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_1571826
_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, 0.289(C6 H12)'
_chemical_formula_sum            'C37.73 H27.46 I6 N12 Zn3'
_chemical_formula_weight         1606.46
_chemical_name_systematic
;catena-[bis(mu-2,4,6-tri(pyridin-4-yl)-1,3,5-triazine)-hexaiodo-tri-zinc
 cyclohexane solvate
;
_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             2024-02-06
_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                 100.996(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4432(11)
_cell_length_b                   15.0627(4)
_cell_length_c                   30.2136(14)
_cell_measurement_reflns_used    13332
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      65.2070
_cell_measurement_theta_min      2.5880
_cell_volume                     15387.3(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 0.987
_diffrn_measured_fraction_theta_max 0.984
_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     17.00  48.00   0.50    1.40    --   83.39 -42.00 -24.00   62
  2  \w    123.00 153.00   0.50    1.40    --   83.39  42.00 127.00   60
  3  \w     76.00 103.00   0.50    1.40    --   83.39  42.00 127.00   54
  4  \w     54.00  96.00   0.50    1.40    --   83.39 -77.00 150.00   84
  5  \w     15.00  44.00   0.50    1.40    --   83.39 -37.00   0.00   58
  6  \w     69.00  99.00   0.50    1.40    --   83.39  77.00-150.00   60
  7  \w     19.00  45.00   0.50    1.40    --   83.39 -57.00-120.00   52
  8  \w    103.00 138.00   0.50    1.40    --   83.39  77.00 150.00   70
  9  \w     25.00  52.00   0.50    1.40    --   83.39 -77.00 150.00   54
 10  \w    121.00 150.00   0.50    1.40    --   83.39  19.00-150.00   58
 11  \w     13.00  41.00   0.50    1.40    --   83.39 -37.00-120.00   56
 12  \w     75.00 103.00   0.50    1.40    --   83.39  57.00-150.00   56
 13  \w     83.00 119.00   0.50    1.40    --   83.39  19.00-150.00   72
 14  \w     86.00 147.00   0.50    1.40    --   83.39 125.00   0.00  122
 15  \w    106.00 133.00   0.50    1.40    --   83.39  57.00-150.00   54
 16  \w     15.00  40.00   0.50    1.40    --   83.39 -37.00  60.00   50
 17  \w     13.00  44.00   0.50    1.40    --   83.39 -37.00  90.00   62
 18  \w     69.00  97.00   0.50    1.40    --   83.39  77.00 150.00   56
 19  \w     39.00  66.00   0.50    1.40    --   83.39 -57.00  90.00   54
 20  \w    119.00 144.00   0.50    1.40    --   83.39  77.00-150.00   50
 21  \w     97.00 123.00   0.50    1.40    --   83.39  57.00-120.00   52
 22  \w     21.00  47.00   0.50    1.40    --   83.39 -57.00 150.00   52
 23  \w   -150.00 -72.00   0.50    1.40    --  -79.34 -42.00 -24.00  156
 24  \w    -44.00 -18.00   0.50    1.40    --  -79.34  42.00 127.00   52
 25  \w   -105.00 -18.00   0.50    1.40    --  -79.34 125.00 150.00  174
 26  \w    -39.00  -8.00   0.50    1.40    --  -79.34  37.00  90.00   62
 27  \w   -125.00 -48.00   0.50    0.60    --  -55.07 -42.00 -24.00  154
 28  \w    -45.00  15.00   0.50    0.60    --  -55.07  42.00 127.00  120
 29  \w    -23.00  14.00   0.50    0.60    --  -55.07  19.00-180.00   74
 30  \w    -23.00  13.00   0.50    0.60    --  -55.07  19.00-120.00   72
 31  \w    -22.00  10.00   0.50    0.60    --  -55.07  19.00 -60.00   64
 32  \w    -19.00  49.00   0.50    0.60    --   51.57 -42.00 -24.00  136
 33  \w     60.00  85.00   0.50    0.60    --   51.57  42.00 127.00   50
;
_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      0.0105960000
_diffrn_orient_matrix_UB_12      -0.0341569000
_diffrn_orient_matrix_UB_13      0.0488967000
_diffrn_orient_matrix_UB_21      0.0380683000
_diffrn_orient_matrix_UB_22      -0.0421747000
_diffrn_orient_matrix_UB_23      -0.0102567000
_diffrn_orient_matrix_UB_31      0.0226625000
_diffrn_orient_matrix_UB_32      0.0866657000
_diffrn_orient_matrix_UB_33      0.0142769000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            66878
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.614
_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    20.201
_exptl_absorpt_correction_T_max  0.475
_exptl_absorpt_correction_T_min  0.056
_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    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             5967
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.425
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         13871
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0902
_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^)+(0.1591P)^2^+158.7637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2797
_refine_ls_wR_factor_ref         0.2970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9808
_reflns_number_total             13871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_1_96b
_cod_database_code               1571826
_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   0.332
_shelx_estimated_absorpt_t_min   0.095
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C2-C3 = C2-C7 = C3-C4 = C4-C5 = C5-C6 = C6-C7
 1.54 with sigma of 0.02
 C2-C4 = C2-C6 = C3-C5 = C4-C6 = C5-C7
 2.54 with sigma of 0.04
 I402-Zn41 \\sim I302-Zn31
 with sigma of 0.02
 I401-Zn41 \\sim I301-Zn31
 with sigma of 0.02
 Zn41-N301 \\sim Zn31-N301
 with sigma of 0.02
 I402-I401 \\sim I302-I301
 with sigma of 0.04
 I402-N301 \\sim I302-N301
 with sigma of 0.04
 I401-N301 \\sim I301-N301
 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
 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
 C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C6 \\sim C6-C7 \\sim C7-C2
 with sigma of 0.02
 C2-C6 \\sim C4-C6 \\sim C3-C7 \\sim C3-C5 \\sim C5-C7 \\sim C2-C4
 with sigma of 0.04
 I503-Zn52 \\sim I404-Zn42
 with sigma of 0.02
 I504-Zn52 \\sim I304-Zn32
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(1)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(1)
 Fixed Sof: I402(0.465) I403(0.39893) I401(0.465) I404(0.39893) Zn41(0.465)
 Zn42(0.39893) I302(0.48184) Zn31(0.48184) I301(0.48184) I304(0.5661)
 Zn32(0.5661) I303(0.5661) I504(0.03498) I503(0.03498) Zn52(0.03498)
 I502(0.05316) Zn51(0.05316) I501(0.05316) C2(0.28851) H2A(0.28851)
 H2B(0.28851) C3(0.28851) H3A(0.28851) H3B(0.28851) C4(0.28851) H4A(0.28851)
 H4B(0.28851) C5(0.28851) H5A(0.28851) H5B(0.28851) C6(0.28851) H6A(0.28851)
 H6B(0.28851) C7(0.28851) H7A(0.28851) H7B(0.28851)
 Fixed Uiso: I504(0.08) I503(0.08) Zn52(0.08) I502(0.08) Zn51(0.08) I501(0.08)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
6.b Aromatic/amide H refined with riding coordinates:
 C336(H336), C335(H335), C311(H311), C331(H331), C310(H310), C304(H304),
 C330(H330), C302(H302), C332(H332), C333(H333), C305(H305), C301(H301),
 C320(H320), C329(H329), C315(H315), C318(H318), C313(H313), C314(H314),
 C312(H312), C322(H322), C317(H317), C328(H328), C323(H323), C319(H319)
;
_shelx_res_checksum              26238
_shelx_hkl_checksum              47561
_olex2_submission_original_sample_id 4_1_96b
_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 4.658
_oxdiff_exptl_absorpt_empirical_full_min 0.438