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_1571879
_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         'C36 H24 I6 N12 Zn3'
_chemical_formula_sum            'C36 H24 I6 N12 Zn3'
_chemical_formula_weight         1582.18
_chemical_name_systematic
catena-[bis(mu-2,4,6-tri(pyridin-4-yl)-1,3,5-triazine)-hexaiodo-tri-zinc
_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             2024-03-26
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.2833(5)
_cell_length_b                   14.9084(2)
_cell_length_c                   31.7352(4)
_cell_measurement_reflns_used    14130
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      68.8620
_cell_measurement_theta_min      2.8470
_cell_volume                     16283.5(4)
_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      100.0(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.992
_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     20.00  46.00   0.50    0.80    --   83.39 -48.00   1.00   52
  2  \w     98.00 132.00   0.50    0.80    --   83.39  48.00 149.00   68
  3  \w     15.00  41.00   0.50    0.80    --   83.39 -37.00-180.00   52
  4  \w     32.00  66.00   0.50    0.80    --   83.39 -57.00-150.00   68
  5  \w     13.00  42.00   0.50    0.80    --   83.39 -37.00 -90.00   58
  6  \w     24.00  50.00   0.50    0.80    --   83.39 -57.00 -30.00   52
  7  \w     15.00  42.00   0.50    0.80    --   83.39 -37.00 150.00   54
  8  \w     12.00  37.00   0.50    0.80    --   83.39 -37.00-120.00   50
  9  \w     26.00 100.00   0.50    0.80    --   83.39 -99.00  30.00  148
 10  \w     15.00  40.00   0.50    0.80    --   83.39 -37.00  30.00   50
 11  \w    113.00 139.00   0.50    0.80    --   83.39  57.00 -30.00   52
 12  \w     80.00 108.00   0.50    0.80    --   83.39  57.00 -30.00   56
 13  \w     75.00 148.00   0.50    0.80    --   83.39  57.00  90.00  146
 14  \w     25.00  51.00   0.50    0.80    --   83.39 -99.00 -60.00   52
 15  \w     65.00 106.00   0.50    0.80    --   83.39 -99.00 -60.00   82
 16  \w     75.00 100.00   0.50    0.80    --   83.39  57.00  60.00   50
 17  \w    126.00 151.00   0.50    0.80    --   83.39  57.00  60.00   50
 18  \w     31.00  64.00   0.50    0.80    --   83.39 -57.00  90.00   66
 19  \w     17.00  68.00   0.50    0.80    --   83.39 -57.00-120.00  102
 20  \w     40.00  65.00   0.50    0.80    --   83.39 -57.00-180.00   50
 21  \w   -134.00-109.00   0.50    0.80    --  -79.34 -48.00   1.00   50
 22  \w    -48.00 -16.00   0.50    0.80    --  -79.34  48.00 149.00   64
 23  \w   -139.00 -95.00   0.50    0.80    --  -79.34 -99.00 120.00   88
 24  \w    -62.00 -15.00   0.50    0.80    --  -79.34  57.00-120.00   94
 25  \w    -36.00 -11.00   0.50    0.80    --  -79.34  37.00 120.00   50
 26  \w    -43.00 -18.00   0.50    0.40    --  -55.07  48.00 149.00   50
 27  \w    -24.00  15.00   0.50    0.40    --  -55.07  19.00-180.00   78
 28  \w   -124.00 -84.00   0.50    0.40    --  -55.07 -48.00   1.00   80
 29  \w    -17.00  17.00   0.50    0.40    --   52.07 -48.00   1.00   68
 30  \w     82.00 108.00   0.50    0.40    --   52.07  48.00 149.00   52
 31  \w     20.00  53.00   0.50    0.40    --   52.07 -48.00   1.00   66
 32  \w     -7.00  19.00   0.50    0.40    --   52.07 -19.00-180.00   52
 33  \w     -4.00  43.00   0.50    0.40    --   52.07 -37.00 120.00   94
;
_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      -0.0252621000
_diffrn_orient_matrix_UB_12      -0.0148595000
_diffrn_orient_matrix_UB_13      0.0332917000
_diffrn_orient_matrix_UB_21      0.0321118000
_diffrn_orient_matrix_UB_22      -0.0591515000
_diffrn_orient_matrix_UB_23      0.0271384000
_diffrn_orient_matrix_UB_31      0.0182542000
_diffrn_orient_matrix_UB_32      0.0833892000
_diffrn_orient_matrix_UB_33      0.0251764000
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            71698
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         2.568
_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    19.082
_exptl_absorpt_correction_T_max  0.379
_exptl_absorpt_correction_T_min  0.063
_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    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         14786
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0472P)^2^+20.8502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13046
_reflns_number_total             14786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_mbp_4_10_96a
_cod_database_code               1571879
_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   0.348
_shelx_estimated_absorpt_t_min   0.054
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I306-Zn33 \\sim I406-Zn43
 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
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I404-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 Zn42-N306 \\sim Zn32-N306
 with sigma of 0.02
 Zn42-N307 \\sim Zn32-N307
 with sigma of 0.02
 I404-I403 \\sim I304-I303
 with sigma of 0.04
 I404-N306 \\sim I304-N306
 with sigma of 0.04
 I404-N307 \\sim I304-N307
 with sigma of 0.04
 I403-N306 \\sim I303-N306
 with sigma of 0.04
 I403-N307 \\sim I303-N307
 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
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I302-I301 \\sim I402-I401
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I501-Zn51 \\sim I401-Zn41
 with sigma of 0.02
 I402-Zn41 \\sim I502-Zn51
 with sigma of 0.02
 Zn51-N301 \\sim Zn41-N301
 with sigma of 0.02
3. Others
 Sof(I405)=Sof(Zn43)=Sof(I406)=1-FVAR(1)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(1)
 Sof(I303)=Sof(Zn32)=Sof(I304)=1-FVAR(2)
 Sof(I404)=Sof(I403)=Sof(Zn42)=FVAR(2)
 Fixed Sof: I302(0.69418) I301(0.69418) Zn31(0.69418) I401(0.27264)
 Zn41(0.27264) I402(0.27264) I501(0.03321) I502(0.03321) Zn51(0.03321)
 Fixed Uiso: I501(0.08) I502(0.08) Zn51(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C302(H302), C301(H301), C331(H331), C314(H314), C311(H311), C330(H330),
 C315(H315), C310(H310), C335(H335), C320(H320), C336(H336), C313(H313),
 C319(H319), C317(H317), C318(H318), C312(H312), C322(H322), C329(H329),
 C304(H304), C323(H323), C328(H328), C305(H305), C333(H333), C332(H332)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78051
_shelx_hkl_checksum              71945
_shelx_fab_checksum              23391
_olex2_date_sample_data_collection 2024-03-25
_olex2_date_sample_submission    2024-03-25
_olex2_submission_original_sample_id '4-Methylbenzophenone 4_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 2.770
_oxdiff_exptl_absorpt_empirical_full_min 0.434