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_1571882
_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         'C144 H96 I24 N48 Zn12, 7.746(C14 H12 O)'
_chemical_formula_sum            'C252.44 H188.95 I24 N48 O7.74 Zn12'
_chemical_formula_weight         7848.75
_chemical_name_systematic
'phenyl(p-tolyl)methanone (absorbed in crystalline sponge)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-27
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                67.9240(10)
_cell_angle_beta                 74.7400(10)
_cell_angle_gamma                73.0100(10)
_cell_formula_units_Z            2
_cell_length_a                   18.8343(3)
_cell_length_b                   29.6438(5)
_cell_length_c                   32.8648(5)
_cell_measurement_reflns_used    53785
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.3170
_cell_measurement_theta_min      2.5360
_cell_volume                     16016.3(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      100.00(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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     29.00  78.00   0.50    0.75    --   51.57-109.00 129.00   98
  2  \w    -76.00  -6.00   0.50    0.75    --  -55.07 109.00-134.00  140
  3  \w    -86.00 -61.00   0.50    1.80    --  -79.34 109.00-134.00   50
  4  \w   -137.00-112.00   0.50    1.80    --  -79.34-109.00 129.00   50
  5  \w     91.00 135.00   0.50    1.80    --   83.39 109.00-134.00   88
  6  \w     63.00 106.00   0.50    1.80    --   83.39-109.00 129.00   86
  7  \w     -9.00  18.00   0.50    0.75    --   51.57 -57.00 -30.00   54
  8  \w     33.00  61.00   0.50    0.75    --   51.57 -57.00 -30.00   56
  9  \w    -13.00  19.00   0.50    0.75    --   51.57 -19.00 150.00   64
 10  \w     46.00 113.00   0.50    0.75    --   51.57  57.00  60.00  134
 11  \w    -12.00  17.00   0.50    0.75    --   51.57 -19.00-180.00   58
 12  \w    -15.00  15.00   0.50    0.75    --  -55.07  19.00 120.00   60
 13  \w   -107.00 -40.00   0.50    0.75    --  -55.07 -77.00   0.00  134
 14  \w    -63.00 -32.00   0.50    1.80    --  -79.34  57.00   0.00   62
 15  \w   -139.00 -91.00   0.50    1.80    --  -79.34 -99.00   0.00   96
 16  \w    -40.00 -15.00   0.50    1.80    --  -79.34  37.00 -30.00   50
 17  \w    -40.00  -8.00   0.50    1.80    --  -79.34  37.00-150.00   64
 18  \w     16.00  41.00   0.50    1.80    --   83.39 -57.00-180.00   50
 19  \w     13.00  43.00   0.50    1.80    --   83.39 -37.00-150.00   60
 20  \w     18.00  43.00   0.50    1.80    --   83.39 -37.00 -30.00   50
 21  \w     17.00  68.00   0.50    1.80    --   83.39 -57.00  30.00  102
 22  \w     24.00  60.00   0.50    1.80    --   83.39 -57.00 150.00   72
 23  \w     13.00  41.00   0.50    1.80    --   83.39 -37.00  30.00   56
 24  \w     14.00  42.00   0.50    1.80    --   83.39 -37.00 -90.00   56
 25  \w     76.00 103.00   0.50    1.80    --   83.39-125.00 120.00   54
 26  \w     12.00  43.00   0.50    1.80    --   83.39 -37.00  90.00   62
 27  \w     26.00  51.00   0.50    1.80    --   83.39-125.00 120.00   50
 28  \w     19.00  45.00   0.50    1.80    --   83.39 -57.00-120.00   52
 29  \w     77.00 124.00   0.50    1.80    --   83.39  57.00  30.00   94
 30  \w     86.00 112.00   0.50    1.80    --   83.39-125.00  30.00   52
 31  \w     24.00 112.00   0.50    1.80    --   83.39-125.00 -60.00  176
 32  \w     17.00  67.00   0.50    1.80    --   83.39 -57.00 -90.00  100
 33  \w     41.00  67.00   0.50    1.80    --   83.39 -77.00-120.00   52
 34  \w     13.00  42.00   0.50    1.80    --   83.39 -37.00-180.00   58
 35  \w     37.00  97.00   0.50    1.80    --   83.39   0.00 150.00  120
 36  \w    105.00 144.00   0.50    1.80    --   83.39   0.00 150.00   78
 37  \w     23.00  67.00   0.50    1.80    --   83.39-125.00  30.00   88
 38  \w     31.00  68.00   0.50    1.80    --   83.39 -57.00  60.00   74
 39  \w     48.00  96.00   0.50    1.80    --   83.39 -99.00-150.00   96
 40  \w     12.00  38.00   0.50    1.80    --   83.39 -37.00 -60.00   52
 41  \w     51.00  85.00   0.50    1.80    --   83.39-125.00   0.00   68
 42  \w     61.00 112.00   0.50    1.80    --   83.39-125.00  90.00  102
 43  \w     75.00 102.00   0.50    1.80    --   83.39  57.00-180.00   54
 44  \w    108.00 149.00   0.50    1.80    --   83.39  57.00-180.00   82
 45  \w     27.00  73.00   0.50    1.80    --   83.39 -99.00-120.00   92
 46  \w     42.00 106.00   0.50    1.80    --   83.39 -99.00 -60.00  128
 47  \w     41.00  68.00   0.50    1.80    --   83.39 -77.00   0.00   54
 48  \w     36.00  89.00   0.50    1.80    --   83.39 -77.00 -30.00  106
 49  \w     13.00  39.00   0.50    1.80    --   83.39 -37.00   0.00   52
 50  \w    102.00 128.00   0.50    1.80    --   83.39  57.00 150.00   52
 51  \w    110.00 143.00   0.50    1.80    --   83.39  77.00 150.00   66
 52  \w     72.00 104.00   0.50    1.80    --   83.39  77.00 120.00   64
 53  \w    108.00 135.00   0.50    1.80    --   83.39  77.00 120.00   54
 54  \w     35.00 107.00   0.50    1.80    --   92.00-103.00 154.83  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, 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      0.0335079000
_diffrn_orient_matrix_UB_12      0.0125217000
_diffrn_orient_matrix_UB_13      -0.0500515000
_diffrn_orient_matrix_UB_21      -0.0025036000
_diffrn_orient_matrix_UB_22      -0.0522375000
_diffrn_orient_matrix_UB_23      0.0018753000
_diffrn_orient_matrix_UB_31      -0.0800744000
_diffrn_orient_matrix_UB_32      0.0203398000
_diffrn_orient_matrix_UB_33      -0.0113635000
_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  0.0699
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            254275
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.491
_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    19.552
_exptl_absorpt_correction_T_max  0.468
_exptl_absorpt_correction_T_min  0.068
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             7467
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.703
_refine_diff_density_min         -2.467
_refine_diff_density_rms         0.289
_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     3592
_refine_ls_number_reflns         58479
_refine_ls_number_restraints     1626
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.1089
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1719P)^2^+344.9750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3369
_refine_ls_wR_factor_ref         0.3547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                43554
_reflns_number_total             58479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_mbp_50_10_96a
_cod_database_code               1571882
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36)2 (C14 H12 O)5 (C6 H12)3'
_chemical_oxdiff_usercomment     4-methylbenzophenone
_shelx_estimated_absorpt_t_max   0.245
_shelx_estimated_absorpt_t_min   0.073
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6D-C5D = C6D-C1D = C2D-C1D = C3D-C2D = C4D-C3D = C5D-C4D
 1.39 with sigma of 0.02
 C2I-C1I = C3I-C2I = C4I-C3I = C5I-C4I = C6I-C5I = C6I-C1I
 1.39 with sigma of 0.02
 C9I-C8I = C9I-C10I = C11I-C10I = C12I-C11I = C13I-C12I = C8I-C13I
 1.39 with sigma of 0.02
 C8I-C7I = C7I-C1I
 1.48 with sigma of 0.02
 C13J-C8J = C8J-C9J = C10J-C9J = C11J-C10J = C11J-C12J = C13J-C12J
 1.39 with sigma of 0.02
 C4I-C14I
 1.5 with sigma of 0.02
 O1I-C7I
 1.22 with sigma of 0.02
 C8J-C7J = C7J-C6J
 1.48 with sigma of 0.02
 O1J-C7J
 1.22 with sigma of 0.01
 C3C-C2C = C4C-C3C = C5C-C4C = C6C-C5C = C6C-C1C = C2C-C1C
 1.39 with sigma of 0.02
 C3J-C14J
 1.5 with sigma of 0.02
 C4H-C3H = C5H-C4H = C6H-C5H = C6H-C1H = C1H-C2H = C2H-C3H
 1.39 with sigma of 0.02
 C8H-C9H = C10H-C9H = C11H-C10H = C11H-C12H = C12H-C13H = C8H-C13H
 1.39 with sigma of 0.02
 O1G-C7G
 1.22 with sigma of 0.02
 C4G-C14G
 1.5 with sigma of 0.02
 O1H-C7H
 1.22 with sigma of 0.02
 C4H-C14H
 1.5 with sigma of 0.01
 C9F-C8F = C10F-C9F = C10F-C11F = C11F-C12F = C12F-C13F = C13F-C8F
 1.39 with sigma of 0.02
 C7F-C1F
 1.48 with sigma of 0.02
 C4F-C14F
 1.5 with sigma of 0.02
 O1F-C7F
 1.22 with sigma of 0.01
 C2E-C1E = C3E-C2E = C4E-C3E = C5E-C4E = C6E-C5E = C6E-C1E
 1.39 with sigma of 0.02
 O1E-C7E
 1.22 with sigma of 0.02
 C4B-C14B
 1.5 with sigma of 0.02
 C8D-C13D = C9D-C8D = C9D-C10D = C11D-C10D = C12D-C11D = C13D-C12D
 1.39 with sigma of 0.02
 O1A-C7A
 1.22 with sigma of 0.02
 O1D-C7D
 1.22 with sigma of 0.02
 C4D-C14D
 1.5 with sigma of 0.02
 C1I-C3I = C2I-C4I = C3I-C5I = C4I-C6I = C5I-C1I = C6I-C2I
 2.4 with sigma of 0.04
 C8I-C10I = C9I-C11I = C10I-C12I = C11I-C13I = C12I-C8I = C13I-C9I
 2.4 with sigma of 0.04
 C1I-C8I
 2.57 with sigma of 0.02
 C3I-C14I
 2.5 with sigma of 0.04
 C1I-O1I
 2.34 with sigma of 0.02
 C8I-O1I
 2.34 with sigma of 0.04
 C5I-C14I
 2.5 with sigma of 0.04
 C8J-C10J = C9J-C11J = C10J-C12J = C11J-C13J = C12J-C8J = C13J-C9J
 2.4 with sigma of 0.04
 C6J-O1J
 2.34 with sigma of 0.04
 C8J-O1J
 2.34 with sigma of 0.02
 C1C-O1C
 2.34 with sigma of 0.04
 C1G-C8G
 2.57 with sigma of 0.04
 C5G-C14G
 2.5 with sigma of 0.04
 C1H-C8H
 2.57 with sigma of 0.02
 C3H-C14H = C5H-C14H
 2.5 with sigma of 0.02
 C8H-O1H
 2.34 with sigma of 0.04
 C8F-C10F = C9F-C11F = C10F-C12F = C11F-C13F = C12F-C8F = C13F-C9F
 2.4 with sigma of 0.04
 C8F-C1F
 2.57 with sigma of 0.02
 C1E-C3E = C2E-C4E = C3E-C5E = C4E-C6E = C5E-C1E = C6E-C2E
 2.4 with sigma of 0.04
 C1E-C8E
 2.57 with sigma of 0.04
 C8E-O1E
 2.4 with sigma of 0.02
 C8B-C1B
 2.57 with sigma of 0.02
 C1D-C3D = C2D-C4D = C3D-C5D = C4D-C6D = C5D-C1D = C6D-C2D
 2.4 with sigma of 0.04
 C1A-C8A
 2.57 with sigma of 0.02
 C8D-C10D = C9D-C11D = C10D-C12D = C11D-C13D = C12D-C8D = C13D-C9D
 2.4 with sigma of 0.04
 C1B-O1B
 2.4 with sigma of 0.04
 C8C-O1C
 2.34 with sigma of 0.04
 I502-Zn51 \\sim I302-Zn31
 with sigma of 0.02
 C1I-C4I \\sim C2I-C5I \\sim C3I-C6I
 with sigma of 0.04
 I501-Zn51 \\sim I301-Zn31
 with sigma of 0.02
 C8I-C11I \\sim C9I-C12I \\sim C10I-C13I
 with sigma of 0.04
 Zn51-N301 \\sim Zn31-N301
 with sigma of 0.02
 I502-I501 \\sim I302-I301
 with sigma of 0.04
 I502-N301 \\sim I302-N301
 with sigma of 0.04
 I501-N301 \\sim I301-N301
 with sigma of 0.04
 I316-Zn38 \\sim I516-Zn58
 with sigma of 0.02
 I315-Zn38 \\sim I515-Zn58
 with sigma of 0.02
 Zn38-N329 \\sim Zn58-N329
 with sigma of 0.02
 I316-I315 \\sim I516-I515
 with sigma of 0.04
 I316-N329 \\sim I516-N329
 with sigma of 0.04
 I315-N329 \\sim I515-N329
 with sigma of 0.04
 I519-Zn50 \\sim I419-Zn40
 with sigma of 0.02
 I520-Zn50 \\sim I420-Zn40
 with sigma of 0.02
 Zn50-N336 \\sim Zn40-N336
 with sigma of 0.02
 Zn50-N337 \\sim Zn40-N337
 with sigma of 0.02
 I519-I520 \\sim I419-I420
 with sigma of 0.04
 I519-N336 \\sim I419-N336
 with sigma of 0.04
 I519-N337 \\sim I419-N337
 with sigma of 0.04
 I520-N336 \\sim I420-N336
 with sigma of 0.04
 I520-N337 \\sim I420-N337
 with sigma of 0.04
 C4J-C14J \\sim C14J-C2J
 with sigma of 0.02
 I323-Zn42 \\sim I523-Zn1
 with sigma of 0.02
 I324-Zn42 \\sim I524-Zn1
 with sigma of 0.02
 Zn42-N343 \\sim Zn1-N343
 with sigma of 0.02
 Zn42-N342 \\sim Zn1-N342
 with sigma of 0.02
 I323-I324 \\sim I523-I524
 with sigma of 0.04
 I323-N343 \\sim I523-N343
 with sigma of 0.04
 C9C-C8C \\sim C9C-C10C \\sim C11C-C10C \\sim C12C-C11C \\sim C13C-C12C \\sim
C8C-C13C
 with sigma of 0.02
 I323-N342 \\sim I523-N342
 with sigma of 0.04
 I324-N343 \\sim I524-N343
 with sigma of 0.04
 I324-N342 \\sim I524-N342
 with sigma of 0.04
 C8C-C7C \\sim C7C-C1C
 with sigma of 0.02
 I310-Zn35 \\sim I510-Zn35
 with sigma of 0.02
 I309-Zn35 \\sim I509-Zn35
 with sigma of 0.02
 I311-Zn36 \\sim I511-Zn56
 with sigma of 0.02
 I312-Zn36 \\sim I512-Zn56
 with sigma of 0.02
 Zn36-N319 \\sim Zn56-N319
 with sigma of 0.02
 Zn36-N318 \\sim Zn56-N318
 with sigma of 0.02
 I311-I312 \\sim I511-I512
 with sigma of 0.04
 I311-N319 \\sim I511-N319
 with sigma of 0.04
 I311-N318 \\sim I511-N318
 with sigma of 0.04
 I312-N319 \\sim I512-N319
 with sigma of 0.04
 I312-N318 \\sim I512-N318
 with sigma of 0.04
 I720-Zn70 \\sim I420-Zn40
 with sigma of 0.02
 I719-Zn70 \\sim I519-Zn50
 with sigma of 0.02
 I712-Zn76 \\sim I312-Zn36
 with sigma of 0.02
 I311-Zn36 \\sim I711-Zn76
 with sigma of 0.02
 I304-Zn32 \\sim I504-Zn52
 with sigma of 0.02
 I303-Zn32 \\sim I503-Zn52
 with sigma of 0.02
 Zn32-N305 \\sim Zn52-N305
 with sigma of 0.02
 I304-I303 \\sim I504-I503
 with sigma of 0.04
 I304-N305 \\sim I504-N305
 with sigma of 0.04
 I303-N305 \\sim I503-N305
 with sigma of 0.04
 I313-Zn37 \\sim I513-Zn57
 with sigma of 0.02
 I314-Zn37 \\sim I514-Zn57
 with sigma of 0.02
 C4G-C3G \\sim C5G-C4G \\sim C6G-C5G \\sim C6G-C1G \\sim C2G-C1G \\sim C3G-C2G
 with sigma of 0.02
 Zn37-N324 \\sim Zn57-N324
 with sigma of 0.02
 Zn37-N325 \\sim Zn57-N325
 with sigma of 0.02
 I313-I314 \\sim I513-I514
 with sigma of 0.04
 I313-N324 \\sim I513-N324
 with sigma of 0.04
 I313-N325 \\sim I513-N325
 with sigma of 0.04
 I314-N324 \\sim I514-N324
 with sigma of 0.04
 I314-N325 \\sim I514-N325
 with sigma of 0.04
 I724-Zn82 \\sim I324-Zn42
 with sigma of 0.02
 I723-Zn82 \\sim I523-Zn1
 with sigma of 0.02
 C9G-C8G \\sim C9G-C10G \\sim C11G-C10G \\sim C12G-C11G \\sim C13G-C12G \\sim
C8G-C13G
 with sigma of 0.02
 C1G-C3G \\sim C2G-C4G \\sim C3G-C5G \\sim C4G-C6G \\sim C5G-C1G \\sim C6G-C2G
 with sigma of 0.04
 C8G-C10G \\sim C9G-C11G \\sim C10G-C12G \\sim C11G-C13G
 with sigma of 0.04
 C7G-C1G \\sim C8G-C7G
 with sigma of 0.02
 C8H-C10H \\sim C9H-C11H \\sim C10H-C12H \\sim C11H-C13H \\sim C12H-C8H
 with sigma of 0.04
 C7H-C1H \\sim C8H-C7H
 with sigma of 0.02
 C2F-C3F \\sim C4F-C3F \\sim C5F-C4F \\sim C6F-C5F \\sim C6F-C1F \\sim C2F-C1F
 with sigma of 0.02
 C1F-C3F \\sim C3F-C5F \\sim C5F-C1F \\sim C6F-C2F
 with sigma of 0.04
 C9E-C8E \\sim C9E-C10E \\sim C11E-C10E \\sim C12E-C11E \\sim C13E-C12E \\sim
C8E-C13E
 with sigma of 0.02
 C7E-C1E \\sim C8E-C7E
 with sigma of 0.02
 C13B-C12B \\sim C8B-C13B \\sim C9B-C8B \\sim C9B-C10B \\sim C11B-C10B \\sim
C12B-C11B
 with sigma of 0.02
 C1E-C4E \\sim C2E-C5E \\sim C3E-C6E
 with sigma of 0.04
 C1B-C3B \\sim C2B-C4B \\sim C3B-C5B \\sim C4B-C6B \\sim C5B-C1B \\sim C6B-C2B
 with sigma of 0.04
 C12B-C8B \\sim C13B-C9B
 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
 C9A-C8A \\sim C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim C13A-C12A \\sim
C8A-C13A
 with sigma of 0.02
 C2B-C1B \\sim C3B-C2B \\sim C4B-C3B \\sim C5B-C4B \\sim C6B-C5B \\sim C6B-C1B
 with sigma of 0.02
 C1A-C3A \\sim C2A-C4A \\sim C3A-C5A
 with sigma of 0.04
 C13A-C9A \\sim C8A-C10A
 with sigma of 0.04
 C7A-C1A \\sim C8A-C7A
 with sigma of 0.02
 C7D-C1D \\sim C8D-C7D
 with sigma of 0.02
 C8E-C10E \\sim C13E-C9E
 with sigma of 0.04
3. Restrained planarity
 C4I, C6I, C1I, C3I, C5I, C2I
 with sigma of 0.1
 C6I, C5I, C4I, C1I, C2I, C3I, C7I, C14I
 with sigma of 0.1
 C9J, C12J, C13J, C11J, C8J, C10J
 with sigma of 0.1
 C6C, C2C, C4C, C3C, C5C, C1C
 with sigma of 0.1
 C8G, C11G, C13G, C12G, C9G, C10G
 with sigma of 0.1
 C4G, C5G, C3G, C14G
 with sigma of 0.1
 C8H, C12H, C11H, C9H, C13H, C10H
 with sigma of 0.1
 C4E, C5E, C6E, C1E, C2E, C3E
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7I \\sim C6I \\sim C5I \\sim C1I \\sim C4I \\sim C2I \\sim C3I \\sim C14I
\\sim O1I \\sim C8I \\sim C9I \\sim C13I \\sim C10I \\sim C12I \\sim C11I:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C7J \\sim C4J \\sim C5J \\sim C3J \\sim C6J \\sim C2J \\sim C14J \\sim C1J
\\sim O1J \\sim C8J \\sim C9J \\sim C13J \\sim C10J \\sim C12J \\sim C11J:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C8H \\sim O1H \\sim C7H \\sim C1H \\sim C13H \\sim C9H \\sim C2H \\sim C6H
\\sim C12H \\sim C10H \\sim C3H \\sim C5H \\sim C11H \\sim C4H \\sim C14H:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C13F \\sim O1F \\sim C7F \\sim C1F \\sim C8F \\sim C2F \\sim C6F \\sim C9F
\\sim C3F \\sim C5F \\sim C12F \\sim C10F \\sim C4F \\sim C11F \\sim C14F:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O1A \\sim C7A \\sim C1A \\sim C8A \\sim C6A \\sim C2A \\sim C13A \\sim C9A
\\sim C5A \\sim C3A \\sim C12A \\sim C10A \\sim C4A \\sim C11A \\sim C14A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C5D \\sim O1D \\sim C7D \\sim C8D \\sim C1D \\sim C13D \\sim C9D \\sim C6D
\\sim C2D \\sim C12D \\sim C10D \\sim C3D \\sim C11D \\sim C4D \\sim C14D:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C7B \\sim C8B \\sim C13B \\sim C9B \\sim C12B \\sim O1B \\sim C1B \\sim C10B
\\sim C11B \\sim C6B \\sim C2B \\sim C5B \\sim C3B \\sim C4B \\sim C14B: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C1E \\sim C4E \\sim C5E \\sim C14E \\sim C3E \\sim C6E \\sim C2E \\sim C7E
\\sim O1E \\sim C8E \\sim C9E \\sim C13E \\sim C10E \\sim C12E \\sim C11E:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C7G \\sim C8G \\sim C13G \\sim C9G \\sim O1G \\sim C1G \\sim C12G \\sim C10G
\\sim C2G \\sim C6G \\sim C11G \\sim C3G \\sim C5G \\sim C4G \\sim C14G: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C7C \\sim C6C \\sim C5C \\sim C1C \\sim C4C \\sim C2C \\sim C3C \\sim C14C
\\sim O1C \\sim C8C \\sim C9C \\sim C13C \\sim C10C \\sim C12C \\sim C11C:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C7I, C6I, C5I, C1I, C4I, C2I, C3I, C14I, O1I, C8I, C9I, C13I, C10I, C12I, C11I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7J, C4J, C5J, C3J, C6J, C2J, C14J, C1J, O1J, C8J, C9J, C13J, C10J, C12J, C11J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I302)=Sof(Zn31)=Sof(I301)=1-FVAR(1)
 Sof(I502)=Sof(I501)=Sof(Zn51)=FVAR(1)
 Sof(I516)=Sof(Zn58)=Sof(I515)=1-FVAR(2)
 Sof(I316)=Sof(I315)=Sof(Zn38)=FVAR(2)
 Sof(I510)=Sof(I509)=1-FVAR(3)
 Sof(I310)=Sof(I309)=FVAR(3)
 Sof(I503)=Sof(I504)=Sof(Zn52)=1-FVAR(4)
 Sof(I304)=Sof(I303)=Sof(Zn32)=FVAR(4)
 Sof(I514)=Sof(Zn57)=Sof(I513)=1-FVAR(5)
 Sof(I313)=Sof(I314)=Sof(Zn37)=FVAR(5)
 Fixed Sof: I519(0.3679) I311(0.95857) I520(0.3679) I323(0.60474)
 I324(0.60474) I312(0.95857) Zn50(0.3679) Zn42(0.60474) Zn36(0.95857)
 C4E(0.9645) O1F(0.75333) O1H(0.73368) C3F(0.75333) H3F(0.75333) C5E(0.9645)
 H5E(0.9645) C1F(0.75333) O1E(0.9645) C9E(0.9645) H9E(0.9645) C10E(0.9645)
 H10E(0.9645) C6E(0.9645) H6E(0.9645) C1E(0.9645) C8G(0.65187) C13E(0.9645)
 H13E(0.9645) C13H(0.73368) H13H(0.73368) C8E(0.9645) C7F(0.75333) C11E(0.9645)
 H11E(0.9645) C12E(0.9645) H12E(0.9645) C2E(0.9645) H2E(0.9645) C6C(0.71084)
 H6C(0.71084) C2C(0.71084) H2C(0.71084) C12C(0.71084) H12C(0.71084)
 C8F(0.75333) C2F(0.75333) H2F(0.75333) C7E(0.9645) C11G(0.65187) H11G(0.65187)
 O1G(0.65187) C13F(0.75333) H13F(0.75333) C14E(0.9645) H14J(0.9645)
 H14K(0.9645) H14L(0.9645) C9C(0.71084) H9C(0.71084) C7G(0.65187) C4C(0.71084)
 C13C(0.71084) H13C(0.71084) C3E(0.9645) H3E(0.9645) C3H(0.73368) H3H(0.73368)
 O1C(0.71084) C8C(0.71084) C9F(0.75333) H9F(0.75333) C1G(0.65187) C3C(0.71084)
 H3C(0.71084) C4F(0.75333) C2H(0.73368) H2H(0.73368) C4H(0.73368) C13G(0.65187)
 H13G(0.65187) C9H(0.73368) H9H(0.73368) C2G(0.65187) H2G(0.65187)
 C12H(0.73368) H12H(0.73368) C5F(0.75333) H5F(0.75333) C12G(0.65187)
 H12G(0.65187) C8H(0.73368) C5C(0.71084) H5C(0.71084) C1H(0.73368) C4G(0.65187)
 C10C(0.71084) H10C(0.71084) C1C(0.71084) C12F(0.75333) H12F(0.75333)
 C10H(0.73368) H10H(0.73368) C14F(0.75333) H14M(0.75333) H14N(0.75333)
 H14O(0.75333) C7H(0.73368) C11F(0.75333) H11F(0.75333) C6G(0.65187)
 H6G(0.65187) C5H(0.73368) H5H(0.73368) C10F(0.75333) H10F(0.75333)
 C11C(0.71084) H11C(0.71084) C6H(0.73368) H6H(0.73368) C6F(0.75333)
 H6F(0.75333) C14C(0.71084) H14V(0.71084) H14W(0.71084) H14X(0.71084)
 C7C(0.71084) C5G(0.65187) H5G(0.65187) C9G(0.65187) H9G(0.65187) C10G(0.65187)
 H10G(0.65187) Zn40(0.57315) I420(0.57315) I419(0.57315) C4J(0.44391)
 H4J(0.44391) C5J(0.44391) H5J(0.44391) C6J(0.44391) C1J(0.44391) H1J(0.44391)
 C2J(0.44391) H2J(0.44391) C3J(0.44391) Zn1(0.38267) I524(0.38267)
 I523(0.38267) I724(0.01259) I723(0.01259) Zn82(0.01259) C11H(0.73368)
 H11H(0.73368) C3G(0.65187) H3G(0.65187) C14H(0.73368) H14P(0.73368)
 H14Q(0.73368) H14R(0.73368) C9J(0.44391) H9J(0.44391) C12J(0.44391)
 H12J(0.44391) C13J(0.44391) H13J(0.44391) C11J(0.44391) H11J(0.44391)
 O1J(0.44391) C8J(0.44391) C7J(0.44391) C10J(0.44391) H10J(0.44391)
 C14G(0.65187) H14S(0.65187) H14T(0.65187) H14U(0.65187) I511(0.02525)
 Zn56(0.02525) I512(0.02525) I720(0.05896) Zn70(0.05896) I719(0.05896)
 C6I(0.48786) H6I(0.48786) C9I(0.48786) H9I(0.48786) C12I(0.48786)
 H12I(0.48786) C5I(0.48786) H5I(0.48786) C4I(0.48786) O1I(0.48786)
 C13I(0.48786) H13I(0.48786) C1I(0.48786) C2I(0.48786) H2I(0.48786)
 C3I(0.48786) H3I(0.48786) C8I(0.48786) C7I(0.48786) C14I(0.48786)
 H14Z(0.48786) H(0.48786) HA(0.48786) C11I(0.48786) H11I(0.48786) C10I(0.48786)
 H10I(0.48786) Zn76(0.01619) I711(0.01619) I712(0.01619) C14J(0.44391)
 H14Y(0.44391) HB(0.44391) HC(0.44391)
 Fixed Uiso: I724(0.08) I723(0.08) Zn82(0.08) I510(0.08) I509(0.08) I511(0.08)
 Zn56(0.08) I512(0.08) I720(0.08) Zn70(0.08) I719(0.08) Zn76(0.08) I711(0.08)
 I712(0.08) I503(0.08) I504(0.08) Zn52(0.08)
7.a Aromatic/amide H refined with riding coordinates:
 C395(H395), C315(H315), C323(H323), C394(H394), C322(H322), C405(H405),
 C409(H409), C347(H347), C333(H333), C412(H412), C400(H400), C430(H430),
 C319(H319), C351(H351), C401(H401), C331(H331), C337(H337), C372(H372),
 C5D(H5D), C328(H328), C340(H340), C336(H336), C329(H329), C371(H371),
 C318(H318), C441(H441), C408(H408), C385(H385), C423(H423), C413(H413),
 C427(H427), C410(H410), C436(H436), C364(H364), C403(H403), C332(H332),
 C439(H439), C6A(H6A), C422(H422), C341(H341), C391(H391), C338(H338),
 C431(H431), C13D(H13D), C356(H356), C384(H384), C368(H368), C335(H335),
 C314(H314), C359(H359), C444(H444), C350(H350), C358(H358), C407(H407),
 C419(H419), C420(H420), C374(H374), C383(H383), C11B(H11B), C348(H348),
 C320(H320), C428(H428), C366(H366), C301(H301), C369(H369), C302(H302),
 C12B(H12B), C425(H425), C330(H330), C349(H349), C355(H355), C386(H386),
 C437(H437), C13B(H13B), C392(H392), C438(H438), C13A(H13A), C389(H389),
 C346(H346), C404(H404), C317(H317), C440(H440), C6B(H6B), C5A(H5A), C382(H382),
  C6D(H6D), C9A(H9A), C3D(H3D), C373(H373), C9D(H9D), C377(H377), C443(H443),
 C387(H387), C310(H310), C365(H365), C12A(H12A), C376(H376), C367(H367),
 C313(H313), C3F(H3F), C353(H353), C402(H402), C305(H305), C5E(H5E), C421(H421),
  C2D(H2D), C418(H418), C390(H390), C304(H304), C354(H354), C311(H311),
 C2B(H2B), C426(H426), C9E(H9E), C11D(H11D), C312(H312), C12D(H12D), C11A(H11A),
  C9B(H9B), C3A(H3A), C10E(H10E), C10B(H10B), C6E(H6E), C3B(H3B), C10A(H10A),
 C13E(H13E), C13H(H13H), C5B(H5B), C10D(H10D), C11E(H11E), C12E(H12E), C2E(H2E),
  C6C(H6C), C2C(H2C), C12C(H12C), C2F(H2F), C11G(H11G), C2A(H2A), C13F(H13F),
 C9C(H9C), C13C(H13C), C3E(H3E), C3H(H3H), C9F(H9F), C3C(H3C), C2H(H2H),
 C13G(H13G), C9H(H9H), C2G(H2G), C12H(H12H), C5F(H5F), C12G(H12G), C5C(H5C),
 C10C(H10C), C12F(H12F), C10H(H10H), C11F(H11F), C6G(H6G), C5H(H5H), C10F(H10F),
  C11C(H11C), C6H(H6H), C6F(H6F), C5G(H5G), C9G(H9G), C10G(H10G), C4J(H4J),
 C5J(H5J), C1J(H1J), C2J(H2J), C11H(H11H), C3G(H3G), C9J(H9J), C12J(H12J),
 C13J(H13J), C11J(H11J), C10J(H10J), C6I(H6I), C9I(H9I), C12I(H12I), C5I(H5I),
 C13I(H13I), C2I(H2I), C3I(H3I), C11I(H11I), C10I(H10I)
7.b Fitted hexagon refined as free rotating group:
 C4J(C5J,C6J,C1J,C2J,C3J)
7.c Idealised Me refined as rotating group:
 C14D(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C14B(H14G,H14H,H14I), C14E(H14J,
 H14K,H14L), C14F(H14M,H14N,H14O), C14C(H14V,H14W,H14X), C14H(H14P,H14Q,H14R),
 C14G(H14S,H14T,H14U), C14I(H14Z,H,HA), C14J(H14Y,HB,HC)
;
_shelx_res_checksum              84671
_shelx_hkl_checksum              38102
_olex2_date_sample_data_collection 2024-03-19
_olex2_date_sample_submission    2024-03-19
_olex2_submission_original_sample_id '4-Methylbenzophenone 50_10_96a'
_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 2.670
_oxdiff_exptl_absorpt_empirical_full_min 0.407