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_1571841
_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
; (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             2024-01-26
_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                 101.242(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.458(2)
_cell_length_b                   15.0078(4)
_cell_length_c                   30.486(3)
_cell_measurement_reflns_used    6447
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.3910
_cell_measurement_theta_min      2.9470
_cell_volume                     15463.0(19)
_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 0.994
_diffrn_measured_fraction_theta_max 0.993
_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    -61.00 -35.00   0.50    5.00    -- -103.00  56.00 164.00   52
  2  \w   -157.00 -89.00   0.50    5.00    -- -103.00 -56.00  22.00  136
  3  \w    -63.00 -36.00   0.50    5.00    -- -103.00  61.00 -60.00   54
  4  \w    -59.00 -30.00   0.50    5.00    -- -103.00  61.00 -30.00   58
  5  \w   -104.00 -39.00   0.50    5.00    -- -103.00  77.00 -90.00  130
  6  \w    -56.00 -31.00   0.50    5.00    -- -103.00  61.00-180.00   50
  7  \w    -59.00 -30.00   0.50    5.00    -- -103.00  61.00-150.00   58
  8  \w    -68.00 -37.00   0.50    5.00    -- -103.00  61.00  30.00   62
  9  \w   -173.00 -99.00   0.50    5.00    -- -103.00 -61.00  90.00  148
 10  \w   -100.00 -35.00   0.50    5.00    -- -103.00  77.00 120.00  130
 11  \w   -172.00 -86.00   0.50    5.00    -- -103.00 -77.00 120.00  172
 12  \w    -83.00 -57.00   0.50    5.00    -- -103.00  77.00  30.00   52
 13  \w    -57.00 -32.00   0.50    5.00    -- -103.00  61.00   0.00   50
 14  \w    147.00 172.00   0.50    5.00    --  101.75  56.00 164.00   50
 15  \w     29.00  65.00   0.50    5.00    --  101.75 -56.00  22.00   72
 16  \w     29.00  73.00   0.50    5.00    --  101.75 -61.00 120.00   88
 17  \w     41.00  66.00   0.50    5.00    --  101.75 -94.00  30.00   50
 18  \w     30.00  73.00   0.50    5.00    --  101.75 -61.00 150.00   86
 19  \w    119.00 164.00   0.50    5.00    --  101.75  45.00  90.00   90
 20  \w    -11.00  26.00   0.50    0.75    --  -46.36  56.00 164.00   74
 21  \w    -88.00 -62.00   0.50    0.75    --  -46.36 -56.00  22.00   52
 22  \w    -25.00  32.00   0.50    0.75    --   46.36 -56.00  22.00  114
 23  \w     36.00 119.00   0.50    0.75    --   46.36  56.00 164.00  166
 24  \w    -24.00  22.00   0.50    0.75    --  -46.36  19.00 -30.00   92
 25  \w    -19.00  28.00   0.50    0.75    --  -46.36  19.00 150.00   94
 26  \w     -9.00  17.00   0.50    0.75    --  -46.36  19.00 120.00   52
;
_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      0.0158043000
_diffrn_orient_matrix_UB_12      0.0047170000
_diffrn_orient_matrix_UB_13      0.0507569000
_diffrn_orient_matrix_UB_21      0.0320466000
_diffrn_orient_matrix_UB_22      -0.0692052000
_diffrn_orient_matrix_UB_23      -0.0044257000
_diffrn_orient_matrix_UB_31      0.0283725000
_diffrn_orient_matrix_UB_32      0.0756343000
_diffrn_orient_matrix_UB_33      -0.0071912000
_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  0.0553
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            51956
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_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    20.094
_exptl_absorpt_correction_T_max  0.412
_exptl_absorpt_correction_T_min  0.105
_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    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         14069
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1819P)^2^+28.0903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2952
_refine_ls_wR_factor_ref         0.3206
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8590
_reflns_number_total             14069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_1_48b
_cod_original_cell_volume        15463.2(18)
_cod_database_code               1571841
_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   0.433
_shelx_estimated_absorpt_t_min   0.123
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 I405-I406 \\sim I305-I306
 with sigma of 0.04
 I303-N306 \\sim I403-N306
 with sigma of 0.04
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I304-N00W \\sim I404-N00W
 with sigma of 0.04
 I303-C323 \\sim I403-C323
 with sigma of 0.04
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-C323 \\sim I404-C323
 with sigma of 0.04
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 Zn32-N00W \\sim Zn42-N00W
 with sigma of 0.02
 Zn32-C323 \\sim Zn42-C323
 with sigma of 0.02
 I303-N00W \\sim I403-N00W
 with sigma of 0.04
 I304-I303 \\sim I404-I403
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I402-I401 \\sim I302-I301
 with sigma of 0.04
 I402-N301 \\sim I302-N301
 with sigma of 0.04
 Zn41-N301 \\sim Zn31-N301
 with sigma of 0.02
 I402-Zn41 \\sim I302-Zn31
 with sigma of 0.02
 I401-N301 \\sim I301-N301
 with sigma of 0.04
 I401-Zn41 \\sim I301-Zn31
 with sigma of 0.02
 C334-C333 \\sim C334-C433
 with sigma of 0.02
 C333-C332 \\sim C433-C432
 with sigma of 0.02
 N312-C332 \\sim N312-C432
 with sigma of 0.02
 C334-C332 \\sim C334-C432
 with sigma of 0.04
 C333-N312 \\sim C433-N312
 with sigma of 0.04
 N301-C305 \\sim N301-C405
 with sigma of 0.02
 C303-C304 \\sim C303-C404
 with sigma of 0.02
 C304-C305 \\sim C404-C405
 with sigma of 0.02
 N301-C304 \\sim N301-C404
 with sigma of 0.04
 C303-C305 \\sim C303-C405
 with sigma of 0.04
 Zn32-N00W \\sim Zn32-N307
 with sigma of 0.02
 N00W-C323 \\sim N307-C423
 with sigma of 0.02
 N00W-C419 \\sim N307-C319
 with sigma of 0.02
 N00W-Zn42 \\sim N307-Zn42
 with sigma of 0.02
 C321-C422 \\sim C321-C322
 with sigma of 0.02
 C321-C420 \\sim C321-C320
 with sigma of 0.02
 C323-C422 \\sim C423-C322
 with sigma of 0.02
 C420-C419 \\sim C320-C319
 with sigma of 0.02
 Zn32-C323 \\sim Zn32-C423
 with sigma of 0.04
 Zn32-C419 \\sim Zn32-C319
 with sigma of 0.04
 N00W-C422 \\sim N307-C322
 with sigma of 0.04
 N00W-C420 \\sim N307-C320
 with sigma of 0.04
 C321-C323 \\sim C321-C423
 with sigma of 0.04
 C321-C419 \\sim C321-C319
 with sigma of 0.04
 C323-C419 \\sim C423-C319
 with sigma of 0.04
 C323-Zn42 \\sim C423-Zn42
 with sigma of 0.04
 C419-Zn42 \\sim C319-Zn42
 with sigma of 0.04
 I502-Zn51 \\sim I501-Zn51
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C432) = Uanis(C332) = Uanis(C333) = Uanis(C433)
Uanis(C302) = Uanis(C301) = Uanis(C304) = Uanis(C305) = Uanis(C404) =
Uanis(C405)
Uanis(C305) = Uanis(C405) = Uanis(C304) = Uanis(C404) = Uanis(C301) =
Uanis(C302)
Uanis(N00W) = Uanis(C323) = Uanis(C422) = Uanis(C420) = Uanis(C419) =
Uanis(N307) = Uanis(C319) = Uanis(C320) = Uanis(C423) = Uanis(C322)
4. Others
 Sof(I305)=Sof(Zn33)=Sof(I306)=1-FVAR(1)
 Sof(I405)=Sof(I406)=Sof(Zn43)=FVAR(1)
 Sof(I404)=Sof(Zn42)=Sof(I403)=1-FVAR(2)
 Sof(I304)=Sof(I303)=Sof(Zn32)=FVAR(2)
 Sof(C404)=Sof(H404)=Sof(C405)=Sof(H405)=1-FVAR(3)
 Sof(C304)=Sof(H304)=Sof(C305)=Sof(H305)=FVAR(3)
 Sof(C320)=Sof(H320)=Sof(C423)=Sof(H423)=Sof(N307)=Sof(C319)=Sof(H319)=
 Sof(C322)=Sof(H322)=1-FVAR(4)
 Sof(N00W)=Sof(C323)=Sof(H323)=Sof(C420)=Sof(H420)=Sof(C419)=Sof(H419)=
 Sof(C422)=Sof(H422)=FVAR(4)
 Fixed Sof: I402(0.41303) I401(0.41303) Zn41(0.41303) C333(0.76101)
 H333(0.76101) I301(0.55323) Zn31(0.55323) I302(0.55323) C332(0.76101)
 H332(0.76101) I501(0.03374) I502(0.03374) Zn51(0.03374) C432(0.23899)
 H432(0.23899) C433(0.23899) H433(0.23899)
 Fixed Uiso: I501(0.08) I502(0.08) Zn51(0.08)
5.a Aromatic/amide H refined with riding coordinates:
 C331(H331), C330(H330), C336(H336), C302(H302), C335(H335), C313(H313),
 C310(H310), C301(H301), C311(H311), C312(H312), C329(H329), C328(H328),
 C323(H323), C304(H304), C315(H315), C317(H317), C314(H314), C305(H305),
 C318(H318), C420(H420), C419(H419), C333(H333), C332(H332), C432(H432),
 C433(H433), C404(H404), C405(H405), C320(H320), C422(H422), C423(H423),
 C319(H319), C322(H322)
5.b Fitted hexagon refined as free rotating group:
 C320(C321,C422,C423,N307,C319)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44408
_shelx_hkl_checksum              76442
_shelx_fab_checksum              7186
_olex2_date_sample_data_collection 2022-07-28
_olex2_date_sample_submission    2022-07-28
_olex2_submission_original_sample_id 25_1_48b
_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 3.999
_oxdiff_exptl_absorpt_empirical_full_min 0.436