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_1571831
_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                 99.334(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.994(5)
_cell_length_b                   15.0640(7)
_cell_length_c                   29.295(5)
_cell_measurement_reflns_used    3407
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.8930
_cell_measurement_theta_min      2.6260
_cell_volume                     14803(3)
_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 0.984
_diffrn_measured_fraction_theta_max 0.983
_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   -156.00-131.00   0.50   10.00    -- -103.00 -40.00-174.00   50
  2  \w   -112.00 -67.00   0.50   10.00    -- -103.00 125.00  60.00   90
  3  \w    -67.00 -41.00   0.50   10.00    -- -103.00  61.00   0.00   52
  4  \w    -61.00 -30.00   0.50   10.00    -- -103.00  61.00  60.00   62
  5  \w    -66.00 -39.00   0.50   10.00    -- -103.00  61.00 120.00   54
  6  \w    -55.00 -30.00   0.50   10.00    -- -103.00 125.00  60.00   50
  7  \w    -69.00 -44.00   0.50   10.00    -- -103.00  61.00 -90.00   50
  8  \w    -66.00 -30.00   0.50   10.00    -- -103.00  61.00-180.00   72
  9  \w    -65.00 -30.00   0.50   10.00    -- -103.00  61.00  90.00   70
 10  \w    -69.00 -44.00   0.50   10.00    -- -103.00  61.00 150.00   50
 11  \w     89.00 174.00   0.50   10.00    --  101.75  40.00 -20.00  170
 12  \w     34.00  72.00   0.50   10.00    --  101.75 -61.00 -90.00   76
 13  \w     31.00  80.00   0.50   10.00    --  101.75 -94.00  30.00   98
 14  \w     48.00 107.00   0.50   10.00    --  101.75 -77.00-150.00  118
 15  \w     29.00  65.00   0.50   10.00    --  101.75 -61.00-180.00   72
 16  \w    102.00 166.00   0.50   10.00    --  101.75  61.00 -90.00  128
 17  \w     29.00  83.00   0.50   10.00    --  101.75 -94.00-150.00  108
 18  \w     89.00 150.00   0.50   10.00    --  101.75  45.00 -90.00  122
 19  \w   -114.00 -34.00   0.50    0.50    --  -46.11 -40.00-174.00  160
 20  \w    -32.00  -7.00   0.50    0.50    --  -46.11  40.00 -20.00   50
 21  \w    -23.00  17.00   0.50    0.50    --   46.11 -40.00-174.00   80
 22  \w     37.00 112.00   0.50    0.50    --   46.11  40.00 -20.00  150
 23  \w    -23.00  24.00   0.50    0.50    --  -46.11  19.00 -30.00   94
 24  \w    -27.00  28.00   0.50    0.50    --   46.11 -19.00  30.00  110
;
_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      0.0056491000
_diffrn_orient_matrix_UB_12      0.0069721000
_diffrn_orient_matrix_UB_13      0.0531439000
_diffrn_orient_matrix_UB_21      0.0393653000
_diffrn_orient_matrix_UB_22      0.0507769000
_diffrn_orient_matrix_UB_23      -0.0000794000
_diffrn_orient_matrix_UB_31      -0.0230221000
_diffrn_orient_matrix_UB_32      0.0883983000
_diffrn_orient_matrix_UB_33      -0.0041088000
_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  0.1134
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            43344
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         2.635
_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    20.990
_exptl_absorpt_correction_T_max  0.337
_exptl_absorpt_correction_T_min  0.088
_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    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         13329
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.1738
_refine_ls_R_factor_gt           0.1223
_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          0.3725
_refine_ls_wR_factor_ref         0.4221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6347
_reflns_number_total             13329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_10_24a
_cod_database_code               1571831
_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   0.321
_shelx_estimated_absorpt_t_min   0.125
_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
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 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-N306 \\sim Zn43-N306
 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
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 Zn41-N301 \\sim Zn41-N401
 with sigma of 0.02
 Zn32-N305 \\sim Zn32-N405
 with sigma of 0.02
 Zn33-N306 \\sim Zn33-N406
 with sigma of 0.02
 N302-C308 \\sim N402-C408
 with sigma of 0.02
 N302-C306 \\sim N402-C406
 with sigma of 0.02
 N304-C308 \\sim N404-C408
 with sigma of 0.02
 N304-C307 \\sim N404-C407
 with sigma of 0.02
 N301-C301 \\sim N401-C401
 with sigma of 0.02
 N301-C305 \\sim N401-C405
 with sigma of 0.02
 N301-Zn31 \\sim N401-Zn31
 with sigma of 0.02
 N303-C307 \\sim N403-C407
 with sigma of 0.02
 N303-C306 \\sim N403-C406
 with sigma of 0.02
 C313-C309 \\sim C413-C409
 with sigma of 0.02
 C313-C312 \\sim C413-C412
 with sigma of 0.02
 C308-C316 \\sim C408-C416
 with sigma of 0.02
 C307-C309 \\sim C407-C409
 with sigma of 0.02
 C306-C303 \\sim C406-C403
 with sigma of 0.02
 C309-C310 \\sim C409-C410
 with sigma of 0.02
 C303-C302 \\sim C403-C402
 with sigma of 0.02
 C303-C304 \\sim C403-C404
 with sigma of 0.02
 C316-C317 \\sim C416-C417
 with sigma of 0.02
 C316-C315 \\sim C416-C415
 with sigma of 0.02
 N306-C318 \\sim N406-C418
 with sigma of 0.02
 N306-Zn43 \\sim N406-Zn43
 with sigma of 0.02
 N306-C314 \\sim N406-C414
 with sigma of 0.02
 C312-N305 \\sim C412-N405
 with sigma of 0.02
 C302-C301 \\sim C402-C401
 with sigma of 0.02
 C318-C317 \\sim C418-C417
 with sigma of 0.02
 C311-C310 \\sim C411-C410
 with sigma of 0.02
 C311-N305 \\sim C411-N405
 with sigma of 0.02
 C305-C304 \\sim C405-C404
 with sigma of 0.02
 Zn42-N305 \\sim Zn42-N405
 with sigma of 0.02
 C315-C314 \\sim C415-C414
 with sigma of 0.02
 Zn41-C301 \\sim Zn41-C401
 with sigma of 0.04
 Zn41-C305 \\sim Zn41-C405
 with sigma of 0.04
 Zn32-C312 \\sim Zn32-C412
 with sigma of 0.04
 Zn32-C311 \\sim Zn32-C411
 with sigma of 0.04
 Zn33-C318 \\sim Zn33-C418
 with sigma of 0.04
 Zn33-C314 \\sim Zn33-C414
 with sigma of 0.04
 N302-N304 \\sim N402-N404
 with sigma of 0.04
 N302-N303 \\sim N402-N403
 with sigma of 0.04
 N302-C303 \\sim N402-C403
 with sigma of 0.04
 N302-C316 \\sim N402-C416
 with sigma of 0.04
 N304-N303 \\sim N404-N403
 with sigma of 0.04
 N304-C309 \\sim N404-C409
 with sigma of 0.04
 N304-C316 \\sim N404-C416
 with sigma of 0.04
 N301-C302 \\sim N401-C402
 with sigma of 0.04
 N301-C304 \\sim N401-C404
 with sigma of 0.04
 N303-C309 \\sim N403-C409
 with sigma of 0.04
 N303-C303 \\sim N403-C403
 with sigma of 0.04
 C313-C307 \\sim C413-C407
 with sigma of 0.04
 C313-C310 \\sim C413-C410
 with sigma of 0.04
 C313-N305 \\sim C413-N405
 with sigma of 0.04
 C308-C307 \\sim C408-C407
 with sigma of 0.04
 C308-C306 \\sim C408-C406
 with sigma of 0.04
 C308-C317 \\sim C408-C417
 with sigma of 0.04
 C308-C315 \\sim C408-C415
 with sigma of 0.04
 C307-C306 \\sim C407-C406
 with sigma of 0.04
 C307-C310 \\sim C407-C410
 with sigma of 0.04
 C306-C302 \\sim C406-C402
 with sigma of 0.04
 C306-C304 \\sim C406-C404
 with sigma of 0.04
 C309-C312 \\sim C409-C412
 with sigma of 0.04
 C309-C311 \\sim C409-C411
 with sigma of 0.04
 C303-C301 \\sim C403-C401
 with sigma of 0.04
 C303-C305 \\sim C403-C405
 with sigma of 0.04
 C316-C318 \\sim C416-C418
 with sigma of 0.04
 C316-C314 \\sim C416-C414
 with sigma of 0.04
 N306-C317 \\sim N406-C417
 with sigma of 0.04
 N306-C315 \\sim N406-C415
 with sigma of 0.04
 C312-C311 \\sim C412-C411
 with sigma of 0.04
 C312-Zn42 \\sim C412-Zn42
 with sigma of 0.04
 C302-C304 \\sim C402-C404
 with sigma of 0.04
 C318-Zn43 \\sim C418-Zn43
 with sigma of 0.04
 C318-C314 \\sim C418-C414
 with sigma of 0.04
 C301-C305 \\sim C401-C405
 with sigma of 0.04
 C301-Zn31 \\sim C401-Zn31
 with sigma of 0.04
 C317-C315 \\sim C417-C415
 with sigma of 0.04
 C311-Zn42 \\sim C411-Zn42
 with sigma of 0.04
 C310-N305 \\sim C410-N405
 with sigma of 0.04
 C305-Zn31 \\sim C405-Zn31
 with sigma of 0.04
 Zn43-C314 \\sim Zn43-C414
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(N301) = Uanis(C303) = Uanis(C302) = Uanis(C301) = Uanis(C305) =
Uanis(C304) = Uanis(N401) = Uanis(C403) = Uanis(C402) = Uanis(C401) =
Uanis(C405) = Uanis(C404)
Uanis(N302) = Uanis(N304) = Uanis(N303) = Uanis(C308) = Uanis(C307) =
Uanis(C306) = Uanis(N402) = Uanis(N404) = Uanis(N403) = Uanis(C408) =
Uanis(C407) = Uanis(C406)
Uanis(C313) = Uanis(C309) = Uanis(C312) = Uanis(C311) = Uanis(C310) =
Uanis(N305) = Uanis(C413) = Uanis(C409) = Uanis(C412) = Uanis(C411) =
Uanis(C410) = Uanis(N405)
Uanis(C316) = Uanis(N306) = Uanis(C318) = Uanis(C317) = Uanis(C315) =
Uanis(C314) = Uanis(C416) = Uanis(N406) = Uanis(C418) = Uanis(C417) =
Uanis(C415) = Uanis(C414)
Uanis(C321) = Uanis(C322) = Uanis(C323) = Uanis(N307) = Uanis(C319) =
Uanis(C320)
Uanis(N309) = Uanis(N308) = Uanis(N310) = Uanis(C325) = Uanis(C324) =
Uanis(C326)
Uanis(C334) = Uanis(C335) = Uanis(C336) = Uanis(C333) = Uanis(N312) =
Uanis(C332)
Uanis(N311) = Uanis(C327) = Uanis(C331) = Uanis(C330) = Uanis(C328) =
Uanis(C329)
4. Others
 Sof(I301)=Sof(Zn31)=Sof(I302)=1-FVAR(1)
 Sof(I401)=Sof(I402)=Sof(Zn41)=FVAR(1)
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(2)
 Sof(I305)=Sof(I306)=Sof(Zn33)=FVAR(2)
 Sof(N402)=Sof(N404)=Sof(N401)=Sof(N403)=Sof(C413)=Sof(H413)=Sof(C408)=
 Sof(C407)=Sof(C406)=Sof(C409)=Sof(C403)=Sof(C416)=Sof(N406)=Sof(C412)=
 Sof(H412)=Sof(C402)=Sof(H402)=Sof(C418)=Sof(H418)=Sof(C401)=Sof(H401)=
 Sof(C417)=Sof(H417)=Sof(C411)=Sof(H411)=Sof(C410)=Sof(H410)=Sof(C405)=
 Sof(H405)=Sof(C404)=Sof(H404)=Sof(N405)=Sof(C415)=Sof(H415)=Sof(C414)=
 Sof(H414)=1-FVAR(3)
 Sof(N302)=Sof(N304)=Sof(N301)=Sof(N303)=Sof(C313)=Sof(H313)=Sof(C308)=
 Sof(C307)=Sof(C306)=Sof(C309)=Sof(C303)=Sof(C316)=Sof(N306)=Sof(C312)=
 Sof(H312)=Sof(C302)=Sof(H302)=Sof(C318)=Sof(H318)=Sof(C301)=Sof(H301)=
 Sof(C317)=Sof(H317)=Sof(C311)=Sof(H311)=Sof(C310)=Sof(H310)=Sof(C305)=
 Sof(H305)=Sof(C304)=Sof(H304)=Sof(N305)=Sof(C315)=Sof(H315)=Sof(C314)=
 Sof(H314)=FVAR(3)
 Fixed Sof: I303(0.489) I304(0.489) Zn32(0.489) I403(0.511) Zn42(0.511)
 I404(0.511)
5.a Aromatic/amide H refined with riding coordinates:
 C331(H331), C313(H313), C322(H322), C323(H323), C319(H319), C320(H320),
 C330(H330), C312(H312), C302(H302), C328(H328), C318(H318), C301(H301),
 C317(H317), C311(H311), C310(H310), C305(H305), C304(H304), C335(H335),
 C336(H336), C333(H333), C329(H329), C315(H315), C314(H314), C332(H332),
 C413(H413), C412(H412), C402(H402), C418(H418), C401(H401), C417(H417),
 C411(H411), C410(H410), C405(H405), C404(H404), C415(H415), C414(H414)
5.b Fitted hexagon refined as free rotating group:
 C321(C322,C323,N307,C319,C320)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2923
_shelx_hkl_checksum              51733
_shelx_fab_checksum              47214
_olex2_date_sample_data_collection 2022-03-10
_olex2_date_sample_submission    2022-03-10
_olex2_submission_original_sample_id 4_10_24a
_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 4.119
_oxdiff_exptl_absorpt_empirical_full_min 0.208