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_1571847
_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)-hexachloro-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             2024-02-26
_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                 101.026(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4933(18)
_cell_length_b                   15.0280(4)
_cell_length_c                   30.223(2)
_cell_measurement_reflns_used    6122
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.6820
_cell_measurement_theta_min      2.5720
_cell_volume                     15377.4(14)
_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_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 0.993
_diffrn_measured_fraction_theta_max 0.992
_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   -128.00 -98.00   0.50    6.00    -- -103.00 -30.00 177.00   60
  2  \w    -99.00 -72.00   0.50    6.00    -- -103.00  77.00 150.00   54
  3  \w    -68.00 -31.00   0.50    6.00    -- -103.00  61.00  60.00   74
  4  \w    -58.00 -31.00   0.50    6.00    -- -103.00  77.00 150.00   54
  5  \w    -68.00 -34.00   0.50    6.00    -- -103.00  77.00  90.00   68
  6  \w   -102.00 -74.00   0.50    6.00    -- -103.00  77.00  90.00   56
  7  \w    -58.00 -30.00   0.50    6.00    -- -103.00  77.00 120.00   56
  8  \w    -60.00 -35.00   0.50    6.00    -- -103.00  61.00 120.00   50
  9  \w    -96.00 -69.00   0.50    6.00    -- -103.00  77.00 120.00   54
 10  \w    -56.00 -30.00   0.50    6.00    -- -103.00  61.00-180.00   52
 11  \w    -67.00 -38.00   0.50    6.00    -- -103.00  61.00  90.00   58
 12  \w    -64.00 -37.00   0.50    6.00    -- -103.00  61.00 150.00   54
 13  \w     91.00 175.00   0.50    6.00    --  101.75  30.00 -22.00  168
 14  \w     40.00  67.00   0.50    6.00    --  101.75 -61.00 -60.00   54
 15  \w     30.00  55.00   0.50    6.00    --  101.75 -61.00-150.00   50
 16  \w     87.00 165.00   0.50    6.00    --  101.75  61.00-120.00  156
 17  \w     40.00  67.00   0.50    6.00    --  101.75 -61.00   0.00   54
 18  \w     31.00  87.00   0.50    6.00    --  101.75 -94.00-150.00  112
 19  \w     31.00  69.00   0.50    6.00    --  101.75 -61.00-180.00   76
 20  \w     30.00  73.00   0.50    6.00    --  101.75 -61.00 -90.00   86
 21  \w     38.00  67.00   0.50    6.00    --  101.75 -61.00-120.00   58
 22  \w   -101.00 -76.00   0.50    1.00    --  -46.36 -30.00 177.00   50
 23  \w    -33.00  25.00   0.50    1.00    --  -46.36  30.00 -22.00  116
 24  \w     43.00 117.00   0.50    1.00    --   46.36  30.00 -22.00  148
 25  \w    -19.00   6.00   0.50    1.00    --   46.36 -30.00 177.00   50
 26  \w    -23.00  27.00   0.50    1.00    --  -46.36  19.00  90.00  100
 27  \w    -21.00  25.00   0.50    1.00    --  -46.36  19.00-120.00   92
 28  \w    -23.00  29.00   0.50    1.00    --  -46.36  19.00 120.00  104
;
_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      0.0450435000
_diffrn_orient_matrix_UB_12      0.0086380000
_diffrn_orient_matrix_UB_13      0.0037238000
_diffrn_orient_matrix_UB_21      -0.0065291000
_diffrn_orient_matrix_UB_22      0.0385991000
_diffrn_orient_matrix_UB_23      -0.0480632000
_diffrn_orient_matrix_UB_31      -0.0014751000
_diffrn_orient_matrix_UB_32      0.0945510000
_diffrn_orient_matrix_UB_33      0.0192494000
_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  0.0671
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            47934
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         2.610
_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    20.206
_exptl_absorpt_correction_T_max  0.248
_exptl_absorpt_correction_T_min  0.111
_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    1.367
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.559
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         13978
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1619
_refine_ls_R_factor_gt           0.1390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3408P)^2^+0.1200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4334
_refine_ls_wR_factor_ref         0.4599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8739
_reflns_number_total             13978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_5_24b
_cod_original_cell_volume        15377.6(15)
_cod_database_code               1571847
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.195
_shelx_estimated_absorpt_t_min   0.101
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 Zn31-N00W \\sim Zn41-N00W
 with sigma of 0.02
 I302-I301 \\sim I402-I401
 with sigma of 0.04
 I302-N00W \\sim I402-N00W
 with sigma of 0.04
 I301-N00W \\sim I401-N00W
 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-N00I \\sim Zn42-N00I
 with sigma of 0.02
 Zn32-N00J \\sim Zn42-N00J
 with sigma of 0.02
 I304-I303 \\sim I404-I403
 with sigma of 0.04
 I304-N00I \\sim I404-N00I
 with sigma of 0.04
 I304-N00J \\sim I404-N00J
 with sigma of 0.04
 I303-N00I \\sim I403-N00I
 with sigma of 0.04
 I303-N00J \\sim I403-N00J
 with sigma of 0.04
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 Zn43-N00O \\sim Zn33-N00O
 with sigma of 0.02
 I406-I405 \\sim I306-I305
 with sigma of 0.04
 I406-N00O \\sim I306-N00O
 with sigma of 0.04
 I405-N00O \\sim I305-N00O
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C327 \\sim C328 \\sim C329 \\sim N00X \\sim C330 \\sim C331: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C309 \\sim C313 \\sim C312 \\sim N21 \\sim C311 \\sim C310: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Others
 Sof(I305)=Sof(Zn33)=Sof(I306)=1-FVAR(1)
 Sof(I406)=Sof(I405)=Sof(Zn43)=FVAR(1)
 Fixed Sof: I304(0.47384) I303(0.47384) I302(0.547) Zn32(0.47384) I301(0.547)
 Zn31(0.547) Zn41(0.453) I401(0.453) I402(0.453) I404(0.46412) Zn42(0.46412)
 I403(0.46412) I504(0.06204) I503(0.06204) Zn52(0.06204)
 Fixed Uiso: I504(0.08) I503(0.08) Zn52(0.08)
5.a Aromatic/amide H refined with riding coordinates:
 C319(H319), C329(H329), C320(H320), C315(H315), C323(H323), C304(H304),
 C317(H317), C328(H328), C302(H302), C314(H314), C310(H310), C305(H305),
 C336(H336), C312(H312), C301(H301), C335(H335), C313(H313), C333(H333),
 C311(H311), C322(H322), C331(H331), C318(H318), C330(H330), C332(H332)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44158
_shelx_hkl_checksum              73212
_shelx_fab_checksum              35612
_olex2_submission_original_sample_id 25_5_24b
_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 21.702
_oxdiff_exptl_absorpt_empirical_full_min 0.170