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_1571822
_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                 100.834(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4506(11)
_cell_length_b                   15.0594(4)
_cell_length_c                   30.1018(14)
_cell_measurement_reflns_used    8081
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.8000
_cell_measurement_theta_min      2.5920
_cell_volume                     15338.6(10)
_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 2014/5 (Sheldrick, 2014)'
_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 0.977
_diffrn_measured_fraction_theta_max 0.974
_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   -146.00 -77.00   0.50    2.59    -- -103.00  -5.00  94.00  138
  2  \w   -169.00 -97.00   0.50    2.59    -- -103.00 -45.00-150.00  144
  3  \w    -69.00 -44.00   0.50    2.59    -- -103.00  61.00-180.00   50
  4  \w   -103.00 -78.00   0.50    2.59    -- -103.00  77.00 120.00   50
  5  \w    -75.00 -47.00   0.50    2.59    -- -103.00 125.00  90.00   56
  6  \w    -66.00 -38.00   0.50    2.59    -- -103.00  77.00 120.00   56
  7  \w   -112.00 -79.00   0.50    2.59    -- -103.00 125.00  90.00   66
  8  \w    -68.00 -41.00   0.50    2.59    -- -103.00  61.00 120.00   54
  9  \w    -85.00 -58.00   0.50    2.59    -- -103.00  77.00-120.00   54
 10  \w     61.00 166.00   0.50    2.59    --  101.75   5.00 -87.00  210
 11  \w     35.00  71.00   0.50    2.59    --  101.75-125.00-150.00   72
 12  \w     33.00 106.00   0.50    2.59    --  101.75 -94.00  30.00  146
 13  \w     74.00 105.00   0.50    2.59    --  101.75-125.00-150.00   62
 14  \w   -117.00 -39.00   0.50    0.65    --  -46.36  -5.00  94.00  156
 15  \w      2.00 120.00   0.50    0.65    --   46.36   5.00 -87.00  236
 16  \w    -19.00   7.00   0.50    0.65    --   46.36  -5.00  94.00   52
 17  \w     33.00  88.00   0.50    0.65    --   46.36-125.00   0.00  110
 18  \w     -3.00  22.00   0.50    0.65    --   46.36 -19.00 -90.00   50
;
_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      -0.0213559000
_diffrn_orient_matrix_UB_12      -0.0061834000
_diffrn_orient_matrix_UB_13      -0.0497536000
_diffrn_orient_matrix_UB_21      0.0401892000
_diffrn_orient_matrix_UB_22      -0.0002945000
_diffrn_orient_matrix_UB_23      -0.0153587000
_diffrn_orient_matrix_UB_31      0.0011784000
_diffrn_orient_matrix_UB_32      -0.1020345000
_diffrn_orient_matrix_UB_33      0.0030960000
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            40957
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_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    20.257
_exptl_absorpt_correction_T_max  0.398
_exptl_absorpt_correction_T_min  0.093
_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    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         13694
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0588
_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^)+(0.1279P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.1926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9962
_reflns_number_total             13694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_1_48a
_cod_database_code               1571822
_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   0.376
_shelx_estimated_absorpt_t_min   0.070
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I302-Zn30 \\sim I402-Zn41
 with sigma of 0.02
 I301-Zn30 \\sim I401-Zn41
 with sigma of 0.02
 Zn30-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
 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
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 I304-I303 \\sim I404-I403
 with sigma of 0.04
 I304-N307 \\sim I404-N307
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I303-N307 \\sim I403-N307
 with sigma of 0.04
 I303-N306 \\sim I403-N306
 with sigma of 0.04
3. Others
 Fixed Sof: I304(0.77537) I303(0.77537) I302(0.48454) I306(0.45024)
 I301(0.48454) Zn32(0.77537) I305(0.45024) Zn30(0.48454) Zn33(0.45024)
 I402(0.45541) Zn41(0.45541) I401(0.45541) I405(0.51684) Zn43(0.51684)
 I406(0.51684) I505(0.03292) I506(0.03292) Zn53(0.03292) I502(0.06004)
 I501(0.06004) Zn51(0.06004) I404(0.1768) Zn42(0.1768) I403(0.1768)
 I504(0.04784) I503(0.04784) Zn52(0.04784)
 Fixed Uiso: I505(0.08) I506(0.08) Zn53(0.08) 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:
 C320(H320), C319(H319), C314(H314), C315(H315), C328(H328), C327(H327),
 C5(H5), C304(H304), C302(H302), C322(H322), C301(H301), C334(H334), C329(H329),
  C305(H305), C317(H317), C310(H310), C311(H311), C330(H330), C332(H332),
 C318(H318), C335(H335), C331(H331), C312(H312), C313(H313)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32029
_shelx_hkl_checksum              44107
_shelx_fab_checksum              79499
_olex2_date_sample_data_collection 2022-03-10
_olex2_date_sample_submission    2022-03-10
_olex2_submission_original_sample_id 4_1_48a
_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 4.656
_oxdiff_exptl_absorpt_empirical_full_min 0.392