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_1571875
_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, 0.25[]'
_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             2024-01-30
_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                 101.107(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.3804(16)
_cell_length_b                   15.0439(5)
_cell_length_c                   30.3200(17)
_cell_measurement_reflns_used    6745
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.3730
_cell_measurement_theta_min      2.9220
_cell_volume                     15388.2(13)
_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  (Sheldrick, 2015)'
_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 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   -172.00-104.00   0.50    4.00    -- -103.00-120.00  40.00  136
  2  \w   -103.00 -77.00   0.50    4.00    -- -103.00 120.00 124.00   52
  3  \w   -132.00 -32.00   0.50    4.00    -- -103.00 154.00 -78.00  200
  4  \w    -88.00 -30.00   0.50    4.00    -- -103.00  77.00 -30.00  116
  5  \w   -113.00 -81.00   0.50    4.00    -- -103.00-125.00  90.00   64
  6  \w    -68.00 -43.00   0.50    4.00    -- -103.00  61.00 120.00   50
  7  \w   -172.00-136.00   0.50    4.00    -- -103.00-125.00  90.00   72
  8  \w    -69.00 -44.00   0.50    4.00    -- -103.00  61.00  90.00   50
  9  \w   -174.00-119.00   0.50    4.00    -- -103.00 -30.00 -60.00  110
 10  \w    -67.00 -32.00   0.50    4.00    -- -103.00  61.00 -60.00   70
 11  \w     47.00  72.00   0.50    4.00    --  101.75-120.00  40.00   50
 12  \w     60.00  85.00   0.50    4.00    --  101.75-154.00-117.00   50
 13  \w     88.00 113.00   0.50    4.00    --  101.75 154.00 -78.00   50
 14  \w     73.00 106.00   0.50    4.00    --  101.75 -94.00  60.00   66
 15  \w     37.00 107.00   0.50    4.00    --  101.75 -77.00  30.00  140
 16  \w     29.00  73.00   0.50    4.00    --  101.75 -61.00-180.00   88
 17  \w     90.00 173.00   0.50    4.00    --  101.75  45.00 120.00  166
 18  \w   -102.00 -76.00   0.50    1.00    --  -46.01-154.00-117.00   52
 19  \w     48.00  78.00   0.50    1.00    --   46.01-120.00  40.00   60
 20  \w     63.00 100.00   0.50    1.00    --   46.01 154.00 -78.00   74
 21  \w     50.00  75.00   0.50    1.00    --   46.01-154.00-117.00   50
 22  \w    -24.00  29.00   0.50    1.00    --  -46.01  19.00 120.00  106
 23  \w   -119.00 -34.00   0.50    1.00    --  -46.01 -37.00 120.00  170
 24  \w    -18.00  23.00   0.50    1.00    --  -46.01  19.00  30.00   82
 25  \w    -27.00  26.00   0.50    1.00    --   46.01 -19.00 -90.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details
'Rigaku Oxford Difffraction, 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      -0.0280977000
_diffrn_orient_matrix_UB_12      0.0136417000
_diffrn_orient_matrix_UB_13      0.0333744000
_diffrn_orient_matrix_UB_21      -0.0006248000
_diffrn_orient_matrix_UB_22      0.1007148000
_diffrn_orient_matrix_UB_23      -0.0093084000
_diffrn_orient_matrix_UB_31      -0.0360289000
_diffrn_orient_matrix_UB_32      -0.0123944000
_diffrn_orient_matrix_UB_33      -0.0384312000
_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  0.0607
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            51653
_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         68.248
_diffrn_reflns_theta_min         2.971
_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    20.192
_exptl_absorpt_correction_T_max  0.293
_exptl_absorpt_correction_T_min  0.037
_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    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.901
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         13991
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.1191
_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^)+(0.3064P)^2^+1.2800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3901
_refine_ls_wR_factor_ref         0.4189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9120
_reflns_number_total             13991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_10_48c
_cod_database_code               1571875
_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   0.237
_shelx_estimated_absorpt_t_min   0.077
_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
 I403-I404 \\sim I303-I304
 with sigma of 0.04
 I403-N305 \\sim I303-N305
 with sigma of 0.04
 I404-N305 \\sim I304-N305
 with sigma of 0.04
 I401-Zn41 \\sim I301-Zn31
 with sigma of 0.02
 I402-Zn41 \\sim I302-Zn31
 with sigma of 0.02
 Zn41-N301 \\sim Zn31-N301
 with sigma of 0.02
 I401-I402 \\sim I301-I302
 with sigma of 0.04
 I401-N301 \\sim I301-N301
 with sigma of 0.04
 I402-N301 \\sim I302-N301
 with sigma of 0.04
 I502-Zn51 \\sim I501-Zn51
 with sigma of 0.02
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I306-I506 \\sim I406-I506
 with sigma of 0.02
 Zn33-N306 \\sim Zn43-N306
 with sigma of 0.02
 Zn33-N307 \\sim Zn43-N307
 with sigma of 0.02
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I305-N307 \\sim I405-N307
 with sigma of 0.04
 I305-I505 \\sim I405-I505
 with sigma of 0.04
 I305-Zn53 \\sim I405-Zn53
 with sigma of 0.04
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 I306-N307 \\sim I406-N307
 with sigma of 0.04
 I306-I505 \\sim I406-I505
 with sigma of 0.04
 I306-Zn53 \\sim I406-Zn53
 with sigma of 0.04
 Zn33-I505 \\sim Zn43-I505
 with sigma of 0.04
 Zn33-I506 \\sim Zn43-I506
 with sigma of 0.04
 Zn33-Zn53 \\sim Zn43-Zn53
 with sigma of 0.04
 C333-C335 \\sim C332-C336
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C309 \\sim C313 \\sim C312 \\sim N305 \\sim C311 \\sim C310: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn41) = Uanis(Zn51)
4. Rigid body (RIGU) restrains
 C309, C313, C312, N305, C311, C310
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: I305(0.58585) I306(0.58585) I401(0.3606) I402(0.3606)
 I403(0.46794) Zn33(0.58585) I404(0.46794) Zn41(0.3606) Zn42(0.46794)
 I303(0.50244) Zn32(0.50244) I304(0.50244) I503(0.02962) I504(0.02962)
 Zn52(0.02962) Zn31(0.48521) I301(0.48521) I302(0.48521) I501(0.15419)
 Zn51(0.15419) I502(0.15419) I505(0.04939) I506(0.04939) Zn53(0.04939)
 I406(0.36476) Zn43(0.36476) I405(0.36476)
 Fixed Uiso: I503(0.08) I504(0.08) Zn52(0.08) I505(0.08) I506(0.08) Zn53(0.08)
6.a Aromatic/amide H refined with riding coordinates:
 C319(H319), C320(H320), C315(H315), C305(H305), C314(H314), C328(H328),
 C329(H329), C304(H304), C302(H302), C301(H301), C318(H318), C312(H312),
 C317(H317), C323(H323), C311(H311), C310(H310), C335(H335), C313(H313),
 C322(H322), C333(H333), C332(H332), C336(H336), C331(H331), C330(H330)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67212
_shelx_hkl_checksum              47766
_shelx_fab_checksum              28107
_platon_squeeze_void_probe_radius 1.20
_olex2_date_sample_data_collection 2023-04-19
_olex2_date_sample_submission    2023-04-19
_olex2_submission_original_sample_id 50_10_48c
_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 3.281
_oxdiff_exptl_absorpt_empirical_full_min 0.381