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_1571856
_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             2024-01-26
_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                 101.076(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4800(19)
_cell_length_b                   15.0207(4)
_cell_length_c                   30.258(2)
_cell_measurement_reflns_used    7145
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.5150
_cell_measurement_theta_min      2.6600
_cell_volume                     15379.1(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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(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 0.985
_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 -93.00   0.50    6.00    -- -103.00 -24.00 170.00  158
  2  \w    -90.00 -64.00   0.50    6.00    -- -103.00  77.00 120.00   52
  3  \w    -69.00 -31.00   0.50    6.00    -- -103.00  61.00   0.00   76
  4  \w    -63.00 -32.00   0.50    6.00    -- -103.00  61.00  90.00   62
  5  \w    -60.00 -30.00   0.50    6.00    -- -103.00  61.00 -30.00   60
  6  \w   -147.00-104.00   0.50    6.00    -- -103.00 -30.00-120.00   86
  7  \w   -103.00 -31.00   0.50    6.00    -- -103.00  77.00 -60.00  144
  8  \w    -66.00 -31.00   0.50    6.00    -- -103.00  61.00-120.00   70
  9  \w    -98.00 -68.00   0.50    6.00    -- -103.00  77.00  90.00   60
 10  \w    -55.00 -30.00   0.50    6.00    -- -103.00  77.00  90.00   50
 11  \w    -57.00 -30.00   0.50    6.00    -- -103.00  61.00 -60.00   54
 12  \w    -68.00 -33.00   0.50    6.00    -- -103.00  61.00  60.00   70
 13  \w    -65.00 -30.00   0.50    6.00    -- -103.00  61.00-180.00   70
 14  \w    -61.00 -36.00   0.50    6.00    -- -103.00  61.00 120.00   50
 15  \w    102.00 128.00   0.50    6.00    --  101.75  24.00 -24.00   52
 16  \w    104.00 139.00   0.50    6.00    --  101.75 125.00 150.00   70
 17  \w     34.00  62.00   0.50    6.00    --  101.75 -61.00-150.00   56
 18  \w     50.00  96.00   0.50    6.00    --  101.75 -77.00  90.00   92
 19  \w   -118.00 -42.00   0.50    1.00    --  -46.36 -24.00 170.00  152
 20  \w    -24.00   1.00   0.50    1.00    --  -46.36  24.00 -24.00   50
 21  \w    -21.00  24.00   0.50    1.00    --   46.36 -24.00 170.00   90
 22  \w     35.00 116.00   0.50    1.00    --   46.36  24.00 -24.00  162
 23  \w     33.00  90.00   0.50    1.00    --   46.36-125.00-150.00  114
 24  \w    -23.00  20.00   0.50    1.00    --   46.36 -19.00  30.00   86
;
_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      -0.0058274000
_diffrn_orient_matrix_UB_12      0.0092592000
_diffrn_orient_matrix_UB_13      -0.0515163000
_diffrn_orient_matrix_UB_21      -0.0429187000
_diffrn_orient_matrix_UB_22      0.0309109000
_diffrn_orient_matrix_UB_23      -0.0017734000
_diffrn_orient_matrix_UB_31      0.0141620000
_diffrn_orient_matrix_UB_32      0.0973096000
_diffrn_orient_matrix_UB_33      0.0054282000
_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  0.0429
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45320
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.240
_diffrn_reflns_theta_min         2.612
_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    20.204
_exptl_absorpt_correction_T_max  0.388
_exptl_absorpt_correction_T_min  0.124
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         13874
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1436P)^2^+7.3530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2252
_refine_ls_wR_factor_ref         0.2425
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8734
_reflns_number_total             13874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_10_48b
_cod_original_cell_volume        15379.3(14)
_cod_database_code               1571856
_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   0.090
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I303-N306 \\sim I403-N306
 with sigma of 0.04
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 I303-N307 \\sim I403-N307
 with sigma of 0.04
 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
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 Zn33-N312 \\sim Zn43-N312
 with sigma of 0.02
 I12-Zn52 \\sim I303-Zn32
 with sigma of 0.02
 I2-Zn52 \\sim I304-Zn32
 with sigma of 0.02
 Zn52-N307 \\sim Zn42-N307
 with sigma of 0.02
 Zn52-N306 \\sim Zn42-N306
 with sigma of 0.02
 I301-Zn31 \\sim I1-Zn
 with sigma of 0.02
 I302-Zn31 \\sim I3-Zn
 with sigma of 0.02
 Zn31-N301 \\sim Zn-N301
 with sigma of 0.02
 I301-I302 \\sim I1-I3
 with sigma of 0.04
 I301-N301 \\sim I1-N301
 with sigma of 0.04
 I302-N301 \\sim I3-N301
 with sigma of 0.04
 I4-Zn10 \\sim I3-Zn
 with sigma of 0.02
 I6-Zn10 \\sim I1-Zn
 with sigma of 0.02
3. Others
 1*[Sof(I301)+Sof(I302)+Sof(Zn31)]+1*[Sof(Zn)+Sof(I3)+Sof(I1)]+1*[Sof(I4)+
 Sof(I6)+Sof(Zn10)]=1 with esd of 0.00001
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(1)
 Sof(I305)=Sof(I306)=Sof(Zn33)=FVAR(1)
 Sof(I301)=Sof(I302)=Sof(Zn31)=FVAR(2)
 Sof(Zn)=Sof(I3)=Sof(I1)=FVAR(3)
 Sof(I4)=Sof(I6)=Sof(Zn10)=FVAR(4)
 Fixed Sof: I304(0.41044) I303(0.41044) Zn32(0.41044) I404(0.55975)
 Zn42(0.55975) I403(0.55975) I2(0.02981) Zn52(0.02981) I12(0.02981)
 Fixed Uiso: I2(0.08) Zn52(0.08) I12(0.08) I4(0.08) I6(0.08) Zn10(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C332(H332), C333(H333), C313(H313), C312(H312), C322(H322), C323(H323),
 C336(H336), C335(H335), C314(H314), C315(H315), C317(H317), C305(H305),
 C304(H304), C318(H318), C301(H301), C310(H310), C328(H328), C329(H329),
 C311(H311), C302(H302), C330(H330), C331(H331), C320(H320), C319(H319)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              1666
_shelx_hkl_checksum              75360
_shelx_fab_checksum              26133
_olex2_date_sample_data_collection 2022-07-28
_olex2_date_sample_submission    2022-07-28
_olex2_submission_original_sample_id 25_10_48b
_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 3.298
_oxdiff_exptl_absorpt_empirical_full_min 0.386