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_1571845
_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, 0.944(C15 H16 O3)'
_chemical_formula_sum            'C122.16 H87.11 I18 N36 O2.83 Zn9'
_chemical_formula_weight         4977.17
_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             2024-02-07
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.01.24 svn.r2f8d729c for OlexSys, GUI svn.r6923)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.342(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   77.257(6)
_cell_length_b                   15.0021(8)
_cell_length_c                   41.5124(18)
_cell_measurement_reflns_used    4599
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.0120
_cell_measurement_theta_min      3.3800
_cell_volume                     47332(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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   -107.00 -82.00   0.50    5.00    -- -103.00-157.00 159.00   50
  2  \w    -96.00 -71.00   0.50    5.00    -- -103.00 119.00  40.00   50
  3  \w   -107.00 -82.00   0.50    5.00    -- -103.00 157.00-164.00   50
  4  \w   -126.00 -82.00   0.50    5.00    -- -103.00-119.00 -45.00   88
  5  \w    -99.00 -74.00   0.50    5.00    -- -103.00  77.00 -90.00   50
  6  \w    -68.00 -31.00   0.50    5.00    -- -103.00  61.00 120.00   74
  7  \w    -68.00 -43.00   0.50    5.00    -- -103.00  61.00 150.00   50
  8  \w    -67.00 -42.00   0.50    5.00    -- -103.00  61.00  60.00   50
  9  \w    -62.00 -30.00   0.50    5.00    -- -103.00  61.00-150.00   64
 10  \w     33.00 107.00   0.50    5.00    --  101.75-119.00 -45.00  148
 11  \w     75.00 132.00   0.50    5.00    --  101.75-157.00 159.00  114
 12  \w    111.00 137.00   0.50    5.00    --  101.75 119.00  40.00   52
 13  \w     50.00  76.00   0.50    5.00    --  101.75 -94.00 -30.00   52
 14  \w     94.00 174.00   0.50    5.00    --  101.75  45.00  30.00  160
 15  \w     32.00  62.00   0.50    5.00    --  101.75 -61.00 -30.00   60
 16  \w     30.00 107.00   0.50    5.00    --  101.75 -77.00 -30.00  154
 17  \w     87.00 174.00   0.50    5.00    --  101.75  61.00 -60.00  174
 18  \w     80.00 106.00   0.50    5.00    --  101.75 -94.00 -30.00   52
 19  \w   -111.00 -70.00   0.50    1.00    --  -46.26 157.00-164.00   82
 20  \w    -98.00 -54.00   0.50    1.00    --  -46.26-157.00 159.00   88
 21  \w     70.00 117.00   0.50    1.00    --   46.26 157.00-164.00   94
 22  \w     62.00  87.00   0.50    1.00    --   46.26-157.00 159.00   50
 23  \w    -22.00  22.00   0.50    1.00    --  -46.26  19.00-120.00   88
 24  \w    -23.00   7.00   0.50    1.00    --  -46.26  19.00 -30.00   60
 25  \w    -22.00  28.00   0.50    1.00    --   46.26 -19.00 -30.00  100
 26  \w    -23.00  28.00   0.50    1.00    --   46.26 -19.00-180.00  102
;
_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      0.0014516000
_diffrn_orient_matrix_UB_12      -0.1016992000
_diffrn_orient_matrix_UB_13      0.0048148000
_diffrn_orient_matrix_UB_21      0.0196386000
_diffrn_orient_matrix_UB_22      0.0039145000
_diffrn_orient_matrix_UB_23      -0.0025090000
_diffrn_orient_matrix_UB_31      0.0048209000
_diffrn_orient_matrix_UB_32      0.0133773000
_diffrn_orient_matrix_UB_33      0.0373440000
_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  0.0819
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       92
_diffrn_reflns_limit_h_min       -92
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            156082
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.164
_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    19.730
_exptl_absorpt_correction_T_max  0.257
_exptl_absorpt_correction_T_min  0.103
_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    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             18550
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.366
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2310
_refine_ls_number_reflns         43077
_refine_ls_number_restraints     1034
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1928
_refine_ls_R_factor_gt           0.1289
_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^)+(0.2235P)^2^+478.5298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3878
_refine_ls_wR_factor_ref         0.4460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20894
_reflns_number_total             43077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_1_96c
_cod_database_code               1571845
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     9300-04
_shelx_estimated_absorpt_t_max   0.184
_shelx_estimated_absorpt_t_min   0.117
_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
 C2C-C1C = C3C-C2C = C4C-C3C = C5C-C4C = C6C-C5C = C6C-C1C
 1.39 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 O3A-C15A
 1.43 with sigma of 0.02
 C8C-C7C = C9C-C8C = C9C-C10C = C11C-C10C = C12C-C11C = C7C-C12C
 1.39 with sigma of 0.02
 O3A-C12A = O2A-C8A
 1.37 with sigma of 0.02
 C8B-C7B = C9B-C8B = C9B-C10B = C11B-C10B = C12B-C11B = C7B-C12B
 1.39 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
 O2C-C8C = O3C-C12C
 1.37 with sigma of 0.02
 C1B-C3B = C2B-C4B = C3B-C5B = C4B-C6B = C5B-C1B = C6B-C2B
 2.4 with sigma of 0.04
 C7A-O3A
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.04
 C2C-C4C = C3C-C5C = C5C-C1C = C6C-C2C
 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
 C7C-C9C = C8C-C10C = C9C-C11C = C10C-C12C = C11C-C7C = C12C-C8C
 2.4 with sigma of 0.04
 C5B-O1B
 2.4 with sigma of 0.04
 O1C-C5C
 2.4 with sigma of 0.04
 C14B-C8B
 2.4 with sigma of 0.02
 C8C-C14C
 2.4 with sigma of 0.02
 C12C-C15C
 2.4 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
 C1A-C4A \\sim C2A-C5A \\sim C3A-C6A
 with sigma of 0.04
 O1A-C13A \\sim O2A-C14A
 with sigma of 0.02
 C7C-C4C \\sim C5C-C13C
 with sigma of 0.02
 O3C-C15C \\sim O2C-C14C \\sim O1C-C13C
 with sigma of 0.02
 C7B-O2B \\sim O2B-C9B
 with sigma of 0.04
 C4C-C13C \\sim C13C-C6C
 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 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
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 Zn33-N312 \\sim Zn43-N312
 with sigma of 0.02
 Zn39-N334 \\sim Zn49-N334
 with sigma of 0.02
 Zn33-N01O \\sim Zn43-N01O
 with sigma of 0.02
 I318-I317 \\sim I418-I417
 with sigma of 0.04
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I318-N334 \\sim I418-N334
 with sigma of 0.04
 I317-N334 \\sim I417-N334
 with sigma of 0.04
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 I306-N01O \\sim I406-N01O
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I305-N01O \\sim I405-N01O
 with sigma of 0.04
 I310-Zn35 \\sim I410-Zn45
 with sigma of 0.02
 I309-Zn35 \\sim I409-Zn45
 with sigma of 0.02
 Zn35-N318 \\sim Zn45-N318
 with sigma of 0.02
 I310-I309 \\sim I410-I409
 with sigma of 0.04
 I310-N318 \\sim I410-N318
 with sigma of 0.04
 I309-N318 \\sim I409-N318
 with sigma of 0.04
 I311-Zn36 \\sim I411-Zn46
 with sigma of 0.02
 I312-Zn36 \\sim I412-Zn46
 with sigma of 0.02
 Zn36-N01P \\sim Zn46-N01P
 with sigma of 0.02
 Zn36-N323 \\sim Zn46-N323
 with sigma of 0.02
 I311-I312 \\sim I411-I412
 with sigma of 0.04
 I311-N01P \\sim I411-N01P
 with sigma of 0.04
 I311-N323 \\sim I411-N323
 with sigma of 0.04
 I312-N01P \\sim I412-N01P
 with sigma of 0.04
 I312-N323 \\sim I412-N323
 with sigma of 0.04
 I316-Zn38 \\sim I416-Zn48
 with sigma of 0.02
 I315-Zn38 \\sim I415-Zn48
 with sigma of 0.02
 Zn38-N329 \\sim Zn48-N329
 with sigma of 0.02
 Zn38-N328 \\sim Zn48-N328
 with sigma of 0.02
 I316-I315 \\sim I416-I415
 with sigma of 0.04
 I316-N329 \\sim I416-N329
 with sigma of 0.04
 I316-N328 \\sim I416-N328
 with sigma of 0.04
 I315-N329 \\sim I415-N329
 with sigma of 0.04
 I315-N328 \\sim I415-N328
 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
 I407-Zn44 \\sim I307-Zn34
 with sigma of 0.02
 I408-Zn44 \\sim I308-Zn34
 with sigma of 0.02
 Zn44-N316 \\sim Zn34-N316
 with sigma of 0.02
 I407-I408 \\sim I307-I308
 with sigma of 0.04
 I407-N316 \\sim I307-N316
 with sigma of 0.04
 I408-N316 \\sim I308-N316
 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-N327 \\sim Zn47-N327
 with sigma of 0.02
 I313-I314 \\sim I413-I414
 with sigma of 0.04
 I313-N327 \\sim I413-N327
 with sigma of 0.04
 I314-N327 \\sim I414-N327
 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-N307 \\sim Zn42-N307
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 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
 I304-N307 \\sim I404-N307
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 Zn56-N01P \\sim Zn46-N01P
 with sigma of 0.02
 Zn56-N323 \\sim Zn46-N323
 with sigma of 0.02
 I511-Zn56 \\sim I411-Zn46
 with sigma of 0.02
 I312-Zn36 \\sim I512-Zn56
 with sigma of 0.02
 Zn31-N301 \\sim Zn51-N301 \\sim Zn41-N301
 with sigma of 0.02
 I301-Zn31 \\sim I501-Zn51
 with sigma of 0.02
 I302-Zn31 \\sim I502-Zn51
 with sigma of 0.02
 N323-C377 \\sim N323-C477
 with sigma of 0.02
 C375-C376 \\sim C375-C476
 with sigma of 0.02
 C376-C377 \\sim C476-C477
 with sigma of 0.02
 N323-C376 \\sim N323-C476
 with sigma of 0.04
 C375-C377 \\sim C375-C477
 with sigma of 0.04
 N312-C341 \\sim N312-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
 N312-C340 \\sim N312-C440
 with sigma of 0.04
 C339-C341 \\sim C339-C441
 with sigma of 0.04
 I513-Zn57 \\sim I313-Zn37
 with sigma of 0.02
 I414-Zn47 \\sim I514-Zn57
 with sigma of 0.02
 Zn57-N327 \\sim Zn37-N327
 with sigma of 0.02
 Zn53-N01O \\sim Zn53-N312
 with sigma of 0.02
3. Restrained planarity
 C4B, C5B, C1B, C6B, C3B, C2B
 with sigma of 0.1
 C12B, C7B, C11B, C10B, C9B, C8B
 with sigma of 0.1
 C4C, C5C, C1C, C6C, C3C, C2C
 with sigma of 0.1
 C12C, C11C, C7C, C9C, C10C, C8C
 with sigma of 0.1
 O2B, C8B, C7B, C12B, O3B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4A \\sim O3A \\sim C12A \\sim C15A \\sim C7A \\sim C11A \\sim C8A \\sim C10A
\\sim C5A \\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
C4B \\sim O2B \\sim C14B \\sim C8B \\sim C7B \\sim C9B \\sim C12B \\sim C10B
\\sim C5B \\sim C3B \\sim O3B \\sim C11B \\sim C6B \\sim C13B \\sim C2B \\sim
C15B \\sim C1B \\sim O1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C5C \\sim O2C \\sim C14C \\sim C8C \\sim C7C \\sim C9C \\sim C4C \\sim C12C
\\sim C10C \\sim C3C \\sim O3C \\sim C11C \\sim C6C \\sim C13C \\sim C2C \\sim
C15C \\sim C1C \\sim O1C: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
I416 \\sim I316 \\sim Zn48 \\sim Zn38 \\sim I415 \\sim I315: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I403 \\sim I303 \\sim Zn42 \\sim Zn32 \\sim I404 \\sim I304: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I417 \\sim I317 \\sim Zn49 \\sim Zn39 \\sim I418 \\sim I318: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Zn43 \\sim Zn33 \\sim I406 \\sim I306 \\sim I405 \\sim I305: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C440) = Uanis(C340) = Uanis(C441) = Uanis(C341)
Uanis(C377) = Uanis(C477) = Uanis(C376) = Uanis(C476)
5. Rigid body (RIGU) restrains
 C4A, O3A, C12A, C15A, C7A, C11A, C8A, C10A, C5A, C3A, O2A, C9A, C6A, C13A,
 C2A, C14A, C1A, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4B, O2B, C14B, C8B, C7B, C9B, C12B, C10B, C5B, C3B, O3B, C11B, C6B, C13B,
 C2B, C15B, C1B, O1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13C, O2C, C14C, C8C, C7C, C9C, C4C, C12C, C10C, C5C, C3C, O3C, C11C, C6C,
 C2C, C15C, C1C, O1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(I306)+Sof(I305)+Sof(Zn33)]+1*[Sof(I406)+Sof(Zn43)+Sof(I405)]+1*
 [Sof(I506)+Sof(Zn53)+Sof(I505)]=1 with esd of 0.00001
 Sof(I410)=Sof(Zn45)=Sof(I409)=1-FVAR(1)
 Sof(I310)=Sof(I309)=Sof(Zn35)=FVAR(1)
 Sof(I416)=Sof(Zn48)=Sof(I415)=1-FVAR(2)
 Sof(I316)=Sof(I315)=Sof(Zn38)=FVAR(2)
 Sof(I308)=Sof(Zn34)=Sof(I307)=1-FVAR(3)
 Sof(I407)=Sof(I408)=Sof(Zn44)=FVAR(3)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(4)
 Sof(I406)=Sof(Zn43)=Sof(I405)=FVAR(5)
 Sof(I506)=Sof(Zn53)=Sof(I505)=FVAR(6)
 Sof(C476)=Sof(H476)=Sof(C477)=Sof(H477)=1-FVAR(7)
 Sof(C376)=Sof(H376)=Sof(C377)=Sof(H377)=FVAR(7)
 Sof(C441)=Sof(H441)=Sof(C440)=Sof(H440)=1-FVAR(8)
 Sof(C340)=Sof(H340)=Sof(C341)=Sof(H341)=FVAR(8)
 Fixed Sof: I318(0.49954) I311(0.43524) I301(0.44833) I313(0.40064)
 I302(0.44833) I314(0.40064) I312(0.43524) I317(0.49954) I303(0.52693)
 I304(0.52693) Zn39(0.49954) Zn31(0.44833) Zn36(0.43524) Zn37(0.40064)
 Zn32(0.52693) O3A(0.49351) O1A(0.49351) H1A(0.49351) O2A(0.49351) C4A(0.49351)
 C5A(0.49351) C6A(0.49351) H6A(0.49351) C1A(0.49351) H1AA(0.49351) C2A(0.49351)
 H2A(0.49351) C3A(0.49351) H3A(0.49351) C7A(0.49351) C12A(0.49351)
 C11A(0.49351) H11A(0.49351) C10A(0.49351) H10A(0.49351) C9A(0.49351)
 H9A(0.49351) C8A(0.49351) C13A(0.49351) H13A(0.49351) H13B(0.49351)
 C15A(0.49351) H15A(0.49351) H15B(0.49351) H15C(0.49351) I418(0.50046)
 Zn49(0.50046) I417(0.50046) I411(0.50982) Zn46(0.50982) I412(0.50982)
 I402(0.53274) Zn41(0.53274) I401(0.53274) I414(0.58149) Zn47(0.58149)
 I413(0.58149) I404(0.41267) Zn42(0.41267) I403(0.41267) C14A(0.49351)
 H14A(0.49351) H14B(0.49351) H14C(0.49351) I504(0.06041) I503(0.06041)
 Zn52(0.06041) I511(0.05495) I512(0.05495) Zn56(0.05495) I502(0.01893)
 I501(0.01893) Zn51(0.01893) I514(0.01786) I513(0.01786) Zn57(0.01786)
 O2C(0.21948) O2B(0.23115) O3C(0.21948) O1B(0.23115) H1B(0.23115) O3B(0.23115)
 O1C(0.21948) H1C(0.21948) C4B(0.23115) C4C(0.21948) C5C(0.21948) C5B(0.23115)
 C12C(0.21948) C12B(0.23115) C1C(0.21948) H1CA(0.21948) C14B(0.23115)
 H14G(0.23115) H14H(0.23115) H14I(0.23115) C7B(0.23115) C1B(0.23115)
 H1BA(0.23115) C11B(0.23115) H11B(0.23115) C10B(0.23115) H10B(0.23115)
 C6C(0.21948) H6C(0.21948) C14C(0.21948) H14D(0.21948) H14E(0.21948)
 H14F(0.21948) C11C(0.21948) H11C(0.21948) C13C(0.21948) H13C(0.21948)
 H13D(0.21948) C7C(0.21948) C15B(0.23115) H15G(0.23115) H15H(0.23115)
 H15I(0.23115) C9C(0.21948) H9C(0.21948) C9B(0.23115) H9B(0.23115) C6B(0.23115)
 H6B(0.23115) C15C(0.21948) H15D(0.21948) H15E(0.21948) H15F(0.21948)
 C3C(0.21948) H3C(0.21948) C13B(0.23115) H13E(0.23115) H13F(0.23115)
 C2C(0.21948) H2C(0.21948) C10C(0.21948) H10C(0.21948) C3B(0.23115)
 H3B(0.23115) C2B(0.23115) H2B(0.23115) C8C(0.21948) C8B(0.23115)
 Fixed Uiso: I506(0.08) Zn53(0.08) I505(0.08) I504(0.08) I503(0.08) Zn52(0.08)
 I511(0.08) I512(0.08) Zn56(0.08) I502(0.08) I501(0.08) Zn51(0.08) I514(0.08)
 I513(0.08) Zn57(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13C(H13C,H13D), C13B(H13E,H13F)
7.b Aromatic/amide H refined with riding coordinates:
 C331(H331), C302(H302), C319(H319), C301(H301), C347(H347), C371(H371),
 C346(H346), C367(H367), C322(H322), C323(H323), C335(H335), C320(H320),
 C328(H328), C408(H408), C402(H402), C382(H382), C333(H333), C312(H312),
 C404(H404), C330(H330), C407(H407), C405(H405), C383(H383), C336(H336),
 C311(H311), C358(H358), C403(H403), C368(H368), C317(H317), C332(H332),
 C374(H374), C394(H394), C391(H391), C369(H369), C356(H356), C329(H329),
 C338(H338), C348(H348), C372(H372), C373(H373), C349(H349), C359(H359),
 C337(H337), C392(H392), C395(H395), C366(H366), C313(H313), C304(H304),
 C364(H364), C315(H315), C385(H385), C318(H318), C310(H310), C400(H400),
 C390(H390), C355(H355), C365(H365), C401(H401), C384(H384), C314(H314),
 C389(H389), C353(H353), C6A(H6A), C1A(H1AA), C2A(H2A), C3A(H3A), C387(H387),
 C386(H386), C351(H351), C11A(H11A), C10A(H10A), C9A(H9A), C350(H350),
 C376(H376), C340(H340), C305(H305), C341(H341), C354(H354), C377(H377),
 C476(H476), C477(H477), C441(H441), C440(H440), C1C(H1CA), C1B(H1BA),
 C11B(H11B), C10B(H10B), C6C(H6C), C11C(H11C), C9C(H9C), C9B(H9B), C6B(H6B),
 C3C(H3C), C2C(H2C), C10C(H10C), C3B(H3B), C2B(H2B)
7.c Fitted hexagon refined as free rotating group:
 C7A(C12A,C11A,C10A,C9A,C8A)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1B(H1B), O1C(H1C)
7.e Idealised Me refined with everything fixed:
 C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C), C14B(H14G,H14H,H14I), C14C(H14D,
 H14E,H14F), C15B(H15G,H15H,H15I), C15C(H15D,H15E,H15F)
;
_shelx_res_checksum              37483
_shelx_hkl_checksum              49218
_olex2_date_sample_data_collection 2023-04-03
_olex2_date_sample_submission    2023-04-03
_olex2_submission_original_sample_id 25_1_96c
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.272
_oxdiff_exptl_absorpt_empirical_full_min 0.297