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_1571830
_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         'C37.024 H26.049 I6 N12 Zn3, 0.23(C6 H12)'
_chemical_formula_sum            'C38.4 H28.81 I6 N12 Zn3'
_chemical_formula_weight         1615.89
_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             2024-02-01
_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                 100.291(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.3373(11)
_cell_length_b                   15.0894(3)
_cell_length_c                   29.5872(11)
_cell_measurement_reflns_used    8602
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.8820
_cell_measurement_theta_min      2.6200
_cell_volume                     15083.4(8)
_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_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 Arc-100'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_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   -127.00 -91.00   0.50    4.04    -- -103.00 -40.00-169.00   72
  2  \w    -69.00 -37.00   0.50    4.04    -- -103.00  61.00 120.00   64
  3  \w    -69.00 -32.00   0.50    4.04    -- -103.00  61.00  90.00   74
  4  \w    -67.00 -36.00   0.50    4.04    -- -103.00  61.00 -30.00   62
  5  \w    -67.00 -35.00   0.50    4.04    -- -103.00  61.00 -90.00   64
  6  \w     92.00 161.00   0.50    4.04    --  101.75  40.00 -15.00  138
  7  \w     65.00 106.00   0.50    4.04    --  101.75 -94.00  30.00   82
  8  \w     33.00  67.00   0.50    4.04    --  101.75 -61.00 -30.00   68
  9  \w     29.00  54.00   0.50    4.04    --  101.75 -61.00  30.00   50
 10  \w     30.00  73.00   0.50    4.04    --  101.75 -61.00-180.00   86
 11  \w     74.00  99.00   0.50    4.04    --  101.75 -94.00 -90.00   50
 12  \w     37.00  69.00   0.50    4.04    --  101.75 -77.00-180.00   64
 13  \w     72.00 101.00   0.50    4.04    --  101.75 -77.00-180.00   58
 14  \w     38.00  64.00   0.50    4.04    --  101.75 -61.00  90.00   52
 15  \w     89.00 171.00   0.50    4.04    --  101.75  15.00 -60.00  164
 16  \w     39.00  73.00   0.50    4.04    --  101.75 -61.00-120.00   68
 17  \w     63.00  89.00   0.50    4.04    --  101.75 -77.00 -60.00   52
 18  \w     29.00  65.00   0.50    4.04    --  101.75 -61.00   0.00   72
 19  \w     30.00  56.00   0.50    4.04    --  101.75 -94.00  30.00   52
 20  \w    -15.00  14.00   0.50    1.01    --  -46.26  40.00 -15.00   58
 21  \w   -113.00 -41.00   0.50    1.01    --  -46.26 -40.00-169.00  144
 22  \w     35.00 114.00   0.50    1.01    --   46.26  40.00 -15.00  158
 23  \w      5.00  31.00   0.50    1.01    --   46.26 -40.00-169.00   52
 24  \w    -22.00  17.00   0.50    1.01    --  -46.26  19.00 120.00   78
 25  \w    -23.00  28.00   0.50    1.01    --  -46.26  19.00 -30.00  102
 26  \w    -26.00   0.00   0.50    1.01    --   46.26 -19.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details
'Rigaku Oxford Difffraction, 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      0.0012364000
_diffrn_orient_matrix_UB_12      -0.0023104000
_diffrn_orient_matrix_UB_13      0.0523334000
_diffrn_orient_matrix_UB_21      -0.0393756000
_diffrn_orient_matrix_UB_22      -0.0512791000
_diffrn_orient_matrix_UB_23      -0.0075159000
_diffrn_orient_matrix_UB_31      0.0229140000
_diffrn_orient_matrix_UB_32      -0.0882182000
_diffrn_orient_matrix_UB_33      0.0029773000
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_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            44524
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_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    20.612
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_T_min  0.149
_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    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             6010
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.492
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         13605
_refine_ls_number_restraints     251
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0746
_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^)+(0.1664P)^2^+23.4188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2339
_refine_ls_wR_factor_ref         0.2527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9808
_reflns_number_total             13605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_5_48c
_cod_original_formula_sum        'C38.40 H28.81 I6 N12 Zn3'
_cod_database_code               1571830
_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   0.371
_shelx_estimated_absorpt_t_min   0.098
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C801-C806 = C801-C802 = C806-C805 = C805-C804 = C804-C803 = C803-C802
 1.54 with sigma of 0.02
 C809-C808 = C809-C810 = C808-C807 = C807-C812 = C812-C811 = C811-C810
 1.54 with sigma of 0.02
 C801-C805 = C801-C803 = C806-C804 = C805-C803 = C804-C802
 2.54 with sigma of 0.04
 C809-C807 = C809-C811 = C808-C812 = C807-C811 = C812-C810
 2.54 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
 C801-C806 \\sim C806-C805 \\sim C805-C804 \\sim C804-C803 \\sim C803-C802
\\sim C802-C801
 with sigma of 0.02
 I302-I301 \\sim I402-I401
 with sigma of 0.04
 C801-C803 \\sim C805-C803 \\sim C806-C802 \\sim C806-C804 \\sim C804-C802
\\sim C801-C805
 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
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 Zn43-N306 \\sim Zn33-N306
 with sigma of 0.02
 Zn43-N307 \\sim Zn33-N307
 with sigma of 0.02
 I406-I405 \\sim I306-I305
 with sigma of 0.04
 I406-N306 \\sim I306-N306
 with sigma of 0.04
 I406-N307 \\sim I306-N307
 with sigma of 0.04
 I405-N306 \\sim I305-N306
 with sigma of 0.04
 I405-N307 \\sim I305-N307
 with sigma of 0.04
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 Zn32-N305 \\sim Zn42-N305
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I303-N305 \\sim I403-N305
 with sigma of 0.04
 I304-N305 \\sim I404-N305
 with sigma of 0.04
 I503-Zn52 \\sim I504-Zn52
 with sigma of 0.02
 Zn32-N305 \\sim Zn52-N305
 with sigma of 0.02
 C809-C808 \\sim C808-C807 \\sim C807-C812 \\sim C812-C811 \\sim C811-C810
\\sim C810-C809
 with sigma of 0.02
 C809-C811 \\sim C807-C811 \\sim C808-C810 \\sim C808-C812 \\sim C812-C810
\\sim C809-C807
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C801 \\sim C806 \\sim C805 \\sim C804 \\sim C803 \\sim C802: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C809 \\sim C808 \\sim C807 \\sim C812 \\sim C811 \\sim C810: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C801, C806, C805, C804, C803, C802
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C809, C808, C807, C812, C811, C810
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(I406)+Sof(I405)+Sof(Zn43)]+1*[Sof(I306)+Sof(Zn33)+Sof(I305)]+1*
 [Sof(I505)+Sof(I506)+Sof(Zn53)]=1 with esd of 0.00001
 Sof(I406)=Sof(I405)=Sof(Zn43)=FVAR(1)
 Sof(I306)=Sof(Zn33)=Sof(I305)=FVAR(2)
 Sof(I505)=Sof(I506)=Sof(Zn53)=FVAR(3)
 Fixed Sof: I303(0.57364) I304(0.57364) I302(0.53776) Zn32(0.57364)
 I301(0.53776) Zn31(0.53776) I402(0.40707) Zn41(0.40707) I401(0.40707)
 I502(0.05514) I501(0.05514) Zn51(0.05514) Zn42(0.37043) I403(0.37043)
 I404(0.37043) I503(0.05595) I504(0.05595) Zn52(0.05595) C809(0.17074)
 H80A(0.17074) H80B(0.17074) C808(0.17074) H80C(0.17074) H80D(0.17074)
 C807(0.17074) H80E(0.17074) H80F(0.17074) C812(0.17074) H81A(0.17074)
 H81B(0.17074) C811(0.17074) H81C(0.17074) H81D(0.17074) C810(0.17074)
 H81E(0.17074) H81F(0.17074) C801(0.22982) H80G(0.22982) H80H(0.22982)
 C806(0.22982) H80I(0.22982) H80J(0.22982) C805(0.22982) H80K(0.22982)
 H80L(0.22982) C804(0.22982) H80M(0.22982) H80N(0.22982) C803(0.22982)
 H80P(0.22982) H80O(0.22982) C802(0.22982) H80Q(0.22982) H80R(0.22982)
 Fixed Uiso: I502(0.08) I501(0.08) Zn51(0.08) I505(0.08) I506(0.08) Zn53(0.08)
 I503(0.08) I504(0.08) Zn52(0.08)
6.a Secondary CH2 refined with riding coordinates:
 C809(H80A,H80B), C808(H80C,H80D), C807(H80E,H80F), C812(H81A,H81B), C811(H81C,
 H81D), C810(H81E,H81F), C801(H80G,H80H), C806(H80I,H80J), C805(H80K,H80L),
 C804(H80M,H80N), C803(H80P,H80O), C802(H80Q,H80R)
6.b Aromatic/amide H refined with riding coordinates:
 C335(H335), C336(H336), C333(H333), C311(H311), C310(H310), C331(H331),
 C332(H332), C304(H304), C330(H330), C315(H315), C302(H302), C305(H305),
 C301(H301), C328(H328), C320(H320), C322(H322), C313(H313), C314(H314),
 C319(H319), C323(H323), C312(H312), C318(H318), C317(H317), C329(H329)
;
_shelx_res_checksum              96246
_shelx_hkl_checksum              26324
_olex2_submission_original_sample_id 4_5_48c
_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 3.392
_oxdiff_exptl_absorpt_empirical_full_min 0.405