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_1571833
_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             2024-02-07
_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                 100.460(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.3369(12)
_cell_length_b                   15.0656(4)
_cell_length_c                   29.8140(12)
_cell_measurement_reflns_used    12682
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.2540
_cell_measurement_theta_min      2.6620
_cell_volume                     15166.7(9)
_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 0.995
_diffrn_measured_fraction_theta_max 0.993
_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     22.00  47.00   0.50    2.10    --   83.27 -62.00 -35.00   50
  2  \w    102.00 138.00   0.50    2.10    --   83.27  62.00 102.00   72
  3  \w    106.00 149.00   0.50    2.10    --   83.27  57.00-120.00   86
  4  \w     45.00  91.00   0.50    2.10    --   83.27 -77.00-150.00   92
  5  \w     12.00  44.00   0.50    2.10    --   83.27 -37.00 150.00   64
  6  \w     16.00  68.00   0.50    2.10    --   83.27 -57.00 -60.00  104
  7  \w     12.00  43.00   0.50    2.10    --   83.27 -37.00-180.00   62
  8  \w     13.00  38.00   0.50    2.10    --   83.27 -37.00 -30.00   50
  9  \w     95.00 145.00   0.50    2.10    --   83.27  77.00 -30.00  100
 10  \w     30.00  65.00   0.50    2.10    --   83.27 -77.00-180.00   70
 11  \w     70.00  96.00   0.50    2.10    --   83.27 -77.00  90.00   52
 12  \w     17.00  43.00   0.50    2.10    --   83.27 -37.00   0.00   52
 13  \w     22.00  63.00   0.50    2.10    --   83.27 -77.00  90.00   82
 14  \w     31.00  57.00   0.50    2.10    --   83.27 -77.00 -90.00   52
 15  \w     69.00  95.00   0.50    2.10    --   83.27 -77.00 -90.00   52
 16  \w     31.00  57.00   0.50    2.10    --   83.27-125.00  60.00   52
 17  \w     87.00 142.00   0.50    2.10    --   83.27 125.00 -90.00  110
 18  \w     84.00 109.00   0.50    2.10    --   83.27 125.00-120.00   50
 19  \w     16.00  63.00   0.50    2.10    --   83.27 -57.00 -90.00   94
 20  \w     66.00  94.00   0.50    2.10    --   83.27 -77.00-120.00   56
 21  \w    -71.00 -13.00   0.50    2.10    --  -79.30  62.00 102.00  116
 22  \w   -146.00 -82.00   0.50    2.10    --  -79.30 -62.00 -35.00  128
 23  \w    -40.00 -15.00   0.50    2.10    --  -79.30  37.00-120.00   50
 24  \w    -39.00  -8.00   0.50    2.10    --  -79.30  37.00 -60.00   62
 25  \w    -39.00  -8.00   0.50    2.10    --  -79.30  37.00 -90.00   62
 26  \w   -122.00 -44.00   0.50    0.70    --  -55.02 -62.00 -35.00  156
 27  \w    -50.00 -17.00   0.50    0.70    --  -55.02 125.00-150.00   66
 28  \w    -24.00  14.00   0.50    0.70    --  -55.02  19.00  60.00   76
 29  \w    -99.00 -59.00   0.50    0.70    --  -55.02 125.00-150.00   80
 30  \w     41.00 118.00   0.50    0.70    --   51.52  62.00 102.00  154
 31  \w    -15.00  62.00   0.50    0.70    --   51.52 -62.00 -35.00  154
;
_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      -0.0276596000
_diffrn_orient_matrix_UB_12      -0.0157691000
_diffrn_orient_matrix_UB_13      -0.0461276000
_diffrn_orient_matrix_UB_21      -0.0185155000
_diffrn_orient_matrix_UB_22      0.0924076000
_diffrn_orient_matrix_UB_23      0.0032103000
_diffrn_orient_matrix_UB_31      0.0312214000
_diffrn_orient_matrix_UB_32      0.0407671000
_diffrn_orient_matrix_UB_33      -0.0249622000
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            70635
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.252
_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    20.487
_exptl_absorpt_correction_T_max  0.312
_exptl_absorpt_correction_T_min  0.058
_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    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         13796
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0653
_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^)+(0.1328P)^2^+19.9313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2153
_refine_ls_wR_factor_ref         0.2282
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9615
_reflns_number_total             13796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_10_24c
_cod_database_code               1571833
_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   0.260
_shelx_estimated_absorpt_t_min   0.105
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 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
 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-N312 \\sim Zn33-N312
 with sigma of 0.02
 I405-I406 \\sim I305-I306
 with sigma of 0.04
 I405-N312 \\sim I305-N312
 with sigma of 0.04
 I406-N312 \\sim I306-N312
 with sigma of 0.04
3. Others
 Fixed Sof: I405(0.44604) I406(0.44604) I303(0.48436) I402(0.4781)
 Zn43(0.44604) I401(0.4781) I304(0.48436) Zn32(0.48436) Zn41(0.4781)
 I403(0.46778) Zn42(0.46778) I404(0.46778) I301(0.49339) Zn31(0.49339)
 I302(0.49339) I305(0.51584) Zn33(0.51584) I306(0.51584) I503(0.04785)
 I504(0.04785) Zn52(0.04785) I501(0.02851) I502(0.02851) Zn51(0.02851)
 I505(0.03812) I506(0.03812) Zn53(0.03812)
 Fixed Uiso: I503(0.08) I504(0.08) Zn52(0.08) I501(0.08) I502(0.08) Zn51(0.08)
 I505(0.08) I506(0.08) Zn53(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C313(H313), C314(H314), C334(H334), C333(H333), C311(H311), C318(H318),
 C321(H321), C310(H310), C319(H319), C323(H323), C320(H320), C304(H304),
 C302(H302), C329(H329), C324(H324), C330(H330), C336(H336), C337(H337),
 C305(H305), C316(H316), C301(H301), C332(H332), C331(H331), C315(H315)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87873
_shelx_hkl_checksum              4256
_shelx_fab_checksum              67475
_olex2_date_sample_data_collection 2024-02-06
_olex2_date_sample_submission    2024-02-06
_olex2_submission_original_sample_id 4_10_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 3.148
_oxdiff_exptl_absorpt_empirical_full_min 0.434