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_1571818
_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         'C15 H16 O3'
_chemical_formula_sum            'C15 H16 O3'
_chemical_formula_weight         244.28
_chemical_name_systematic        (2',6'dimethoxy-[1,1'-biphenyl]-2-yl)methanol
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-03-18
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.244(7)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.913(2)
_cell_length_b                   7.6350(7)
_cell_length_c                   27.048(2)
_cell_measurement_reflns_used    1441
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      63.7260
_cell_measurement_theta_min      3.1970
_cell_volume                     4930.4(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    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_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 0.983
_diffrn_measured_fraction_theta_max 0.968
_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     43.00 109.00   0.50    4.50    --   51.51  30.00 148.00  132
  2  \w    -17.00  37.00   0.50    4.50    --   51.51 -30.00 -11.00  108
  3  \w   -110.00 -85.00   0.50    4.50    --  -55.01 -30.00 -11.00   50
  4  \w    -33.00  -8.00   0.50    4.50    --  -55.01  30.00 148.00   50
  5  \w   -135.00-109.00   0.50   11.00    --  -79.37 -30.00 -11.00   52
  6  \w    111.00 154.00   0.50   11.00    --   83.47  30.00 148.00   86
  7  \w    -17.00  24.00   0.50    4.50    --   51.51 -19.00 -60.00   82
  8  \w    -18.00  23.00   0.50    4.50    --   51.51 -19.00-150.00   82
  9  \w    -63.00 -13.00   0.50   11.00    --  -79.37  57.00 -30.00  100
 10  \w    -39.00 -12.00   0.50   11.00    --  -79.37  57.00-120.00   54
 11  \w    -56.00 -29.00   0.50   11.00    --  -79.37  77.00  90.00   54
 12  \w     87.00 112.00   0.50   11.00    --   83.47-125.00 -30.00   50
 13  \w     23.00  49.00   0.50   11.00    --   83.47-125.00 -30.00   52
 14  \w     25.00  60.00   0.50   11.00    --   83.47 -57.00  30.00   70
 15  \w     12.00  37.00   0.50   11.00    --   83.47 -37.00 -30.00   50
 16  \w     13.00  43.00   0.50   11.00    --   83.47 -37.00  90.00   60
 17  \w     12.00  39.00   0.50   11.00    --   83.47 -37.00 -90.00   54
 18  \w     14.00  43.00   0.50   11.00    --   83.47 -37.00  60.00   58
 19  \w     16.00  68.00   0.50   11.00    --   83.47 -57.00 150.00  104
 20  \w     18.00  44.00   0.50   11.00    --   83.47 -37.00-120.00   52
 21  \w    104.00 153.00   0.50   11.00    --   83.47  37.00-120.00   98
 22  \w     84.00 146.00   0.50   11.00    --   83.47 125.00 150.00  124
 23  \w    106.00 131.00   0.50   11.00    --   83.47  57.00-180.00   50
;
_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      -0.0366345000
_diffrn_orient_matrix_UB_12      0.0301835000
_diffrn_orient_matrix_UB_13      0.0442667000
_diffrn_orient_matrix_UB_21      -0.0470307000
_diffrn_orient_matrix_UB_22      0.0737300000
_diffrn_orient_matrix_UB_23      -0.0352679000
_diffrn_orient_matrix_UB_31      -0.0246135000
_diffrn_orient_matrix_UB_32      -0.1855899000
_diffrn_orient_matrix_UB_33      -0.0068613000
_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_unetI/netI     0.0774
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            7946
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.689
_diffrn_reflns_theta_min         3.273
_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    0.737
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.949
_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    1.316
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         7946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1524
_refine_ls_R_factor_gt           0.0797
_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^)+(0.1039P)^2^+7.8365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.2463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4183
_reflns_number_total             7946
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 98.3032\% 
around [-0.00 1.00 0.01] (reciprocal) or [-0.00 1.00 0.00] (direct)
;
_cod_data_source_file            lt5068.cif
_cod_data_source_block           BBA_8_12_OMe
_cod_original_cell_volume        4930.4(8)
_cod_database_code               1571818
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(C15 H16 O3)2'
_chemical_oxdiff_usercomment     '9300-04 Pure'
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.910
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.689(2)
 0.311(2)
2. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
3.a Idealised tetrahedral OH refined as rotating group:
 O1A(H1AA), O1B(H1BA)
;
_shelx_res_checksum              58989
_shelx_hkl_checksum              20505
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.739
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2