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_7227777
_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'
_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                   31.3031(11)
_cell_length_b                   31.3031(11)
_cell_length_c                   31.3031(11)
_cell_measurement_reflns_used    2435
_cell_measurement_temperature    295
_cell_measurement_theta_max      13.2400
_cell_measurement_theta_min      1.7750
_cell_volume                     30673.4(19)
_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      'diamond-anvil cell'
_diffrn_ambient_pressure         250000
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.727
_diffrn_measured_fraction_theta_max 0.727
_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   -105.00 -74.00   0.20    0.70    --   15.00  70.00 155.77  155
  2  \w   -105.00 -74.00   0.20    0.70    --   15.00  70.00 -24.23  155
  3  \w   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00-155.77  200
  4  \w   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00  24.23  200
  5  \w   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 -24.23  280
  6  \w   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 155.77  280
  7  \w    -96.00 -30.00   0.20    0.70    --   15.00 -70.00  24.23  330
  8  \w    -96.00 -30.00   0.20    0.70    --   15.00 -70.00-155.77  330
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Newport IS4CCD (4 circle), Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0037906000
_diffrn_orient_matrix_UB_12      -0.0001763000
_diffrn_orient_matrix_UB_13      0.0217748000
_diffrn_orient_matrix_UB_21      -0.0111240000
_diffrn_orient_matrix_UB_22      0.0188683000
_diffrn_orient_matrix_UB_23      -0.0017932000
_diffrn_orient_matrix_UB_31      -0.0185468000
_diffrn_orient_matrix_UB_32      -0.0112634000
_diffrn_orient_matrix_UB_33      -0.0032637000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.727
_diffrn_reflns_Laue_measured_fraction_max 0.727
_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       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4737
_diffrn_reflns_point_group_measured_fraction_full 0.731
_diffrn_reflns_point_group_measured_fraction_max 0.731
_diffrn_reflns_theta_full        13.252
_diffrn_reflns_theta_max         13.252
_diffrn_reflns_theta_min         1.784
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76028
_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    0.915
_exptl_crystal_description       plate
_exptl_crystal_F_000             8928
_exptl_crystal_recrystallization_method
'Compressed crystal that was grown in situ at 0.16 GPa in the diamond-anvil cell from methanol:water mixture by heating and subsequent cooling of the cell'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 140 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.36(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         594
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.452
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0955
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2583
_refine_ls_wR_factor_ref         0.2807
_reflns_Friedel_coverage         0.605
_reflns_Friedel_fraction_full    0.737
_reflns_Friedel_fraction_max     0.737
_reflns_number_gt                466
_reflns_number_total             594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cp00593h3.cif
_cod_data_source_block           CDMOF_a_0_25GPa
_cod_depositor_comments
'Adding full bibliography for 7227776--7227790.cif.'
_cod_original_cell_volume        30673(2)
_cod_database_code               7227777
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C48 H82 K2 O40'
_reflns_odcompleteness_completeness 77.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.25
_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
 C14-C15
 1.5 with sigma of 0.02
 O14-C15
 2.4 with sigma of 0.02
 C14-O14
 1.45 with sigma of 0.02
 C14-C13
 1.5 with sigma of 0.02
 O13-C13
 1.45 with sigma of 0.02
 O3-C3
 1.45 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.02
 C6-C5
 1.5 with sigma of 0.02
 C16-C15
 1.5 with sigma of 0.02
 C16-O16
 1.45 with sigma of 0.02
 K1-C16
 4 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C2-O3
 2.3 with sigma of 0.02
 C2-C5
 3 with sigma of 0.02
 C5-C2
 3 with sigma of 0.02
 C1-C4
 2.8 with sigma of 0.02
 C5-C1
 2.3 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.02
 C12-C15
 3 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.02
 C15-C12
 3 with sigma of 0.02
 C11-C14
 3 with sigma of 0.02
 K1-C11
 4 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.02
 C2-O2
 1.45 with sigma of 0.02
 O2-C3
 2.2 with sigma of 0.02
 C12-O12
 1.45 with sigma of 0.02
 C6-O6
 1.45 with sigma of 0.02
 O5-C3
 3 with sigma of 0.02
 O15-C15
 1.45 with sigma of 0.02
 O15-C13
 3 with sigma of 0.02
 O5-C6
 2.5 with sigma of 0.02
 O5-C5
 1.45 with sigma of 0.02
 O15-C16
 2.2 with sigma of 0.02
 O5-C1
 1.45 with sigma of 0.02
 O15-C11
 1.45 with sigma of 0.02
 C13-C15
 2.4 with sigma of 0.02
 O14-C15
 2.5 with sigma of 0.04
 C13-O14
 2.5 with sigma of 0.04
 C5-C3
 2.5 with sigma of 0.02
 C4-C2
 2.5 with sigma of 0.02
 C3-C1
 2.5 with sigma of 0.02
 C1-C5
 2.5 with sigma of 0.02
 C12-C14
 2.4 with sigma of 0.02
 C4-C11
 2.5 with sigma of 0.04
 C11-C4
 2.5 with sigma of 0.04
 C11-C13
 2.4 with sigma of 0.02
 C15-C11
 2.4 with sigma of 0.02
 O2-C1
 2.5 with sigma of 0.04
 O4-C12
 2.5 with sigma of 0.04
 O6-C5
 2.7 with sigma of 0.04
 O5-C4
 2.5 with sigma of 0.02
 C14-O15
 2.4 with sigma of 0.02
 C2-O5
 2.5 with sigma of 0.02
 O15-C12
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(K1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Uiso(C1)=Uiso(C2)=Uiso(C3)=Uiso(C4)=Uiso(C5)=Uiso(C6)=Uiso(C11)=Uiso(C12)=
 Uiso(C13)=Uiso(C14)=Uiso(C15)=Uiso(C16)=FVAR(1)
 Uiso(O2)=Uiso(O3)=Uiso(O4)=Uiso(O5)=Uiso(O6)=Uiso(O12)=Uiso(O13)=Uiso(O14)=
 Uiso(O15)=Uiso(O16)=Uiso(OA)=FVAR(2)
5.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)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C16(H16A,H16B)
5.c Tetrahedral OH refined with riding coordinates:
 O2(H2A), O3(H3A), O6(H6), O12(H12A), O13(H13A), O16(H16)
;
_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_olex2_submission_original_sample_id CDMOF_alpha_2_025
_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 1.937
_oxdiff_exptl_absorpt_empirical_full_min 0.678