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_1571836
_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             2024-01-30
_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                 101.346(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.5442(16)
_cell_length_b                   15.0184(3)
_cell_length_c                   30.549(2)
_cell_measurement_reflns_used    7365
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.4400
_cell_measurement_theta_min      2.6440
_cell_volume                     15539.0(13)
_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   -158.00 -85.80   0.38    5.00    -- -103.00  -9.00  80.00  190
  2  \w    -61.00 -30.98   0.38    5.00    -- -103.00  61.00 120.00   79
  3  \w   -111.00 -35.00   0.38    5.00    -- -103.00 125.00  90.00  200
  4  \w    -77.00 -50.40   0.38    5.00    -- -103.00 125.00 -90.00   70
  5  \w   -111.00 -79.08   0.38    5.00    -- -103.00 125.00 -90.00   84
  6  \w   -171.00 -98.80   0.38    5.00    -- -103.00 -94.00-150.00  190
  7  \w    -56.00 -32.06   0.38    5.00    -- -103.00  61.00-120.00   63
  8  \w   -145.00-118.78   0.38    5.00    -- -103.00 -30.00 150.00   69
  9  \w    -64.00 -39.30   0.38    5.00    -- -103.00  61.00  90.00   65
 10  \w   -146.00 -94.70   0.38    5.00    -- -103.00 -30.00   0.00  135
 11  \w     86.00 151.74   0.38    5.00    --  101.75   9.00-104.00  173
 12  \w     43.00 104.56   0.38    5.00    --  101.75 -77.00-180.00  162
 13  \w     31.00  71.66   0.38    5.00    --  101.75 -61.00-150.00  107
 14  \w     30.00  95.74   0.38    5.00    --  101.75 -94.00-180.00  173
 15  \w     38.00  66.12   0.38    5.00    --  101.75 -61.00 -90.00   74
 16  \w     35.00  70.72   0.38    5.00    --  101.75 -61.00-120.00   94
 17  \w     62.00  98.86   0.38    5.00    --  101.75 -94.00  30.00   97
 18  \w   -119.00 -28.94   0.38    1.50    --  -46.26  -9.00  80.00  237
 19  \w    -10.00  16.22   0.38    1.50    --  -46.26   9.00-104.00   69
 20  \w    -25.00   0.08   0.38    1.50    --   46.26  -9.00  80.00   66
 21  \w     28.00 117.30   0.38    1.50    --   46.26   9.00-104.00  235
 22  \w    -16.00  10.22   0.38    1.50    --  -46.26  19.00  30.00   69
 23  \w    -23.00  16.14   0.38    1.50    --  -46.26  19.00  60.00  103
 24  \w     28.00  89.94   0.38    1.50    --   46.26-125.00 -60.00  163
;
_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      0.0353468000
_diffrn_orient_matrix_UB_12      0.0117361000
_diffrn_orient_matrix_UB_13      0.0390944000
_diffrn_orient_matrix_UB_21      0.0284462000
_diffrn_orient_matrix_UB_22      -0.0025836000
_diffrn_orient_matrix_UB_23      -0.0329969000
_diffrn_orient_matrix_UB_31      -0.0033705000
_diffrn_orient_matrix_UB_32      0.1018398000
_diffrn_orient_matrix_UB_33      -0.0053649000
_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  0.0488
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            51976
_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         68.247
_diffrn_reflns_theta_min         2.609
_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    19.996
_exptl_absorpt_correction_T_max  0.397
_exptl_absorpt_correction_T_min  0.157
_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    1.353
_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          0.07
_refine_diff_density_max         1.138
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         14144
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0920
_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^)+(0.1706P)^2^+47.6676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2865
_refine_ls_wR_factor_ref         0.3057
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9183
_reflns_number_total             14144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_10_96c
_cod_database_code               1571836
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     9300-90
_shelx_estimated_absorpt_t_max   0.335
_shelx_estimated_absorpt_t_min   0.142
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I404-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 I404-I403 \\sim I304-I303
 with sigma of 0.04
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 Zn43-N306 \\sim Zn33-N306
 with sigma of 0.02
 Zn43-N00W \\sim Zn33-N00W
 with sigma of 0.02
 I405-I406 \\sim I305-I306
 with sigma of 0.04
 I405-N306 \\sim I305-N306
 with sigma of 0.04
 I405-N00W \\sim I305-N00W
 with sigma of 0.04
 I406-N306 \\sim I306-N306
 with sigma of 0.04
 I406-N00W \\sim I306-N00W
 with sigma of 0.04
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I302-I301 \\sim I402-I401
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
3. Others
 Fixed Sof: I302(0.52174) I301(0.52174) I404(0.25489) I403(0.25489)
 I405(0.40494) I406(0.40494) Zn31(0.52174) Zn42(0.25489) Zn43(0.40494)
 I304(0.7451) Zn32(0.7451) I303(0.7451) I305(0.55389) Zn33(0.55389)
 I306(0.55389) I505(0.04117) I506(0.04117) Zn53(0.04117) Zn41(0.28579)
 I402(0.28579) I401(0.28579) I501(0.19247) I502(0.19247) Zn51(0.19247)
 Fixed Uiso: I505(0.08) I506(0.08) Zn53(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C302(H302), C301(H301), C311(H311), C336(H336), C310(H310), C330(H330),
 C333(H333), C335(H335), C331(H331), C332(H332), C319(H319), C329(H329),
 C323(H323), C322(H322), C320(H320), C328(H328), C305(H305), C317(H317),
 C304(H304), C313(H313), C315(H315), C312(H312), C314(H314), C318(H318)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44399
_shelx_hkl_checksum              80910
_shelx_fab_checksum              30265
_olex2_date_sample_data_collection 2023-03-04
_olex2_date_sample_submission    2023-03-04
_olex2_submission_original_sample_id 4_10_96c
_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 3.188
_oxdiff_exptl_absorpt_empirical_full_min 0.355