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_1571851
_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, 0.232(C15 H16 O3)'
_chemical_formula_sum            'C39.49 H27.72 I6 N12 O0.7 Zn3'
_chemical_formula_weight         1638.96
_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             2024-01-31
_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                 101.744(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.4145(9)
_cell_length_b                   14.9918(3)
_cell_length_c                   31.0574(10)
_cell_measurement_reflns_used    13212
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.4360
_cell_measurement_theta_min      2.6440
_cell_volume                     15688.2(7)
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_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 0.993
_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     83.00 137.00   0.50    2.00    --   83.36  56.00 151.00  108
  2  \w     21.00  58.00   0.50    2.00    --   83.36 -56.00   9.00   74
  3  \w     39.00  67.00   0.50    2.00    --   83.36 -57.00 -30.00   56
  4  \w     34.00  77.00   0.50    2.00    --   83.36 -77.00-180.00   86
  5  \w     84.00 128.00   0.50    2.00    --   83.36 125.00   0.00   88
  6  \w     31.00  68.00   0.50    2.00    --   83.36 -57.00  30.00   74
  7  \w     17.00  42.00   0.50    2.00    --   83.36 -37.00 150.00   50
  8  \w     16.00  41.00   0.50    2.00    --   83.36 -37.00 -30.00   50
  9  \w     17.00  43.00   0.50    2.00    --   83.36 -37.00  90.00   52
 10  \w     44.00  97.00   0.50    2.00    --   83.36 -99.00-180.00  106
 11  \w    111.00 146.00   0.50    2.00    --   83.36 125.00  30.00   70
 12  \w     27.00  53.00   0.50    2.00    --   83.36 -57.00  90.00   52
 13  \w     85.00 110.00   0.50    2.00    --   83.36 125.00  30.00   50
 14  \w     48.00 105.00   0.50    2.00    --   83.36 -99.00 -60.00  114
 15  \w     42.00  68.00   0.50    2.00    --   83.36 -77.00 -30.00   52
 16  \w     18.00  61.00   0.50    2.00    --   83.36 -57.00  60.00   86
 17  \w    106.00 131.00   0.50    2.00    --   83.36  57.00  90.00   50
 18  \w     31.00  65.00   0.50    2.00    --   83.36 -57.00-180.00   68
 19  \w   -132.00-107.00   0.50    2.00    --  -79.36 -56.00   9.00   50
 20  \w    -61.00 -35.00   0.50    2.00    --  -79.36  56.00 151.00   52
 21  \w    -37.00  -8.00   0.50    2.00    --  -79.36  37.00 120.00   58
 22  \w   -138.00-107.00   0.50    2.00    --  -79.36 -99.00 120.00   62
 23  \w    -64.00 -19.00   0.50    2.00    --  -79.36  57.00   0.00   90
 24  \w    -99.00 -69.00   0.50    1.00    --  -55.06 -56.00   9.00   60
 25  \w    -35.00  13.00   0.50    1.00    --  -55.06  56.00 151.00   96
 26  \w    -23.00  14.00   0.50    1.00    --  -55.06  19.00 -30.00   74
 27  \w    -23.00  12.00   0.50    1.00    --  -55.06  19.00 -90.00   70
 28  \w    -23.00  14.00   0.50    1.00    --  -55.06  19.00-150.00   74
 29  \w    -13.00  57.00   0.50    1.00    --   51.81 -56.00   9.00  140
 30  \w     81.00 118.00   0.50    1.00    --   51.81  56.00 151.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, 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      0.0125394000
_diffrn_orient_matrix_UB_12      0.0119425000
_diffrn_orient_matrix_UB_13      0.0502056000
_diffrn_orient_matrix_UB_21      -0.0335001000
_diffrn_orient_matrix_UB_22      0.0686726000
_diffrn_orient_matrix_UB_23      -0.0011159000
_diffrn_orient_matrix_UB_31      -0.0284414000
_diffrn_orient_matrix_UB_32      -0.0755110000
_diffrn_orient_matrix_UB_33      0.0068814000
_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  0.0417
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            64404
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         2.623
_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    19.833
_exptl_absorpt_correction_T_max  0.439
_exptl_absorpt_correction_T_min  0.100
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             6098
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.069
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     753
_refine_ls_number_reflns         14239
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.0933
_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^)+(0.2248P)^2^+20.1300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3037
_refine_ls_wR_factor_ref         0.3307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9307
_reflns_number_total             14239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_5_96c
_cod_original_formula_sum        'C39.49 H27.72 I6 N12 O0.70 Zn3'
_cod_database_code               1571851
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     9300-04
_shelx_estimated_absorpt_t_max   0.382
_shelx_estimated_absorpt_t_min   0.069
_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
 O1A-C13A = O3A-C15A = O2A-C14A
 1.43 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 C8A-C14A
 2.4 with sigma of 0.04
 O2A-C8A \\sim O3A-C12A
 with sigma of 0.02
 C7A-O2A \\sim O2A-C9A
 with sigma of 0.02
 I301-Zn31 \\sim I401-Zn1
 with sigma of 0.02
 I302-Zn31 \\sim I402-Zn1
 with sigma of 0.02
 Zn31-N301 \\sim Zn1-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
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 Zn33-N312 \\sim Zn43-N312
 with sigma of 0.02
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 I303-Zn32 \\sim I403-Zn2
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn2
 with sigma of 0.02
 Zn32-N307 \\sim Zn2-N307
 with sigma of 0.02
 Zn32-N306 \\sim Zn2-N306
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 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-N307 \\sim I404-N307
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I504-Zn52 \\sim I304-Zn32
 with sigma of 0.02
 I503-Zn52 \\sim I303-Zn32
 with sigma of 0.02
 N311-C430 \\sim N311-C330
 with sigma of 0.02
 C327-C431 \\sim C327-C331
 with sigma of 0.02
 C431-C430 \\sim C331-C330
 with sigma of 0.02
 N311-C431 \\sim N311-C331
 with sigma of 0.04
 C327-C430 \\sim C327-C330
 with sigma of 0.04
3. Restrained planarity
 O2A, C8A, C7A, C12A, O3A
 with sigma of 0.1
 C4A, C5A, C6A, C13A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4A \\sim O3A \\sim C12A \\sim C15A \\sim C7A \\sim C11A \\sim C8A \\sim C10A
\\sim C9A \\sim O2A \\sim C5A \\sim C3A \\sim C14A \\sim C6A \\sim C13A \\sim
C2A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C431) = Uanis(C430) = Uanis(C330) = Uanis(C331)
5. Rigid body (RIGU) restrains
 C4A, O3A, C12A, C15A, C7A, C11A, C8A, C10A, C9A, O2A, C5A, C3A, C14A, C6A,
 C13A, C2A, C1A, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(1)
 Sof(I305)=Sof(I306)=Sof(Zn33)=FVAR(1)
 Sof(C330)=Sof(H330)=Sof(C331)=Sof(H331)=1-FVAR(2)
 Sof(C431)=Sof(H431)=Sof(C430)=Sof(H430)=FVAR(2)
 Fixed Sof: I303(0.49302) I304(0.49302) I301(0.47326) I302(0.47326)
 Zn32(0.49302) Zn31(0.47326) I401(0.50036) Zn1(0.50036) I402(0.50036)
 I403(0.47435) Zn2(0.47435) I404(0.47435) I504(0.03263) I503(0.03263)
 Zn52(0.03263) I501(0.02637) I502(0.02637) Zn51(0.02637) O3A(0.23239)
 C7A(0.23239) C12A(0.23239) C11A(0.23239) H11A(0.23239) C10A(0.23239)
 H10A(0.23239) C9A(0.23239) H9A(0.23239) C8A(0.23239) O2A(0.23239)
 C15A(0.23239) H15A(0.23239) H15B(0.23239) H15C(0.23239) C14A(0.23239)
 H14A(0.23239) H14B(0.23239) H14C(0.23239) C1A(0.23239) H1A(0.23239)
 C2A(0.23239) H2A(0.23239) C3A(0.23239) H3A(0.23239) C4A(0.23239) C5A(0.23239)
 C6A(0.23239) H6A(0.23239) O1A(0.23239) H1AA(0.23239) C13A(0.23239)
 H13A(0.23239) H13B(0.23239)
 Fixed Uiso: I504(0.08) I503(0.08) Zn52(0.08) I501(0.08) I502(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:
 C320(H320), C315(H315), C319(H319), C314(H314), C305(H305), C329(H329),
 C328(H328), C304(H304), C302(H302), C301(H301), C310(H310), C313(H313),
 C317(H317), C311(H311), C322(H322), C323(H323), C312(H312), C332(H332),
 C318(H318), C335(H335), C333(H333), C336(H336), C431(H431), C430(H430),
 C11A(H11A), C10A(H10A), C9A(H9A), C330(H330), C331(H331), C1A(H1A), C2A(H2A),
 C3A(H3A), C6A(H6A)
7.c Fitted hexagon refined as free rotating group:
 C7A(C12A,C11A,C10A,C9A,C8A), C1A(C2A,C3A,C4A,C5A,C6A)
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              52163
_shelx_hkl_checksum              55458
_olex2_date_sample_data_collection 2023-10-03
_olex2_date_sample_submission    2023-10-03
_olex2_submission_original_sample_id 25_5_96c
_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 4.184
_oxdiff_exptl_absorpt_empirical_full_min 0.296