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_1571859
_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, 0.271(C15 H16 O3)'
_chemical_formula_sum            'C40.06 H28.33 I6 N12 O0.81 Zn3'
_chemical_formula_weight         1648.34
_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             2024-01-12
_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                 102.080(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.561(2)
_cell_length_b                   14.9900(6)
_cell_length_c                   31.380(3)
_cell_measurement_reflns_used    8721
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.8910
_cell_measurement_theta_min      2.6310
_cell_volume                     15897.0(19)
_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_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 0.994
_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   -115.00 -90.00   0.50    6.00    -- -103.00 -35.00-176.00   50
  2  \w    -69.00 -42.00   0.50    6.00    -- -103.00  61.00   0.00   54
  3  \w    -75.00 -32.00   0.50    6.00    -- -103.00 125.00  30.00   86
  4  \w    -65.00 -33.00   0.50    6.00    -- -103.00  61.00 -30.00   64
  5  \w   -111.00 -76.00   0.50    6.00    -- -103.00 125.00  30.00   70
  6  \w    -65.00 -40.00   0.50    6.00    -- -103.00  61.00-120.00   50
  7  \w   -117.00 -86.00   0.50    6.00    -- -103.00 -61.00 120.00   62
  8  \w    -98.00 -32.00   0.50    6.00    -- -103.00  77.00  60.00  132
  9  \w   -162.00-128.00   0.50    6.00    -- -103.00 -61.00 120.00   68
 10  \w    -94.00 -69.00   0.50    6.00    -- -103.00  77.00  90.00   50
 11  \w    -65.00 -32.00   0.50    6.00    -- -103.00  61.00 -60.00   66
 12  \w     90.00 175.00   0.50    6.00    --  101.75  35.00 -19.00  170
 13  \w     34.00  65.00   0.50    6.00    --  101.75 -61.00-150.00   62
 14  \w     37.00 105.00   0.50    6.00    --  101.75 -94.00 -90.00  136
 15  \w     30.00  70.00   0.50    6.00    --  101.75 -61.00 150.00   80
 16  \w     47.00  72.00   0.50    6.00    --  101.75 -61.00  60.00   50
 17  \w     29.00  65.00   0.50    6.00    --  101.75 -61.00   0.00   72
 18  \w     35.00  61.00   0.50    6.00    --  101.75 -61.00  30.00   52
 19  \w     34.00  70.00   0.50    6.00    --  101.75 -61.00-180.00   72
 20  \w     46.00  71.00   0.50    6.00    --  101.75 -61.00 -60.00   50
 21  \w     35.00  62.00   0.50    6.00    --  101.75 -61.00 -30.00   54
 22  \w    -33.00  17.00   0.50    1.00    --  -46.36  35.00 -19.00  100
 23  \w   -120.00 -46.00   0.50    1.00    --  -46.36 -35.00-176.00  148
 24  \w     34.00 117.00   0.50    1.00    --   46.36  35.00 -19.00  166
 25  \w    -17.00   8.00   0.50    1.00    --   46.36 -35.00-176.00   50
 26  \w    -40.00  24.00   0.50    1.00    --  -46.36  37.00 120.00  128
 27  \w    -24.00  24.00   0.50    1.00    --  -46.36  19.00 120.00   96
;
_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      0.0125738000
_diffrn_orient_matrix_UB_12      -0.0056729000
_diffrn_orient_matrix_UB_13      0.0500127000
_diffrn_orient_matrix_UB_21      -0.0397332000
_diffrn_orient_matrix_UB_22      -0.0447561000
_diffrn_orient_matrix_UB_23      0.0018785000
_diffrn_orient_matrix_UB_31      0.0184795000
_diffrn_orient_matrix_UB_32      -0.0923661000
_diffrn_orient_matrix_UB_33      -0.0039774000
_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_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            51491
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_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    19.576
_exptl_absorpt_correction_T_max  0.339
_exptl_absorpt_correction_T_min  0.101
_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            'pale yellow'
_exptl_crystal_colour_modifier   pale
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             6138
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.090
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         14455
_refine_ls_number_restraints     309
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0964
_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^)+(0.1811P)^2^+90.1494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3059
_refine_ls_wR_factor_ref         0.3264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10046
_reflns_number_total             14455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_1_24b
_cod_original_cell_volume        15897.2(18)
_cod_database_code               1571859
_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   0.303
_shelx_estimated_absorpt_t_min   0.111
_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
 O2A-C8A = O3A-C12A
 1.37 with sigma of 0.02
 C8A-C14A
 2.35 with sigma of 0.04
 C6A-C5A \\sim C5A-C4A \\sim C4A-C3A \\sim C3A-C2A \\sim C2A-C1A \\sim C6A-C1A
 with sigma of 0.02
 O2A-C14A \\sim O3A-C15A \\sim O1A-C13A
 with sigma of 0.02
 C1A-C3A \\sim C2A-C4A \\sim C3A-C5A \\sim C4A-C6A \\sim C5A-C1A \\sim C6A-C2A
 with sigma of 0.02
 C7A-C4A \\sim C5A-C13A
 with sigma of 0.02
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I302-I301 \\sim I402-I401
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I301-N301 \\sim I401-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
 N307-C319 \\sim N307-C419
 with sigma of 0.02
 C321-C320 \\sim C321-C420
 with sigma of 0.02
 C319-C320 \\sim C419-C420
 with sigma of 0.02
 N307-C320 \\sim N307-C420
 with sigma of 0.04
 C321-C319 \\sim C321-C419
 with sigma of 0.04
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 I304-I303 \\sim I404-I403
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I304-N307 \\sim I404-N307
 with sigma of 0.04
 I303-N306 \\sim I403-N306
 with sigma of 0.04
 I303-N307 \\sim I403-N307
 with sigma of 0.04
3. Restrained angles
 C7A-C12A-C11A
 fixed at 120 with sigma of 0.02
 C11A-C10A-C9A
 fixed at 120 with sigma of 0.02
 C10A-C9A-C8A
 fixed at 120 with sigma of 0.02
 C9A-C8A-C7A
 fixed at 120 with sigma of 0.02
 C8A-C7A-C12A
 fixed at 120 with sigma of 0.02
 C4A-C5A-C6A
 fixed at 120 with sigma of 0.02
 C5A-C6A-C1A
 fixed at 120 with sigma of 0.02
 C6A-C1A-C2A
 fixed at 120 with sigma of 0.02
 C1A-C2A-C3A
 fixed at 120 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C8A \\sim O2A \\sim C14A \\sim C7A \\sim C9A \\sim C12A \\sim C4A \\sim C10A
\\sim O3A \\sim C11A \\sim C3A \\sim C5A \\sim C15A \\sim C2A \\sim C13A \\sim
C6A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C420) = Uanis(C320) = Uanis(C319) = Uanis(C419)
5. Rigid body (RIGU) restrains
 C3A, O2A, C8A, C14A, C7A, C9A, H14A, H14B, H14C, C12A, C4A, H9A, C10A, O3A,
 C11A, C5A, H10A, C15A, H11A, H3A, C2A, C13A, C6A, H15A, H15B, H15C, C1A, H2A,
 O1A, H13A, H13B, H6A, H1A, H1AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I402)=Sof(Zn41)=Sof(I401)=1-FVAR(1)
 Sof(I302)=Sof(I301)=Sof(Zn31)=FVAR(1)
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(2)
 Sof(I305)=Sof(I306)=Sof(Zn33)=FVAR(2)
 Sof(C419)=Sof(H419)=Sof(C420)=Sof(H420)=1-FVAR(3)
 Sof(C319)=Sof(H319)=Sof(C320)=Sof(H320)=FVAR(3)
 Fixed Sof: I304(0.64502) I303(0.64502) Zn32(0.64502) I404(0.31764)
 Zn42(0.31764) I403(0.31764) I504(0.03735) I503(0.03735) Zn52(0.03735)
 O2A(0.27081) O3A(0.27081) C7A(0.27081) C8A(0.27081) C9A(0.27081) H9A(0.27081)
 C10A(0.27081) H10A(0.27081) C11A(0.27081) H11A(0.27081) C12A(0.27081)
 C4A(0.27081) C15A(0.27081) H15A(0.27081) H15B(0.27081) H15C(0.27081)
 O1A(0.27081) H1AA(0.27081) C1A(0.27081) H1A(0.27081) C3A(0.27081) H3A(0.27081)
 C2A(0.27081) H2A(0.27081) C13A(0.27081) H13A(0.27081) H13B(0.27081)
 C14A(0.27081) H14A(0.27081) H14B(0.27081) H14C(0.27081) C5A(0.27081)
 C6A(0.27081) H6A(0.27081)
 Fixed Uiso: I504(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:
 C313(H313), C333(H333), C318(H318), C312(H312), C322(H322), C323(H323),
 C332(H332), C317(H317), C304(H304), C314(H314), C315(H315), C302(H302),
 C305(H305), C336(H336), C335(H335), C310(H310), C328(H328), C311(H311),
 C331(H331), C329(H329), C319(H319), C320(H320), C301(H301), C330(H330),
 C419(H419), C420(H420), C9A(H9A), C10A(H10A), C11A(H11A), C1A(H1A), C3A(H3A),
 C2A(H2A), C6A(H6A)
7.c Fitted hexagon refined as free rotating group:
 C7A(C8A,C9A,C10A,C11A,C12A)
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              24672
_shelx_hkl_checksum              58603
_olex2_date_sample_data_collection 2022-06-06
_olex2_date_sample_submission    2022-06-06
_olex2_submission_original_sample_id 50_1_24b
_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 3.443
_oxdiff_exptl_absorpt_empirical_full_min 0.312