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_1571866
_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
' [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             2024-01-17
_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                 100.858(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.412(2)
_cell_length_b                   15.0303(5)
_cell_length_c                   29.994(3)
_cell_measurement_reflns_used    8962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.1220
_cell_measurement_theta_min      3.1750
_cell_volume                     15235.8(19)
_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(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -106.00 -78.00   0.50    2.02    -- -103.00 149.00 106.00   56
  2  \w   -109.00 -34.00   0.50    2.02    -- -103.00 123.00 -56.00  150
  3  \w   -137.00-112.00   0.50    2.02    -- -103.00-149.00  59.00   50
  4  \w   -117.00 -79.00   0.50    2.02    -- -103.00-123.00-137.00   76
  5  \w    -70.00 -45.00   0.50    2.02    -- -103.00  77.00 -60.00   50
  6  \w    -98.00 -73.00   0.50    2.02    -- -103.00  77.00 -60.00   50
  7  \w    -64.00 -37.00   0.50    2.02    -- -103.00  61.00  90.00   54
  8  \w    -97.00 -38.00   0.50    2.02    -- -103.00 125.00   0.00  118
  9  \w   -166.00 -82.00   0.50    2.02    -- -103.00-125.00 -90.00  168
 10  \w   -131.00-105.00   0.50    2.02    -- -103.00 -77.00 150.00   52
 11  \w    -87.00 -54.00   0.50    2.02    -- -103.00  77.00 150.00   66
 12  \w    -69.00 -31.00   0.50    2.02    -- -103.00  61.00 150.00   76
 13  \w   -163.00-104.00   0.50    2.02    -- -103.00 -15.00 -90.00  118
 14  \w     74.00 101.00   0.50    2.02    --  101.75-123.00-137.00   54
 15  \w    147.00 172.00   0.50    2.02    --  101.75 123.00 -56.00   50
 16  \w     93.00 126.00   0.50    2.02    --  101.75-149.00  59.00   66
 17  \w    109.00 136.00   0.50    2.02    --  101.75 123.00 -56.00   54
 18  \w     30.00 105.00   0.50    2.02    --  101.75 -94.00  90.00  150
 19  \w     89.00 128.00   0.50    2.02    --  101.75  30.00-120.00   78
 20  \w     39.00 105.00   0.50    2.02    --  101.75 -94.00-120.00  132
 21  \w     86.00 171.00   0.50    2.02    --  101.75  61.00 -60.00  170
 22  \w     63.00 107.00   0.50    2.02    --  101.75 -77.00-120.00   88
 23  \w     90.00 173.00   0.50    2.02    --  101.75  45.00  30.00  166
 24  \w     35.00  67.00   0.50    2.02    --  101.75 -61.00-120.00   64
 25  \w     30.00  58.00   0.50    2.02    --  101.75 -61.00-180.00   56
 26  \w     44.00 106.00   0.50    2.02    --  101.75 -94.00 -30.00  124
 27  \w    146.00 172.00   0.50    2.02    --  101.75  30.00-120.00   52
 28  \w     90.00 175.00   0.50    2.02    --  101.75  30.00 120.00  170
 29  \w     77.00 106.00   0.50    2.02    --  101.75 -98.00  63.59   58
 30  \w     77.00 130.00   0.50    2.02    --  101.75 149.00 106.00  106
 31  \w     31.00 106.00   0.50    2.02    --  101.75 -98.00-177.32  150
 32  \w     30.00  57.00   0.50    2.02    --  101.75 -77.00-120.00   54
 33  \w    -87.00 -22.00   0.50    0.50    --  -46.01 123.00 -56.00  130
 34  \w    -89.00 -60.00   0.50    0.50    --  -46.01-149.00  59.00   58
 35  \w   -106.00 -65.00   0.50    0.50    --  -46.01 149.00 106.00   82
 36  \w     22.00  90.00   0.50    0.50    --   46.01-123.00-137.00  136
 37  \w     77.00 111.00   0.50    0.50    --   46.01 149.00 106.00   68
 38  \w     47.00  72.00   0.50    0.50    --   46.01-149.00  59.00   50
 39  \w   -118.00 -26.00   0.50    0.50    --  -46.01 -77.00  90.00  184
 40  \w    -13.00  28.00   0.50    0.50    --   46.01 -19.00 120.00   82
 41  \w    -27.00  27.00   0.50    0.50    --   46.01 -19.00  90.00  108
 42  \w     55.00 113.00   0.50    0.50    --   46.01  77.00  30.00  116
;
_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      -0.0071440000
_diffrn_orient_matrix_UB_12      0.0092216000
_diffrn_orient_matrix_UB_13      -0.0520691000
_diffrn_orient_matrix_UB_21      0.0375262000
_diffrn_orient_matrix_UB_22      -0.0551214000
_diffrn_orient_matrix_UB_23      -0.0012782000
_diffrn_orient_matrix_UB_31      -0.0248370000
_diffrn_orient_matrix_UB_32      -0.0858512000
_diffrn_orient_matrix_UB_33      -0.0048539000
_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  0.0825
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            90613
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_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    20.394
_exptl_absorpt_correction_T_max  0.350
_exptl_absorpt_correction_T_min  0.067
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             5856
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         13941
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0899
_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^)+(0.1949P)^2^+22.6024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3042
_refine_ls_wR_factor_ref         0.3336
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8014
_reflns_number_total             13941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_5_48c
_cod_original_cell_volume        15235.8(18)
_cod_database_code               1571866
_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   0.329
_shelx_estimated_absorpt_t_min   0.113
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 I402-Zn41 \\sim I302-Zn31
 with sigma of 0.02
 I401-Zn41 \\sim I301-Zn31
 with sigma of 0.02
 I402-I401 \\sim I302-I301
 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
 I501-Zn51 \\sim I401-Zn41
 with sigma of 0.02
 I502-Zn51 \\sim I302-Zn31
 with sigma of 0.02
 Zn51-N301 \\sim Zn31-N301
 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
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 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
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I304-N307 \\sim I404-N307
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(Zn33) = Uanis(Zn43)
4. Others
 1*[Sof(I305)+Sof(I306)+Sof(Zn33)]+1*[Sof(I405)+Sof(Zn43)+Sof(I406)]+1*
 [Sof(I505)+Sof(I506)+Sof(Zn53)]=1 with esd of 0.00001
 Sof(I305)=Sof(I306)=Sof(Zn33)=FVAR(1)
 Sof(I405)=Sof(Zn43)=Sof(I406)=FVAR(2)
 Sof(I505)=Sof(I506)=Sof(Zn53)=FVAR(3)
 Fixed Sof: I303(0.49005) I304(0.49005) I402(0.38056) I401(0.38056)
 Zn32(0.49005) Zn41(0.38056) I302(0.59969) Zn31(0.59969) I301(0.59969)
 I502(0.01975) Zn51(0.01975) I501(0.01975) I403(0.46458) Zn42(0.46458)
 I404(0.46458) I503(0.04536) I504(0.04536) Zn52(0.04536)
 Fixed Uiso: I502(0.08) Zn51(0.08) I501(0.08) I505(0.08) I506(0.08) Zn53(0.08)
 I503(0.08) I504(0.08) Zn52(0.08)
5.a Aromatic/amide H refined with riding coordinates:
 C319(H319), C320(H320), C315(H315), C314(H314), C304(H304), C302(H302),
 C301(H301), C323(H323), C322(H322), C311(H311), C335(H335), C305(H305),
 C318(H318), C317(H317), C310(H310), C336(H336), C332(H332), C312(H312),
 C333(H333), C313(H313), C331(H331), C328(H328), C329(H329), C330(H330)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              6940
_shelx_hkl_checksum              31576
_shelx_fab_checksum              27309
_olex2_date_sample_data_collection 2023-04-19
_olex2_date_sample_submission    2023-04-19
_olex2_submission_original_sample_id 50_5_48c
_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 2.874
_oxdiff_exptl_absorpt_empirical_full_min 0.398