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_1571839
_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 I6.006 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)-hexachloro-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             2024-01-25
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.634(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.3531(8)
_cell_length_b                   15.0637(4)
_cell_length_c                   29.9781(11)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      70.9980
_cell_measurement_theta_min      2.6460
_cell_volume                     15246.8(8)
_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 0.992
_diffrn_measured_fraction_theta_max 0.991
_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   -115.00 -88.00   0.50    2.50    -- -103.00-142.00-119.00   54
  2  \w   -101.00 -76.00   0.50    2.50    -- -103.00 142.00 -63.00   50
  3  \w   -127.00-102.00   0.50    2.50    -- -103.00-127.00  51.00   50
  4  \w    -73.00 -48.00   0.50    2.50    -- -103.00 127.00 126.00   50
  5  \w    -82.00 -31.00   0.50    2.50    -- -103.00  77.00 -30.00  102
  6  \w    -55.00 -30.00   0.50    2.50    -- -103.00  61.00-150.00   50
  7  \w   -112.00 -33.00   0.50    2.50    -- -103.00 125.00  60.00  158
  8  \w     72.00 108.00   0.50    2.50    --  101.75-127.00  51.00   72
  9  \w     74.00 123.00   0.50    2.50    --  101.75-142.00-119.00   98
 10  \w     97.00 122.00   0.50    2.50    --  101.75 142.00 -63.00   50
 11  \w    116.00 142.00   0.50    2.50    --  101.75 127.00 126.00   52
 12  \w     33.00 108.00   0.50    2.50    --  101.75-110.00  10.61  150
 13  \w     79.00 146.00   0.50    2.50    --  101.75  77.00-150.00  134
 14  \w     86.00 135.00   0.50    2.50    --  101.75  61.00   0.00   98
 15  \w     90.00 175.00   0.50    2.50    --  101.75  30.00 -60.00  170
 16  \w    140.00 166.00   0.50    2.50    --  101.75  61.00   0.00   52
 17  \w     45.00 109.00   0.50    2.50    --  101.75-125.00 120.00  128
 18  \w     49.00  80.00   0.50    2.50    --  101.75 -94.00-120.00   62
 19  \w   -117.00 -64.00   0.50    0.50    --  -46.26-142.00-119.00  106
 20  \w     74.00 117.00   0.50    0.50    --   46.26 142.00 -63.00   86
 21  \w     43.00  94.00   0.50    0.50    --   46.26-127.00  51.00  102
 22  \w     62.00  90.00   0.50    0.50    --   46.26-142.00-119.00   56
 23  \w    -18.00   9.00   0.50    0.50    --  -46.26  19.00 -60.00   54
 24  \w    -22.00   8.00   0.50    0.50    --  -46.26  19.00-150.00   60
 25  \w     25.00 115.00   0.50    0.50    --   46.26  77.00 120.00  180
;
_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      0.0187290000
_diffrn_orient_matrix_UB_12      0.0028094000
_diffrn_orient_matrix_UB_13      -0.0428140000
_diffrn_orient_matrix_UB_21      0.0017331000
_diffrn_orient_matrix_UB_22      0.1020986000
_diffrn_orient_matrix_UB_23      0.0027569000
_diffrn_orient_matrix_UB_31      0.0415897000
_diffrn_orient_matrix_UB_32      -0.0054930000
_diffrn_orient_matrix_UB_33      0.0297931000
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            50575
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         2.617
_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    20.379
_exptl_absorpt_correction_T_max  0.299
_exptl_absorpt_correction_T_min  0.057
_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    1.379
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         13839
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1460P)^2^+12.5369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2214
_refine_ls_wR_factor_ref         0.2322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10225
_reflns_number_total             13839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_1_24c
_cod_database_code               1571839
_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   0.235
_shelx_estimated_absorpt_t_min   0.067
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I402-Zn41 \\sim I302-Zn31
 with sigma of 0.02
 I401-Zn41 \\sim I301-Zn31
 with sigma of 0.02
 Zn41-N301 \\sim Zn31-N301
 with sigma of 0.02
 I402-I401 \\sim I302-I301
 with sigma of 0.04
 I402-N301 \\sim I302-N301
 with sigma of 0.04
 I401-N301 \\sim I301-N301
 with sigma of 0.04
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 Zn43-N307 \\sim Zn33-N307
 with sigma of 0.02
 Zn43-N306 \\sim Zn33-N306
 with sigma of 0.02
 I405-I406 \\sim I305-I306
 with sigma of 0.04
 I405-N307 \\sim I305-N307
 with sigma of 0.04
 I405-N306 \\sim I305-N306
 with sigma of 0.04
 I406-N307 \\sim I306-N307
 with sigma of 0.04
 I406-N306 \\sim I306-N306
 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-N305 \\sim Zn42-N305
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I303-N305 \\sim I403-N305
 with sigma of 0.04
 I304-N305 \\sim I404-N305
 with sigma of 0.04
3. Others
 Sof(I404)=Sof(Zn42)=Sof(I403)=1-FVAR(1)
 Sof(I303)=Sof(I304)=Sof(Zn32)=FVAR(1)
 Fixed Sof: I402(0.19971) I405(0.4545) I406(0.4545) I401(0.19971)
 Zn41(0.19971) Zn43(0.4545) I302(0.72558) Zn31(0.72558) I301(0.72558)
 I306(0.51828) Zn33(0.51828) I305(0.51828) I502(0.07471) I501(0.0804)
 Zn51(0.07471) I506(0.02723) I505(0.02723) Zn53(0.02723)
 Fixed Uiso: I502(0.08) I501(0.08) Zn51(0.08) I506(0.08) I505(0.08) Zn53(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C310(H310), C311(H311), C336(H336), C302(H302), C328(H328), C335(H335),
 C313(H313), C312(H312), C301(H301), C331(H331), C320(H320), C315(H315),
 C329(H329), C330(H330), C319(H319), C333(H333), C305(H305), C304(H304),
 C332(H332), C317(H317), C322(H322), C318(H318), C314(H314), C323(H323)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              79785
_shelx_hkl_checksum              11154
_shelx_fab_checksum              5716
_olex2_date_sample_data_collection 2023-03-30
_olex2_date_sample_submission    2023-03-30
_olex2_submission_original_sample_id 50_1_24c
_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 6.508
_oxdiff_exptl_absorpt_empirical_full_min 0.411