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_1571850
_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, 0.964(C15 H16 O3), 1.89(C6 H12)'
_chemical_formula_sum            'C133.79 H110.09 I18 N36 O2.89 Zn9'
_chemical_formula_weight         5140.97
_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             2024-01-29
_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                 100.008(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   78.4975(16)
_cell_length_b                   14.9701(2)
_cell_length_c                   41.6228(6)
_cell_measurement_reflns_used    21047
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.2880
_cell_measurement_theta_min      2.2360
_cell_volume                     48167.3(14)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -174.00 -91.16   0.38    1.00    -- -103.00 -49.00-174.00  218
  2  \w    -69.00 -31.00   0.38    1.00    -- -103.00  61.00 -60.00  100
  3  \w   -104.00 -31.04   0.38    1.00    -- -103.00  77.00-120.00  192
  4  \w   -174.00 -91.16   0.38    1.00    -- -103.00 -45.00 -90.00  218
  5  \w    -69.00 -31.00   0.38    1.00    -- -103.00  61.00 -90.00  100
  6  \w    -69.00 -31.00   0.38    1.00    -- -103.00  61.00   0.00  100
  7  \w    -69.00 -31.00   0.38    1.00    -- -103.00  61.00 -30.00  100
  8  \w   -112.00 -31.06   0.38    1.00    -- -103.00 125.00  60.00  213
  9  \w    -69.00 -31.00   0.38    1.00    -- -103.00  61.00  30.00  100
 10  \w    -69.00 -31.00   0.38    1.00    -- -103.00  61.00-180.00  100
 11  \w    -69.00 -31.00   0.38    1.00    -- -103.00  61.00 150.00  100
 12  \w     89.00 172.98   0.38    1.00    --  101.75  49.00 -26.00  221
 13  \w     29.00  55.98   0.38    1.00    --  101.75 -49.00-174.00   71
 14  \w     29.00  71.94   0.38    1.00    --  101.75 -61.00  30.00  113
 15  \w     89.00 172.98   0.38    1.00    --  101.75  45.00  90.00  221
 16  \w     29.00 105.00   0.38    1.00    --  101.75 -94.00-180.00  200
 17  \w     29.00  71.94   0.38    1.00    --  101.75 -61.00   0.00  113
 18  \w    -53.00  24.90   0.38    0.20    --  -46.48  49.00 -26.00  205
 19  \w     33.00 117.74   0.38    0.20    --   46.48  49.00 -26.00  223
 20  \w    -25.00  55.94   0.38    0.20    --   46.48 -49.00-174.00  213
 21  \w   -118.00 -34.02   0.38    0.20    --  -46.48 -49.00-174.00  221
 22  \w    -24.00  27.68   0.38    0.20    --  -46.48  19.00 120.00  136
 23  \w    -40.00  25.74   0.38    0.20    --  -46.48  37.00 120.00  173
 24  \w     24.00  96.20   0.38    0.20    --   46.48  77.00  60.00  190
;
_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      0.0140120000
_diffrn_orient_matrix_UB_12      0.0115967000
_diffrn_orient_matrix_UB_13      -0.0214058000
_diffrn_orient_matrix_UB_21      -0.0122869000
_diffrn_orient_matrix_UB_22      0.0606236000
_diffrn_orient_matrix_UB_23      -0.0233621000
_diffrn_orient_matrix_UB_31      0.0070615000
_diffrn_orient_matrix_UB_32      0.0823489000
_diffrn_orient_matrix_UB_33      0.0202004000
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            224407
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.156
_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    19.406
_exptl_absorpt_correction_T_max  0.383
_exptl_absorpt_correction_T_min  0.089
_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    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             19296
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.955
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2493
_refine_ls_number_reflns         44037
_refine_ls_number_restraints     1166
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0931
_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^)+(0.1206P)^2^+875.7648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2669
_refine_ls_wR_factor_ref         0.2849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31697
_reflns_number_total             44037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_5_96b
_cod_database_code               1571850
_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   0.344
_shelx_estimated_absorpt_t_min   0.120
_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
 O1A-C13A = O2A-C14A = O3A-C15A
 1.43 with sigma of 0.02
 C2B-C1B = C2B-C3B = C3B-C4B = C5B-C4B = C6B-C5B = C1B-C6B
 1.39 with sigma of 0.02
 C8B-C7B = C8B-C9B = C10B-C9B = C11B-C10B = C12B-C11B = C7B-C12B
 1.39 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 C7B-C4B
 1.5 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
 C831-C836 = C831-C832 = C836-C835 = C835-C834 = C834-C833 = C833-C832
 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
 C810-C811 = C810-C809 = C811-C812 = C812-C807 = C807-C808 = C808-C809
 1.54 with sigma of 0.02
 C1-C8 = C1-C12 = C8-C9 = C9-C10 = C10-C11 = C11-C12
 1.54 with sigma of 0.02
 C813-C818 = C813-C814 = C818-C817 = C817-C816 = C816-C815 = C815-C814
 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
 C830-C829 = C830-C825 = C829-C828 = C828-C827 = C827-C826 = C826-C825
 1.54 with sigma of 0.02
 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
 C5A-O1A
 2.4 with sigma of 0.01
 C5B-O1B
 2.4 with sigma of 0.02
 C12B-C15B
 2.4 with sigma of 0.04
 C9B-O2B
 2.45 with sigma of 0.04
 C8B-C14B
 2.4 with sigma of 0.02
 C831-C835 = C831-C833 = C836-C834 = C835-C833 = C834-C832
 2.54 with sigma of 0.04
 C804-C802 = C804-C806 = C803-C801 = C802-C806 = C801-C805
 2.54 with sigma of 0.04
 C810-C812 = C810-C808 = C811-C807 = C812-C808 = C807-C809
 2.54 with sigma of 0.04
 C1-C9 = C1-C11 = C8-C10 = C9-C11 = C10-C12
 2.54 with sigma of 0.04
 C813-C817 = C813-C815 = C818-C816 = C817-C815 = C816-C814
 2.54 with sigma of 0.04
 C823-C821 = C823-C819 = C822-C820 = C821-C819 = C820-C824
 2.54 with sigma of 0.04
 C830-C828 = C830-C826 = C829-C827 = C828-C826 = C827-C825
 2.54 with sigma of 0.04
 C9A-C8A \\sim C8A-C7A \\sim C12A-C7A \\sim C12A-C11A \\sim C10A-C11A \\sim
C10A-C9A
 with sigma of 0.02
 C8A-C10A \\sim C9A-C11A
 with sigma of 0.04
 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
 C831-C836 \\sim C836-C835 \\sim C835-C834 \\sim C834-C833 \\sim C833-C832
\\sim C832-C831
 with sigma of 0.02
 C831-C833 \\sim C835-C833 \\sim C836-C832 \\sim C836-C834 \\sim C834-C832
\\sim C831-C835
 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
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 Zn43-N311 \\sim Zn33-N311
 with sigma of 0.02
 I404-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 I403-N307 \\sim I303-N307
 with sigma of 0.04
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 Zn42-N306 \\sim Zn32-N306
 with sigma of 0.02
 Zn42-N307 \\sim Zn32-N307
 with sigma of 0.02
 I403-N306 \\sim I303-N306
 with sigma of 0.04
 I404-I403 \\sim I304-I303
 with sigma of 0.04
 I404-N306 \\sim I304-N306
 with sigma of 0.04
 I404-N307 \\sim I304-N307
 with sigma of 0.04
 I311-N318 \\sim I411-N318
 with sigma of 0.04
 I312-N318 \\sim I412-N318
 with sigma of 0.04
 I311-Zn36 \\sim I411-Zn46
 with sigma of 0.02
 I311-I312 \\sim I411-I412
 with sigma of 0.04
 I312-Zn36 \\sim I412-Zn46
 with sigma of 0.02
 I311-N319 \\sim I411-N319
 with sigma of 0.04
 Zn36-N318 \\sim Zn46-N318
 with sigma of 0.02
 Zn36-N319 \\sim Zn46-N319
 with sigma of 0.02
 I312-N319 \\sim I412-N319
 with sigma of 0.04
 I405-N311 \\sim I305-N311
 with sigma of 0.04
 I406-N311 \\sim I306-N311
 with sigma of 0.04
 I405-I406 \\sim I305-I306
 with sigma of 0.04
 I301-I302 \\sim I401-I402
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I302-N301 \\sim I402-N301
 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
 I313-N324 \\sim I413-N324
 with sigma of 0.04
 I314-N324 \\sim I414-N324
 with sigma of 0.04
 I313-I314 \\sim I413-I414
 with sigma of 0.04
 Zn37-N324 \\sim Zn47-N324
 with sigma of 0.02
 I313-N325 \\sim I413-N325
 with sigma of 0.04
 Zn37-N325 \\sim Zn47-N325
 with sigma of 0.02
 I314-N325 \\sim I414-N325
 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
 I316-N329 \\sim I416-N329
 with sigma of 0.04
 I315-N329 \\sim I415-N329
 with sigma of 0.04
 I315-Zn38 \\sim I415-Zn48
 with sigma of 0.02
 Zn38-N329 \\sim Zn48-N329
 with sigma of 0.02
 I316-I315 \\sim I416-I415
 with sigma of 0.04
 I316-Zn38 \\sim I416-Zn48
 with sigma of 0.02
 I310-I309 \\sim I410-I409
 with sigma of 0.04
 I310-Zn35 \\sim I410-Zn45
 with sigma of 0.02
 I310-N317 \\sim I410-N317
 with sigma of 0.04
 I309-Zn35 \\sim I409-Zn45
 with sigma of 0.02
 I309-N317 \\sim I409-N317
 with sigma of 0.04
 Zn35-N317 \\sim Zn45-N317
 with sigma of 0.02
 I307-Zn34 \\sim I407-Zn44
 with sigma of 0.02
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 I308-N313 \\sim I408-N313
 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-N312 \\sim I408-N312
 with sigma of 0.04
 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
 I318-N331 \\sim I418-N331
 with sigma of 0.04
 I317-N331 \\sim I417-N331
 with sigma of 0.04
 I318-I317 \\sim I418-I417
 with sigma of 0.04
 I318-Zn39 \\sim I418-Zn49
 with sigma of 0.02
 I318-N330 \\sim I418-N330
 with sigma of 0.04
 I317-N330 \\sim I417-N330
 with sigma of 0.04
 I317-Zn39 \\sim I417-Zn49
 with sigma of 0.02
 Zn39-N331 \\sim Zn49-N331
 with sigma of 0.02
 Zn39-N330 \\sim Zn49-N330
 with sigma of 0.02
 I509-Zn55 \\sim I309-Zn35
 with sigma of 0.02
 I310-Zn35 \\sim I510-Zn55
 with sigma of 0.02
 Zn55-N317 \\sim Zn35-N317
 with sigma of 0.02
 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
 C1-C8 \\sim C8-C9 \\sim C9-C10 \\sim C10-C11 \\sim C11-C12 \\sim C12-C1
 with sigma of 0.02
 C1-C11 \\sim C9-C11 \\sim C8-C12 \\sim C8-C10 \\sim C10-C12 \\sim C1-C9
 with sigma of 0.04
 C813-C818 \\sim C818-C817 \\sim C817-C816 \\sim C816-C815 \\sim C815-C814
\\sim C814-C813
 with sigma of 0.02
 C813-C815 \\sim C817-C815 \\sim C818-C814 \\sim C818-C816 \\sim C816-C814
\\sim C813-C817
 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
 C830-C829 \\sim C829-C828 \\sim C828-C827 \\sim C827-C826 \\sim C826-C825
\\sim C825-C830
 with sigma of 0.02
 C830-C826 \\sim C828-C826 \\sim C829-C825 \\sim C829-C827 \\sim C827-C825
\\sim C830-C828
 with sigma of 0.04
3. Restrained planarity
 C1B, C2B, C3B, C4B, C5B, C6B
 with sigma of 0.1
 C9B, C10B, C7B, C8B, C11B, C12B
 with sigma of 0.1
 O2B, C8B, C7B, C12B, O3B
 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 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 C3B \\sim C2B \\sim C5B \\sim C7B \\sim C1B \\sim C6B \\sim C13B
\\sim C8B \\sim C12B \\sim O1B \\sim C9B \\sim O2B \\sim C11B \\sim O3B \\sim
C10B \\sim C14B \\sim C15B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C831 \\sim C836 \\sim C835 \\sim C834 \\sim C833 \\sim C832: 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
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
C1 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C813 \\sim C818 \\sim C817 \\sim C816 \\sim C815 \\sim C814: 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
C830 \\sim C829 \\sim C828 \\sim C827 \\sim C826 \\sim C825: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn33) = Uanis(Zn43)
5. Rigid body (RIGU) restrains
 C4B, C3B, C2B, C5B, C7B, C1B, C6B, C13B, C8B, C12B, O1B, C9B, O2B, C11B, O3B,
 C10B, C14B, C15B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C831, C836, C835, C834, C833, C832
 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
 C810, C811, C812, C807, C808, C809
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C813, C818, C817, C816, C815, C814
 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
 C830, C829, C828, C827, C826, C825
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(I316)+Sof(I315)+Sof(Zn38)]+1*[Sof(Zn48)+Sof(I415)+Sof(I416)]+1*
 [Sof(I515)+Sof(I516)+Sof(Zn58)]=1 with esd of 0.00001
 1*[Sof(I310)+Sof(I309)+Sof(Zn35)]+1*[Sof(I409)+Sof(Zn45)+Sof(I410)]+1*
 [Sof(I510)+Sof(I509)+Sof(Zn55)]=1 with esd of 0.00001
 Sof(I303)=Sof(Zn32)=Sof(I304)=1-FVAR(1)
 Sof(I404)=Sof(I403)=Sof(Zn42)=FVAR(1)
 Sof(I417)=Sof(Zn49)=Sof(I418)=1-FVAR(2)
 Sof(I318)=Sof(I317)=Sof(Zn39)=FVAR(2)
 Sof(I316)=Sof(I315)=Sof(Zn38)=FVAR(3)
 Sof(Zn48)=Sof(I415)=Sof(I416)=FVAR(4)
 Sof(I515)=Sof(I516)=Sof(Zn58)=FVAR(5)
 Sof(I310)=Sof(I309)=Sof(Zn35)=FVAR(6)
 Sof(I409)=Sof(Zn45)=Sof(I410)=FVAR(7)
 Sof(I510)=Sof(I509)=Sof(Zn55)=FVAR(8)
 Fixed Sof: I311(0.55619) I307(0.53905) I308(0.53905) I313(0.32648)
 I405(0.29549) I312(0.55619) I314(0.32648) I406(0.29549) I301(0.39665)
 I302(0.39665) Zn36(0.55619) Zn43(0.29549) Zn34(0.53905) Zn37(0.32648)
 Zn31(0.39665) O2A(0.7253) O3A(0.7253) O1A(0.7253) H1A(0.7253) C7A(0.7253)
 C4A(0.7253) C5A(0.7253) C6A(0.7253) H6A(0.7253) C1A(0.7253) H1AA(0.7253)
 C2A(0.7253) H2A(0.7253) C3A(0.7253) H3A(0.7253) C8A(0.7253) C11A(0.7253)
 H11A(0.7253) C12A(0.7253) C14A(0.7253) H14A(0.7253) H14B(0.7253) H14C(0.7253)
 C9A(0.7253) H9A(0.7253) C10A(0.7253) H10A(0.7253) C13A(0.7253) H13A(0.7253)
 H13B(0.7253) I411(0.4438) Zn46(0.4438) I412(0.4438) I305(0.65836)
 Zn33(0.65836) I306(0.65836) I401(0.26029) Zn41(0.26029) I402(0.26029)
 I413(0.48278) Zn47(0.48278) I414(0.48278) I407(0.40995) Zn44(0.40995)
 I408(0.40995) I505(0.04615) I506(0.04615) Zn53(0.04615) I501(0.34306)
 I502(0.34306) Zn51(0.34306) I514(0.19075) I513(0.19075) Zn57(0.19075)
 I508(0.051) I507(0.051) Zn54(0.051) C15A(0.7253) H15A(0.7253) H15B(0.7253)
 H15C(0.7253) C3B(0.23832) H3B(0.23832) C4B(0.23832) C5B(0.23832) C6B(0.23832)
 H6B(0.23832) C9B(0.23832) H9B(0.23832) C10B(0.23832) H10B(0.23832)
 C1B(0.23832) H1B(0.23832) C2B(0.23832) H2B(0.23832) C7B(0.23832) O2B(0.23832)
 C8B(0.23832) C810(0.33677) H81A(0.33677) H81B(0.33677) C811(0.33677)
 H81C(0.33677) H81D(0.33677) C812(0.33677) H81E(0.33677) H81F(0.33677)
 C807(0.33677) H80A(0.33677) H80B(0.33677) C808(0.33677) H80C(0.33677)
 H80D(0.33677) C809(0.33677) H80E(0.33677) H80F(0.33677) C1(0.17696)
 H1C(0.17696) H1D(0.17696) C8(0.17696) H8A(0.17696) H8B(0.17696) C9(0.17696)
 H9C(0.17696) H9D(0.17696) C10(0.17696) H10C(0.17696) H10D(0.17696)
 C11(0.17696) H11C(0.17696) H11D(0.17696) C12(0.17696) H12A(0.17696)
 H12B(0.17696) C813(0.27525) H81G(0.27525) H81H(0.27525) C818(0.27525)
 H81I(0.27525) H81J(0.27525) C817(0.27525) H81K(0.27525) H81L(0.27525)
 C816(0.27525) H81M(0.27525) H81N(0.27525) C815(0.27525) H81O(0.27525)
 H81P(0.27525) C814(0.27525) H81Q(0.27525) H81R(0.27525) C823(0.24323)
 H82A(0.24323) H82B(0.24323) C822(0.24323) H82C(0.24323) H82D(0.24323)
 C821(0.24323) H82E(0.24323) H82F(0.24323) C820(0.24323) H82G(0.24323)
 H82H(0.24323) C819(0.24323) H81S(0.24323) H81T(0.24323) C824(0.24323)
 H82I(0.24323) H82J(0.24323) C11B(0.23832) H11B(0.23832) O3B(0.23832)
 C12B(0.23832) C13B(0.23832) H13C(0.23832) H13D(0.23832) O1B(0.23832)
 H1BA(0.23832) C830(0.28876) H83A(0.28876) H83B(0.28876) C829(0.28876)
 H82K(0.28876) H82L(0.28876) C828(0.28876) H82M(0.28876) H82N(0.28876)
 C827(0.28876) H82O(0.28876) H82P(0.28876) C826(0.28876) H82Q(0.28876)
 H82R(0.28876) C825(0.28876) H82S(0.28876) H82T(0.28876) C14B(0.23832)
 H14D(0.23832) H14E(0.23832) H14F(0.23832) C15B(0.23832) H15D(0.23832)
 H15E(0.23832) H15F(0.23832) C804(0.35291) H80G(0.35291) H80H(0.35291)
 C803(0.35291) H80I(0.35291) H80J(0.35291) C802(0.35291) H80K(0.35291)
 H80L(0.35291) C801(0.35291) H80M(0.35291) H80N(0.35291) C806(0.35291)
 H80O(0.35291) H80P(0.35291) C805(0.35291) H80Q(0.35291) H80R(0.35291)
 C831(0.21574) H83C(0.21574) H83D(0.21574) C836(0.21574) H83E(0.21574)
 H83F(0.21574) C835(0.21574) H83G(0.21574) H83H(0.21574) C834(0.21574)
 H83I(0.21574) H83J(0.21574) C833(0.21574) H83K(0.21574) H83L(0.21574)
 C832(0.21574) H83M(0.21574) H83N(0.21574)
 Fixed Uiso: I505(0.08) I506(0.08) Zn53(0.08) I515(0.08) I516(0.08) Zn58(0.08)
 I508(0.08) I507(0.08) Zn54(0.08) I510(0.08) I509(0.08) Zn55(0.08) C810(0.08)
 C811(0.08) C812(0.08) C807(0.08) C808(0.08) C809(0.08) C831(0.08) C836(0.08)
 C835(0.08) C834(0.08) C833(0.08) C832(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C810(H81A,H81B), C811(H81C,H81D), C812(H81E,H81F), C807(H80A,
 H80B), C808(H80C,H80D), C809(H80E,H80F), C1(H1C,H1D), C8(H8A,H8B), C9(H9C,H9D),
  C10(H10C,H10D), C11(H11C,H11D), C12(H12A,H12B), C813(H81G,H81H), C818(H81I,
 H81J), C817(H81K,H81L), C816(H81M,H81N), C815(H81O,H81P), C814(H81Q,H81R),
 C823(H82A,H82B), C822(H82C,H82D), C821(H82E,H82F), C820(H82G,H82H), C819(H81S,
 H81T), C824(H82I,H82J), C13B(H13C,H13D), C830(H83A,H83B), C829(H82K,H82L),
 C828(H82M,H82N), C827(H82O,H82P), C826(H82Q,H82R), C825(H82S,H82T), C804(H80G,
 H80H), C803(H80I,H80J), C802(H80K,H80L), C801(H80M,H80N), C806(H80O,H80P),
 C805(H80Q,H80R), C831(H83C,H83D), C836(H83E,H83F), C835(H83G,H83H), C834(H83I,
 H83J), C833(H83K,H83L), C832(H83M,H83N)
7.b Aromatic/amide H refined with riding coordinates:
 C317(H317), C346(H346), C320(H320), C332(H332), C333(H333), C336(H336),
 C347(H347), C318(H318), C319(H319), C329(H329), C312(H312), C354(H354),
 C322(H322), C328(H328), C313(H313), C364(H364), C335(H335), C400(H400),
 C349(H349), C353(H353), C371(H371), C356(H356), C6A(H6A), C1A(H1AA), C2A(H2A),
 C3A(H3A), C348(H348), C355(H355), C372(H372), C368(H368), C359(H359),
 C315(H315), C338(H338), C391(H391), C341(H341), C351(H351), C331(H331),
 C323(H323), C358(H358), C314(H314), C369(H369), C340(H340), C392(H392),
 C390(H390), C365(H365), C394(H394), C404(H404), C385(H385), C408(H408),
 C337(H337), C330(H330), C11A(H11A), C389(H389), C401(H401), C407(H407),
 C405(H405), C395(H395), C376(H376), C366(H366), C305(H305), C384(H384),
 C304(H304), C403(H403), C367(H367), C373(H373), C377(H377), C9A(H9A),
 C302(H302), C10A(H10A), C350(H350), C301(H301), C382(H382), C374(H374),
 C402(H402), C310(H310), C383(H383), C311(H311), C387(H387), C386(H386),
 C3B(H3B), C6B(H6B), C9B(H9B), C10B(H10B), C1B(H1B), C2B(H2B), C11B(H11B)
7.c Fitted hexagon refined as free rotating group:
 C4A(C5A,C6A,C1A,C2A,C3A)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1B(H1BA)
7.e Idealised Me refined with everything fixed:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C14B(H14D,H14E,H14F), C15B(H15D,
 H15E,H15F)
;
_shelx_res_checksum              56324
_shelx_hkl_checksum              52051
_olex2_date_sample_data_collection 2022-06-13
_olex2_date_sample_submission    2022-06-13
_olex2_submission_original_sample_id 25_5_96b
_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 3.000
_oxdiff_exptl_absorpt_empirical_full_min 0.535