Pressure inverse solubility and polymorphism of an edible γ-cyclodextrin-based metal-organic framework.
Patyk-Kaźmierczak, Ewa; Warren, Mark R.; Allan, David R.; Katrusiak, Andrzej; Physical chemistry chemical physics : PCCP 19 (2017) 9086–9091; doi:10.1039/c7cp00593h

data_7227789
_publ_section_title
;
 Pressure inverse solubility and polymorphism of an edible
 \g-cyclodextrin-based metal-organic framework.
;
_journal_issue                   13
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              9086
_journal_page_last               9091
_journal_paper_doi               10.1039/c7cp00593h
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_name_common            '\g-cyclodextrin-metal-organic framework'
_chemical_name_systematic
'catena-((\m8-\g-Cyclodextrin)-di-potassium dihydroxide)'
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_Hall           'I 4 2 3'
_space_group_name_H-M_alt        'I 4 3 2'
_symmetry_space_group_name_Hall  'I 4 2 3'
_symmetry_space_group_name_H-M   'I 4 3 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            12
_cell_length_a                   31.2093(16)
_cell_length_b                   31.2093(16)
_cell_length_c                   31.2093(16)
_cell_measurement_reflns_used    1891
_cell_measurement_temperature    269.99(10)
_cell_measurement_theta_max      12.9810
_cell_measurement_theta_min      3.1560
_cell_volume                     30398(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      'ispropanol:water mother liquor'
_diffrn_ambient_temperature      269.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_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    -68.00  54.00   1.00   15.00    --  -18.72   0.00-150.00  122
  2  \w    -73.00  20.00   1.00   15.00    --  -18.72 -19.00  60.00   93
  3  \w    -40.00   8.00   1.00   15.00    --  -18.72  57.00  60.00   48
  4  \w    -25.00  23.00   1.00   15.00    --  -18.72 -99.00   0.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0032543000
_diffrn_orient_matrix_UB_12      0.0169472000
_diffrn_orient_matrix_UB_13      0.0147675000
_diffrn_orient_matrix_UB_21      0.0001663000
_diffrn_orient_matrix_UB_22      -0.0149725000
_diffrn_orient_matrix_UB_23      0.0171089000
_diffrn_orient_matrix_UB_31      0.0224746000
_diffrn_orient_matrix_UB_32      -0.0023531000
_diffrn_orient_matrix_UB_33      -0.0023986000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1616
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20814
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        13.690
_diffrn_reflns_theta_max         13.690
_diffrn_reflns_theta_min         2.919
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.924
_exptl_crystal_description       cube
_exptl_crystal_F_000             8928
_exptl_crystal_recrystallization_method
'Crystal grown from water solution by isopropanol vapour difussion method'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.47
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.138
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 241 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.17(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         766
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0986P)^2^+25.3536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.623
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                694
_reflns_number_total             766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cp00593h5.cif
_cod_data_source_block           CDMOF_a_270K
_cod_depositor_comments
'Adding full bibliography for 7227776--7227790.cif.'
_cod_original_cell_volume        30399(3)
_cod_database_code               7227789
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C48 H82 K2 O40'
_reflns_odcompleteness_completeness 97.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.66
_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 O(H) groups
2. Restrained distances
 C4-C3
 1.5 with sigma of 0.02
 C5-C6
 1.5 with sigma of 0.02
 O4-C4
 1.45 with sigma of 0.02
 C16-C15
 1.5 with sigma of 0.01
 C15-C16
 1.45 with sigma of 0.01
 C11-O4
 1.45 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.02
 C1-O5
 1.45 with sigma of 0.02
 O15-C15
 1.45 with sigma of 0.02
 C11-O15
 1.45 with sigma of 0.02
 O13-C13
 1.45 with sigma of 0.01
 C13-O13
 1.42 with sigma of 0.01
 C11-C13
 2.5 with sigma of 0.04
 C11-C15
 2.5 with sigma of 0.04
 C11-C4
 2.5 with sigma of 0.04
 C2-C4
 2.5 with sigma of 0.04
 O15-C12
 2.5 with sigma of 0.04
 O15-C14
 2.5 with sigma of 0.04
 C2-O5
 2.5 with sigma of 0.04
3. Others
 Uiso(O2)=Uiso(O3)=Uiso(O5)=Uiso(O6)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C16(H16A,H16B)
4.c Tetrahedral OH refined with riding coordinates:
 O2(H2A), O3(H3A), O6(H6), O12(H12A), O13(H13A), O16(H16)
;
_olex2_exptl_crystal_mounting_method
'Crystal coated in isopropanol:water mother liquor and mounted in a quarts capillary'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.904
_oxdiff_exptl_absorpt_empirical_full_min 0.652