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_1571829
_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             2024-02-01
_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                 100.538(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.3094(9)
_cell_length_b                   15.0823(3)
_cell_length_c                   29.8583(10)
_cell_measurement_reflns_used    5596
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.0030
_cell_measurement_theta_min      2.5990
_cell_volume                     15190.0(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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   -116.00 -45.00   0.50    4.00    -- -103.00  84.00 154.00  142
  2  \w   -166.00-112.00   0.50    4.00    -- -103.00 -84.00  34.00  108
  3  \w    -84.00 -50.00   0.50    4.00    -- -103.00  77.00 -90.00   68
  4  \w   -172.00 -85.00   0.50    4.00    -- -103.00 -94.00 120.00  174
  5  \w    -66.00 -39.00   0.50    4.00    -- -103.00  61.00 -60.00   54
  6  \w    -66.00 -33.00   0.50    4.00    -- -103.00  61.00 150.00   66
  7  \w    -61.00 -32.00   0.50    4.00    -- -103.00  61.00   0.00   58
  8  \w     53.00  79.00   0.50    4.00    --  101.75 -84.00  34.00   52
  9  \w    120.00 175.00   0.50    4.00    --  101.75  84.00 154.00  110
 10  \w     33.00  72.00   0.50    4.00    --  101.75 -61.00  60.00   78
 11  \w     88.00 173.00   0.50    4.00    --  101.75  15.00 120.00  170
 12  \w     30.00  73.00   0.50    4.00    --  101.75 -61.00  30.00   86
 13  \w     37.00  63.00   0.50    4.00    --  101.75 -61.00-180.00   52
 14  \w     39.00  73.00   0.50    4.00    --  101.75 -61.00 -60.00   68
 15  \w     90.00 151.00   0.50    4.00    --  101.75  45.00-150.00  122
 16  \w    -69.00  22.00   0.50    1.00    --  -46.61  84.00 154.00  182
 17  \w    -13.00  48.00   0.50    1.00    --   46.61 -84.00  34.00  122
 18  \w    -40.00   5.00   0.50    1.00    --  -46.61  37.00 -90.00   90
 19  \w   -117.00 -32.00   0.50    1.00    --  -46.61 -57.00 -30.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details
'Rigaku Oxford Difffraction, UG2 \k goniometer'
_diffrn_measurement_device_type
; Rigaku 007HF equipped with Varimax confocal mirrors and a UG2 goniometer
 and HyPix 6000HE 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      0.0181516000
_diffrn_orient_matrix_UB_12      -0.0075318000
_diffrn_orient_matrix_UB_13      -0.0433671000
_diffrn_orient_matrix_UB_21      0.0212503000
_diffrn_orient_matrix_UB_22      0.0894348000
_diffrn_orient_matrix_UB_23      0.0112583000
_diffrn_orient_matrix_UB_31      0.0361234000
_diffrn_orient_matrix_UB_32      -0.0487748000
_diffrn_orient_matrix_UB_33      0.0273304000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            47451
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         2.620
_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    20.455
_exptl_absorpt_correction_T_max  0.491
_exptl_absorpt_correction_T_min  0.211
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         13821
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0851P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8597
_reflns_number_total             13821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_5_48b
_cod_database_code               1571829
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.428
_shelx_estimated_absorpt_t_min   0.212
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I301-Zn41 \\sim I401-Zn
 with sigma of 0.02
 I302-Zn41 \\sim I402-Zn
 with sigma of 0.02
 Zn41-N301 \\sim Zn-N301
 with sigma of 0.02
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I301-I302 \\sim I401-I402
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 Zn33-N312 \\sim Zn43-N312
 with sigma of 0.02
 I404-N306 \\sim I304-N306
 with sigma of 0.04
 I403-N306 \\sim I303-N306
 with sigma of 0.04
 I404-I403 \\sim I304-I303
 with sigma of 0.04
 I404-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 I404-N307 \\sim I304-N307
 with sigma of 0.04
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 I403-N307 \\sim I303-N307
 with sigma of 0.04
 Zn42-N306 \\sim Zn32-N306
 with sigma of 0.02
 Zn42-N307 \\sim Zn32-N307
 with sigma of 0.02
3. Others
 Sof(I405)=Sof(Zn43)=Sof(I406)=1-FVAR(1)
 Sof(I305)=Sof(I306)=Sof(Zn33)=FVAR(1)
 Fixed Sof: I301(0.53921) I404(0.43936) I302(0.53921) I403(0.43936)
 Zn41(0.53921) Zn42(0.43936) I401(0.40142) Zn(0.40142) I402(0.40142)
 I304(0.51537) Zn32(0.51537) I303(0.51537) I501(0.05936) I502(0.05936)
 Zn51(0.05936) I503(0.04529) I504(0.04529) Zn52(0.04529)
 Fixed Uiso: I501(0.08) I502(0.08) Zn51(0.08) I503(0.08) I504(0.08) Zn52(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C335(H335), C336(H336), C310(H310), C331(H331), C311(H311), C333(H333),
 C332(H332), C304(H304), C330(H330), C302(H302), C305(H305), C315(H315),
 C313(H313), C329(H329), C301(H301), C312(H312), C322(H322), C314(H314),
 C328(H328), C320(H320), C319(H319), C318(H318), C323(H323), C317(H317)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92250
_shelx_hkl_checksum              868
_shelx_fab_checksum              8008
_olex2_date_sample_data_collection 2022-08-10
_olex2_date_sample_submission    2022-08-10
_olex2_submission_original_sample_id 4_5_48b
_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 3.159
_oxdiff_exptl_absorpt_empirical_full_min 0.314