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_1571864
_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, 0.295(C15 H16 O3)'
_chemical_formula_sum            'C40.42 H28.72 I6 N12 O0.88 Zn3'
_chemical_formula_weight         1654.24
_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             2024-01-22
_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                 102.106(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.5810(14)
_cell_length_b                   14.9867(3)
_cell_length_c                   31.5551(15)
_cell_measurement_reflns_used    9171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.4060
_cell_measurement_theta_min      2.6580
_cell_volume                     15989.9(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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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   -134.00 -84.00   0.50    3.00    -- -103.00  -8.00 152.00  100
  2  \w   -151.00 -82.00   0.50    3.00    -- -103.00 -94.00 -90.00  138
  3  \w   -157.00 -90.00   0.50    3.00    -- -103.00 -30.00  90.00  134
  4  \w    -64.00 -39.00   0.50    3.00    -- -103.00  61.00 -90.00   50
  5  \w    -82.00 -57.00   0.50    3.00    -- -103.00 125.00  60.00   50
  6  \w   -112.00 -84.00   0.50    3.00    -- -103.00 125.00  60.00   56
  7  \w     92.00 174.00   0.50    3.00    --  101.75   8.00 -32.00  164
  8  \w    136.00 174.00   0.50    3.00    --  101.75  61.00  30.00   76
  9  \w     33.00 106.00   0.50    3.00    --  101.75 -94.00-120.00  146
 10  \w     34.00  63.00   0.50    3.00    --  101.75 -61.00 -30.00   58
 11  \w     87.00 144.00   0.50    3.00    --  101.75  61.00   0.00  114
 12  \w     31.00  73.00   0.50    3.00    --  101.75 -94.00 120.00   84
 13  \w     64.00  92.00   0.50    3.00    --  101.75 -94.00-180.00   56
 14  \w     77.00 106.00   0.50    3.00    --  101.75 -94.00 120.00   58
 15  \w     31.00  98.00   0.50    3.00    --  101.75 -94.00-150.00  134
 16  \w     30.00  69.00   0.50    3.00    --  101.75 -61.00 -60.00   78
 17  \w   -110.00 -31.00   0.50    0.50    --  -46.36  -8.00 152.00  158
 18  \w    -14.00  11.00   0.50    0.50    --  -46.36   8.00 -32.00   50
 19  \w    -27.00  -2.00   0.50    0.50    --   46.36  -8.00 152.00   50
 20  \w     31.00 120.00   0.50    0.50    --   46.36   8.00 -32.00  178
 21  \w    -20.00  17.00   0.50    0.50    --  -46.36  19.00 120.00   74
 22  \w     23.00  94.00   0.50    0.50    --   46.36-125.00   0.00  142
;
_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      -0.0118581000
_diffrn_orient_matrix_UB_12      0.0055125000
_diffrn_orient_matrix_UB_13      -0.0498524000
_diffrn_orient_matrix_UB_21      -0.0437035000
_diffrn_orient_matrix_UB_22      0.0100788000
_diffrn_orient_matrix_UB_23      0.0028416000
_diffrn_orient_matrix_UB_31      0.0049539000
_diffrn_orient_matrix_UB_32      0.1020975000
_diffrn_orient_matrix_UB_33      0.0023918000
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            52421
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         2.614
_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    19.466
_exptl_absorpt_correction_T_max  0.356
_exptl_absorpt_correction_T_min  0.084
_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             6163
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.126
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         14569
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.1233
_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^)+(0.1620P)^2^+325.7856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3522
_refine_ls_wR_factor_ref         0.3650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10971
_reflns_number_total             14569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_5_48a
_cod_database_code               1571864
_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   0.343
_shelx_estimated_absorpt_t_min   0.089
_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
 C4A-C3A = C4A-C5A = C6A-C5A = C1A-C6A = C1A-C2A = C2A-C3A
 1.39 with sigma of 0.02
 C4A-C7A
 1.5 with sigma of 0.02
 C5A-C13A
 1.51 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
 C4A-C6A = C5A-C1A = C6A-C2A = C1A-C3A
 2.4 with sigma of 0.04
 C8A-C14A
 2.4 with sigma of 0.02
 C12A-C15A
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.04
 C7A-O2A = C7A-O3A
 2.4 with sigma of 0.04
 C7A-C12A \\sim C12A-C11A \\sim C11A-C10A \\sim C9A-C10A \\sim C9A-C8A \\sim
C8A-C7A
 with sigma of 0.02
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 C7A-C9A \\sim C8A-C10A \\sim C9A-C11A \\sim C10A-C12A \\sim C11A-C7A \\sim
C12A-C8A
 with sigma of 0.04
 C7A-O2A \\sim O2A-C9A
 with sigma of 0.04
 C7A-O3A \\sim O3A-C11A
 with sigma of 0.04
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 Zn43-N312 \\sim Zn33-N312
 with sigma of 0.02
 I405-I406 \\sim I305-I306
 with sigma of 0.04
 I405-N312 \\sim I305-N312
 with sigma of 0.04
 I406-N312 \\sim I306-N312
 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
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 I504-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 Zn42-N306 \\sim Zn32-N306
 with sigma of 0.02
 Zn42-N307 \\sim Zn32-N307
 with sigma of 0.02
 I403-I504 \\sim I303-I304
 with sigma of 0.04
 I403-N306 \\sim I303-N306
 with sigma of 0.04
 I403-N307 \\sim I303-N307
 with sigma of 0.04
 I504-N306 \\sim I304-N306
 with sigma of 0.04
 I504-N307 \\sim I304-N307
 with sigma of 0.04
 N312-C336 \\sim N312-C436
 with sigma of 0.02
 C334-C335 \\sim C334-C435
 with sigma of 0.02
 C335-C336 \\sim C435-C436
 with sigma of 0.02
 N312-C335 \\sim N312-C435
 with sigma of 0.04
 C334-C336 \\sim C334-C436
 with sigma of 0.04
 N306-C414 \\sim N306-C314
 with sigma of 0.02
 C316-C415 \\sim C316-C315
 with sigma of 0.02
 C415-C414 \\sim C315-C314
 with sigma of 0.02
 N306-C415 \\sim N306-C315
 with sigma of 0.04
 C316-C414 \\sim C316-C314
 with sigma of 0.04
3. Restrained planarity
 C4A, C5A, C6A, C1A, C2A, C3A
 with sigma of 0.1
 C7A, C12A, C11A, C10A, C9A, C8A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7A \\sim O2A \\sim C8A \\sim C14A \\sim C9A \\sim C12A \\sim C4A \\sim C10A
\\sim C11A \\sim O3A \\sim C5A \\sim C3A \\sim C15A \\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(C336) = Uanis(C436)
Uanis(C335) = Uanis(C435)
Uanis(C329) = Uanis(C328) = Uanis(C327) = Uanis(C331) = Uanis(C330) =
Uanis(N311)
Uanis(C314) = Uanis(C414) = Uanis(C415) = Uanis(C315)
5. Rigid body (RIGU) restrains
 C7A, O2A, C8A, C14A, C9A, C12A, C4A, C10A, C11A, O3A, C5A, C3A, C15A, 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
 1*[Sof(I301)+Sof(I302)+Sof(Zn31)]+1*[Sof(I402)+Sof(Zn41)+Sof(I401)]+1*
 [Sof(I501)+Sof(I502)+Sof(Zn51)]=1 with esd of 0.00001
 Sof(I306)=Sof(Zn33)=Sof(I305)=1-FVAR(1)
 Sof(I405)=Sof(I406)=Sof(Zn43)=FVAR(1)
 Sof(I301)=Sof(I302)=Sof(Zn31)=FVAR(2)
 Sof(I402)=Sof(Zn41)=Sof(I401)=FVAR(3)
 Sof(I501)=Sof(I502)=Sof(Zn51)=FVAR(4)
 Sof(C435)=Sof(H435)=Sof(C436)=Sof(H436)=1-FVAR(5)
 Sof(C335)=Sof(H335)=Sof(C336)=Sof(H336)=FVAR(5)
 Sof(C314)=Sof(H314)=Sof(C315)=Sof(H315)=1-FVAR(6)
 Sof(C415)=Sof(H415)=Sof(C414)=Sof(H414)=FVAR(6)
 Fixed Sof: I403(0.20981) I504(0.20981) Zn42(0.20981) O2A(0.29499)
 C7A(0.29499) C12A(0.29499) C11A(0.29499) H11A(0.29499) C10A(0.29499)
 H10A(0.29499) C9A(0.29499) H9A(0.29499) C8A(0.29499) O3A(0.29499) C4A(0.29499)
 C5A(0.29499) C6A(0.29499) H6A(0.29499) C2A(0.29499) H2A(0.29499) O1A(0.29499)
 H1A(0.29499) C14A(0.29499) H14A(0.29499) H14B(0.29499) H14C(0.29499)
 C13A(0.29499) H13A(0.29499) H13B(0.29499) C1A(0.29499) H1AA(0.29499)
 C15A(0.29499) H15A(0.29499) H15B(0.29499) H15C(0.29499) C3A(0.29499)
 H3A(0.29499) I304(0.56254) Zn32(0.56254) I303(0.56254) I503(0.22766)
 I404(0.22766) Zn52(0.22766)
 Fixed Uiso: I501(0.08) I502(0.08) Zn51(0.08) I503(0.08) Zn52(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B)
7.b Aromatic/amide H refined with riding coordinates:
 C317(H317), C301(H301), C322(H322), C333(H333), C302(H302), C332(H332),
 C311(H311), C323(H323), C312(H312), C304(H304), C318(H318), C310(H310),
 C313(H313), C415(H415), C320(H320), C319(H319), C414(H414), C328(H328),
 C335(H335), C331(H331), C329(H329), C330(H330), C305(H305), C11A(H11A),
 C10A(H10A), C9A(H9A), C6A(H6A), C2A(H2A), C1A(H1AA), C3A(H3A), C336(H336),
 C435(H435), C436(H436), C314(H314), C315(H315)
7.c Tetrahedral OH refined with riding coordinates:
 O1A(H1A)
7.d Idealised Me refined with everything fixed:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C)
;
_shelx_res_checksum              8407
_shelx_hkl_checksum              90437
_olex2_date_sample_data_collection 2022-02-01
_olex2_date_sample_submission    2022-02-01
_olex2_submission_original_sample_id 50_5_48a
_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 2.967
_oxdiff_exptl_absorpt_empirical_full_min 0.454