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_1571835
_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         'C38.783 H26.968 I6 N12 O0.557 Zn3'
_chemical_formula_sum            'C38.78 H26.97 I6 N12 O0.56 Zn3'
_chemical_formula_weight         1627.49
_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             2024-02-01
_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                 102.185(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.7075(8)
_cell_length_b                   14.9722(3)
_cell_length_c                   31.1023(9)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.3800
_cell_measurement_theta_min      2.8970
_cell_volume                     15798.1(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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   -174.00 -88.00   0.50    4.50    -- -103.00 -55.00  24.00  172
  2  \w    -61.00 -30.00   0.50    4.50    -- -103.00  55.00 167.00   62
  3  \w    -62.00 -37.00   0.50    4.50    -- -103.00  61.00  90.00   50
  4  \w   -174.00 -83.00   0.50    4.50    -- -103.00 -94.00 -30.00  182
  5  \w   -174.00-123.00   0.50    4.50    -- -103.00 -45.00  90.00  102
  6  \w    -67.00 -31.00   0.50    4.50    -- -103.00  61.00  60.00   72
  7  \w    -65.00 -40.00   0.50    4.50    -- -103.00  61.00 120.00   50
  8  \w   -103.00 -73.00   0.50    4.50    -- -103.00  77.00-150.00   60
  9  \w    -69.00 -44.00   0.50    4.50    -- -103.00  61.00  30.00   50
 10  \w    -55.00 -30.00   0.50    4.50    -- -103.00  77.00-150.00   50
 11  \w   -100.00 -41.00   0.50    4.50    -- -103.00  77.00-120.00  118
 12  \w   -162.00 -88.00   0.50    4.50    -- -103.00 -61.00 120.00  148
 13  \w     95.00 131.00   0.50    4.50    --  101.75  55.00 167.00   72
 14  \w     36.00  63.00   0.50    4.50    --  101.75 -55.00  24.00   54
 15  \w     30.00  69.00   0.50    4.50    --  101.75 -61.00-120.00   78
 16  \w     90.00 135.00   0.50    4.50    --  101.75  45.00 -90.00   90
 17  \w     33.00  70.00   0.50    4.50    --  101.75 -61.00 -30.00   74
 18  \w     33.00  72.00   0.50    4.50    --  101.75 -61.00 -90.00   78
 19  \w     47.00  73.00   0.50    4.50    --  101.75 -61.00 150.00   52
 20  \w    -23.00  26.00   0.50    0.73    --  -46.48  55.00 167.00   98
 21  \w   -117.00 -43.00   0.50    0.73    --  -46.48 -55.00  24.00  148
 22  \w     49.00  77.00   0.50    0.73    --   46.48  55.00 167.00   56
 23  \w     -6.00  19.00   0.50    0.73    --   46.48 -55.00  24.00   50
 24  \w    -23.00  28.00   0.50    0.73    --  -46.48  19.00 -30.00  102
 25  \w    -23.00  28.00   0.50    0.73    --  -46.48  19.00 150.00  102
 26  \w    -23.00  17.00   0.50    0.73    --  -46.48  19.00 -60.00   80
;
_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      -0.0048521000
_diffrn_orient_matrix_UB_12      -0.0068646000
_diffrn_orient_matrix_UB_13      -0.0502515000
_diffrn_orient_matrix_UB_21      0.0336458000
_diffrn_orient_matrix_UB_22      0.0679628000
_diffrn_orient_matrix_UB_23      0.0018018000
_diffrn_orient_matrix_UB_31      0.0301268000
_diffrn_orient_matrix_UB_32      -0.0769988000
_diffrn_orient_matrix_UB_33      0.0060795000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            53948
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.605
_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    19.689
_exptl_absorpt_correction_T_max  0.364
_exptl_absorpt_correction_T_min  0.130
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             6049
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.221
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         14397
_refine_ls_number_restraints     293
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0936
_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^)+(0.1960P)^2^+82.0058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3026
_refine_ls_wR_factor_ref         0.3224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10040
_reflns_number_total             14397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           4_10_96b
_cod_database_code               1571835
_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   0.339
_shelx_estimated_absorpt_t_min   0.145
_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
 C13A-C5A
 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
 O3A-C12A
 1.37 with sigma of 0.02
 C5A-O1A
 2.4 with sigma of 0.04
 C8A-C14A
 2.4 with sigma of 0.04
 C6A-C13A
 2.5 with sigma of 0.04
 C4A-C13A
 2.5 with sigma of 0.04
 C7A-O3A
 2.35 with sigma of 0.04
 C12A-C15A
 2.4 with sigma of 0.02
 C12A-C4A \\sim C4A-C8A
 with sigma of 0.04
 C3A-C7A \\sim C7A-C5A
 with sigma of 0.04
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 I406-N307 \\sim I306-N307
 with sigma of 0.04
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 Zn43-N307 \\sim Zn33-N307
 with sigma of 0.02
 Zn43-N306 \\sim Zn33-N306
 with sigma of 0.02
 I406-N306 \\sim I306-N306
 with sigma of 0.04
 I405-I406 \\sim I305-I306
 with sigma of 0.04
 I405-N307 \\sim I305-N307
 with sigma of 0.04
 I405-N306 \\sim I305-N306
 with sigma of 0.04
 I401-N301 \\sim I301-N301
 with sigma of 0.04
 I402-I401 \\sim I302-I301
 with sigma of 0.04
 I402-Zn41 \\sim I302-Zn31
 with sigma of 0.02
 I402-N301 \\sim I302-N301
 with sigma of 0.04
 I401-Zn41 \\sim I301-Zn31
 with sigma of 0.02
 Zn41-N301 \\sim Zn31-N301
 with sigma of 0.02
 I304-N305 \\sim I404-N305
 with sigma of 0.04
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I303-N305 \\sim I403-N305
 with sigma of 0.04
 Zn32-N305 \\sim Zn42-N305
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I501-Zn51 \\sim I401-Zn41
 with sigma of 0.02
 I402-Zn41 \\sim I502-Zn51
 with sigma of 0.02
 Zn41-N301 \\sim Zn51-N301
 with sigma of 0.02
 N307-C323 \\sim N307-C423
 with sigma of 0.02
 C321-C322 \\sim C321-C422
 with sigma of 0.02
 C323-C322 \\sim C423-C422
 with sigma of 0.02
 N307-C322 \\sim N307-C422
 with sigma of 0.04
 C321-C323 \\sim C321-C423
 with sigma of 0.04
3. Restrained planarity
 C4A, C5A, C6A, C13A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7A \\sim O2A \\sim C8A \\sim C14A \\sim C9A \\sim C10A \\sim C12A \\sim C4A
\\sim C11A \\sim O3A \\sim C5A \\sim C3A \\sim C15A \\sim C13A \\sim C6A \\sim
C2A \\sim O1A \\sim C1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C422) = Uanis(C423) = Uanis(C323) = Uanis(C322)
5. Rigid body (RIGU) restrains
 C7A, O2A, C8A, C14A, C9A, C10A, C12A, C4A, C11A, O3A, C5A, C3A, C15A, C13A,
 C6A, C2A, O1A, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I305)=Sof(Zn33)=Sof(I306)=1-FVAR(1)
 Sof(I405)=Sof(I406)=Sof(Zn43)=FVAR(1)
 Sof(C423)=Sof(H423)=Sof(C422)=Sof(H422)=1-FVAR(2)
 Sof(C323)=Sof(H323)=Sof(C322)=Sof(H322)=FVAR(2)
 Fixed Sof: I402(0.38642) I401(0.38642) I303(0.52003) I304(0.52003)
 Zn41(0.38642) Zn32(0.52003) I302(0.57441) Zn31(0.57441) I301(0.57441)
 Zn42(0.43315) I403(0.43315) I404(0.43315) I504(0.04681) I503(0.04681)
 Zn52(0.04681) I502(0.03918) I501(0.03918) Zn51(0.03918) O2A(0.18551)
 O3A(0.18551) C8A(0.18551) C9A(0.18551) H9A(0.18551) C10A(0.18551)
 H10A(0.18551) C11A(0.18551) H11A(0.18551) C12A(0.18551) C7A(0.18551)
 C15A(0.18551) H15A(0.18551) H15B(0.18551) H15C(0.18551) C14A(0.18551)
 H14A(0.18551) H14B(0.18551) H14C(0.18551) C13A(0.18551) H13A(0.18551)
 H13B(0.18551) C4A(0.18551) C5A(0.18551) C6A(0.18551) H6A(0.18551) C1A(0.18551)
 H1A(0.18551) C2A(0.18551) H2A(0.18551) C3A(0.18551) H3A(0.18551) O1A(0.18551)
 H1AA(0.18551)
 Fixed Uiso: I504(0.08) I503(0.08) Zn52(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:
 C328(H328), C304(H304), C305(H305), C329(H329), C314(H314), C320(H320),
 C315(H315), C319(H319), C317(H317), C318(H318), C313(H313), C312(H312),
 C311(H311), C310(H310), C01C(H01C), C302(H302), C334(H334), C335(H335),
 C332(H332), C301(H301), C330(H330), C331(H331), C323(H323), C322(H322),
 C9A(H9A), C10A(H10A), C11A(H11A), C423(H423), C422(H422), C6A(H6A), C1A(H1A),
 C2A(H2A), C3A(H3A)
7.c Fitted hexagon refined as free rotating group:
 C8A(C9A,C10A,C11A,C12A,C7A), C4A(C5A,C6A,C1A,C2A,C3A)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1AA)
7.e Idealised Me refined with everything fixed:
 C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C)
;
_shelx_res_checksum              18590
_shelx_hkl_checksum              73881
_olex2_date_sample_data_collection 2022-08-01
_olex2_date_sample_submission    2022-08-01
_olex2_submission_original_sample_id 4_10_96b
_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 2.706
_oxdiff_exptl_absorpt_empirical_full_min 0.359