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_1571819
_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         'C115.572 H79.804 I18 N36 O1.514 Zn9'
_chemical_formula_sum            'C115.57 H79.8 I18 N36 O1.52 Zn9'
_chemical_formula_weight         4869.59
_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                 99.709(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   78.549(10)
_cell_length_b                   14.9682(8)
_cell_length_c                   41.688(3)
_cell_measurement_reflns_used    5081
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.1420
_cell_measurement_theta_min      2.2990
_cell_volume                     48312(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_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_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 0.991
_diffrn_measured_fraction_theta_max 0.990
_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   -148.00-103.90   0.15    3.00    -- -103.00-112.00-124.00  294
  2  \w    -95.00 -56.00   0.15    3.00    -- -103.00 112.00 -31.00  260
  3  \w    -67.00 -31.00   0.15    3.00    -- -103.00  61.00-180.00  240
  4  \w   -171.00 -90.00   0.15    3.00    -- -103.00 -45.00  60.00  540
  5  \w   -173.00 -90.95   0.15    3.00    -- -103.00 -15.00 -60.00  547
  6  \w    -64.00 -34.90   0.15    3.00    -- -103.00  61.00 120.00  194
  7  \w    -55.00 -30.85   0.15    3.00    -- -103.00  61.00 150.00  161
  8  \w     90.00 156.00   0.15    3.00    --  101.75 112.00 -31.00  440
  9  \w     44.00  69.05   0.15    3.00    --  101.75-112.00-124.00  167
 10  \w     30.00 110.10   0.15    3.00    --  101.75-125.00-150.00  534
 11  \w     42.00  74.10   0.15    3.00    --  101.75 -61.00 -90.00  214
 12  \w     91.00 148.15   0.15    3.00    --  101.75  45.00-120.00  381
 13  \w     31.00  74.05   0.15    3.00    --  101.75 -61.00-120.00  287
 14  \w     33.00  96.00   0.15    3.00    --  101.75 -77.00-120.00  420
 15  \w     30.00  99.00   0.15    3.00    --  101.75 -94.00-120.00  460
 16  \w    -47.00 -21.95   0.15    0.75    --  -45.99 112.00 -31.00  167
 17  \w     43.00  79.00   0.15    0.75    --   45.99-112.00-124.00  240
 18  \w    -19.00  28.10   0.15    0.75    --  -45.99  19.00 -30.00  314
 19  \w    -19.00  22.10   0.15    0.75    --  -45.99  19.00-150.00  274
 20  \w    -12.00  20.10   0.15    0.75    --  -45.99  19.00 -90.00  214
 21  \w    -19.00  18.05   0.15    0.75    --  -45.99  19.00 120.00  247
 22  \w     24.00 110.10   0.15    0.75    --   45.99  77.00 -30.00  574
;
_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      -0.0135220000
_diffrn_orient_matrix_UB_12      -0.0042732000
_diffrn_orient_matrix_UB_13      0.0227980000
_diffrn_orient_matrix_UB_21      -0.0144681000
_diffrn_orient_matrix_UB_22      0.0191971000
_diffrn_orient_matrix_UB_23      -0.0290458000
_diffrn_orient_matrix_UB_31      -0.0020766000
_diffrn_orient_matrix_UB_32      -0.1010538000
_diffrn_orient_matrix_UB_33      -0.0063626000
_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_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       94
_diffrn_reflns_limit_h_min       -93
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            146635
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.283
_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    19.313
_exptl_absorpt_correction_T_max  0.274
_exptl_absorpt_correction_T_min  0.043
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
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    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             18091
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.566
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1877
_refine_ls_number_reflns         43775
_refine_ls_number_restraints     958
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.2071
_refine_ls_R_factor_gt           0.1738
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2254P)^2^+2478.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4738
_refine_ls_wR_factor_ref         0.5004
_reflns_Friedel_coverage         0.000
_reflns_number_gt                29042
_reflns_number_total             43775
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_1_24a
_cod_original_formula_sum        'C115.57 H79.80 I18 N36 O1.52 Zn9'
_cod_database_code               1571819
_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   0.225
_shelx_estimated_absorpt_t_min   0.082
_reflns_odcompleteness_completeness 98.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C2A-C1A = C3A-C2A = C4A-C3A = C5A-C4A = C6A-C5A = C6A-C1A
 1.39 with sigma of 0.02
 O2A-C14A = O1A-C13A = O3A-C15A
 1.43 with sigma of 0.02
 C1A-C3A = C2A-C4A = C3A-C5A = C4A-C6A = C5A-C1A = C6A-C2A
 2.4 with sigma of 0.04
 C8A-C14A
 2.4 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 C12A-C8A
 with sigma of 0.04
 I416-Zn48 \\sim I316-Zn38
 with sigma of 0.02
 C7A-C4A \\sim C5A-C13A
 with sigma of 0.02
 O3A-C12A \\sim O2A-C8A
 with sigma of 0.02
 Zn35-N318 \\sim Zn45-N318
 with sigma of 0.02
 Zn39-N331 \\sim Zn49-N331
 with sigma of 0.02
 I309-N318 \\sim I409-N318
 with sigma of 0.04
 I415-Zn48 \\sim I315-Zn38
 with sigma of 0.02
 I310-N318 \\sim I410-N318
 with sigma of 0.04
 I317-N331 \\sim I417-N331
 with sigma of 0.04
 I318-N331 \\sim I418-N331
 with sigma of 0.04
 Zn48-N329 \\sim Zn38-N329
 with sigma of 0.02
 I416-I415 \\sim I316-I315
 with sigma of 0.04
 I416-N329 \\sim I316-N329
 with sigma of 0.04
 I415-N329 \\sim I315-N329
 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-N319 \\sim Zn45-N319
 with sigma of 0.02
 I309-I310 \\sim I409-I410
 with sigma of 0.04
 I309-N319 \\sim I409-N319
 with sigma of 0.04
 I310-N319 \\sim I410-N319
 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 Zn33-N311 \\sim Zn43-N311
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N311 \\sim I406-N311
 with sigma of 0.04
 I305-N311 \\sim I405-N311
 with sigma of 0.04
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I302-I301 \\sim I402-I401
 with sigma of 0.04
 I413-Zn47 \\sim I313-Zn37
 with sigma of 0.02
 I414-Zn47 \\sim I314-Zn37
 with sigma of 0.02
 Zn47-N324 \\sim Zn37-N324
 with sigma of 0.02
 Zn47-N325 \\sim Zn37-N325
 with sigma of 0.02
 I413-I414 \\sim I313-I314
 with sigma of 0.04
 I413-N324 \\sim I313-N324
 with sigma of 0.04
 I413-N325 \\sim I313-N325
 with sigma of 0.04
 I414-N324 \\sim I314-N324
 with sigma of 0.04
 I414-N325 \\sim I314-N325
 with sigma of 0.04
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I303-N306 \\sim I403-N306
 with sigma of 0.04
 I303-N307 \\sim I403-N307
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I304-N307 \\sim I404-N307
 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
 N312-Zn34 \\sim N312-Zn44
 with sigma of 0.02
 N313-Zn34 \\sim N313-Zn44
 with sigma of 0.02
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 Zn34-I307 \\sim Zn44-I407
 with sigma of 0.02
 N312-I308 \\sim N312-I408
 with sigma of 0.04
 N312-I307 \\sim N312-I407
 with sigma of 0.04
 N313-I308 \\sim N313-I408
 with sigma of 0.04
 N313-I307 \\sim N313-I407
 with sigma of 0.04
 I308-I307 \\sim I408-I407
 with sigma of 0.04
 I308-Zn34 \\sim I508-Zn54
 with sigma of 0.02
 I307-Zn34 \\sim I507-Zn54
 with sigma of 0.02
 I317-Zn39 \\sim I417-Zn49
 with sigma of 0.02
 I318-Zn39 \\sim I418-Zn49
 with sigma of 0.02
 Zn39-N330 \\sim Zn49-N330
 with sigma of 0.02
 I317-I318 \\sim I417-I418
 with sigma of 0.04
 I317-N330 \\sim I417-N330
 with sigma of 0.04
 I318-N330 \\sim I418-N330
 with sigma of 0.04
 I518-Zn59 \\sim I418-Zn49
 with sigma of 0.02
 I517-Zn59 \\sim I417-Zn49
 with sigma of 0.02
 N325-C373 \\sim N325-C473
 with sigma of 0.02
 N325-C377 \\sim N325-C477
 with sigma of 0.02
 C375-C374 \\sim C375-C474
 with sigma of 0.02
 C375-C376 \\sim C375-C476
 with sigma of 0.02
 C374-C373 \\sim C474-C473
 with sigma of 0.02
 C376-C377 \\sim C476-C477
 with sigma of 0.02
 N325-C374 \\sim N325-C474
 with sigma of 0.04
 N325-C376 \\sim N325-C476
 with sigma of 0.04
 C375-C373 \\sim C375-C473
 with sigma of 0.04
 C375-C377 \\sim C375-C477
 with sigma of 0.04
 Zn33-N311 \\sim Zn33-N411
 with sigma of 0.02
 N311-C329 \\sim N411-C429
 with sigma of 0.02
 N311-C330 \\sim N411-C430
 with sigma of 0.02
 N311-Zn43 \\sim N411-Zn43
 with sigma of 0.02
 C327-C325 \\sim C427-C325
 with sigma of 0.02
 C327-C328 \\sim C427-C428
 with sigma of 0.02
 C327-C331 \\sim C427-C431
 with sigma of 0.02
 C329-C328 \\sim C429-C428
 with sigma of 0.02
 C331-C330 \\sim C431-C430
 with sigma of 0.02
 Zn33-C329 \\sim Zn33-C429
 with sigma of 0.04
 Zn33-C330 \\sim Zn33-C430
 with sigma of 0.04
 N311-C328 \\sim N411-C428
 with sigma of 0.04
 N311-C331 \\sim N411-C431
 with sigma of 0.04
 C327-C329 \\sim C427-C429
 with sigma of 0.04
 C327-C330 \\sim C427-C430
 with sigma of 0.04
 C325-C328 \\sim C325-C428
 with sigma of 0.04
 C325-C331 \\sim C325-C431
 with sigma of 0.04
 C329-C330 \\sim C429-C430
 with sigma of 0.04
 C329-Zn43 \\sim C429-Zn43
 with sigma of 0.04
 C328-C331 \\sim C428-C431
 with sigma of 0.04
 C330-Zn43 \\sim C430-Zn43
 with sigma of 0.04
3. Restrained planarity
 C7A, C8A, C9A, C10A, C11A, C12A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4A \\sim O3A \\sim C12A \\sim C15A \\sim C11A \\sim C7A \\sim C10A \\sim C8A
\\sim C9A \\sim C5A \\sim C3A \\sim O2A \\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
N318 \\sim C352 \\sim C353 \\sim C354 \\sim C350 \\sim C351: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I310 \\sim I410 \\sim Zn45 \\sim Zn35 \\sim I409 \\sim I309: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I312 \\sim I412 \\sim Zn36 \\sim Zn46 \\sim I311 \\sim I411: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C323 \\sim N307 \\sim C319 \\sim C320 \\sim C321 \\sim C322: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C403 \\sim C399 \\sim C400 \\sim C401 \\sim N335 \\sim C402: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C393 \\sim C395 \\sim C394 \\sim C392 \\sim C391 \\sim N331: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C309 \\sim C310 \\sim C311 \\sim N305 \\sim C312 \\sim C313: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N323 \\sim C363 \\sim C364 \\sim C367 \\sim C365 \\sim C366: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(I309) = Uanis(I409)
Uanis(Zn45) = Uanis(Zn35)
Uanis(Zn44) = Uanis(Zn34)
Uanis(Zn33) = Uanis(Zn43)
Uanis(Zn48) = Uanis(Zn38)
Uanis(I415) = Uanis(I315)
Uanis(N311) = Uanis(C327) = Uanis(C329) = Uanis(C328) = Uanis(C331) =
Uanis(C330) = Uanis(C430) = Uanis(C429) = Uanis(C431) = Uanis(C428) =
Uanis(C427) = Uanis(N411)
Uanis(C374) = Uanis(C376) = Uanis(C373) = Uanis(C377) = Uanis(C473) =
Uanis(C474) = Uanis(C476) = Uanis(C477)
5. Rigid body (RIGU) restrains
 C4A, O3A, C12A, C15A, C11A, C7A, C10A, C8A, C9A, C5A, C3A, O2A, C6A, C13A,
 C2A, C14A, C1A, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N318, C352, C353, C354, C350, C351
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C323, N307, C319, C320, C321, C322
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N335, C402, C399, C401, C403, C400
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N331, C393, C395, C394, C392, C391
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C309, C310, C311, N305, C312, C313
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N323, C364, C367, C365, C366, C363
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C345, C349, C346, N317, C347, C348
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N312, C336, C335, C333, C332, C334
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I317, I417, Zn49, Zn39, I418, I318
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I409)=Sof(Zn45)=Sof(I410)=1-FVAR(1)
 Sof(I309)=Sof(I310)=Sof(Zn35)=FVAR(1)
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(2)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(2)
 Sof(I402)=Sof(Zn41)=Sof(I401)=1-FVAR(3)
 Sof(I302)=Sof(I301)=Sof(Zn31)=Sof(H402)=FVAR(3)
 Sof(I314)=Sof(Zn37)=Sof(I313)=1-FVAR(4)
 Sof(I413)=Sof(I414)=Sof(Zn47)=FVAR(4)
 Sof(I404)=Sof(Zn42)=Sof(I403)=1-FVAR(5)
 Sof(I303)=Sof(I304)=Sof(Zn32)=FVAR(5)
 Sof(Zn46)=Sof(I412)=Sof(I411)=1-FVAR(6)
 Sof(I312)=Sof(I311)=Sof(Zn36)=FVAR(6)
 Sof(C473)=Sof(H473)=Sof(C474)=Sof(H474)=Sof(C476)=Sof(H476)=Sof(C477)=
 Sof(H477)=1-FVAR(7)
 Sof(C374)=Sof(H374)=Sof(C376)=Sof(H376)=Sof(C373)=Sof(H373)=Sof(C377)=
 Sof(H377)=FVAR(7)
 Fixed Sof: I416(0.21481) I415(0.21481) I317(0.44815) I318(0.44815)
 Zn48(0.21481) Zn39(0.44815) N311(0.71541) C327(0.71541) C329(0.71541)
 H329(0.71541) C328(0.71541) H328(0.71541) C331(0.71541) H331(0.71541)
 C330(0.71541) H330(0.71541) I316(0.78519) Zn38(0.78519) I315(0.78519)
 I308(0.42339) Zn34(0.42339) I307(0.42339) I408(0.53218) Zn44(0.53218)
 I407(0.53218) I508(0.04442) I507(0.04442) Zn54(0.04442) I417(0.51162)
 Zn49(0.51162) I418(0.51162) I517(0.04023) Zn59(0.04023) I518(0.04023)
 O3A(0.5048) C1A(0.5048) H1A(0.5048) O1A(0.5048) H1AA(0.5048) O2A(0.5048)
 C5A(0.5048) C12A(0.5048) C4A(0.5048) C6A(0.5048) H6A(0.5048) C8A(0.5048)
 C11A(0.5048) H11A(0.5048) C9A(0.5048) H9A(0.5048) C14A(0.5048) H14A(0.5048)
 H14B(0.5048) H14C(0.5048) C2A(0.5048) H2A(0.5048) C15A(0.5048) H15A(0.5048)
 H15B(0.5048) H15C(0.5048) C7A(0.5048) C13A(0.5048) H13A(0.5048) H13B(0.5048)
 C430(0.28459) H430(0.28459) C429(0.28459) H429(0.28459) C431(0.28459)
 H431(0.28459) C428(0.28459) H428(0.28459) C427(0.28459) N411(0.28459)
 C3A(0.5048) H3A(0.5048) C10A(0.5048) H10A(0.5048)
 Fixed Uiso: I508(0.08) I507(0.08) Zn54(0.08) I517(0.08) Zn59(0.08) I518(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B)
7.b Aromatic/amide H refined with riding coordinates:
 C385(H385), C310(H310), C311(H311), C312(H312), C313(H313), C395(H395),
 C402(H402), C404(H404), C384(H384), C405(H405), C317(H317), C382(H382),
 C329(H329), C353(H353), C355(H355), C328(H328), C389(H389), C364(H364),
 C401(H401), C320(H320), C354(H354), C368(H368), C318(H318), C403(H403),
 C356(H356), C390(H390), C358(H358), C407(H407), C323(H323), C359(H359),
 C400(H400), C336(H336), C372(H372), C394(H394), C335(H335), C314(H314),
 C337(H337), C319(H319), C383(H383), C366(H366), C374(H374), C315(H315),
 C408(H408), C322(H322), C331(H331), C392(H392), C340(H340), C333(H333),
 C367(H367), C376(H376), C332(H332), C391(H391), C369(H369), C373(H373),
 C371(H371), C338(H338), C377(H377), C341(H341), C330(H330), C387(H387),
 C386(H386), C305(H305), C304(H304), C302(H302), C301(H301), C349(H349),
 C346(H346), C347(H347), C365(H365), C348(H348), C1A(H1A), C6A(H6A), C11A(H11A),
  C9A(H9A), C2A(H2A), C473(H473), C474(H474), C476(H476), C477(H477),
 C350(H350), C351(H351), C430(H430), C429(H429), C431(H431), C428(H428),
 C3A(H3A), C10A(H10A)
7.c Fitted hexagon refined as free rotating group:
 C309(C310,C311,N305,C312,C313), N301(C305,C304,C303,C302,C301)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1AA)
7.e Idealised Me refined with everything fixed:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C)
;
_shelx_res_checksum              9062
_shelx_hkl_checksum              46719
_olex2_date_sample_data_collection 2022-01-25
_olex2_date_sample_submission    2022-01-25
_olex2_submission_original_sample_id 4_1_24a
_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 4.047
_oxdiff_exptl_absorpt_empirical_full_min 0.169