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_1571820
_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, 1.727(C6 H12)'
_chemical_formula_sum            'C46.36 H44.73 I6 N12 Zn3'
_chemical_formula_weight         1727.54
_chemical_name_systematic
; catena-[bis(mu-2,4,6-tri(pyridin-4-yl)-1,3,5-triazine)-hexaiodo-tri-zinc 
cyclohexane solvate
;
_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             2024-01-31
_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                 100.420(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.3474(9)
_cell_length_b                   15.1342(3)
_cell_length_c                   29.5974(9)
_cell_measurement_reflns_used    8256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.4780
_cell_measurement_theta_min      2.6830
_cell_volume                     15131.6(7)
_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 0.992
_diffrn_measured_fraction_theta_max 0.991
_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   -144.00-101.00   0.50    1.60    -- -103.00 -29.00 178.00   86
  2  \w    -69.00 -44.00   0.50    1.60    -- -103.00  61.00-180.00   50
  3  \w    -68.00 -37.00   0.50    1.60    -- -103.00  61.00 -90.00   62
  4  \w    -56.00 -31.00   0.50    1.60    -- -103.00  61.00-120.00   50
  5  \w    -63.00 -35.00   0.50    1.60    -- -103.00 125.00   0.00   56
  6  \w   -106.00 -79.00   0.50    1.60    -- -103.00 125.00   0.00   54
  7  \w    -72.00 -46.00   0.50    1.60    -- -103.00  77.00 -60.00   52
  8  \w    -61.00 -36.00   0.50    1.60    -- -103.00  61.00 -30.00   50
  9  \w    -68.00 -43.00   0.50    1.60    -- -103.00  61.00  90.00   50
 10  \w   -104.00 -34.00   0.50    1.60    -- -103.00  77.00 150.00  140
 11  \w     89.00 149.00   0.50    1.60    --  101.75  29.00 -20.00  120
 12  \w     30.00  70.00   0.50    1.60    --  101.75 -61.00 -90.00   80
 13  \w     37.00  72.00   0.50    1.60    --  101.75 -61.00  30.00   70
 14  \w     29.00  67.00   0.50    1.60    --  101.75 -61.00  90.00   76
 15  \w     34.00  68.00   0.50    1.60    --  101.75 -61.00-120.00   68
 16  \w     30.00  73.00   0.50    1.60    --  101.75 -61.00  60.00   86
 17  \w     29.00  64.00   0.50    1.60    --  101.75 -61.00 -30.00   70
 18  \w     37.00  63.00   0.50    1.60    --  101.75 -61.00   0.00   52
 19  \w     32.00  73.00   0.50    1.60    --  101.75 -61.00 150.00   82
 20  \w     31.00  72.00   0.50    1.60    --  101.75 -61.00-150.00   82
 21  \w    -10.00  17.00   0.50    0.40    --  -46.61  29.00 -20.00   54
 22  \w    -90.00 -44.00   0.50    0.40    --  -46.61 -29.00 178.00   92
 23  \w     34.00 121.00   0.50    0.40    --   46.61  29.00 -20.00  174
 24  \w    -25.00  21.00   0.50    0.40    --   46.61 -29.00 178.00   92
 25  \w    -12.00  13.00   0.50    0.40    --  -46.61  19.00 150.00   50
 26  \w     -4.00  29.00   0.50    0.40    --  -46.61  19.00-120.00   66
 27  \w    -23.00  27.00   0.50    0.40    --   46.61 -19.00  30.00  100
;
_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      -0.0088827000
_diffrn_orient_matrix_UB_12      -0.0075407000
_diffrn_orient_matrix_UB_13      -0.0527630000
_diffrn_orient_matrix_UB_21      0.0417848000
_diffrn_orient_matrix_UB_22      -0.0378844000
_diffrn_orient_matrix_UB_23      0.0007581000
_diffrn_orient_matrix_UB_31      -0.0160312000
_diffrn_orient_matrix_UB_32      -0.0941447000
_diffrn_orient_matrix_UB_33      0.0039385000
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            48974
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_min         2.616
_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    20.584
_exptl_absorpt_correction_T_max  0.426
_exptl_absorpt_correction_T_min  0.132
_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    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             6519
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.378
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         13719
_refine_ls_number_restraints     586
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0641
_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^)+(0.1156P)^2^+78.6523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10910
_reflns_number_total             13719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_1_24b
_cod_database_code               1571820
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 H12 N24 C36) (C15 H16 O3) (C6 H12)3'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.426
_shelx_estimated_absorpt_t_min   0.093
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C829-C830 = C829-C828 = C830-C825 = C825-C826 = C826-C827 = C827-C828
 1.54 with sigma of 0.02
 C808-C809 = C808-C807 = C809-C810 = C810-C811 = C811-C812 = C812-C807
 1.54 with sigma of 0.02
 C806-C805 = C806-C801 = C805-C804 = C804-C803 = C803-C802 = C802-C801
 1.54 with sigma of 0.02
 C819-C824 = C819-C820 = C824-C823 = C823-C822 = C822-C821 = C821-C820
 1.54 with sigma of 0.02
 C813-C818 = C813-C814 = C818-C817 = C817-C816 = C816-C815 = C815-C814
 1.54 with sigma of 0.02
 C829-C825 = C829-C827 = C830-C826 = C825-C827 = C826-C828
 2.54 with sigma of 0.04
 C808-C810 = C808-C812 = C809-C811 = C810-C812 = C811-C807
 2.54 with sigma of 0.04
 C806-C804 = C806-C802 = C805-C803 = C804-C802 = C803-C801
 2.54 with sigma of 0.04
 C819-C823 = C819-C821 = C824-C822 = C823-C821 = C822-C820
 2.54 with sigma of 0.04
 C813-C817 = C813-C815 = C818-C816 = C817-C815 = C816-C814
 2.54 with sigma of 0.04
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 C829-C830 \\sim C830-C825 \\sim C825-C826 \\sim C826-C827 \\sim C827-C828
\\sim C828-C829
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 C829-C827 \\sim C825-C827 \\sim C830-C828 \\sim C830-C826 \\sim C826-C828
\\sim C829-C825
 with sigma of 0.04
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 I301-I302 \\sim I401-I402
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 Zn33-N312 \\sim Zn43-N312
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I304-N307 \\sim I404-N307
 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
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 C808-C809 \\sim C809-C810 \\sim C810-C811 \\sim C811-C812 \\sim C812-C807
\\sim C807-C808
 with sigma of 0.02
 C808-C812 \\sim C810-C812 \\sim C809-C807 \\sim C809-C811 \\sim C811-C807
\\sim C808-C810
 with sigma of 0.04
 C806-C805 \\sim C805-C804 \\sim C804-C803 \\sim C803-C802 \\sim C802-C801
\\sim C801-C806
 with sigma of 0.02
 C806-C802 \\sim C804-C802 \\sim C805-C801 \\sim C805-C803 \\sim C803-C801
\\sim C806-C804
 with sigma of 0.04
 C819-C824 \\sim C824-C823 \\sim C823-C822 \\sim C822-C821 \\sim C821-C820
\\sim C820-C819
 with sigma of 0.02
 C819-C821 \\sim C823-C821 \\sim C824-C820 \\sim C824-C822 \\sim C822-C820
\\sim C819-C823
 with sigma of 0.04
 C813-C818 \\sim C818-C817 \\sim C817-C816 \\sim C816-C815 \\sim C815-C814
\\sim C814-C813
 with sigma of 0.02
 C813-C815 \\sim C817-C815 \\sim C818-C814 \\sim C818-C816 \\sim C816-C814
\\sim C813-C817
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C829 \\sim C830 \\sim C825 \\sim C826 \\sim C827 \\sim C828: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C808 \\sim C809 \\sim C810 \\sim C811 \\sim C812 \\sim C807: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C806 \\sim C805 \\sim C804 \\sim C803 \\sim C802 \\sim C801: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C819 \\sim C824 \\sim C823 \\sim C822 \\sim C821 \\sim C820: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C813 \\sim C818 \\sim C817 \\sim C816 \\sim C815 \\sim C814: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C829, C830, C825, C826, C827, C828
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C808, C809, C810, C811, C812, C807
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C806, C805, C804, C803, C802, C801
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C819, C824, C823, C822, C821, C820
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C813, C818, C817, C816, C815, C814
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: I303(0.57301) I304(0.57301) I305(0.59909) I306(0.59909)
 Zn32(0.57301) I301(0.41539) I302(0.41539) Zn33(0.59909) Zn31(0.41539)
 I402(0.53797) Zn41(0.53797) I401(0.53797) I405(0.37368) Zn43(0.37368)
 I406(0.37368) I502(0.04661) I501(0.04661) Zn51(0.04661) I505(0.02724)
 Zn53(0.02724) I506(0.02724) I404(0.42699) Zn42(0.42699) I403(0.42699)
 C808(0.35875) H80A(0.35875) H80B(0.35875) C809(0.35875) H80C(0.35875)
 H80D(0.35875) C810(0.35875) H81A(0.35875) H81B(0.35875) C811(0.35875)
 H81C(0.35875) H81D(0.35875) C812(0.35875) H81E(0.35875) H81F(0.35875)
 C807(0.35875) H80E(0.35875) H80F(0.35875) C806(0.37602) H80G(0.37602)
 H80H(0.37602) C805(0.37602) H80I(0.37602) H80J(0.37602) C804(0.37602)
 H80K(0.37602) H80L(0.37602) C803(0.37602) H80M(0.37602) H80N(0.37602)
 C802(0.37602) H80O(0.37602) H80P(0.37602) C801(0.37602) H80Q(0.37602)
 H80R(0.37602) C832(0.32563) H83C(0.32563) H83D(0.32563) C831(0.32563)
 H83E(0.32563) H83F(0.32563) C833(0.32563) H83G(0.32563) H83H(0.32563)
 C819(0.30334) H81G(0.30334) H81H(0.30334) C824(0.30334) H82A(0.30334)
 H82B(0.30334) C823(0.30334) H82C(0.30334) H82D(0.30334) C822(0.30334)
 H82E(0.30334) H82F(0.30334) C821(0.30334) H82G(0.30334) H82H(0.30334)
 C820(0.30334) H82I(0.30334) H82J(0.30334) C813(0.25808) H81I(0.25808)
 H81J(0.25808) C818(0.25808) H81K(0.25808) H81L(0.25808) C817(0.25808)
 H81M(0.25808) H81N(0.25808) C816(0.25808) H81O(0.25808) H81P(0.25808)
 C815(0.25808) H81Q(0.25808) H81R(0.25808) C814(0.25808) H81S(0.25808)
 H81T(0.25808) C829(0.2682) H82K(0.2682) H82L(0.2682) C830(0.2682) H83A(0.2682)
 H83B(0.2682) C825(0.2682) H82M(0.2682) H82N(0.2682) C826(0.2682) H82O(0.2682)
 H82P(0.2682) C827(0.2682) H82Q(0.2682) H82R(0.2682) C828(0.2682) H82S(0.2682)
 H82T(0.2682)
 Fixed Uiso: I502(0.08) I501(0.08) Zn51(0.08) I505(0.08) Zn53(0.08) I506(0.08)
6.a Secondary CH2 refined with riding coordinates:
 C808(H80A,H80B), C809(H80C,H80D), C810(H81A,H81B), C811(H81C,H81D), C812(H81E,
 H81F), C807(H80E,H80F), C806(H80G,H80H), C805(H80I,H80J), C804(H80K,H80L),
 C803(H80M,H80N), C802(H80O,H80P), C801(H80Q,H80R), C832(H83C,H83D), C831(H83E,
 H83F), C833(H83G,H83H), C819(H81G,H81H), C824(H82A,H82B), C823(H82C,H82D),
 C822(H82E,H82F), C821(H82G,H82H), C820(H82I,H82J), C813(H81I,H81J), C818(H81K,
 H81L), C817(H81M,H81N), C816(H81O,H81P), C815(H81Q,H81R), C814(H81S,H81T),
 C829(H82K,H82L), C830(H83A,H83B), C825(H82M,H82N), C826(H82O,H82P), C827(H82Q,
 H82R), C828(H82S,H82T)
6.b Aromatic/amide H refined with riding coordinates:
 C317(H317), C318(H318), C313(H313), C315(H315), C335(H335), C314(H314),
 C312(H312), C322(H322), C323(H323), C336(H336), C333(H333), C311(H311),
 C331(H331), C332(H332), C330(H330), C320(H320), C304(H304), C319(H319),
 C310(H310), C328(H328), C305(H305), C329(H329), C301(H301), C302(H302)
;
_shelx_res_checksum              46971
_shelx_hkl_checksum              24464
_olex2_date_sample_data_collection 2022-07-28
_olex2_date_sample_submission    2022-07-28
_olex2_submission_original_sample_id 4_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 0.592