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_1571846
_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, 0.259(C15 H16 O3)'
_chemical_formula_sum            'C39.88 H28.14 I6 N12 O0.78 Zn3'
_chemical_formula_weight         1645.46
_chemical_name_systematic
; (2',6'-dimethoxy-[1,1'-biphenyl]-2-yl)methanol 
(absorbed in crystalline sponge)
;
_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             2024-02-06
_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                 101.916(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.5084(12)
_cell_length_b                   14.9904(4)
_cell_length_c                   31.4216(16)
_cell_measurement_reflns_used    6986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.5100
_cell_measurement_theta_min      2.6110
_cell_volume                     15904.0(11)
_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 0.989
_diffrn_measured_fraction_theta_max 0.987
_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    -60.00 -33.00   0.50    3.99    -- -103.00  55.00 -25.00   54
  2  \w   -125.00 -97.00   0.50    3.99    -- -103.00 -55.00-168.00   56
  3  \w   -154.00-129.00   0.50    3.99    -- -103.00 -55.00-168.00   50
  4  \w    -96.00 -59.00   0.50    3.99    -- -103.00 125.00-150.00   74
  5  \w    -68.00 -31.00   0.50    3.99    -- -103.00  61.00 -60.00   74
  6  \w    -56.00 -31.00   0.50    3.99    -- -103.00  61.00-180.00   50
  7  \w    -62.00 -34.00   0.50    3.99    -- -103.00  61.00   0.00   56
  8  \w     30.00  65.00   0.50    3.99    --  101.75 -55.00-168.00   70
  9  \w    106.00 131.00   0.50    3.99    --  101.75  55.00 -25.00   50
 10  \w     90.00 173.00   0.50    3.99    --  101.75  30.00-150.00  166
 11  \w     89.00 116.00   0.50    3.99    --  101.75  45.00 -90.00   54
 12  \w     45.00  73.00   0.50    3.99    --  101.75 -61.00   0.00   56
 13  \w     39.00  71.00   0.50    3.99    --  101.75 -61.00 -60.00   64
 14  \w     38.00 107.00   0.50    3.99    --  101.75 -77.00 120.00  138
 15  \w    119.00 175.00   0.50    3.99    --  101.75  61.00-120.00  112
 16  \w     30.00  67.00   0.50    3.99    --  101.75 -77.00   0.00   74
 17  \w     72.00  98.00   0.50    3.99    --  101.75 -77.00   0.00   52
 18  \w     96.00 138.00   0.50    3.99    --  101.75  61.00  60.00   84
 19  \w    120.00 169.00   0.50    3.99    --  101.75  45.00 -90.00   98
 20  \w    -33.00  25.00   0.50    1.00    --  -46.48  55.00 -25.00  116
 21  \w   -106.00 -80.00   0.50    1.00    --  -46.48 -55.00-168.00   52
 22  \w    -77.00 -41.00   0.50    1.00    --  -46.48 -55.00-168.00   72
 23  \w    -25.00  37.00   0.50    1.00    --   46.48 -55.00-168.00  124
 24  \w    -27.00  26.00   0.50    1.00    --   46.48 -19.00  30.00  106
 25  \w     35.00 118.00   0.50    1.00    --   46.48  55.00 -25.00  166
;
_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      0.0064841000
_diffrn_orient_matrix_UB_12      0.0078436000
_diffrn_orient_matrix_UB_13      0.0499253000
_diffrn_orient_matrix_UB_21      0.0335272000
_diffrn_orient_matrix_UB_22      0.0677162000
_diffrn_orient_matrix_UB_23      -0.0000688000
_diffrn_orient_matrix_UB_31      -0.0302166000
_diffrn_orient_matrix_UB_32      0.0768135000
_diffrn_orient_matrix_UB_33      -0.0050438000
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            49830
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.246
_diffrn_reflns_theta_min         2.617
_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    19.567
_exptl_absorpt_correction_T_max  0.436
_exptl_absorpt_correction_T_min  0.135
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       block
_exptl_crystal_F_000             6125
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.107
_refine_diff_density_min         -1.184
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         14369
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.1258
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1997P)^2^+231.4372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3841
_refine_ls_wR_factor_ref         0.4060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9492
_reflns_number_total             14369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_5_24a
_cod_database_code               1571846
_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   0.441
_shelx_estimated_absorpt_t_min   0.105
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C2A-C1A = C2A-C3A = C4A-C3A = C4A-C5A = C5A-C6A = C1A-C6A
 1.39 with sigma of 0.02
 C8A-C7A = C8A-C9A = C10A-C9A = C11A-C10A = C12A-C11A = C12A-C7A
 1.39 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 O1A-C13A = O2A-C14A = O3A-C15A
 1.43 with sigma of 0.02
 O2A-C8A = O3A-C12A
 1.37 with sigma of 0.02
 C1A-C3A = C2A-C4A = C3A-C5A = C4A-C6A = C5A-C1A = C6A-C2A
 2.4 with sigma of 0.04
 C7A-C9A = C8A-C10A = C9A-C11A = C10A-C12A = C11A-C7A = C12A-C8A
 2.4 with sigma of 0.04
 C12A-C15A
 2.4 with sigma of 0.02
 C8A-C14A
 2.4 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 C8A-C4A \\sim C4A-C12A
 with sigma of 0.04
 C5A-C7A \\sim C7A-C3A
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 Zn33-N306 \\sim Zn43-N306
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 I305-N306 \\sim I405-N306
 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
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 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
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 N311-C332 \\sim N311-C432
 with sigma of 0.02
 C334-C333 \\sim C334-C433
 with sigma of 0.02
 C332-C333 \\sim C432-C433
 with sigma of 0.02
 N311-C333 \\sim N311-C433
 with sigma of 0.04
 C334-C332 \\sim C334-C432
 with sigma of 0.04
 Zn53-N306 \\sim Zn53-N307
 with sigma of 0.02
3. Restrained planarity
 C10A, C8A, C7A, C11A, C9A, C12A
 with sigma of 0.1
 O3A, C12A, C7A, C8A, O2A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C8A \\sim O2A \\sim C14A \\sim C7A \\sim C9A \\sim C4A \\sim C12A \\sim C10A
\\sim C3A \\sim C5A \\sim O3A \\sim C11A \\sim C2A \\sim C6A \\sim C13A \\sim
C15A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C305 \\sim C304 \\sim C303 \\sim C302 \\sim C301: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn42) = Uanis(Zn52)
Uanis(C432) = Uanis(C332) = Uanis(C333) = Uanis(C433)
5. Rigid body (RIGU) restrains
 C8A, O2A, C14A, C7A, C9A, C4A, C12A, C10A, C3A, C5A, O3A, C11A, C2A, C6A,
 C13A, C15A, C1A, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: I301(0.50842) I302(0.50842) I303(0.48625) I304(0.48625)
 I306(0.53396) I305(0.53396) Zn31(0.50842) Zn32(0.48625) Zn33(0.53396)
 C332(0.55065) H332(0.55065) C333(0.55065) H333(0.55065) Zn43(0.41938)
 I406(0.41938) I405(0.41938) I403(0.3085) Zn42(0.3085) I404(0.3085)
 I401(0.45006) Zn41(0.45006) I402(0.45006) I503(0.20525) Zn52(0.20525)
 I504(0.20525) C433(0.44935) H433(0.44935) C432(0.44935) H432(0.44935)
 O2A(0.25902) O3A(0.25902) C7A(0.25902) C4A(0.25902) C12A(0.25902) C8A(0.25902)
 C9A(0.25902) H9A(0.25902) C3A(0.25902) H3A(0.25902) C14A(0.25902)
 H14A(0.25902) H14B(0.25902) H14C(0.25902) C11A(0.25902) H11A(0.25902)
 C5A(0.25902) C15A(0.25902) H15A(0.25902) H15B(0.25902) H15C(0.25902)
 C2A(0.25902) H2A(0.25902) C6A(0.25902) H6A(0.25902) C1A(0.25902) H1A(0.25902)
 C10A(0.25902) H10A(0.25902) O1A(0.25902) H1AA(0.25902) C13A(0.25902)
 H13A(0.25902) H13B(0.25902) I505(0.04665) I506(0.04665) Zn53(0.04665)
 I502(0.04152) I501(0.04152) Zn51(0.04152)
 Fixed Uiso: I505(0.08) I506(0.08) Zn53(0.08) I502(0.08) I501(0.08) Zn51(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B)
7.b Aromatic/amide H refined with riding coordinates:
 C302(H302), C331(H331), C335(H335), C317(H317), C318(H318), C311(H311),
 C310(H310), C312(H312), C313(H313), C330(H330), C301(H301), C315(H315),
 C336(H336), C304(H304), C305(H305), C328(H328), C314(H314), C329(H329),
 C332(H332), C333(H333), C323(H323), C322(H322), C320(H320), C319(H319),
 C433(H433), C432(H432), C9A(H9A), C3A(H3A), C11A(H11A), C2A(H2A), C6A(H6A),
 C1A(H1A), C10A(H10A)
7.c Fitted hexagon refined as free rotating group:
 N307(C323,C322,C321,C320,C319)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1AA)
7.e Idealised Me refined with everything fixed:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C)
;
_shelx_res_checksum              35616
_shelx_hkl_checksum              71418
_olex2_date_sample_data_collection 2022-03-15
_olex2_date_sample_submission    2022-03-15
_olex2_submission_original_sample_id 25_5_24a
_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 4.403
_oxdiff_exptl_absorpt_empirical_full_min 0.273