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_1571853
_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, 0.502(C15 H16 O3)'
_chemical_formula_sum            'C115.54 H80.04 I18 N36 O1.51 Zn9'
_chemical_formula_weight         4869.29
_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             2024-01-31
_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                 99.913(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   78.288(6)
_cell_length_b                   14.9666(7)
_cell_length_c                   41.6314(19)
_cell_measurement_reflns_used    5360
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.2300
_cell_measurement_theta_min      2.2660
_cell_volume                     48051(5)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -113.00 -37.76   0.38    1.20    -- -103.00 136.00  28.00  198
  2  \w   -145.00-121.06   0.38    1.20    -- -103.00-136.00 -35.00   63
  3  \w   -115.00 -58.00   0.38    1.20    -- -103.00 132.00-148.00  150
  4  \w   -124.00 -92.08   0.38    1.20    -- -103.00-132.00 141.00   84
  5  \w    -67.00 -30.14   0.38    1.20    -- -103.00  61.00-150.00   97
  6  \w   -112.00 -76.66   0.38    1.20    -- -103.00-125.00-180.00   93
  7  \w   -173.00-118.28   0.38    1.20    -- -103.00-125.00-180.00  144
  8  \w   -159.00 -94.78   0.38    1.20    -- -103.00 -45.00 -90.00  169
  9  \w   -160.00 -93.12   0.38    1.20    -- -103.00 -45.00 120.00  176
 10  \w   -107.00 -41.64   0.38    1.20    -- -103.00 125.00 120.00  172
 11  \w    -83.00 -29.80   0.38    1.20    -- -103.00  77.00-120.00  140
 12  \w    -92.00 -68.06   0.38    1.20    -- -103.00  77.00-150.00   63
 13  \w   -166.00 -91.14   0.38    1.20    -- -103.00 -45.00  30.00  197
 14  \w   -141.00-112.88   0.38    1.20    -- -103.00 -15.00   0.00   74
 15  \w   -170.00-143.78   0.38    1.20    -- -103.00 -15.00   0.00   69
 16  \w    100.00 125.08   0.38    1.20    --  101.75 136.00  28.00   66
 17  \w    111.00 160.40   0.38    1.20    --  101.75 132.00-148.00  130
 18  \w     87.00 118.92   0.38    1.20    --  101.75-136.00 -35.00   84
 19  \w     49.00  74.08   0.38    1.20    --  101.75-132.00 141.00   66
 20  \w     42.00  69.36   0.38    1.20    --  101.75 -61.00-180.00   72
 21  \w     75.00 101.22   0.38    1.20    --  101.75 -77.00 -30.00   69
 22  \w     31.00  65.20   0.38    1.20    --  101.75 -61.00 -60.00   90
 23  \w     32.00 104.20   0.38    1.20    --  101.75-103.00 137.25  190
 24  \w     37.00 105.02   0.38    1.20    --  101.75-103.00  62.71  179
 25  \w     37.00  72.34   0.38    1.20    --  101.75 -61.00-150.00   93
 26  \w     30.00  71.80   0.38    1.20    --  101.75 -61.00  30.00  110
 27  \w     31.00  99.02   0.38    1.20    --  101.75 -97.00  -6.35  179
 28  \w     91.00 171.94   0.38    1.20    --  101.75  45.00-150.00  213
 29  \w     37.00  70.06   0.38    1.20    --  101.75 -61.00 -30.00   87
 30  \w     68.00 104.86   0.38    1.20    --  101.75 -97.00 152.25   97
 31  \w     31.00  56.46   0.38    1.20    --  101.75 -61.00 150.00   67
 32  \w     40.00 104.22   0.38    1.20    --  101.75 -94.00 -60.00  169
 33  \w     89.00 173.74   0.38    1.20    --  101.75  45.00 -60.00  223
 34  \w     29.00  54.08   0.38    1.20    --  101.75 -77.00 -30.00   66
 35  \w   -116.00 -68.88   0.38    0.40    --  -46.48-136.00 -35.00  124
 36  \w    -98.00 -50.88   0.38    0.40    --  -46.48 136.00  28.00  124
 37  \w    -83.00 -56.78   0.38    0.40    --  -46.48 132.00-148.00   69
 38  \w     28.00  95.26   0.38    0.40    --   46.48-132.00 141.00  177
 39  \w     40.00  65.08   0.38    0.40    --   46.48-136.00 -35.00   66
 40  \w    -39.00  26.36   0.38    0.40    --  -46.48  37.00   0.00  172
 41  \w    -22.00  18.28   0.38    0.40    --  -46.48  19.00 -30.00  106
 42  \w    -56.00 -25.98   0.38    0.40    --  -46.48 -77.00-180.00   79
 43  \w      1.00  26.08   0.38    0.40    --  -46.48  19.00 -90.00   66
 44  \w   -117.00 -89.64   0.38    0.40    --  -46.48 -77.00-180.00   72
 45  \w     24.00 114.06   0.38    0.40    --   46.48  77.00-150.00  237
 46  \w     52.00 117.36   0.38    0.40    --   46.48  37.00-180.00  172
;
_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      0.0129377000
_diffrn_orient_matrix_UB_12      -0.0066976000
_diffrn_orient_matrix_UB_13      -0.0239106000
_diffrn_orient_matrix_UB_21      -0.0098440000
_diffrn_orient_matrix_UB_22      -0.0815565000
_diffrn_orient_matrix_UB_23      -0.0163346000
_diffrn_orient_matrix_UB_31      -0.0116250000
_diffrn_orient_matrix_UB_32      0.0623721000
_diffrn_orient_matrix_UB_33      -0.0239130000
_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  0.2215
_diffrn_reflns_av_unetI/netI     0.0995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       94
_diffrn_reflns_limit_h_min       -94
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            325146
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.155
_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    19.418
_exptl_absorpt_correction_T_max  0.510
_exptl_absorpt_correction_T_min  0.048
_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    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             18091
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.786
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1941
_refine_ls_number_reflns         43965
_refine_ls_number_restraints     532
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.2225
_refine_ls_R_factor_gt           0.1636
_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^)+(0.2253P)^2^+2303.6001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4455
_refine_ls_wR_factor_ref         0.4906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23904
_reflns_number_total             43965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_10_24b
_cod_database_code               1571853
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 H12 N24 C36) (C15 H16 O3)2 (C6 H12)'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.112
_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
 C2A-C1A = C3A-C2A = C4A-C3A = C5A-C4A = C6A-C5A = C6A-C1A
 1.39 with sigma of 0.02
 C8A-C7A = C9A-C8A = C9A-C10A = C11A-C10A = C12A-C11A = C7A-C12A
 1.39 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 O1A-C13A = O2A-C14A = O3A-C15A
 1.43 with sigma of 0.02
 C1A-C3A = C2A-C4A = C4A-C6A = C5A-C1A = C6A-C2A
 2.4 with sigma of 0.04
 C7A-C9A = C8A-C10A = C9A-C11A = C10A-C12A = C11A-C7A = C12A-C8A
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.02
 C8A-C14A
 2.4 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-N306 \\sim Zn42-N306
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I303-N306 \\sim I403-N306
 with sigma of 0.04
 I309-Zn35 \\sim I409-Zn45
 with sigma of 0.02
 I303-N307 \\sim I403-N307
 with sigma of 0.04
 I310-Zn35 \\sim I410-Zn45
 with sigma of 0.02
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 Zn35-N318 \\sim Zn45-N318
 with sigma of 0.02
 I304-N307 \\sim I404-N307
 with sigma of 0.04
 Zn35-N319 \\sim Zn45-N319
 with sigma of 0.02
 I309-I310 \\sim I409-I410
 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
 I310-N318 \\sim I410-N318
 with sigma of 0.04
 I310-N319 \\sim I410-N319
 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-N311 \\sim Zn43-N311
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.02
 I306-N311 \\sim I406-N311
 with sigma of 0.02
 I305-N311 \\sim I405-N311
 with sigma of 0.02
 I318-Zn39 \\sim I418-Zn49
 with sigma of 0.02
 I317-Zn39 \\sim I417-Zn49
 with sigma of 0.02
 Zn39-N330 \\sim Zn49-N330
 with sigma of 0.02
 Zn39-N331 \\sim Zn49-N331
 with sigma of 0.02
 I318-I317 \\sim I418-I417
 with sigma of 0.04
 I318-N330 \\sim I418-N330
 with sigma of 0.04
 I318-N331 \\sim I418-N331
 with sigma of 0.04
 I317-N330 \\sim I417-N330
 with sigma of 0.04
 I317-N331 \\sim I417-N331
 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
 I313-Zn37 \\sim I413-Zn47
 with sigma of 0.02
 I314-Zn37 \\sim I414-Zn47
 with sigma of 0.02
 Zn37-N324 \\sim Zn47-N324
 with sigma of 0.02
 Zn37-N325 \\sim Zn47-N325
 with sigma of 0.02
 I313-I314 \\sim I413-I414
 with sigma of 0.04
 I313-N324 \\sim I413-N324
 with sigma of 0.04
 I313-N325 \\sim I413-N325
 with sigma of 0.04
 I314-N324 \\sim I414-N324
 with sigma of 0.04
 I314-N325 \\sim I414-N325
 with sigma of 0.04
 I312-Zn36 \\sim I412-Zn46
 with sigma of 0.02
 I311-Zn36 \\sim I411-Zn46
 with sigma of 0.02
 Zn36-N323 \\sim Zn46-N323
 with sigma of 0.02
 I312-I311 \\sim I412-I411
 with sigma of 0.04
 I312-N323 \\sim I412-N323
 with sigma of 0.04
 I311-N323 \\sim I411-N323
 with sigma of 0.04
 I312-Zn36 \\sim I2-Zn56
 with sigma of 0.02
 I316-Zn38 \\sim I416-Zn48
 with sigma of 0.02
 Zn38-N329 \\sim Zn48-N329
 with sigma of 0.02
 Zn38-I315 \\sim Zn48-I415
 with sigma of 0.02
 I316-N329 \\sim I416-N329
 with sigma of 0.04
 I316-I315 \\sim I416-I415
 with sigma of 0.04
 N329-I315 \\sim N329-I415
 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
 N318-C450 \\sim N318-C350
 with sigma of 0.02
 C352-C451 \\sim C352-C351
 with sigma of 0.02
 C451-C450 \\sim C351-C350
 with sigma of 0.02
 N318-C451 \\sim N318-C351
 with sigma of 0.04
 C352-C450 \\sim C352-C350
 with sigma of 0.04
 N313-C341 \\sim N313-C441
 with sigma of 0.02
 C339-C340 \\sim C339-C440
 with sigma of 0.02
 C340-C341 \\sim C440-C441
 with sigma of 0.02
 N313-C340 \\sim N313-C440
 with sigma of 0.04
 C339-C341 \\sim C339-C441
 with sigma of 0.04
 C363-C467 \\sim C363-C367
 with sigma of 0.02
 N323-C466 \\sim N323-C366
 with sigma of 0.02
 C467-C466 \\sim C367-C366
 with sigma of 0.02
 C363-C466 \\sim C363-C366
 with sigma of 0.04
 N323-C467 \\sim N323-C367
 with sigma of 0.04
 N325-C377 \\sim N325-C477
 with sigma of 0.02
 N325-C373 \\sim N325-C473
 with sigma of 0.02
 C375-C376 \\sim C375-C476
 with sigma of 0.02
 C375-C374 \\sim C375-C474
 with sigma of 0.02
 C377-C376 \\sim C477-C476
 with sigma of 0.02
 C373-C374 \\sim C473-C474
 with sigma of 0.02
 N325-C376 \\sim N325-C476
 with sigma of 0.04
 N325-C374 \\sim N325-C474
 with sigma of 0.04
 C375-C377 \\sim C375-C477
 with sigma of 0.04
 C375-C373 \\sim C375-C473
 with sigma of 0.04
 I417-Zn49 \\sim I517-Zn59
 with sigma of 0.02
 I518-Zn59 \\sim I318-Zn39
 with sigma of 0.02
 I504-Zn52 \\sim I304-Zn32
 with sigma of 0.02
 I503-Zn52 \\sim I303-Zn32
 with sigma of 0.02
 I502-Zn51 \\sim I402-Zn41
 with sigma of 0.02
 I501-Zn51 \\sim I401-Zn41
 with sigma of 0.02
 Zn51-N301 \\sim Zn41-N301 \\sim Zn31-N301
 with sigma of 0.02
 I501-Zn51 \\sim I301-Zn31
 with sigma of 0.02
 I502-Zn51 \\sim I302-Zn31
 with sigma of 0.02
3. Restrained planarity
 O3A, C12A, C7A, C8A, O2A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O2A \\sim C8A \\sim C14A \\sim C7A \\sim C9A \\sim C4A \\sim C12A \\sim C10A
\\sim C5A \\sim C3A \\sim O3A \\sim C11A \\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
C327 \\sim C331 \\sim C330 \\sim N311 \\sim C329 \\sim C328: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I308 \\sim I408 \\sim Zn44 \\sim Zn34 \\sim I407 \\sim I307: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I301 \\sim I401 \\sim Zn31 \\sim Zn41 \\sim I302 \\sim I402: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn49) = Uanis(Zn39)
Uanis(Zn35) = Uanis(Zn45)
Uanis(C366) = Uanis(C466) = Uanis(C367) = Uanis(C467)
Uanis(C450) = Uanis(C350) = Uanis(C351) = Uanis(C451)
Uanis(C340) = Uanis(C440) = Uanis(C441) = Uanis(C341)
Uanis(C374) = Uanis(C474) = Uanis(C473) = Uanis(C373) = Uanis(C376) =
Uanis(C476) = Uanis(C477) = Uanis(C377)
5. Rigid body (RIGU) restrains
 O2A, C8A, C14A, C7A, C9A, C4A, C12A, C10A, C5A, C3A, O3A, C11A, C6A, C13A,
 C2A, C15A, C1A, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C327, C331, C330, N311, C329, C328
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I308, I408, Zn44, Zn34, I407, I307
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I301, I401, Zn31, Zn41, I302, I402
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I409)=Sof(Zn45)=Sof(I410)=1-FVAR(1)
 Sof(I309)=Sof(I310)=Sof(Zn35)=FVAR(1)
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(2)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(2)
 Sof(I413)=Sof(Zn47)=Sof(I414)=1-FVAR(3)
 Sof(I313)=Sof(I314)=Sof(Zn37)=FVAR(3)
 Sof(Zn44)=Sof(I407)=Sof(I408)=1-FVAR(4)
 Sof(I307)=Sof(I308)=Sof(Zn34)=FVAR(4)
 Sof(C351)=Sof(H351)=Sof(C350)=Sof(H350)=1-FVAR(5)
 Sof(C451)=Sof(H451)=Sof(C450)=Sof(H450)=FVAR(5)
 Sof(C440)=Sof(H440)=Sof(C441)=Sof(H441)=1-FVAR(6)
 Sof(C340)=Sof(H340)=Sof(C341)=Sof(H341)=FVAR(6)
 Sof(C367)=Sof(H367)=Sof(C366)=Sof(H366)=1-FVAR(7)
 Sof(C467)=Sof(H467)=Sof(C466)=Sof(H466)=FVAR(7)
 Sof(C473)=Sof(H473)=Sof(C474)=Sof(H474)=Sof(C476)=Sof(H476)=Sof(C477)=
 Sof(H477)=1-FVAR(8)
 Sof(C377)=Sof(H377)=Sof(C376)=Sof(H376)=Sof(C373)=Sof(H373)=Sof(C374)=
 Sof(H374)=FVAR(8)
 Fixed Sof: I318(0.62398) I303(0.81978) I317(0.62398) I316(0.51276)
 I312(0.6974) I304(0.81978) I311(0.6974) I301(0.59374) I302(0.59374)
 Zn39(0.62398) Zn38(0.51276) Zn32(0.81978) Zn36(0.6974) Zn31(0.59374)
 O2A(0.50248) O3A(0.50248) O1A(0.50248) H1A(0.50248) C11A(0.50248)
 H11A(0.50248) C7A(0.50248) C4A(0.50248) C5A(0.50248) C6A(0.50248) H6A(0.50248)
 C1A(0.50248) H1AA(0.50248) C2A(0.50248) H2A(0.50248) C3A(0.50248) H3A(0.50248)
 C8A(0.50248) C9A(0.50248) H9A(0.50248) C10A(0.50248) H10A(0.50248)
 C13A(0.50248) H13A(0.50248) H13B(0.50248) C12A(0.50248) I418(0.35019)
 Zn49(0.35019) I417(0.35019) I403(0.08671) Zn42(0.08671) I404(0.08671)
 I401(0.31543) I402(0.31543) Zn41(0.31543) I315(0.51276) I412(0.24469)
 Zn46(0.24469) I411(0.24469) I1(0.05792) I2(0.05792) Zn56(0.05792)
 Zn48(0.48724) I416(0.48724) I415(0.48724) C15A(0.50248) H15A(0.50248)
 H15B(0.50248) H15C(0.50248) C14A(0.50248) H14A(0.50248) H14B(0.50248)
 H14C(0.50248) I517(0.02584) I518(0.02584) Zn59(0.02584) Zn52(0.09351)
 I504(0.09351) I503(0.09351) I502(0.09083) I501(0.09083) Zn51(0.09083)
 Fixed Uiso: I403(0.08) Zn42(0.08) I404(0.08) I1(0.08) I2(0.08) Zn56(0.08)
 I517(0.08) I518(0.08) Zn59(0.08) Zn52(0.08) I504(0.08) I503(0.08) I502(0.08)
 I501(0.08) Zn51(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B)
7.b Aromatic/amide H refined with riding coordinates:
 C317(H317), C389(H389), C364(H364), C328(H328), C336(H336), C318(H318),
 C384(H384), C353(H353), C354(H354), C390(H390), C394(H394), C395(H395),
 C404(H404), C405(H405), C387(H387), C372(H372), C312(H312), C385(H385),
 C359(H359), C322(H322), C329(H329), C335(H335), C355(H355), C386(H386),
 C402(H402), C358(H358), C356(H356), C407(H407), C401(H401), C403(H403),
 C320(H320), C371(H371), C313(H313), C319(H319), C323(H323), C392(H392),
 C400(H400), C368(H368), C315(H315), C365(H365), C333(H333), C408(H408),
 C377(H377), C304(H304), C369(H369), C305(H305), C340(H340), C376(H376),
 C331(H331), C310(H310), C301(H301), C338(H338), C11A(H11A), C467(H467),
 C337(H337), C466(H466), C314(H314), C302(H302), C341(H341), C311(H311),
 C373(H373), C382(H382), C6A(H6A), C1A(H1AA), C2A(H2A), C3A(H3A), C330(H330),
 C374(H374), C391(H391), C332(H332), C451(H451), C450(H450), C9A(H9A),
 C10A(H10A), C346(H346), C349(H349), C347(H347), C348(H348), C383(H383),
 C351(H351), C350(H350), C440(H440), C441(H441), C367(H367), C366(H366),
 C473(H473), C474(H474), C476(H476), C477(H477)
7.c Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C)
7.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1A)
;
_shelx_res_checksum              75611
_shelx_hkl_checksum              5724
_olex2_date_sample_data_collection 2022-08-09
_olex2_date_sample_submission    2022-08-09
_olex2_submission_original_sample_id 25_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 9.006
_oxdiff_exptl_absorpt_empirical_full_min 0.331