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_1571842
_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, 1.018(C15 H16 O3), 1.116(C6 H12)'
_chemical_formula_sum            'C129.97 H101.68 I18 N36 O3.06 Zn9'
_chemical_formula_weight         5089.17
_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             2024-01-26
_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                 100.259(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   78.5587(18)
_cell_length_b                   14.9697(2)
_cell_length_c                   41.6779(6)
_cell_measurement_reflns_used    19374
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.8000
_cell_measurement_theta_min      2.2610
_cell_volume                     48229.6(15)
_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 6000HE'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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   -167.00 -82.00   0.25    3.00    -- -103.00 -74.00-157.00  340
  2  \w    -93.00 -37.00   0.25    3.00    -- -103.00  74.00 -29.00  224
  3  \w   -174.00 -90.00   0.25    3.00    -- -103.00 -45.00-120.00  336
  4  \w    -69.00 -38.00   0.25    3.00    -- -103.00  61.00 150.00  124
  5  \w    -98.00 -48.00   0.25    3.00    -- -103.00  77.00  90.00  200
  6  \w   -174.00 -94.00   0.25    3.00    -- -103.00 -45.00 -90.00  320
  7  \w     30.00  94.00   0.25    3.00    --  101.75 -74.00-157.00  256
  8  \w    143.00 168.00   0.25    3.00    --  101.75  74.00 -29.00  100
  9  \w     34.00  60.00   0.25    3.00    --  101.75 -61.00 120.00  104
 10  \w     97.00 174.00   0.25    3.00    --  101.75  45.00  90.00  308
 11  \w     48.00  73.00   0.25    3.00    --  101.75 -61.00 -30.00  100
 12  \w     29.00  54.00   0.25    3.00    --  101.75 -61.00   0.00  100
 13  \w    -17.00  17.00   0.25    1.00    --  -46.51  74.00 -29.00  136
 14  \w    -59.00 -33.00   0.25    1.00    --  -46.51  74.00 -29.00  104
 15  \w     27.00 105.00   0.25    1.00    --   46.51  74.00 -29.00  312
 16  \w    -25.00  67.00   0.25    1.00    --   46.51 -74.00-157.00  368
 17  \w    -96.00 -71.00   0.25    1.00    --  -46.51 -74.00-157.00  100
 18  \w    -23.00  27.00   0.25    1.00    --  -46.51  19.00 -30.00  200
;
_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      0.0118848000
_diffrn_orient_matrix_UB_12      -0.0048655000
_diffrn_orient_matrix_UB_13      -0.0256568000
_diffrn_orient_matrix_UB_21      0.0087682000
_diffrn_orient_matrix_UB_22      -0.0839762000
_diffrn_orient_matrix_UB_23      0.0167931000
_diffrn_orient_matrix_UB_31      -0.0133878000
_diffrn_orient_matrix_UB_32      -0.0592722000
_diffrn_orient_matrix_UB_33      -0.0216934000
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       94
_diffrn_reflns_limit_h_min       -94
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            143224
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         2.252
_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    19.376
_exptl_absorpt_correction_T_max  0.470
_exptl_absorpt_correction_T_min  0.182
_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    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             19055
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.981
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2390
_refine_ls_number_reflns         43855
_refine_ls_number_restraints     999
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1358P)^2^+270.6525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2201
_refine_ls_wR_factor_ref         0.2396
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30847
_reflns_number_total             43855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_1_48c
_cod_database_code               1571842
_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   0.444
_shelx_estimated_absorpt_t_min   0.187
_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
 C2B-C1B = C3B-C2B = C4B-C3B = C5B-C4B = C6B-C5B = C6B-C1B
 1.39 with sigma of 0.02
 O1A-C13A
 1.43 with sigma of 0.01
 O2A-C14A = O3A-C15A
 1.43 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.01
 C5B-C13B
 1.51 with sigma of 0.02
 C7B-C4B
 1.5 with sigma of 0.02
 O1B-C13B = O2B-C14B = O3B-C15B
 1.43 with sigma of 0.02
 O3B-C12B = O2B-C8B
 1.37 with sigma of 0.02
 C809-C810 = C809-C808 = C810-C811 = C811-C812 = C812-C807 = C807-C808
 1.54 with sigma of 0.02
 C829-C828 = C829-C830 = C828-C827 = C827-C826 = C826-C825 = C825-C830
 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
 C819-C824 = C819-C820 = C824-C823 = C823-C822 = C822-C821 = C821-C820
 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
 C5A-O1A
 2.4 with sigma of 0.01
 C1B-C3B = C2B-C4B = C3B-C5B = C4B-C6B = C5B-C1B = C6B-C2B
 2.4 with sigma of 0.04
 C5B-O1B
 2.4 with sigma of 0.04
 C15B-C12B
 2.4 with sigma of 0.04
 C809-C811 = C809-C807 = C810-C812 = C811-C807 = C812-C808
 2.54 with sigma of 0.04
 C829-C827 = C829-C825 = C828-C826 = C827-C825 = C826-C830
 2.54 with sigma of 0.04
 C813-C817 = C813-C815 = C818-C816 = C817-C815 = C816-C814
 2.54 with sigma of 0.04
 C819-C823 = C819-C821 = C824-C822 = C823-C821 = C822-C820
 2.54 with sigma of 0.04
 C804-C802 = C804-C806 = C803-C801 = C802-C806 = C801-C805
 2.54 with sigma of 0.04
 C8A-C7A \\sim C9A-C8A \\sim C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim
C7A-C12A
 with sigma of 0.02
 C7A-C9A \\sim C8A-C10A \\sim C9A-C11A \\sim C10A-C12A \\sim C11A-C7A \\sim
C12A-C8A
 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-N306 \\sim Zn43-N306
 with sigma of 0.02
 Zn33-N307 \\sim Zn43-N307
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 I306-N307 \\sim I406-N307
 with sigma of 0.04
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I305-N307 \\sim I405-N307
 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-N305 \\sim Zn42-N305
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I303-N305 \\sim I403-N305
 with sigma of 0.04
 I304-N305 \\sim I404-N305
 with sigma of 0.04
 I309-Zn35 \\sim I409-Zn45
 with sigma of 0.02
 I310-Zn35 \\sim I410-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
 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
 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-N331 \\sim Zn48-N331
 with sigma of 0.02
 Zn38-N330 \\sim Zn48-N330
 with sigma of 0.02
 I315-I316 \\sim I415-I416
 with sigma of 0.04
 I315-N331 \\sim I415-N331
 with sigma of 0.04
 I315-N330 \\sim I415-N330
 with sigma of 0.04
 I316-N331 \\sim I416-N331
 with sigma of 0.04
 I316-N330 \\sim I416-N330
 with sigma of 0.04
 I317-Zn39 \\sim I417-Zn49
 with sigma of 0.02
 I318-Zn39 \\sim I418-Zn49
 with sigma of 0.02
 Zn39-N336 \\sim Zn49-N336
 with sigma of 0.02
 I317-I318 \\sim I417-I418
 with sigma of 0.04
 I317-N336 \\sim I417-N336
 with sigma of 0.04
 I318-N336 \\sim I418-N336
 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
 I407-Zn44 \\sim I307-Zn34
 with sigma of 0.02
 I408-Zn44 \\sim I308-Zn34
 with sigma of 0.02
 Zn44-N312 \\sim Zn34-N312
 with sigma of 0.02
 Zn44-N313 \\sim Zn34-N313
 with sigma of 0.02
 I407-I408 \\sim I307-I308
 with sigma of 0.04
 I407-N312 \\sim I307-N312
 with sigma of 0.04
 I407-N313 \\sim I307-N313
 with sigma of 0.04
 I408-N312 \\sim I308-N312
 with sigma of 0.04
 I408-N313 \\sim I308-N313
 with sigma of 0.04
 I519-Zn59 \\sim I518-Zn59
 with sigma of 0.02
 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
 I503-Zn52 \\sim I403-Zn42
 with sigma of 0.02
 I504-Zn52 \\sim I304-Zn32
 with sigma of 0.02
 I512-Zn56 \\sim I511-Zn56
 with sigma of 0.02
 C809-C810 \\sim C810-C811 \\sim C811-C812 \\sim C812-C807 \\sim C807-C808
\\sim C808-C809
 with sigma of 0.02
 C809-C807 \\sim C811-C807 \\sim C810-C808 \\sim C810-C812 \\sim C812-C808
\\sim C809-C811
 with sigma of 0.04
 C829-C828 \\sim C828-C827 \\sim C827-C826 \\sim C826-C825 \\sim C825-C830
\\sim C830-C829
 with sigma of 0.02
 C829-C825 \\sim C827-C825 \\sim C828-C830 \\sim C828-C826 \\sim C826-C830
\\sim C829-C827
 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
 C819-C824 \\sim C824-C823 \\sim C823-C822 \\sim C822-C821 \\sim C821-C820
\\sim C820-C819
 with sigma of 0.02
 C819-C821 \\sim C823-C821 \\sim C824-C820 \\sim C824-C822 \\sim C822-C820
\\sim C819-C823
 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
3. Restrained planarity
 C5B, C3B, C2B, C6B, C4B, C1B
 with sigma of 0.1
 O3B, C12B, C7B, C8B, O2B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C5A \\sim O2A \\sim C8A \\sim C14A \\sim C7A \\sim C9A \\sim C4A \\sim C12A
\\sim C10A \\sim C3A \\sim C11A \\sim O3A \\sim C2A \\sim C6A \\sim C13A \\sim
C15A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C10B \\sim C4B \\sim C3B \\sim C5B \\sim C7B \\sim C2B \\sim C6B \\sim C13B
\\sim C12B \\sim C8B \\sim C1B \\sim O1B \\sim C11B \\sim O3B \\sim O2B \\sim
C9B \\sim C15B \\sim C14B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C809 \\sim C810 \\sim C811 \\sim C812 \\sim C807 \\sim C808: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C829 \\sim C828 \\sim C827 \\sim C826 \\sim C825 \\sim C830: 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
C819 \\sim C824 \\sim C823 \\sim C822 \\sim C821 \\sim C820: 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
5. Rigid body (RIGU) restrains
 C10B, C4B, C3B, C5B, C7B, C2B, C6B, C13B, C12B, C8B, C1B, O1B, C11B, O3B, O2B,
  C9B, C15B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C809, C810, C811, C812, C807, C808
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C829, C828, C827, C826, C825, C830
 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
 C819, C824, C823, C822, C821, C820
 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
6. Others
 1*[Sof(I317)+Sof(I318)+Sof(Zn39)]+1*[Sof(I418)+Sof(Zn49)+Sof(I417)]+1*
 [Sof(I518)+Sof(I519)+Sof(Zn59)]=1 with esd of 0.00001
 1*[Sof(I306)+Sof(I305)+Sof(Zn33)]+1*[Sof(I405)+Sof(Zn43)+Sof(I406)]+1*
 [Sof(I505)+Sof(I506)+Sof(Zn53)]=1 with esd of 0.00001
 1*[Sof(I313)+Sof(I312)+Sof(I314)+Sof(I311)+Sof(Zn36)+Sof(Zn37)+Sof(I413)+
 Sof(Zn47)+Sof(I414)]+1*[Sof(I411)+Sof(Zn46)+Sof(I412)]+1*[Sof(I511)+Sof(I512)+
 Sof(Zn56)]=1 with esd of 0.00001
 1*[Sof(I301)+Sof(I302)+Sof(Zn31)]+1*[Sof(Zn41)+Sof(I402)+Sof(I401)]+1*
 [Sof(I501)+Sof(I17)+Sof(Zn51)]+1*[Sof(I602)+Sof(I601)+Sof(Zn61)]=1 with esd of
 0.00001
 Sof(I409)=Sof(Zn45)=Sof(I410)=1-FVAR(1)
 Sof(I309)=Sof(I310)=Sof(Zn35)=FVAR(1)
 Sof(I415)=Sof(Zn48)=Sof(I416)=1-FVAR(2)
 Sof(I315)=Sof(I316)=Sof(Zn38)=FVAR(2)
 Sof(I308)=Sof(Zn34)=Sof(I307)=1-FVAR(3)
 Sof(I407)=Sof(I408)=Sof(Zn44)=FVAR(3)
 Sof(I317)=Sof(I318)=Sof(Zn39)=FVAR(4)
 Sof(I418)=Sof(Zn49)=Sof(I417)=FVAR(5)
 Sof(I518)=Sof(I519)=Sof(Zn59)=FVAR(6)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(7)
 Sof(I405)=Sof(Zn43)=Sof(I406)=FVAR(8)
 Sof(I505)=Sof(I506)=Sof(Zn53)=FVAR(9)
 Sof(I413)=Sof(Zn47)=Sof(I414)=1-FVAR(10)
 Sof(I313)=Sof(I312)=Sof(I314)=Sof(I311)=Sof(Zn36)=Sof(Zn37)=FVAR(10)
 Sof(I411)=Sof(Zn46)=Sof(I412)=FVAR(11)
 Sof(I511)=Sof(I512)=Sof(Zn56)=FVAR(12)
 Sof(I301)=Sof(I302)=Sof(Zn31)=FVAR(13)
 Sof(Zn41)=Sof(I402)=Sof(I401)=FVAR(14)
 Sof(I501)=Sof(I17)=Sof(Zn51)=FVAR(15)
 Sof(I602)=Sof(I601)=Sof(Zn61)=FVAR(16)
 Fixed Sof: I303(0.56859) I304(0.56859) Zn32(0.56859) O2A(0.76853)
 O3A(0.76853) O1A(0.76853) H1AA(0.76853) C7A(0.76853) C8A(0.76853) C1A(0.76853)
 H1A(0.76853) C2A(0.76853) H2A(0.76853) C3A(0.76853) H3A(0.76853) C4A(0.76853)
 C5A(0.76853) C6A(0.76853) H6A(0.76853) C12A(0.76853) C11A(0.76853)
 H11A(0.76853) C9A(0.76853) H9A(0.76853) C10A(0.76853) H10A(0.76853)
 C14A(0.76853) H14A(0.76853) H14B(0.76853) H14C(0.76853) C13A(0.76853)
 H13A(0.76853) H13B(0.76853) I403(0.37438) Zn42(0.37438) I404(0.37438)
 I503(0.05703) I504(0.05703) Zn52(0.05703) C15A(0.76853) H15A(0.76853)
 H15B(0.76853) H15C(0.76853) C4B(0.24975) C3B(0.24975) H3B(0.24975)
 C5B(0.24975) O2B(0.24975) C6B(0.24975) H6B(0.24975) C2B(0.24975) H2B(0.24975)
 C7B(0.24975) C12B(0.24975) C11B(0.24975) H11B(0.24975) C10B(0.24975)
 H10B(0.24975) C9B(0.24975) H9B(0.24975) C8B(0.24975) C1B(0.24975) H1B(0.24975)
 C13B(0.24975) H13C(0.24975) H13D(0.24975) O3B(0.24975) O1B(0.24975)
 H1BA(0.24975) C14B(0.24975) H14D(0.24975) H14E(0.24975) H14F(0.24975)
 C15B(0.24975) H15D(0.24975) H15E(0.24975) H15F(0.24975) C809(0.23295)
 H2C(0.23295) H2D(0.23295) C810(0.23295) H3C(0.23295) H3D(0.23295)
 C811(0.23295) H7A(0.23295) H7B(0.23295) C812(0.23295) H8A(0.23295)
 H8B(0.23295) C807(0.23295) H9C(0.23295) H9D(0.23295) C808(0.23295)
 H10C(0.23295) H10D(0.23295) C829(0.28471) H11C(0.28471) H11D(0.28471)
 C828(0.28471) H15G(0.28471) H15H(0.28471) C827(0.28471) H17A(0.28471)
 H17B(0.28471) C826(0.28471) H19A(0.28471) H19B(0.28471) C825(0.28471)
 H13E(0.28471) H13F(0.28471) C830(0.28471) H22A(0.28471) H22B(0.28471)
 C813(0.17263) H4A(0.17263) H4B(0.17263) C818(0.17263) H5A(0.17263)
 H5B(0.17263) C817(0.17263) H6C(0.17263) H6D(0.17263) C816(0.17263)
 H12A(0.17263) H12B(0.17263) C815(0.17263) H14G(0.17263) H14H(0.17263)
 C814(0.17263) H16A(0.17263) H16B(0.17263) C819(0.18823) H18A(0.18823)
 H18B(0.18823) C824(0.18823) H1CA(0.18823) H1CB(0.18823) C823(0.18823)
 H1DA(0.18823) H1DB(0.18823) C822(0.18823) H1EA(0.18823) H1EB(0.18823)
 C821(0.18823) H1FA(0.18823) H1FB(0.18823) C820(0.18823) H1GA(0.18823)
 H1GB(0.18823) C804(0.23702) H1HA(0.23702) H1HB(0.23702) C803(0.23702)
 H1IA(0.23702) H1IB(0.23702) C802(0.23702) H1JA(0.23702) H1JB(0.23702)
 C801(0.23702) H1KA(0.23702) H1KB(0.23702) C806(0.23702) H1LA(0.23702)
 H1LB(0.23702) C805(0.23702) H1MA(0.23702) H1MB(0.23702)
 Fixed Uiso: I503(0.08) I504(0.08) Zn52(0.08) I518(0.08) I519(0.08) Zn59(0.08)
 I505(0.08) I506(0.08) Zn53(0.08) I501(0.08) I17(0.08) Zn51(0.08) I511(0.08)
 I512(0.08) Zn56(0.08) I602(0.08) I601(0.08) Zn61(0.08) C829(0.08) C828(0.08)
 C827(0.08) C826(0.08) C825(0.08) C830(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13B(H13C,H13D), C809(H2C,H2D), C810(H3C,H3D), C811(H7A,H7B),
  C812(H8A,H8B), C807(H9C,H9D), C808(H10C,H10D), C829(H11C,H11D), C828(H15G,
 H15H), C827(H17A,H17B), C826(H19A,H19B), C825(H13E,H13F), C830(H22A,H22B),
 C813(H4A,H4B), C818(H5A,H5B), C817(H6C,H6D), C816(H12A,H12B), C815(H14G,H14H),
 C814(H16A,H16B), C819(H18A,H18B), C824(H1CA,H1CB), C823(H1DA,H1DB), C822(H1EA,
 H1EB), C821(H1FA,H1FB), C820(H1GA,H1GB), C804(H1HA,H1HB), C803(H1IA,H1IB),
 C802(H1JA,H1JB), C801(H1KA,H1KB), C806(H1LA,H1LB), C805(H1MA,H1MB)
7.b Aromatic/amide H refined with riding coordinates:
 C317(H317), C329(H329), C333(H333), C320(H320), C351(H351), C318(H318),
 C332(H332), C350(H350), C322(H322), C328(H328), C355(H355), C359(H359),
 C319(H319), C336(H336), C364(H364), C405(H405), C323(H323), C348(H348),
 C356(H356), C335(H335), C371(H371), C312(H312), C349(H349), C353(H353),
 C358(H358), C392(H392), C354(H354), C372(H372), C313(H313), C315(H315),
 C314(H314), C365(H365), C395(H395), C368(H368), C404(H404), C331(H331),
 C394(H394), C340(H340), C369(H369), C337(H337), C330(H330), C346(H346),
 C401(H401), C338(H338), C385(H385), C366(H366), C341(H341), C403(H403),
 C390(H390), C389(H389), C400(H400), C402(H402), C367(H367), C407(H407),
 C391(H391), C347(H347), C1A(H1A), C2A(H2A), C3A(H3A), C6A(H6A), C304(H304),
 C383(H383), C376(H376), C305(H305), C377(H377), C373(H373), C311(H311),
 C384(H384), C11A(H11A), C408(H408), C310(H310), C9A(H9A), C10A(H10A),
 C382(H382), C301(H301), C374(H374), C302(H302), C387(H387), C386(H386),
 C3B(H3B), C6B(H6B), C2B(H2B), C11B(H11B), C10B(H10B), C9B(H9B), C1B(H1B)
7.c Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A), C7B(C12B,C11B,C10B,C9B,C8B)
7.d Tetrahedral OH refined with riding coordinates:
 O1B(H1BA)
7.e Idealised Me refined with everything fixed:
 C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F)
7.f Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C)
7.g Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA)
;
_shelx_res_checksum              84015
_shelx_hkl_checksum              96458
_olex2_date_sample_data_collection 2022-03-10
_olex2_date_sample_submission    2022-03-10
_olex2_submission_original_sample_id 25_1_48c
_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 2.204
_oxdiff_exptl_absorpt_empirical_full_min 0.454