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_1571821
_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, 0.734(C15 H16 O3), 1.444(C6 H12)'
_chemical_formula_sum            'C127.68 H101.08 I18 N36 O2.2 Zn9'
_chemical_formula_weight         5047.47
_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             2024-02-01
_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                 99.929(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   78.299(4)
_cell_length_b                   14.9565(3)
_cell_length_c                   41.6827(16)
_cell_measurement_reflns_used    7865
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.9470
_cell_measurement_theta_min      2.5930
_cell_volume                     48083(3)
_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_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 Arc-100'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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   -124.00 -98.92   0.38    2.50    -- -103.00 -20.00  30.00   66
  2  \w   -104.00 -65.24   0.38    2.50    -- -103.00 125.00 -90.00  102
  3  \w    -79.00 -36.82   0.38    2.50    -- -103.00  77.00  60.00  111
  4  \w    -64.00 -39.68   0.38    2.50    -- -103.00  61.00 -60.00   64
  5  \w     88.00 167.42   0.38    2.50    --  101.75  20.00-161.00  209
  6  \w     38.00  65.36   0.38    2.50    --  101.75 -61.00  60.00   72
  7  \w     31.00  69.00   0.38    2.50    --  101.75 -61.00-180.00  100
  8  \w     29.00  71.94   0.38    2.50    --  101.75 -61.00-120.00  113
  9  \w     38.00  71.82   0.38    2.50    --  101.75 -61.00 -90.00   89
 10  \w     35.00 111.00   0.38    2.50    --  101.75-125.00  30.00  200
 11  \w     95.00 173.66   0.38    2.50    --  101.75  15.00 120.00  207
 12  \w     36.00  62.22   0.38    2.50    --  101.75 -61.00  90.00   69
 13  \w     33.00  71.76   0.38    2.50    --  101.75 -61.00 -60.00  102
 14  \w    106.00 170.22   0.38    2.50    --  101.75  61.00-150.00  169
 15  \w     38.00  71.82   0.38    2.50    --  101.75 -61.00-150.00   89
 16  \w     35.00  70.34   0.38    2.50    --  101.75-125.00-150.00   93
 17  \w    -22.00   3.08   0.38    0.70    --  -46.01  20.00-161.00   66
 18  \w   -120.00 -34.12   0.38    0.70    --  -46.01 -20.00  30.00  226
 19  \w     35.00 108.34   0.38    0.70    --   46.01  20.00-161.00  193
 20  \w    -25.00   1.22   0.38    0.70    --   46.01 -20.00  30.00   69
 21  \w    -24.00   1.08   0.38    0.70    --  -46.01  19.00-180.00   66
 22  \w     64.00  90.22   0.38    0.70    --   46.01-125.00-150.00   69
 23  \w    -25.00  41.12   0.38    0.70    --   46.01 -37.00-120.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details
'Rigaku Oxford Difffraction, 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      -0.0198423000
_diffrn_orient_matrix_UB_12      0.0113113000
_diffrn_orient_matrix_UB_13      -0.0050679000
_diffrn_orient_matrix_UB_21      0.0001754000
_diffrn_orient_matrix_UB_22      -0.0245809000
_diffrn_orient_matrix_UB_23      0.0359516000
_diffrn_orient_matrix_UB_31      0.0022895000
_diffrn_orient_matrix_UB_32      0.0993568000
_diffrn_orient_matrix_UB_33      0.0094503000
_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  0.0784
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       93
_diffrn_reflns_limit_h_min       -94
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            151389
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.152
_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    19.427
_exptl_absorpt_correction_T_max  0.336
_exptl_absorpt_correction_T_min  0.133
_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    1.395
_exptl_crystal_description       block
_exptl_crystal_F_000             18886
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.722
_refine_diff_density_min         -1.857
_refine_diff_density_rms         0.310
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2145
_refine_ls_number_reflns         43690
_refine_ls_number_restraints     1144
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.2027
_refine_ls_R_factor_gt           0.1602
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1574P)^2^+3867.7375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4183
_refine_ls_wR_factor_ref         0.4444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26882
_reflns_number_total             43690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_1_24c
_cod_original_formula_sum        'C127.68 H101.08 I18 N36 O2.20 Zn9'
_cod_database_code               1571821
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)3'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.274
_shelx_estimated_absorpt_t_min   0.147
_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
 C1B-C6B = C1B-C2B = C3B-C2B = C3B-C4B = C5B-C4B = C6B-C5B
 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
 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
 C5B-C13B
 1.51 with sigma of 0.02
 O1A-C13A
 1.43 with sigma of 0.02
 C7B-C4B
 1.5 with sigma of 0.02
 O1B-C13B = O3B-C15B = O2B-C14B
 1.43 with sigma of 0.02
 O2B-C8B = O3B-C12B
 1.37 with sigma of 0.02
 C824-C819 = C824-C823 = C819-C820 = C820-C821 = C821-C822 = C822-C823
 1.54 with sigma of 0.02
 C802-C803 = C802-C801 = C803-C804 = C804-C805 = C805-C806 = C806-C801
 1.54 with sigma of 0.02
 C818-C817 = C818-C813 = C817-C816 = C816-C815 = C815-C814 = C814-C813
 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
 C2B-C4B = C4B-C6B = C5B-C1B = C6B-C2B
 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
 C7B-C9B = C8B-C10B = C9B-C11B = C10B-C12B = C11B-C7B = C12B-C8B
 2.4 with sigma of 0.04
 O1B-C5B
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.02
 C8A-C14A = C12A-C15A
 2.4 with sigma of 0.04
 C8B-C14B
 2.4 with sigma of 0.04
 C12B-C15B
 2.4 with sigma of 0.04
 C4B-C13B = C13B-C6B
 2.5 with sigma of 0.04
 C824-C820 = C824-C822 = C819-C821 = C820-C822 = C821-C823
 2.54 with sigma of 0.04
 C802-C804 = C802-C806 = C803-C805 = C804-C806 = C805-C801
 2.54 with sigma of 0.04
 C818-C816 = C818-C814 = C817-C815 = C816-C814 = C815-C813
 2.54 with sigma of 0.04
 C810-C812 = C810-C808 = C811-C807 = C812-C808 = C807-C809
 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
 O2A-C14A \\sim O3A-C15A
 with sigma of 0.02
 O3A-C12A \\sim O2A-C8A
 with sigma of 0.02
 C824-C819 \\sim C819-C820 \\sim C820-C821 \\sim C821-C822 \\sim C822-C823
\\sim C823-C824
 with sigma of 0.02
 C824-C822 \\sim C820-C822 \\sim C819-C823 \\sim C819-C821 \\sim C821-C823
\\sim C824-C820
 with sigma of 0.04
 I415-Zn48 \\sim I315-Zn38
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I416-Zn48 \\sim I316-Zn38
 with sigma of 0.02
 Zn48-N330 \\sim Zn38-N330
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 Zn48-N331 \\sim Zn38-N331
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 I415-I416 \\sim I315-I316
 with sigma of 0.04
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I415-N330 \\sim I315-N330
 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
 I415-N331 \\sim I315-N331
 with sigma of 0.04
 I416-N330 \\sim I316-N330
 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
 I416-N331 \\sim I316-N331
 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
 I305-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I306-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 Zn33-N311 \\sim Zn43-N311
 with sigma of 0.02
 I305-I306 \\sim I406-I405
 with sigma of 0.04
 I305-N311 \\sim I406-N311
 with sigma of 0.04
 I306-N311 \\sim I405-N311
 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
 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
 I314-Zn37 \\sim I414-Zn47
 with sigma of 0.02
 I313-Zn37 \\sim I413-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
 I314-I313 \\sim I414-I413
 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
 I313-N324 \\sim I413-N324
 with sigma of 0.04
 I313-N325 \\sim I413-N325
 with sigma of 0.04
 N324-Zn57 \\sim Zn57-N325
 with sigma of 0.02
 N331-Zn58 \\sim Zn58-N330
 with sigma of 0.02
 Zn56-N323 \\sim Zn36-N323
 with sigma of 0.02
 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
 C818-C817 \\sim C817-C816 \\sim C816-C815 \\sim C815-C814 \\sim C814-C813
\\sim C813-C818
 with sigma of 0.02
 C818-C814 \\sim C816-C814 \\sim C817-C813 \\sim C817-C815 \\sim C815-C813
\\sim C818-C816
 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
 C377-C373 \\sim C376-C374
 with sigma of 0.02
3. Restrained planarity
 C4B, C5B, C2B, C6B, C3B, C1B
 with sigma of 0.1
 C7A, C9A, C10A, C12A, C8A, C11A
 with sigma of 0.1
 C7B, C10B, C9B, C12B, C11B, C8B
 with sigma of 0.1
 O2B, C8B, C7B, C12B, O3B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C5A \\sim O3A \\sim C12A \\sim C15A \\sim C7A \\sim C11A \\sim C4A \\sim C8A
\\sim C10A \\sim C3A \\sim O2A \\sim C9A \\sim C6A \\sim C13A \\sim C2A \\sim
C14A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C824 \\sim C819 \\sim C820 \\sim C821 \\sim C822 \\sim C823: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C391 \\sim C392 \\sim C393 \\sim C394 \\sim C395 \\sim N331: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Zn37 \\sim I314 \\sim I313: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
I413 \\sim I313 \\sim I414 \\sim I314: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C304 \\sim C305 \\sim N301 \\sim C301 \\sim C302 \\sim C303: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C363 \\sim C364 \\sim C365 \\sim N323 \\sim C366 \\sim C367: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N336 \\sim C406 \\sim C404 \\sim C408 \\sim C407 \\sim C405: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I405 \\sim I306 \\sim Zn43 \\sim Zn33 \\sim I406 \\sim I305: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I311 \\sim I411 \\sim Zn36 \\sim Zn46 \\sim I312 \\sim I412: 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
C818 \\sim C817 \\sim C816 \\sim C815 \\sim C814 \\sim C813: 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
Uanis(Zn38) = Uanis(Zn48)
Uanis(Zn47) = Uanis(Zn37)
5. Rigid body (RIGU) restrains
 C824, C819, C820, C821, C822, C823
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Zn37, I314, I313
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I413, I313, I414, I314
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C304, C305, N301, C301, C302, C303
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C363, C364, C365, N323, C366, C367
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N336, C406, C404, C405, C408, C407
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I405, I306, Zn43, Zn33, I406, I305
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I311, I411, Zn36, Zn46, I312, I412
 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
 C818, C817, C816, C815, C814, C813
 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
 N322, N320, N321, C360, C362, C361
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N331, C393, C395, C392, C394, C391
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N306, C316, C318, C317, C314, C315
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N313, C339, C340, C337, C338, C341
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(I318)+Sof(I317)+Sof(Zn39)]+1*[Sof(I418)+Sof(I417)+Sof(Zn49)]=1 with
 esd of 0.00001
 1*[Sof(I301)+Sof(I302)+Sof(Zn31)]+1*[Sof(I401)+Sof(Zn41)+Sof(I402)]=1 with
 esd of 0.00001
 Sof(I407)=Sof(Zn44)=Sof(I408)=1-FVAR(1)
 Sof(I307)=Sof(I308)=Sof(Zn34)=FVAR(1)
 Sof(I318)=Sof(I317)=Sof(Zn39)=FVAR(2)
 Sof(I418)=Sof(I417)=Sof(Zn49)=FVAR(3)
 Sof(I301)=Sof(I302)=Sof(Zn31)=FVAR(4)
 Sof(I401)=Sof(Zn41)=Sof(I402)=FVAR(5)
 Fixed Sof: I415(0.44551) I312(0.48397) I311(0.48397) I314(0.82828)
 I313(0.82828) I416(0.44551) I303(0.49839) I304(0.49839) I305(0.55821)
 I306(0.55821) Zn36(0.48397) Zn48(0.44551) Zn37(0.82828) Zn32(0.49839)
 Zn33(0.55821) O3A(0.62169) O2A(0.62169) C5A(0.62169) C7A(0.62169) C4A(0.62169)
 C3A(0.62169) H3A(0.62169) O1A(0.62169) H1A(0.62169) C1A(0.62169) H1AA(0.62169)
 C12A(0.62169) C6A(0.62169) H6A(0.62169) C8A(0.62169) C11A(0.62169)
 H11A(0.62169) C2A(0.62169) H2A(0.62169) C9A(0.62169) H9A(0.62169)
 C14A(0.62169) H14A(0.62169) H14B(0.62169) H14C(0.62169) C10A(0.62169)
 H10A(0.62169) C15A(0.62169) H15A(0.62169) H15B(0.62169) H15C(0.62169)
 C13A(0.62169) H13A(0.62169) H13B(0.62169) I315(0.51671) Zn38(0.51671)
 I316(0.51671) I403(0.50162) Zn42(0.50162) I404(0.50162) I515(0.03778)
 I516(0.03778) Zn58(0.03778) I405(0.35275) Zn43(0.35275) I406(0.35275)
 I505(0.08904) I506(0.08904) Zn53(0.08904) I411(0.46295) Zn46(0.46295)
 I412(0.46295) I511(0.05309) I512(0.05309) Zn56(0.05309) I414(0.07766)
 Zn47(0.07766) I413(0.07766) Zn57(0.09405) I514(0.09405) I513(0.09405)
 C4B(0.11265) C5B(0.11265) C2B(0.11265) H2B(0.11265) C6B(0.11265) H6B(0.11265)
 C3B(0.11265) H3B(0.11265) C1B(0.11265) H1B(0.11265) C7B(0.11265) C10B(0.11265)
 H10B(0.11265) C13B(0.11265) H13C(0.11265) H13D(0.11265) C9B(0.11265)
 H9B(0.11265) C12B(0.11265) C11B(0.11265) H11B(0.11265) O1B(0.11265)
 H1BA(0.11265) O3B(0.11265) O2B(0.11265) C8B(0.11265) C802(0.3985) H80A(0.3985)
 H80B(0.3985) C803(0.3985) H80C(0.3985) H80D(0.3985) C804(0.3985) H80E(0.3985)
 H80F(0.3985) C805(0.3985) H80G(0.3985) H80H(0.3985) C806(0.3985) H80I(0.3985)
 H80J(0.3985) C801(0.3985) H80K(0.3985) H80L(0.3985) C824(0.35052)
 H82A(0.35052) H82B(0.35052) C819(0.35052) H81A(0.35052) H81B(0.35052)
 C820(0.35052) H82C(0.35052) H82D(0.35052) C821(0.35052) H82E(0.35052)
 H82F(0.35052) C822(0.35052) H82G(0.35052) H82H(0.35052) C823(0.35052)
 H82I(0.35052) H82J(0.35052) C15B(0.11265) H15D(0.11265) H15E(0.11265)
 H15F(0.11265) C818(0.37086) H81C(0.37086) H81D(0.37086) C817(0.37086)
 H81E(0.37086) H81F(0.37086) C816(0.37086) H81G(0.37086) H81H(0.37086)
 C815(0.37086) H81I(0.37086) H81J(0.37086) C814(0.37086) H81K(0.37086)
 H81L(0.37086) C813(0.37086) H81M(0.37086) H81N(0.37086) C810(0.32453)
 H81O(0.32453) H81P(0.32453) C811(0.32453) H81Q(0.32453) H81R(0.32453)
 C812(0.32453) H81S(0.32453) H81T(0.32453) C807(0.32453) H80M(0.32453)
 H80N(0.32453) C808(0.32453) H80O(0.32453) H80P(0.32453) C809(0.32453)
 H80Q(0.32453) H80R(0.32453) C14B(0.11265) H14D(0.11265) H14E(0.11265)
 H14F(0.11265)
 Fixed Uiso: I515(0.08) I516(0.08) Zn58(0.08) I505(0.08) I506(0.08) Zn53(0.08)
 I418(0.08) I417(0.08) Zn49(0.08) I401(0.08) Zn41(0.08) I402(0.08) I511(0.08)
 I512(0.08) Zn56(0.08) Zn57(0.08) I514(0.08) I513(0.08) C4B(0.08) C5B(0.08)
 C2B(0.08) C6B(0.08) C3B(0.08) C1B(0.08) C7B(0.08) C10B(0.08) C13B(0.08)
 C9B(0.08) C12B(0.08) C11B(0.08) O1B(0.08) O3B(0.08) O2B(0.08) C8B(0.08)
 C15B(0.08) C818(0.08) C817(0.08) C816(0.08) C815(0.08) C814(0.08) C813(0.08)
 C14B(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), C824(H82A,H82B),
 C819(H81A,H81B), C820(H82C,H82D), C821(H82E,H82F), C822(H82G,H82H), C823(H82I,
 H82J), C818(H81C,H81D), C817(H81E,H81F), C816(H81G,H81H), C815(H81I,H81J),
 C814(H81K,H81L), C813(H81M,H81N), C810(H81O,H81P), C811(H81Q,H81R), C812(H81S,
 H81T), C807(H80M,H80N), C808(H80O,H80P), C809(H80Q,H80R)
7.b Aromatic/amide H refined with riding coordinates:
 C365(H365), C364(H364), C368(H368), C349(H349), C348(H348), C355(H355),
 C354(H354), C353(H353), C332(H332), C390(H390), C389(H389), C372(H372),
 C371(H371), C404(H404), C395(H395), C392(H392), C387(H387), C394(H394),
 C369(H369), C384(H384), C367(H367), C356(H356), C319(H319), C403(H403),
 C328(H328), C402(H402), C385(H385), C313(H313), C322(H322), C386(H386),
 C401(H401), C373(H373), C346(H346), C376(H376), C374(H374), C405(H405),
 C358(H358), C391(H391), C329(H329), C323(H323), C3A(H3A), C408(H408),
 C347(H347), C366(H366), C400(H400), C336(H336), C330(H330), C359(H359),
 C318(H318), C335(H335), C317(H317), C331(H331), C1A(H1AA), C382(H382),
 C333(H333), C320(H320), C6A(H6A), C312(H312), C377(H377), C301(H301),
 C383(H383), C340(H340), C350(H350), C407(H407), C304(H304), C11A(H11A),
 C314(H314), C310(H310), C337(H337), C338(H338), C305(H305), C2A(H2A),
 C351(H351), C315(H315), C311(H311), C302(H302), C9A(H9A), C10A(H10A),
 C341(H341), C2B(H2B), C6B(H6B), C3B(H3B), C1B(H1B), 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:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C14B(H14D,
 H14E,H14F)
;
_shelx_res_checksum              54258
_shelx_hkl_checksum              13441
_olex2_date_sample_data_collection 2023-03-30
_olex2_date_sample_submission    2023-03-30
_olex2_submission_original_sample_id 4_1_24c
_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 2.467
_oxdiff_exptl_absorpt_empirical_full_min 0.452