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_1571884
_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         'C72 H48 I12 N24 Zn6, 1.655(C14 H12 O1)'
_chemical_formula_sum            'C95.17 H67.86 I12 N24 O1.65 Zn6'
_chemical_formula_weight         3489.13
_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             2024-03-26
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                99.996(3)
_cell_angle_beta                 93.338(3)
_cell_angle_gamma                110.091(3)
_cell_formula_units_Z            2
_cell_length_a                   15.0552(6)
_cell_length_b                   18.9430(7)
_cell_length_c                   30.8258(9)
_cell_measurement_reflns_used    22451
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.4290
_cell_measurement_theta_min      2.5570
_cell_volume                     8064.7(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 0.996
_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     33.00 108.00   0.50    1.50    --   92.00-111.00 -55.41  150
  2  \w     40.00  65.00   0.50    1.50    --   83.39 -96.00 130.00   50
  3  \w    111.00 137.00   0.50    1.50    --   83.39  96.00-120.00   52
  4  \w     88.00 150.00   0.50    1.50    --   83.39  57.00-180.00  124
  5  \w     75.00 150.00   0.50    1.50    --   83.39  57.00 120.00  150
  6  \w     33.00 105.00   0.50    1.50    --   83.39 -99.00 150.00  144
  7  \w    106.00 139.00   0.50    1.50    --   83.39 125.00  60.00   66
  8  \w     70.00 110.00   0.50    1.50    --   83.39-125.00  60.00   80
  9  \w     30.00  99.00   0.50    1.50    --   83.39 -77.00  30.00  138
 10  \w     13.00  42.00   0.50    1.50    --   83.39 -37.00 -90.00   58
 11  \w     84.00 154.00   0.50    1.50    --   83.39  37.00 -90.00  140
 12  \w     86.00 111.00   0.50    1.50    --   83.39-125.00 -90.00   50
 13  \w     47.00  73.00   0.50    1.50    --   83.39 -77.00 -60.00   52
 14  \w     58.00  99.00   0.50    1.50    --   83.39 -77.00-180.00   82
 15  \w     29.00  58.00   0.50    1.50    --   83.39-125.00  60.00   58
 16  \w     81.00 130.00   0.50    1.50    --   83.39  77.00-150.00   98
 17  \w     23.00 110.00   0.50    1.50    --   83.39-125.00 120.00  174
 18  \w     53.00  82.00   0.50    1.50    --   83.39-125.00   0.00   58
 19  \w     31.00  56.00   0.50    1.50    --   83.39 -57.00  30.00   50
 20  \w     12.00  37.00   0.50    1.50    --   83.39 -37.00  30.00   50
 21  \w    101.00 126.00   0.50    1.50    --   83.39  57.00  30.00   50
 22  \w     25.00  52.00   0.50    1.50    --   83.39-125.00   0.00   54
 23  \w     23.00  65.00   0.50    1.50    --   83.39-125.00  30.00   84
 24  \w     58.00 104.00   0.50    1.50    --   83.39 -99.00 120.00   92
 25  \w     41.00  85.00   0.50    1.50    --   83.39 -77.00 150.00   88
 26  \w     77.00 103.00   0.50    1.50    --   83.39-125.00  30.00   52
 27  \w     75.00 136.00   0.50    1.50    --   83.39  57.00-150.00  122
 28  \w     31.00  71.00   0.50    1.50    --   83.39 -77.00 -30.00   80
 29  \w    112.00 137.00   0.50    1.50    --   83.39 125.00-150.00   50
 30  \w     94.00 148.00   0.50    1.50    --   83.39  57.00 150.00  108
 31  \w     67.00  94.00   0.50    1.50    --   83.39  77.00-120.00   54
 32  \w     12.00  37.00   0.50    1.50    --   83.39 -37.00 -30.00   50
 33  \w     15.00  40.00   0.50    1.50    --   83.39 -37.00 -60.00   50
 34  \w     36.00  88.00   0.50    1.50    --   83.39 -77.00   0.00  104
 35  \w   -139.00 -82.00   0.50    1.50    --  -79.34 -96.00 130.00  114
 36  \w    -85.00 -60.00   0.50    1.50    --  -79.34  96.00-120.00   50
 37  \w    -38.00 -12.00   0.50    1.50    --  -79.34  37.00-180.00   52
 38  \w    -37.00  -8.00   0.50    1.50    --  -79.34  37.00 -90.00   58
 39  \w    -95.00 -22.00   0.50    1.50    --  -79.34  77.00  60.00  146
 40  \w    -37.00  -8.00   0.50    1.50    --  -79.34  37.00-120.00   58
 41  \w    -63.00 -38.00   0.50    0.50    --  -55.00  96.00-120.00   50
 42  \w    -13.00  12.00   0.50    0.50    --  -55.00  19.00  90.00   50
 43  \w    -24.00  15.00   0.50    0.50    --  -55.00  19.00   0.00   78
 44  \w    -21.00  11.00   0.50    0.50    --  -55.00  19.00  30.00   64
 45  \w      5.00  77.00   0.50    0.50    --   51.07 -96.00 130.00  144
 46  \w     62.00  99.00   0.50    0.50    --   51.07  57.00-180.00   74
 47  \w    -16.00  43.00   0.50    0.50    --   51.07 -37.00   0.00  118
 48  \w    -11.00  21.00   0.50    0.50    --   51.07 -19.00 -90.00   64
;
_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      0.0367681000
_diffrn_orient_matrix_UB_12      0.0002058000
_diffrn_orient_matrix_UB_13      0.0477351000
_diffrn_orient_matrix_UB_21      0.0706332000
_diffrn_orient_matrix_UB_22      0.0828227000
_diffrn_orient_matrix_UB_23      0.0044383000
_diffrn_orient_matrix_UB_31      -0.0756762000
_diffrn_orient_matrix_UB_32      0.0311943000
_diffrn_orient_matrix_UB_33      0.0178716000
_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  0.0857
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            113925
_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         2.538
_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    19.329
_exptl_absorpt_correction_T_max  0.353
_exptl_absorpt_correction_T_min  0.072
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.486
_refine_diff_density_min         -2.007
_refine_diff_density_rms         0.412
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1440
_refine_ls_number_reflns         29370
_refine_ls_number_restraints     392
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.2155
_refine_ls_R_factor_gt           0.1831
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2661P)^2^+530.3491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5043
_refine_ls_wR_factor_ref         0.5273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20540
_reflns_number_total             29370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_mbp_50_10_96c
_cod_database_code               1571884
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C14 H12 O)2 (C6 H12)4'
_chemical_oxdiff_usercomment     4-methylbenzophenone
_shelx_estimated_absorpt_t_max   0.307
_shelx_estimated_absorpt_t_min   0.066
_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
 C6A-C1A = C2A-C1A = C3A-C2A = C4A-C3A = C5A-C4A = C6A-C5A
 1.39 with sigma of 0.02
 C6B-C1B = C2B-C1B = C3B-C2B = C4B-C3B = C5B-C4B = C6B-C5B
 1.39 with sigma of 0.02
 C9B-C8B = C9B-C10B = C11B-C10B = C12B-C11B = C13B-C12B = C8B-C13B
 1.39 with sigma of 0.02
 C4B-C14B
 1.5 with sigma of 0.02
 C7B-C1B = C8B-C7B
 1.48 with sigma of 0.02
 O1A-C7A
 1.22 with sigma of 0.02
 C4A-C14A
 1.5 with sigma of 0.02
 C1B-C3B = C2B-C4B = C3B-C5B = C4B-C6B = C5B-C1B = C6B-C2B
 2.4 with sigma of 0.04
 C1A-C3A = C2A-C4A = C3A-C5A = C4A-C6A = C5A-C1A = C6A-C2A
 2.4 with sigma of 0.04
 C8B-C10B = C9B-C11B
 2.4 with sigma of 0.04
 C8A-C1A
 2.57 with sigma of 0.02
 C1A-O1A = C8A-O1A
 2.4 with sigma of 0.04
 C9A-C8A \\sim C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim C13A-C12A \\sim
C8A-C13A
 with sigma of 0.02
 C1B-C4B \\sim C2B-C5B \\sim C3B-C6B
 with sigma of 0.04
 C12A-C8A \\sim C8A-C10A \\sim C9A-C13A
 with sigma of 0.04
 C8A-C7A \\sim C7A-C1A
 with sigma of 0.02
 I412-Zn46 \\sim I312-Zn36
 with sigma of 0.02
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 I403-N305 \\sim I303-N305
 with sigma of 0.04
 Zn42-N305 \\sim Zn32-N305
 with sigma of 0.02
 I403-I404 \\sim I303-I304
 with sigma of 0.04
 I411-Zn46 \\sim I311-Zn36
 with sigma of 0.02
 Zn46-N324 \\sim Zn36-N324
 with sigma of 0.02
 Zn42-I404 \\sim Zn32-I304
 with sigma of 0.02
 I411-N324 \\sim I311-N324
 with sigma of 0.04
 I412-I411 \\sim I312-I311
 with sigma of 0.04
 I412-N324 \\sim I312-N324
 with sigma of 0.04
 I410-Zn45 \\sim I310-Zn35
 with sigma of 0.02
 I409-Zn45 \\sim I309-Zn35
 with sigma of 0.02
 Zn45-N318 \\sim Zn35-N318
 with sigma of 0.02
 Zn45-N319 \\sim Zn35-N319
 with sigma of 0.02
 I410-I409 \\sim I310-I309
 with sigma of 0.04
 I410-N318 \\sim I310-N318
 with sigma of 0.04
 I410-N319 \\sim I310-N319
 with sigma of 0.04
 I409-N318 \\sim I309-N318
 with sigma of 0.04
 I409-N319 \\sim I309-N319
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I306-Zn33 \\sim I406-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
 I305-I306 \\sim I405-I406
 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
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 I306-N307 \\sim I406-N307
 with sigma of 0.04
 I307-Zn34 \\sim I407-Zn44
 with sigma of 0.02
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 Zn34-N313 \\sim Zn44-N313
 with sigma of 0.02
 Zn34-N312 \\sim Zn44-N312
 with sigma of 0.02
 I307-I308 \\sim I407-I408
 with sigma of 0.04
 I307-N313 \\sim I407-N313
 with sigma of 0.04
 I307-N312 \\sim I407-N312
 with sigma of 0.04
 I308-N313 \\sim I408-N313
 with sigma of 0.04
 I308-N312 \\sim I408-N312
 with sigma of 0.04
 N305-I404 \\sim N305-I304
 with sigma of 0.04
 I12-Zn51 \\sim I302-Zn31
 with sigma of 0.02
 I11-Zn51 \\sim I301-Zn31
 with sigma of 0.02
3. Restrained planarity
 C6B, C2B, C3B, C5B, C1B, C4B
 with sigma of 0.1
 C13A, C9A, C10A, C12A, C8A, C11A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7B \\sim C6B \\sim C5B \\sim C1B \\sim C4B \\sim C2B \\sim C14B \\sim C3B
\\sim C8B \\sim O1B \\sim C13B \\sim C9B \\sim C12B \\sim C10B \\sim C11B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C7A \\sim C6A \\sim C5A \\sim C1A \\sim C4A \\sim C2A \\sim C14A \\sim C3A
\\sim O1A \\sim C8A \\sim C9A \\sim C13A \\sim C10A \\sim C12A \\sim C11A:
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 I305 \\sim I405: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C336 \\sim N312 \\sim C332 \\sim C333 \\sim C334 \\sim C335: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn42) = Uanis(Zn32)
Uanis(I404) = Uanis(I304)
Uanis(I303) = Uanis(I403)
5. Rigid body (RIGU) restrains
 I409, I309, Zn35, Zn45, I310, I410
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I410, I310, Zn35, Zn45, I309, I409
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I306, I406, Zn33, Zn43, I405, I305
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(I302)+Sof(Zn31)+Sof(I301)]+1*[Sof(I402)+Sof(Zn41)+Sof(I401)]+1*
 [Sof(I11)+Sof(I12)+Sof(Zn51)]=1 with esd of 0.00001
 Sof(I311)=Sof(Zn36)=Sof(I312)=1-FVAR(1)
 Sof(I412)=Sof(I411)=Sof(Zn46)=FVAR(1)
 Sof(I309)=Sof(Zn35)=Sof(I310)=1-FVAR(2)
 Sof(I410)=Sof(I409)=Sof(Zn45)=FVAR(2)
 Sof(I304)=Sof(Zn32)=Sof(I303)=1-FVAR(3)
 Sof(I403)=Sof(Zn42)=Sof(I404)=FVAR(3)
 Sof(I302)=Sof(Zn31)=Sof(I301)=FVAR(4)
 Sof(I402)=Sof(Zn41)=Sof(I401)=FVAR(5)
 Sof(I11)=Sof(I12)=Sof(Zn51)=FVAR(6)
 Fixed Sof: I305(0.58974) I307(0.61395) I306(0.58974) I308(0.61395)
 Zn33(0.58974) Zn34(0.61395) C6A(0.89017) H6A(0.89017) C6B(0.76488)
 H6B(0.76488) C5B(0.76488) H5B(0.76488) O1A(0.89017) C14B(0.76488)
 H14D(0.76488) H14E(0.76488) H14F(0.76488) C8A(0.89017) C4B(0.76488)
 C14A(0.89017) H14A(0.89017) H14B(0.89017) H14C(0.89017) C12B(0.76488)
 H12B(0.76488) C9A(0.89017) H9A(0.89017) C11A(0.89017) H11A(0.89017)
 O1B(0.76488) C13A(0.89017) H13A(0.89017) C12A(0.89017) H12A(0.89017)
 C7A(0.89017) C2A(0.89017) H2A(0.89017) C9B(0.76488) H9B(0.76488) C8B(0.76488)
 C4A(0.89017) C13B(0.76488) H13B(0.76488) C3A(0.89017) H3A(0.89017)
 C11B(0.76488) H11B(0.76488) C2B(0.76488) H2B(0.76488) C5A(0.89017)
 H5A(0.89017) C1A(0.89017) C3B(0.76488) H3B(0.76488) C10B(0.76488)
 H10B(0.76488) C1B(0.76488) C7B(0.76488) C10A(0.89017) H10A(0.89017)
 I406(0.41026) Zn43(0.41026) I405(0.41026) I407(0.38605) Zn44(0.38605)
 I408(0.38605)
 Fixed Uiso: I402(0.08) Zn41(0.08) I401(0.08) I11(0.08) I12(0.08) Zn51(0.08)
7.a Aromatic/amide H refined with riding coordinates:
 C305(H305), C301(H301), C332(H332), C313(H313), C318(H318), C320(H320),
 C322(H322), C312(H312), C304(H304), C366(H366), C336(H336), C311(H311),
 C315(H315), C369(H369), C340(H340), C319(H319), C367(H367), C338(H338),
 C310(H310), C6A(H6A), C302(H302), C314(H314), C337(H337), C354(H354),
 C341(H341), C350(H350), C333(H333), C356(H356), C347(H347), C353(H353),
 C351(H351), C372(H372), C6B(H6B), C368(H368), C323(H323), C355(H355),
 C330(H330), C365(H365), C317(H317), C329(H329), C5B(H5B), C364(H364),
 C331(H331), C328(H328), C371(H371), C12B(H12B), C9A(H9A), C11A(H11A),
 C13A(H13A), C12A(H12A), C346(H346), C2A(H2A), C9B(H9B), C359(H359), C349(H349),
  C335(H335), C13B(H13B), C3A(H3A), C11B(H11B), C2B(H2B), C5A(H5A), C3B(H3B),
 C10B(H10B), C348(H348), C358(H358), C10A(H10A)
7.b Idealised Me refined as rotating group:
 C14B(H14D,H14E,H14F), C14A(H14A,H14B,H14C)
;
_shelx_res_checksum              5764
_shelx_hkl_checksum              46800
_olex2_date_sample_data_collection 2024-03-19
_olex2_date_sample_submission    2024-03-19
_olex2_submission_original_sample_id '4-Methylbenzophenone 50_10_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 3.203
_oxdiff_exptl_absorpt_empirical_full_min 0.379