, C9B, C11B, C8B
 with sigma of 0.1
 C1B, C6B, C3B, C5B, C4B, C2B
 with sigma of 0.1
 O2B, C8B, C7B, C12B, O3B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7A \\sim O3A \\sim C12A \\sim C15A \\sim C11A \\sim C4A \\sim C8A \\sim C10A
\\sim C3A \\sim C5A \\sim O2A \\sim C9A \\sim C2A \\sim C6A \\sim C13A \\sim
C14A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C7B \\sim C1B \\sim C6B \\sim C2B \\sim C5B \\sim C3B \\sim C4B \\sim C13B
\\sim O1B \\sim C12B \\sim C8B \\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
C802 \\sim C803 \\sim C804 \\sim C805 \\sim C806 \\sim C801: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C810 \\sim C811 \\sim C812 \\sim C807 \\sim C808 \\sim C809: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C814 \\sim C813 \\sim C818 \\sim C817 \\sim C816 \\sim C815: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn45) = Uanis(Zn35)
Uanis(I307) = Uanis(I407)
Uanis(Zn34) = Uanis(Zn44)
Uanis(I308) = Uanis(I408)
Uanis(C494) = Uanis(C394) = Uanis(C395) = Uanis(C495)
Uanis(Zn41) = Uanis(Zn31)
5. Rigid body (RIGU) restrains
 C7B, C1B, C6B, C2B, C5B, C3B, C4B, C13B, O1B, C12B, C8B, 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
 C802, C803, C804, C805, C806, C801
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C810, C811, C812, C807, C808, C809
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C814, C813, C818, C817, C816, C815
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I418)=Sof(Zn49)=Sof(I417)=1-FVAR(1)
 Sof(I318)=Sof(Zn39)=Sof(I317)=FVAR(1)
 Sof(I416)=Sof(Zn48)=Sof(I415)=1-FVAR(2)
 Sof(I315)=Sof(I316)=Sof(Zn38)=FVAR(2)
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(3)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(3)
 Sof(C494)=Sof(H494)=Sof(C495)=Sof(H495)=1-FVAR(4)
 Sof(C394)=Sof(H394)=Sof(C395)=Sof(H395)=FVAR(4)
 Fixed Sof: I310(0.52348) I301(0.58957) I309(0.52348) I302(0.58957)
 I313(0.67306) I314(0.67306) I304(0.45216) I303(0.45216) I307(0.630208)
 I308(0.630208) Zn35(0.52348) Zn31(0.58957) Zn32(0.45216) Zn37(0.67306)
 Zn34(0.630208) O3A(0.52075) O2A(0.52075) C3A(0.52075) H3A(0.52075)
 O1A(0.52075) H1A(0.52075) C7A(0.52075) C4A(0.52075) C2A(0.52075) H2A(0.52075)
 C5A(0.52075) C8A(0.52075) C12A(0.52075) C1A(0.52075) H1AA(0.52075)
 C11A(0.52075) H11A(0.52075) C6A(0.52075) H6A(0.52075) C15A(0.52075)
 H15A(0.52075) H15B(0.52075) H15C(0.52075) C13A(0.52075) H13A(0.52075)
 H13B(0.52075) C14A(0.52075) H14A(0.52075) H14B(0.52075) H14C(0.52075)
 C9A(0.52075) H9A(0.52075) I410(0.41758) Zn45(0.41758) I409(0.41758)
 I408(0.19716) Zn44(0.19716) I407(0.19716) I404(0.49279) Zn42(0.49279)
 I403(0.49279) I414(0.32694) Zn47(0.32694) I413(0.32694) I402(0.33413)
 Zn41(0.33413) I401(0.33413) I312(0.5) I311(0.5) I508(0.17263) I507(0.17263)
 Zn54(0.17263) I502(0.0763) I501(0.0763) Zn51(0.0763) C10A(0.52075)
 H10A(0.52075) I503(0.05506) I504(0.05506) Zn52(0.05506) I509(0.05895)
 Zn55(0.05895) I510(0.05895) I412(0.5) I411(0.5) C1B(0.19839) H1B(0.19839)
 C6B(0.19839) H6B(0.19839) C3B(0.19839) H3B(0.19839) C5B(0.19839) C4B(0.19839)
 C2B(0.19839) H2B(0.19839) C7B(0.19839) C12B(0.19839) C10B(0.19839)
 H10B(0.19839) C13B(0.19839) H13C(0.19839) H13D(0.19839) O3B(0.19839)
 C9B(0.19839) H9B(0.19839) O1B(0.19839) H1BA(0.19839) C11B(0.19839)
 H11B(0.19839) C802(0.34093) H80A(0.34093) H80B(0.34093) C803(0.34093)
 H80C(0.34093) H80D(0.34093) C804(0.34093) H80E(0.34093) H80F(0.34093)
 C805(0.34093) H80G(0.34093) H80H(0.34093) C806(0.34093) H80I(0.34093)
 H80J(0.34093) C801(0.34093) H80K(0.34093) H80L(0.34093) C15B(0.19839)
 H15D(0.19839) H15E(0.19839) H15F(0.19839) C8B(0.19839) O2B(0.19839)
 C14B(0.19839) H14D(0.19839) H14E(0.19839) H14F(0.19839) C810(0.33073)
 H81A(0.33073) H81B(0.33073) C811(0.33073) H81C(0.33073) H81D(0.33073)
 C812(0.33073) H81E(0.33073) H81F(0.33073) C807(0.33073) H80M(0.33073)
 H80N(0.33073) C808(0.33073) H80O(0.33073) H80P(0.33073) C809(0.33073)
 H80Q(0.33073) H80R(0.33073) C814(0.19007) H81G(0.19007) H81H(0.19007)
 C813(0.19007) H81I(0.19007) H81J(0.19007) C818(0.19007) H81K(0.19007)
 H81L(0.19007) C817(0.19007) H81M(0.19007) H81N(0.19007) C816(0.19007)
 H81O(0.19007) H81P(0.19007) C815(0.19007) H81Q(0.19007) H81R(0.19007)
 Fixed Uiso: I502(0.08) I501(0.08) Zn51(0.08) I503(0.08) I504(0.08) Zn52(0.08)
 I509(0.08) Zn55(0.08) I510(0.08) C814(0.08) C813(0.08) C818(0.08) C817(0.08)
 C816(0.08) C815(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13B(H13C,H13D), C802(H80A,H80B), C803(H80C,H80D), C804(H80E,
 H80F), C805(H80G,H80H), C806(H80I,H80J), C801(H80K,H80L), C810(H81A,H81B),
 C811(H81C,H81D), C812(H81E,H81F), C807(H80M,H80N), C808(H80O,H80P), C809(H80Q,
 H80R), C814(H81G,H81H), C813(H81I,H81J), C818(H81K,H81L), C817(H81M,H81N),
 C816(H81O,H81P), C815(H81Q,H81R)
7.b Aromatic/amide H refined with riding coordinates:
 C390(H390), C349(H349), C385(H385), C314(H314), C354(H354), C384(H384),
 C353(H353), C313(H313), C348(H348), C328(H328), C315(H315), C373(H373),
 C391(H391), C392(H392), C364(H364), C331(H331), C320(H320), C355(H355),
 C319(H319), C312(H312), C305(H305), C340(H340), C317(H317), C310(H310),
 C341(H341), C351(H351), C338(H338), C389(H389), C332(H332), C301(H301),
 C401(H401), C330(H330), C302(H302), C347(H347), C400(H400), C346(H346),
 C387(H387), C337(H337), C335(H335), C350(H350), C333(H333), C311(H311),
 C329(H329), C356(H356), C336(H336), C383(H383), C374(H374), C386(H386),
 C304(H304), C382(H382), C402(H402), C371(H371), C403(H403), C365(H365),
 C405(H405), C318(H318), C376(H376), C372(H372), C358(H358), C323(H323),
 C322(H322), C369(H369), C3A(H3A), C367(H367), C377(H377), C366(H366),
 C359(H359), C368(H368), C394(H394), C404(H404), C408(H408), C2A(H2A),
 C407(H407), C395(H395), C1A(H1AA), C11A(H11A), C6A(H6A), C9A(H9A), C10A(H10A),
 C494(H494), C495(H495), C1B(H1B), C6B(H6B), C3B(H3B), C2B(H2B), C10B(H10B),
 C9B(H9B), C11B(H11B)
7.c Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1B(H1BA)
7.d 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              96091
_shelx_hkl_checksum              45406
_olex2_date_sample_data_collection 2023-03-04
_olex2_date_sample_submission    2023-03-04
_olex2_submission_original_sample_id 4_1_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 2.267
_oxdiff_exptl_absorpt_empirical_full_min 0.486