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_1571838
_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                 101.219(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4567(17)
_cell_length_b                   15.0045(4)
_cell_length_c                   30.444(2)
_cell_measurement_reflns_used    7111
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.7350
_cell_measurement_theta_min      2.9630
_cell_volume                     15438.9(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 0.995
_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   -165.00 -91.00   0.50    6.00    -- -103.00 -31.00-171.00  148
  2  \w    -58.00 -33.00   0.50    6.00    -- -103.00 125.00  30.00   50
  3  \w   -109.00 -84.00   0.50    6.00    -- -103.00 125.00  30.00   50
  4  \w   -170.00 -94.00   0.50    6.00    -- -103.00 -61.00 120.00  152
  5  \w    -62.00 -37.00   0.50    6.00    -- -103.00  61.00 -30.00   50
  6  \w    -92.00 -67.00   0.50    6.00    -- -103.00  77.00-180.00   50
  7  \w    -56.00 -31.00   0.50    6.00    -- -103.00  61.00-150.00   50
  8  \w    -65.00 -32.00   0.50    6.00    -- -103.00  61.00 -90.00   66
  9  \w     97.00 134.00   0.50    6.00    --  101.75  31.00 -11.00   74
 10  \w     38.00  73.00   0.50    6.00    --  101.75 -61.00  30.00   70
 11  \w     34.00  73.00   0.50    6.00    --  101.75 -61.00  90.00   78
 12  \w     88.00 114.00   0.50    6.00    --  101.75  15.00 120.00   52
 13  \w     39.00  73.00   0.50    6.00    --  101.75 -61.00-180.00   68
 14  \w     29.00  72.00   0.50    6.00    --  101.75 -61.00 -90.00   86
 15  \w     29.00  68.00   0.50    6.00    --  101.75 -61.00 150.00   78
 16  \w     29.00  56.00   0.50    6.00    --  101.75 -61.00 -30.00   54
 17  \w     37.00  70.00   0.50    6.00    --  101.75 -61.00   0.00   66
 18  \w     40.00  72.00   0.50    6.00    --  101.75 -61.00  60.00   64
 19  \w    144.00 171.00   0.50    6.00    --  101.75  15.00 120.00   54
 20  \w     36.00  71.00   0.50    6.00    --  101.75 -61.00-150.00   70
 21  \w     37.00  62.00   0.50    6.00    --  101.75 -77.00   0.00   50
 22  \w     71.00  98.00   0.50    6.00    --  101.75 -77.00   0.00   54
 23  \w   -120.00 -35.00   0.50    1.20    --  -46.48 -31.00-171.00  170
 24  \w    -31.00  26.00   0.50    1.20    --  -46.48  31.00 -11.00  114
 25  \w    -17.00  37.00   0.50    1.20    --   46.48 -31.00-171.00  108
 26  \w     44.00 101.00   0.50    1.20    --   46.48  31.00 -11.00  114
 27  \w    -13.00  20.00   0.50    1.20    --  -46.48  19.00 -30.00   66
 28  \w     25.00  90.00   0.50    1.20    --   46.48-125.00  60.00  130
;
_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      -0.0082157000
_diffrn_orient_matrix_UB_12      -0.0010124000
_diffrn_orient_matrix_UB_13      -0.0515834000
_diffrn_orient_matrix_UB_21      0.0409805000
_diffrn_orient_matrix_UB_22      -0.0418727000
_diffrn_orient_matrix_UB_23      0.0008646000
_diffrn_orient_matrix_UB_31      -0.0181747000
_diffrn_orient_matrix_UB_32      -0.0936825000
_diffrn_orient_matrix_UB_33      0.0001424000
_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  0.0601
_diffrn_reflns_av_unetI/netI     0.0496
_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       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            51251
_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         68.251
_diffrn_reflns_theta_min         2.615
_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    20.126
_exptl_absorpt_correction_T_max  0.469
_exptl_absorpt_correction_T_min  0.123
_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    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         14055
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1744P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2581
_refine_ls_wR_factor_ref         0.2769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8775
_reflns_number_total             14055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_1_24b
_cod_database_code               1571838
_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   0.500
_shelx_estimated_absorpt_t_min   0.108
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I502-Zn51 \\sim I302-Zn31
 with sigma of 0.02
 I501-Zn51 \\sim I301-Zn31
 with sigma of 0.02
 Zn51-N301 \\sim Zn31-N301
 with sigma of 0.02
 I502-I501 \\sim I302-I301
 with sigma of 0.04
 I502-N301 \\sim I302-N301
 with sigma of 0.04
 I501-N301 \\sim I301-N301
 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-N312 \\sim Zn43-N312
 with sigma of 0.02
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I306-N312 \\sim I406-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
 Zn52-N307 \\sim Zn52-N306
 with sigma of 0.02
 I503-Zn52 \\sim I403-Zn42
 with sigma of 0.02
 I504-Zn52 \\sim I304-Zn32
 with sigma of 0.02
3. Others
 1*[Sof(I302)+Sof(Zn31)+Sof(I301)]+1*[Sof(I502)+Sof(I501)+Sof(Zn51)]+1*
 [Sof(I401)+Sof(I402)+Sof(Zn41)]=1 with esd of 0.00001
 Sof(I302)=Sof(Zn31)=Sof(I301)=FVAR(1)
 Sof(I502)=Sof(I501)=Sof(Zn51)=FVAR(2)
 Sof(I401)=Sof(I402)=Sof(Zn41)=FVAR(3)
 Fixed Sof: I304(0.43038) I303(0.43038) I305(0.42064) I306(0.42064)
 Zn32(0.43038) Zn33(0.42064) I405(0.3262) Zn43(0.3262) I406(0.3262)
 I404(0.54285) I403(0.54285) Zn42(0.54285) I503(0.02679) I504(0.02679)
 Zn52(0.02679) I505(0.25317) I506(0.25317) Zn53(0.25317)
 Fixed Uiso: I502(0.08) I501(0.08) Zn51(0.08) I503(0.08) I504(0.08) Zn52(0.08)
 I401(0.08) I402(0.08) Zn41(0.08)
4.a Aromatic/amide H refined with riding coordinates:
 C320(H320), C319(H319), C329(H329), C328(H328), C314(H314), C305(H305),
 C315(H315), C323(H323), C304(H304), C301(H301), C310(H310), C322(H322),
 C311(H311), C312(H312), C318(H318), C302(H302), C317(H317), C331(H331),
 C332(H332), C313(H313), C335(H335), C336(H336), C333(H333), C330(H330)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88
_shelx_hkl_checksum              83757
_shelx_fab_checksum              9490
_olex2_date_sample_data_collection 2022-08-09
_olex2_date_sample_submission    2022-08-09
_olex2_submission_original_sample_id 50_1_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 3.252
_oxdiff_exptl_absorpt_empirical_full_min 0.331