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_1571832
_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                 99.979(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.2193(11)
_cell_length_b                   15.0730(4)
_cell_length_c                   29.5041(12)
_cell_measurement_reflns_used    8098
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.6760
_cell_measurement_theta_min      2.6400
_cell_volume                     14987.6(9)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_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 0.994
_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   -174.00 -93.00   0.50    4.50    -- -103.00 -70.00-158.00  162
  2  \w    -85.00 -57.00   0.50    4.50    -- -103.00  70.00 -26.00   56
  3  \w    -67.00 -31.00   0.50    4.50    -- -103.00  61.00 -30.00   72
  4  \w    -68.00 -43.00   0.50    4.50    -- -103.00  61.00  90.00   50
  5  \w    -67.00 -31.00   0.50    4.50    -- -103.00  61.00-120.00   72
  6  \w    -98.00 -35.00   0.50    4.50    -- -103.00  77.00 -60.00  126
  7  \w    -69.00 -37.00   0.50    4.50    -- -103.00  61.00 -90.00   64
  8  \w    -69.00 -43.00   0.50    4.50    -- -103.00  61.00-150.00   52
  9  \w    -69.00 -30.00   0.50    4.50    -- -103.00  61.00-180.00   78
 10  \w   -168.00 -94.00   0.50    4.50    -- -103.00 -15.00  60.00  148
 11  \w    104.00 129.00   0.50    4.50    --  101.75  70.00 -26.00   50
 12  \w     49.00  75.00   0.50    4.50    --  101.75 -70.00-158.00   52
 13  \w    148.00 175.00   0.50    4.50    --  101.75 125.00 -90.00   54
 14  \w     43.00  72.00   0.50    4.50    --  101.75 -61.00  30.00   58
 15  \w     37.00  62.00   0.50    4.50    --  101.75-125.00 -60.00   50
 16  \w     96.00 174.00   0.50    4.50    --  101.75  45.00 -90.00  156
 17  \w     31.00  73.00   0.50    4.50    --  101.75 -61.00   0.00   84
 18  \w     85.00 119.00   0.50    4.50    --  101.75 125.00 -90.00   68
 19  \w    -50.00  25.00   0.50    1.00    --  -46.48  70.00 -26.00  150
 20  \w   -108.00 -46.00   0.50    1.00    --  -46.48 -70.00-158.00  124
 21  \w    -25.00  48.00   0.50    1.00    --   46.48 -70.00-158.00  146
 22  \w     49.00  74.00   0.50    1.00    --   46.48  70.00 -26.00   50
 23  \w    -22.00  29.00   0.50    1.00    --  -46.48  19.00 -30.00  102
 24  \w    -23.00  22.00   0.50    1.00    --  -46.48  19.00 -60.00   90
;
_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      0.0105209000
_diffrn_orient_matrix_UB_12      -0.0037925000
_diffrn_orient_matrix_UB_13      0.0529036000
_diffrn_orient_matrix_UB_21      -0.0274630000
_diffrn_orient_matrix_UB_22      -0.0809286000
_diffrn_orient_matrix_UB_23      0.0003527000
_diffrn_orient_matrix_UB_31      0.0349876000
_diffrn_orient_matrix_UB_32      -0.0622655000
_diffrn_orient_matrix_UB_33      -0.0036649000
_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  0.0355
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            48842
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.622
_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    20.732
_exptl_absorpt_correction_T_max  0.323
_exptl_absorpt_correction_T_min  0.091
_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    1.402
_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         0.821
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         13632
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0597
_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^)+(0.1271P)^2^+3.4780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1960
_refine_ls_wR_factor_ref         0.2103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9162
_reflns_number_total             13632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_10_24b
_cod_database_code               1571832
_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   0.325
_shelx_estimated_absorpt_t_min   0.127
_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-N00I \\sim Zn43-N00I
 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-N00I \\sim I406-N00I
 with sigma of 0.04
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I305-N00I \\sim I405-N00I
 with sigma of 0.04
 N00I-C318 \\sim N00I-C418
 with sigma of 0.02
 C316-C317 \\sim C316-C417
 with sigma of 0.02
 C317-H317 \\sim C417-H417
 with sigma of 0.02
 C317-C318 \\sim C417-C418
 with sigma of 0.02
 C318-H318 \\sim C418-H418
 with sigma of 0.02
 N00I-C317 \\sim N00I-C417
 with sigma of 0.04
 N00I-H318 \\sim N00I-H418
 with sigma of 0.04
 C316-H317 \\sim C316-H417
 with sigma of 0.04
 C316-C318 \\sim C316-C418
 with sigma of 0.04
 C317-H318 \\sim C417-H418
 with sigma of 0.04
 H317-C318 \\sim H417-C418
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N310 \\sim C327 \\sim C328 \\sim C329 \\sim C330 \\sim C331: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C317) = Uanis(C318) = Uanis(C418) = Uanis(C417)
4. Rigid body (RIGU) restrains
 N310, C327, C328, C329, C330, C331
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(I306)+Sof(I305)+Sof(Zn33)]+1*[Sof(Zn43)+Sof(I405)+Sof(I406)]+1*
 [Sof(I506)+Sof(I505)+Sof(Zn53)]=1 with esd of 0.00001
 Sof(I402)=Sof(Zn41)=Sof(I401)=1-FVAR(1)
 Sof(I302)=Sof(I301)=Sof(Zn31)=FVAR(1)
 Sof(I403)=Sof(Zn42)=Sof(I404)=1-FVAR(2)
 Sof(I304)=Sof(I303)=Sof(Zn32)=FVAR(2)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(3)
 Sof(Zn43)=Sof(I405)=Sof(I406)=FVAR(4)
 Sof(I506)=Sof(I505)=Sof(Zn53)=FVAR(5)
 Sof(C418)=Sof(H418)=Sof(C417)=Sof(H417)=1-FVAR(6)
 Sof(C317)=Sof(H317)=Sof(C318)=Sof(H318)=FVAR(6)
 Fixed Uiso: I506(0.08) I505(0.08) Zn53(0.08)
6.a Aromatic/amide H refined with riding coordinates:
 C320(H320), C319(H319), C328(H328), C323(H323), C322(H322), C315(H315),
 C314(H314), C302(H302), C329(H329), C310(H310), C301(H301), C335(H335),
 C304(H304), C336(H336), C311(H311), C317(H317), C333(H333), C305(H305),
 C318(H318), C332(H332), C312(H312), C313(H313), C331(H331), C330(H330),
 C418(H418), C417(H417)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63656
_shelx_hkl_checksum              99381
_shelx_fab_checksum              95376
_olex2_date_sample_data_collection 2022-06-06
_olex2_date_sample_submission    2022-06-06
_olex2_submission_original_sample_id 4_10_24b
_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 4.269
_oxdiff_exptl_absorpt_empirical_full_min 0.314