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_1571823
_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                 99.542(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.1537(11)
_cell_length_b                   15.1026(3)
_cell_length_c                   29.0899(12)
_cell_measurement_reflns_used    6545
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.2530
_cell_measurement_theta_min      3.0540
_cell_volume                     14797.2(8)
_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 0.993
_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    -65.00 -31.00   0.50    4.00    -- -103.00  61.00   0.00   68
  2  \w    -63.00 -31.00   0.50    4.00    -- -103.00  61.00-150.00   64
  3  \w   -112.00 -33.00   0.50    4.00    -- -103.00 125.00  30.00  158
  4  \w    -62.00 -33.00   0.50    4.00    -- -103.00  61.00 120.00   58
  5  \w    -64.00 -34.00   0.50    4.00    -- -103.00 125.00  90.00   60
  6  \w    -63.00 -30.00   0.50    4.00    -- -103.00  61.00  60.00   66
  7  \w    -64.00 -30.00   0.50    4.00    -- -103.00  61.00-180.00   68
  8  \w    -64.00 -30.00   0.50    4.00    -- -103.00  61.00-120.00   68
  9  \w    -58.00 -33.00   0.50    4.00    -- -103.00  61.00  90.00   50
 10  \w    -63.00 -30.00   0.50    4.00    -- -103.00  61.00 150.00   66
 11  \w    101.00 174.00   0.50    4.00    --  101.75  33.00  -8.00  146
 12  \w     30.00  68.00   0.50    4.00    --  101.75 -61.00-180.00   76
 13  \w     30.00  71.00   0.50    4.00    --  101.75 -61.00-120.00   82
 14  \w     32.00  71.00   0.50    4.00    --  101.75 -61.00-150.00   78
 15  \w     31.00  66.00   0.50    4.00    --  101.75 -61.00 -60.00   70
 16  \w     57.00 105.00   0.50    4.00    --  101.75 -94.00 -90.00   96
 17  \w     42.00  72.00   0.50    4.00    --  101.75 -61.00   0.00   60
 18  \w     35.00  65.00   0.50    4.00    --  101.75 -61.00 -90.00   60
 19  \w    -78.00 -33.00   0.50    1.00    --  -46.61 -33.00-166.00   90
 20  \w    -36.00   1.00   0.50    1.00    --  -46.61  33.00  -8.00   74
 21  \w     38.00 120.00   0.50    1.00    --   46.61  33.00  -8.00  164
 22  \w    -18.00   7.00   0.50    1.00    --   46.61 -33.00-166.00   50
 23  \w    -23.00  12.00   0.50    1.00    --  -46.61  19.00 -90.00   70
 24  \w    -23.00  29.00   0.50    1.00    --  -46.61  19.00 120.00  104
 25  \w    -24.00  26.00   0.50    1.00    --  -46.61  19.00-180.00  100
;
_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      -0.0186669000
_diffrn_orient_matrix_UB_12      0.0020235000
_diffrn_orient_matrix_UB_13      -0.0519914000
_diffrn_orient_matrix_UB_21      0.0375780000
_diffrn_orient_matrix_UB_22      -0.0437552000
_diffrn_orient_matrix_UB_23      -0.0126056000
_diffrn_orient_matrix_UB_31      -0.0182174000
_diffrn_orient_matrix_UB_32      -0.0920789000
_diffrn_orient_matrix_UB_33      0.0048824000
_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  0.0504
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47702
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.624
_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    20.998
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.216
_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    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         13452
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0567
_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^)+(0.1040P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7748
_reflns_number_total             13452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_1_48b
_cod_database_code               1571823
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3) (C6 H12)4'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.572
_shelx_estimated_absorpt_t_min   0.171
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 I404-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 Zn42-N305 \\sim Zn32-N305
 with sigma of 0.02
 I404-N305 \\sim I304-N305
 with sigma of 0.04
 I403-I404 \\sim I303-I304
 with sigma of 0.04
 I403-N305 \\sim I303-N305
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I301-I302 \\sim I401-I402
 with sigma of 0.04
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N307 \\sim I406-N307
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I305-N307 \\sim I405-N307
 with sigma of 0.04
 Zn33-N306 \\sim Zn43-N306
 with sigma of 0.02
 Zn33-N307 \\sim Zn43-N307
 with sigma of 0.02
 I502-Zn51 \\sim I501-Zn51
 with sigma of 0.02
3. Others
 Sof(I303)=Sof(Zn32)=Sof(I304)=1-FVAR(1)
 Sof(I403)=Sof(I404)=Sof(Zn42)=FVAR(1)
 Sof(I405)=Sof(Zn43)=Sof(I406)=1-FVAR(2)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(2)
 Fixed Sof: I301(0.54627) I302(0.54627) Zn31(0.54627) I401(0.41411)
 Zn41(0.41411) I402(0.41411) I501(0.03961) Zn51(0.03961) I502(0.03961)
 Fixed Uiso: I501(0.08) Zn51(0.08) I502(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C335(H335), C336(H336), C331(H331), C332(H332), C311(H311), C333(H333),
 C330(H330), C329(H329), C314(H314), C305(H305), C315(H315), C310(H310),
 C304(H304), C320(H320), C313(H313), C319(H319), C301(H301), C322(H322),
 C302(H302), C318(H318), C323(H323), C312(H312), C328(H328), C317(H317)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68201
_shelx_hkl_checksum              68425
_shelx_fab_checksum              64326
_olex2_date_sample_data_collection 2022-08-10
_olex2_date_sample_submission    2022-08-10
_olex2_submission_original_sample_id 4_1_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 4.066
_oxdiff_exptl_absorpt_empirical_full_min 0.496