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_1571854
_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                 100.709(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4156(9)
_cell_length_b                   15.0804(3)
_cell_length_c                   30.0607(16)
_cell_measurement_reflns_used    8194
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.1470
_cell_measurement_theta_min      2.5940
_cell_volume                     15329.8(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 0.995
_diffrn_measured_fraction_theta_max 0.994
_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   -106.00 -37.00   0.50    4.00    -- -103.00 112.00 -53.00  138
  2  \w   -150.00-125.00   0.50    4.00    -- -103.00-112.00-145.00   50
  3  \w    -65.00 -40.00   0.50    4.00    -- -103.00  61.00 150.00   50
  4  \w   -116.00 -90.00   0.50    4.00    -- -103.00 -45.00-150.00   52
  5  \w   -172.00-136.00   0.50    4.00    -- -103.00 -45.00-150.00   72
  6  \w    -62.00 -33.00   0.50    4.00    -- -103.00  61.00 -30.00   58
  7  \w   -173.00 -94.00   0.50    4.00    -- -103.00 -30.00 120.00  158
  8  \w    -58.00 -33.00   0.50    4.00    -- -103.00  61.00 120.00   50
  9  \w     67.00  94.00   0.50    4.00    --  101.75-112.00-145.00   54
 10  \w     90.00 135.00   0.50    4.00    --  101.75 112.00 -53.00   90
 11  \w     29.00 106.00   0.50    4.00    --  101.75 -94.00-150.00  154
 12  \w     33.00  65.00   0.50    4.00    --  101.75-125.00  60.00   64
 13  \w    140.00 166.00   0.50    4.00    --  101.75  61.00 -90.00   52
 14  \w     30.00  65.00   0.50    4.00    --  101.75 -61.00-150.00   70
 15  \w     85.00 134.00   0.50    4.00    --  101.75  61.00 -90.00   98
 16  \w     38.00  69.00   0.50    4.00    --  101.75 -61.00-120.00   62
 17  \w     63.00 106.00   0.50    4.00    --  101.75 -94.00-120.00   86
 18  \w     43.00  69.00   0.50    4.00    --  101.75 -61.00 -90.00   52
 19  \w     29.00  65.00   0.50    4.00    --  101.75 -61.00   0.00   72
 20  \w     77.00 110.00   0.50    4.00    --  101.75-125.00  60.00   66
 21  \w     34.00  65.00   0.50    4.00    --  101.75 -61.00  60.00   62
 22  \w     93.00 146.00   0.50    4.00    --  101.75 125.00  60.00  106
 23  \w    -83.00 -12.00   0.50    1.00    --  -46.26 112.00 -53.00  142
 24  \w     26.00  61.00   0.50    1.00    --   46.26-112.00-145.00   70
 25  \w     -6.00  29.00   0.50    1.00    --  -46.26  19.00-150.00   70
 26  \w   -117.00 -24.00   0.50    1.00    --  -46.26 -77.00-150.00  186
 27  \w    -22.00  24.00   0.50    1.00    --  -46.26  19.00 -60.00   92
;
_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      0.0015512000
_diffrn_orient_matrix_UB_12      -0.0164678000
_diffrn_orient_matrix_UB_13      -0.0501930000
_diffrn_orient_matrix_UB_21      0.0084093000
_diffrn_orient_matrix_UB_22      -0.0989764000
_diffrn_orient_matrix_UB_23      0.0102544000
_diffrn_orient_matrix_UB_31      -0.0447689000
_diffrn_orient_matrix_UB_32      -0.0191551000
_diffrn_orient_matrix_UB_33      -0.0097082000
_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  0.0507
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            53521
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         2.613
_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    20.269
_exptl_absorpt_correction_T_max  0.425
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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    1.371
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.781
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         13960
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0864
_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^)+(0.1966P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2709
_refine_ls_wR_factor_ref         0.2890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9409
_reflns_number_total             13960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_10_24c
_cod_database_code               1571854
_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   0.376
_shelx_estimated_absorpt_t_min   0.140
_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
 I404-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 Zn42-N305 \\sim Zn32-N305
 with sigma of 0.02
 I404-I403 \\sim I304-I303
 with sigma of 0.04
 I404-N305 \\sim I304-N305
 with sigma of 0.04
 I403-N305 \\sim I303-N305
 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
 Zn33-N307 \\sim Zn43-N307
 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
 I305-N307 \\sim I405-N307
 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
3. Others
 1*[Sof(I401)+Sof(I402)+Sof(Zn41)]+1*[Sof(I302)+Sof(Zn31)+Sof(I301)]+1*
 [Sof(I502)+Sof(I501)+Sof(Zn51)]=1 with esd of 0.00001
 Sof(I401)=Sof(I402)=Sof(Zn41)=FVAR(1)
 Sof(I302)=Sof(Zn31)=Sof(I301)=FVAR(2)
 Sof(I502)=Sof(I501)=Sof(Zn51)=FVAR(3)
 Fixed Sof: I404(0.28968) I403(0.28968) I305(0.55511) Zn42(0.28968)
 I306(0.55511) Zn33(0.55511) Zn32(0.68587) I303(0.68587) I304(0.68587)
 I504(0.02445) I503(0.02445) Zn52(0.02445) I405(0.44489) Zn43(0.44489)
 I406(0.44489)
 Fixed Uiso: I502(0.08) I501(0.08) Zn51(0.08) I504(0.08) I503(0.08) Zn52(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C313(H313), C312(H312), C332(H332), C317(H317), C311(H311), C319(H319),
 C310(H310), C333(H333), C322(H322), C336(H336), C318(H318), C320(H320),
 C323(H323), C305(H305), C328(H328), C329(H329), C301(H301), C330(H330),
 C304(H304), C331(H331), C335(H335), C302(H302), C315(H315), C314(H314)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32479
_shelx_hkl_checksum              63579
_shelx_fab_checksum              79556
_olex2_date_sample_data_collection 2023-04-19
_olex2_date_sample_submission    2023-04-19
_olex2_submission_original_sample_id 25_10_24c
_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 3.462
_oxdiff_exptl_absorpt_empirical_full_min 0.454