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_1571824
_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             2024-01-29
_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                 100.809(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4353(8)
_cell_length_b                   15.0604(3)
_cell_length_c                   30.1558(14)
_cell_measurement_reflns_used    9535
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.4380
_cell_measurement_theta_min      2.5960
_cell_volume                     15361.6(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_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 0.994
_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   -170.00-144.00   0.50    4.00    -- -103.00 -87.00  22.00   52
  2  \w   -104.00 -79.00   0.50    4.00    -- -103.00  87.00 139.00   50
  3  \w   -102.00 -32.00   0.50    4.00    -- -103.00  77.00 -60.00  140
  4  \w    -69.00 -34.00   0.50    4.00    -- -103.00  61.00 150.00   70
  5  \w    -69.00 -44.00   0.50    4.00    -- -103.00  61.00 -90.00   50
  6  \w    -94.00 -30.00   0.50    4.00    -- -103.00  77.00 -30.00  128
  7  \w    -61.00 -35.00   0.50    4.00    -- -103.00  61.00   0.00   52
  8  \w    -69.00 -44.00   0.50    4.00    -- -103.00  61.00 -60.00   50
  9  \w    -63.00 -38.00   0.50    4.00    -- -103.00  61.00 -30.00   50
 10  \w     84.00 161.00   0.50    4.00    --  101.75  87.00 139.00  154
 11  \w     34.00  68.00   0.50    4.00    --  101.75-125.00-120.00   68
 12  \w    121.00 164.00   0.50    4.00    --  101.75  45.00 120.00   86
 13  \w     29.00  72.00   0.50    4.00    --  101.75 -61.00  30.00   86
 14  \w    101.00 172.00   0.50    4.00    --  101.75  45.00  90.00  142
 15  \w     42.00 113.00   0.50    4.00    --  101.75 -87.00  22.00  142
 16  \w     36.00  65.00   0.50    4.00    --  101.75 -61.00-150.00   58
 17  \w     44.00 106.00   0.50    4.00    --  101.75 -77.00  90.00  124
 18  \w     80.00 110.00   0.50    4.00    --  101.75-125.00-120.00   60
 19  \w     73.00 110.00   0.50    4.00    --  101.75-125.00  30.00   74
 20  \w     73.00  99.00   0.50    4.00    --  101.75 -77.00 -90.00   52
 21  \w    -12.00  18.00   0.50    1.00    --  -46.26  87.00 139.00   60
 22  \w    -72.00 -35.00   0.50    1.00    --  -46.26  87.00 139.00   74
 23  \w     15.00  49.00   0.50    1.00    --   46.26 -87.00  22.00   68
 24  \w   -118.00 -31.00   0.50    1.00    --  -46.26 -57.00  30.00  174
 25  \w    -24.00  25.00   0.50    1.00    --  -46.26  19.00-180.00   98
 26  \w    -40.00  25.00   0.50    1.00    --  -46.26  37.00-120.00  130
;
_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      0.0079345000
_diffrn_orient_matrix_UB_12      -0.0143807000
_diffrn_orient_matrix_UB_13      0.0514682000
_diffrn_orient_matrix_UB_21      0.0189648000
_diffrn_orient_matrix_UB_22      -0.0906850000
_diffrn_orient_matrix_UB_23      -0.0062484000
_diffrn_orient_matrix_UB_31      0.0406398000
_diffrn_orient_matrix_UB_32      0.0452171000
_diffrn_orient_matrix_UB_33      0.0037970000
_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  0.0358
_diffrn_reflns_av_unetI/netI     0.0294
_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       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            54183
_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         68.239
_diffrn_reflns_theta_min         2.613
_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    20.227
_exptl_absorpt_correction_T_max  0.400
_exptl_absorpt_correction_T_min  0.150
_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    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         13987
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0893P)^2^+13.1304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9956
_reflns_number_total             13987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_1_48c
_cod_database_code               1571824
_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   0.332
_shelx_estimated_absorpt_t_min   0.151
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I301-I302 \\sim I401-I402
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I303-Zn32 \\sim I403-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
 I304-I303 \\sim I404-I403
 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
 I303-N306 \\sim I403-N306
 with sigma of 0.04
 I303-N307 \\sim I403-N307
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 Zn33-N312 \\sim Zn43-N312
 with sigma of 0.02
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I306-N312 \\sim I406-N312
 with sigma of 0.04
3. Others
 1*[Sof(I304)+Sof(I303)+Sof(Zn32)]+1*[Sof(I403)+Sof(Zn42)+Sof(I404)]+1*
 [Sof(I503)+Sof(I504)+Sof(Zn52)]=1 with esd of 0.000001
 Sof(I304)=Sof(I303)=Sof(Zn32)=FVAR(1)
 Sof(I403)=Sof(Zn42)=Sof(I404)=FVAR(2)
 Sof(I503)=Sof(I504)=Sof(Zn52)=FVAR(3)
 Fixed Sof: I305(0.48813) I306(0.48813) I301(0.89) Zn33(0.48813) I302(0.89)
 Zn31(0.89) I401(0.06) Zn41(0.06) I402(0.06) I406(0.51187) Zn43(0.51187)
 I405(0.51187) I501(0.05) I502(0.05) Zn51(0.05)
 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), C330(H330), C311(H311), C336(H336), C310(H310), C331(H331),
 C332(H332), C333(H333), C302(H302), C320(H320), C301(H301), C304(H304),
 C305(H305), C314(H314), C322(H322), C329(H329), C313(H313), C315(H315),
 C317(H317), C312(H312), C318(H318), C328(H328), C319(H319), C323(H323)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24676
_shelx_hkl_checksum              53398
_shelx_fab_checksum              41932
_olex2_date_sample_data_collection 2023-04-19
_olex2_date_sample_submission    2023-04-19
_olex2_submission_original_sample_id 4_1_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 2.677
_oxdiff_exptl_absorpt_empirical_full_min 0.403