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_1571834
_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                 101.054(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4940(13)
_cell_length_b                   15.0307(3)
_cell_length_c                   30.3347(13)
_cell_measurement_reflns_used    11766
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      64.8900
_cell_measurement_theta_min      3.4170
_cell_volume                     15435.8(10)
_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     84.00 145.00   0.50    4.41    --   83.39  83.00 -15.00  122
  2  \w     22.00 104.00   0.50    4.41    --   83.39 -83.00-135.00  164
  3  \w    105.00 150.00   0.50    4.41    --   83.39  57.00-150.00   90
  4  \w     14.00  39.00   0.50    4.41    --   83.39 -37.00  60.00   50
  5  \w     17.00  44.00   0.50    4.41    --   83.39 -57.00 120.00   54
  6  \w    120.00 145.00   0.50    4.41    --   83.39  77.00 -90.00   50
  7  \w     45.00  98.00   0.50    4.41    --   83.39 -77.00-120.00  106
  8  \w     75.00 147.00   0.50    4.41    --   83.39  57.00-120.00  144
  9  \w     77.00 102.00   0.50    4.41    --   83.39  77.00 -90.00   50
 10  \w     12.00  42.00   0.50    4.41    --   83.39 -37.00 -30.00   60
 11  \w     52.00  78.00   0.50    4.41    --   83.39 -77.00 -60.00   52
 12  \w     12.00  37.00   0.50    4.41    --   83.39 -37.00 -90.00   50
 13  \w     50.00  99.00   0.50    4.41    --   83.39 -77.00  60.00   98
 14  \w     68.00 142.00   0.50    4.41    --   83.39  77.00 -30.00  148
 15  \w     67.00 137.00   0.50    4.41    --   83.39  77.00 -60.00  140
 16  \w    106.00 133.00   0.50    4.41    --   83.39  57.00 -90.00   54
 17  \w     13.00  40.00   0.50    4.41    --   83.39 -37.00  30.00   54
 18  \w   -141.00 -78.00   0.50    4.41    --  -79.34 -83.00-135.00  126
 19  \w   -100.00 -18.00   0.50    4.41    --  -79.34  83.00 -15.00  164
 20  \w    -75.00   6.00   0.50    1.10    --  -55.07  83.00 -15.00  162
 21  \w    -12.00  15.00   0.50    1.10    --  -55.07  19.00-180.00   54
 22  \w    -24.00   8.00   0.50    1.10    --  -55.07  19.00 150.00   64
 23  \w    -23.00  10.00   0.50    1.10    --  -55.07  19.00  90.00   66
 24  \w    -23.00   8.00   0.50    1.10    --  -55.07  19.00 -60.00   62
 25  \w     -9.00  72.00   0.50    1.10    --   51.57 -83.00-135.00  162
 26  \w    -18.00  28.00   0.50    1.10    --   51.57 -19.00 -90.00   92
;
_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      -0.0260724000
_diffrn_orient_matrix_UB_12      -0.0222685000
_diffrn_orient_matrix_UB_13      -0.0458389000
_diffrn_orient_matrix_UB_21      -0.0231735000
_diffrn_orient_matrix_UB_22      0.0871318000
_diffrn_orient_matrix_UB_23      0.0017675000
_diffrn_orient_matrix_UB_31      0.0292962000
_diffrn_orient_matrix_UB_32      0.0490673000
_diffrn_orient_matrix_UB_33      -0.0239000000
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0347
_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       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            69226
_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         68.248
_diffrn_reflns_theta_min         2.610
_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    20.130
_exptl_absorpt_correction_T_max  0.439
_exptl_absorpt_correction_T_min  0.183
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         14036
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0844
_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^)+(0.1612P)^2^+42.9882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2720
_refine_ls_wR_factor_ref         0.2947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8636
_reflns_number_total             14036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_10_96a
_cod_database_code               1571834
_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   0.333
_shelx_estimated_absorpt_t_min   0.196
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 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
 Zn42-N306 \\sim Zn42-N307
 with sigma of 0.02
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 Zn33-N312 \\sim Zn43-N312
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 I404-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 Zn42-N306 \\sim Zn32-N306
 with sigma of 0.02
 Zn42-N307 \\sim Zn32-N307
 with sigma of 0.02
 I403-I404 \\sim I303-I304
 with sigma of 0.04
 I403-N306 \\sim I303-N306
 with sigma of 0.04
 I403-N307 \\sim I303-N307
 with sigma of 0.04
 I404-N306 \\sim I304-N306
 with sigma of 0.04
 I404-N307 \\sim I304-N307
 with sigma of 0.04
 I506-Zn53 \\sim I306-Zn33
 with sigma of 0.02
 I302-Zn31 \\sim I502-Zn51
 with sigma of 0.02
 I501-Zn51 \\sim I301-Zn31
 with sigma of 0.02
3. Others
 1*[Sof(I401)+Sof(I402)+Sof(Zn41)]+1*[Sof(I301)+Sof(Zn31)+Sof(I302)]+1*
 [Sof(I501)+Sof(I502)+Sof(Zn51)]=1 with esd of 0.00001
 Sof(I401)=Sof(I402)=Sof(Zn41)=FVAR(1)
 Sof(I301)=Sof(Zn31)=Sof(I302)=FVAR(2)
 Sof(I501)=Sof(I502)=Sof(Zn51)=FVAR(3)
 Sof(I303)=Sof(Zn32)=Sof(I304)=1-FVAR(4)
 Sof(I403)=Sof(I404)=Sof(Zn42)=FVAR(4)
 Fixed Sof: I306(0.49644) I305(0.49644) Zn33(0.49644) I406(0.39873)
 Zn43(0.39873) I405(0.39873) I505(0.10483) I506(0.10483) Zn53(0.10483)
 Fixed Uiso: 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), C312(H312), C332(H332), C320(H320), C333(H333), C318(H318),
 C317(H317), C319(H319), C310(H310), C304(H304), C311(H311), C322(H322),
 C305(H305), C336(H336), C328(H328), C323(H323), C329(H329), C331(H331),
 C335(H335), C330(H330), C315(H315), C301(H301), C302(H302), C314(H314)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              81829
_shelx_hkl_checksum              10187
_shelx_fab_checksum              79045
_olex2_date_sample_data_collection 2024-02-06
_olex2_date_sample_submission    2024-02-06
_olex2_submission_original_sample_id 4_10_96a
_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 3.004
_oxdiff_exptl_absorpt_empirical_full_min 0.356