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_1571828
_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                 99.380(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.0757(18)
_cell_length_b                   15.0947(6)
_cell_length_c                   29.186(2)
_cell_measurement_reflns_used    6944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.2680
_cell_measurement_theta_min      2.6720
_cell_volume                     14811.5(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_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 6000HE'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_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   -172.00-102.00   0.50    6.00    -- -103.00 -37.00  21.00  140
  2  \w    -63.00 -33.00   0.50    6.00    -- -103.00  61.00 -90.00   60
  3  \w    -61.00 -30.00   0.50    6.00    -- -103.00  61.00-120.00   62
  4  \w   -123.00 -91.00   0.50    6.00    -- -103.00 -15.00 -90.00   64
  5  \w    -71.00 -45.00   0.50    6.00    -- -103.00 125.00   0.00   52
  6  \w   -170.00-139.00   0.50    6.00    -- -103.00 -15.00 -90.00   62
  7  \w   -174.00-138.00   0.50    6.00    -- -103.00 -15.00-120.00   72
  8  \w    -74.00 -32.00   0.50    6.00    -- -103.00  77.00   0.00   84
  9  \w   -115.00 -90.00   0.50    6.00    -- -103.00 -15.00-120.00   50
 10  \w    -58.00 -33.00   0.50    6.00    -- -103.00  61.00-180.00   50
 11  \w    -67.00 -42.00   0.50    6.00    -- -103.00  61.00 -30.00   50
 12  \w    -65.00 -35.00   0.50    6.00    -- -103.00  61.00 -60.00   60
 13  \w    -69.00 -30.00   0.50    6.00    -- -103.00  61.00   0.00   78
 14  \w    108.00 133.00   0.50    6.00    --  101.75  37.00 177.00   50
 15  \w     31.00  73.00   0.50    6.00    --  101.75 -61.00  60.00   84
 16  \w     35.00  62.00   0.50    6.00    --  101.75 -61.00  30.00   54
 17  \w     38.00  72.00   0.50    6.00    --  101.75 -61.00  90.00   68
 18  \w     39.00  72.00   0.50    6.00    --  101.75 -61.00 120.00   66
 19  \w     48.00 104.00   0.50    6.00    --  101.75 -77.00-120.00  112
 20  \w    -27.00  14.00   0.50    1.00    --  -46.36  37.00 177.00   82
 21  \w   -115.00 -42.00   0.50    1.00    --  -46.36 -37.00  21.00  146
 22  \w     36.00 112.00   0.50    1.00    --   46.36  37.00 177.00  152
 23  \w    -16.00   9.00   0.50    1.00    --   46.36 -37.00  21.00   50
 24  \w    -12.00  22.00   0.50    1.00    --  -46.36  19.00 150.00   68
 25  \w    -18.00  19.00   0.50    1.00    --  -46.36  19.00 -60.00   74
 26  \w    -20.00  29.00   0.50    1.00    --  -46.36  19.00 -30.00   98
;
_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      -0.0063268000
_diffrn_orient_matrix_UB_12      -0.0080462000
_diffrn_orient_matrix_UB_13      -0.0532741000
_diffrn_orient_matrix_UB_21      0.0400090000
_diffrn_orient_matrix_UB_22      0.0469427000
_diffrn_orient_matrix_UB_23      -0.0008163000
_diffrn_orient_matrix_UB_31      0.0214236000
_diffrn_orient_matrix_UB_32      -0.0903126000
_diffrn_orient_matrix_UB_33      0.0043615000
_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     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            41560
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         2.629
_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    20.978
_exptl_absorpt_correction_T_max  0.429
_exptl_absorpt_correction_T_min  0.121
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
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    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.382
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         13370
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0918
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3039
_refine_ls_wR_factor_ref         0.3413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7602
_reflns_number_total             13370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_5_48a
_cod_original_cell_volume        14811.6(15)
_cod_database_code               1571828
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.420
_shelx_estimated_absorpt_t_min   0.096
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I305-Zn33 \\sim I405-Zn43
 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
 I306-I305 \\sim I406-I405
 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
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I305-N307 \\sim I405-N307
 with sigma of 0.04
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I302-I301 \\sim I402-I401
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 Zn32-N305 \\sim Zn42-N305
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I303-N305 \\sim I403-N305
 with sigma of 0.04
 I304-N305 \\sim I404-N305
 with sigma of 0.04
 I505-Zn53 \\sim I506-Zn53
 with sigma of 0.02
 I501-Zn51 \\sim I502-Zn51
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N301) = Uanis(C302) = Uanis(C303) = Uanis(C301) = Uanis(C304) =
Uanis(C305)
Uanis(N303) = Uanis(N302) = Uanis(N304) = Uanis(C308) = Uanis(C307) =
Uanis(C306)
Uanis(N306) = Uanis(C316) = Uanis(C314) = Uanis(C315) = Uanis(C317) =
Uanis(C318)
Uanis(N305) = Uanis(C309) = Uanis(C310) = Uanis(C311) = Uanis(C312) =
Uanis(C313)
4. Others
 Sof(I403)=Sof(Zn42)=Sof(I404)=1-FVAR(1)
 Sof(I303)=Sof(I304)=Sof(Zn32)=FVAR(1)
 Fixed Sof: I306(0.50935) I305(0.50935) I302(0.47956) Zn33(0.50935)
 I301(0.47956) Zn31(0.47956) I405(0.41923) Zn43(0.41923) I406(0.41923)
 I402(0.4918) Zn41(0.4918) I401(0.4918) I502(0.02863) Zn51(0.02863)
 I501(0.02863) I506(0.07143) Zn53(0.07143) I505(0.07143)
 Fixed Uiso: I502(0.08) Zn51(0.08) I501(0.08) I506(0.08) Zn53(0.08) I505(0.08)
5.a Aromatic/amide H refined with riding coordinates:
 C320(H320), C319(H319), C328(H328), C322(H322), C302(H302), C329(H329),
 C301(H301), C323(H323), C304(H304), C310(H310), C314(H314), C315(H315),
 C311(H311), C317(H317), C312(H312), C333(H333), C305(H305), C332(H332),
 C331(H331), C318(H318), C336(H336), C313(H313), C335(H335), C330(H330)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67440
_shelx_hkl_checksum              8486
_shelx_fab_checksum              77520
_olex2_date_sample_data_collection 2022-03-10
_olex2_date_sample_submission    2022-03-10
_olex2_submission_original_sample_id 4_5_48a
_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 3.895
_oxdiff_exptl_absorpt_empirical_full_min 0.243