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_7227788
_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      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-19
_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                120.0
_cell_formula_units_Z            18
_cell_length_a                   43.260(16)
_cell_length_b                   43.260(16)
_cell_length_c                   28.104(16)
_cell_measurement_reflns_used    1157
_cell_measurement_temperature    244.98(10)
_cell_measurement_theta_max      10.7500
_cell_measurement_theta_min      2.9290
_cell_volume                     45548(4)
_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      244.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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      -0.0055056000
_diffrn_orient_matrix_UB_12      -0.0128463000
_diffrn_orient_matrix_UB_13      0.0184808000
_diffrn_orient_matrix_UB_21      -0.0169609000
_diffrn_orient_matrix_UB_22      -0.0008132000
_diffrn_orient_matrix_UB_23      0.0007555000
_diffrn_orient_matrix_UB_31      -0.0066023000
_diffrn_orient_matrix_UB_32      -0.0136630000
_diffrn_orient_matrix_UB_33      -0.0172669000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2076
_diffrn_reflns_av_unetI/netI     0.1333
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21233
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        13.681
_diffrn_reflns_theta_max         13.681
_diffrn_reflns_theta_min         2.778
_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  0.14415
_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    0.925
_exptl_crystal_description       cube
_exptl_crystal_F_000             13392
_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         0.169
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 583 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.35(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         3104
_refine_ls_number_restraints     302
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0812
_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^)+(0.0963P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.2034
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                2197
_reflns_number_total             3104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cp00593h5.cif
_cod_data_source_block           CDMOF_b_245K
_cod_depositor_comments
'Adding full bibliography for 7227776--7227790.cif.'
_cod_original_cell_volume        45547(30)
_cod_database_code               7227788
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C48 H82 K2 O40'
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.67
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H73A of O73, All C(H,H) groups
 At 1.5 times of:
  H76 of O76, H72A of O72, H66 of O66, H52A of O52, H46 of O46, H2A of O2,
  H3A of O3, H6 of O6, H12A of O12, H13A of O13, H16 of O16, H22A of O22, H23A
  of O23, H26 of O26, H32A of O32, H33A of O33, H36 of O36, H42A of O42, H43A
  of O43, H63A of O63, H62A of O62, H56 of O56, H53A of O53
2. Restrained distances
 C64-C65
 1.5 with sigma of 0.02
 C71-C72
 1.5 with sigma of 0.02
 C65-C66
 1.5 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.02
 C23-C24
 1.5 with sigma of 0.02
 C23-C22
 1.5 with sigma of 0.02
 C15-C16
 1.5 with sigma of 0.02
 C45-C46
 1.5 with sigma of 0.02
 C44-C45
 1.5 with sigma of 0.02
 C35-C36
 1.5 with sigma of 0.002
 C64-C63
 1.5 with sigma of 0.02
 C4-C3
 1.5 with sigma of 0.005
 C4-C1
 3.5 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.005
 C5-C3
 2.5 with sigma of 0.02
 C13-C14
 1.5 with sigma of 0.02
 C13-C12
 1.5 with sigma of 0.02
 C44-C43
 1.5 with sigma of 0.02
 C43-C44
 1.5 with sigma of 0.02
 C42-C43
 1.5 with sigma of 0.02
 C21-C22
 1.5 with sigma of 0.02
 C6-C5
 1.5 with sigma of 0.005
 C72-C73
 1.5 with sigma of 0.02
 C26-C25
 1.5 with sigma of 0.02
 O15-C11
 1.45 with sigma of 0.02
 C2-O5
 2.5 with sigma of 0.02
 O5-C1
 1.45 with sigma of 0.02
 C31-O44
 1.45 with sigma of 0.02
 C33-O33
 1.45 with sigma of 0.02
 C35-O35
 1.45 with sigma of 0.005
 C31-O35
 1.45 with sigma of 0.005
 C33-O35
 3 with sigma of 0.02
 O73-C73
 1.45 with sigma of 0.02
 O12-C12
 1.45 with sigma of 0.02
 O23-C23
 1.45 with sigma of 0.02
 C26-O26
 1.45 with sigma of 0.005
 C6-O6
 1.45 with sigma of 0.02
 C61-O74
 1.45 with sigma of 0.02
 C61-O65
 1.45 with sigma of 0.02
 C35-O36
 2.45 with sigma of 0.02
 O36-C36
 1.45 with sigma of 0.002
 O22-C22
 1.45 with sigma of 0.02
 C72-O72
 1.45 with sigma of 0.02
 C16-O16
 1.45 with sigma of 0.02
 O4-C4
 1.45 with sigma of 0.02
 O3-C3
 1.45 with sigma of 0.02
 O2-C2
 1.45 with sigma of 0.02
 O63-C63
 1.45 with sigma of 0.005
 O43-C43
 1.45 with sigma of 0.02
 C14-C15
 1.5 with sigma of 0.02
 C24-C25
 1.5 with sigma of 0.02
 C52-C53
 1.5 with sigma of 0.02
 C65-C64
 1.5 with sigma of 0.02
 C71-O4
 1.45 with sigma of 0.01
 O14-C1
 1.45 with sigma of 0.02
 O15-C15
 1.45 with sigma of 0.01
 C21-O25
 1.45 with sigma of 0.01
 O25-C25
 1.45 with sigma of 0.01
 O44-C44
 1.45 with sigma of 0.01
 C41-C42
 1.5 with sigma of 0.02
 C54-C55
 1.5 with sigma of 0.02
 O54-C41
 1.45 with sigma of 0.01
 C1-K2
 3.8 with sigma of 0.02
 C12-K1
 3.8 with sigma of 0.02
 O13-C13
 1.45 with sigma of 0.02
 C12-O12
 1.45 with sigma of 0.02
 C22-O22
 1.45 with sigma of 0.02
 C54-C53
 1.5 with sigma of 0.02
 O14-C14
 1.45 with sigma of 0.01
 C35-C34
 1.5 with sigma of 0.002
 C33-C34
 1.5 with sigma of 0.02
 C31-C32
 1.5 with sigma of 0.02
 C33-C32
 1.5 with sigma of 0.02
 O32-C32
 1.45 with sigma of 0.02
 C5-O5
 1.45 with sigma of 0.01
 C45-O45
 1.45 with sigma of 0.02
 C53-C52
 1.5 with sigma of 0.02
 O54-C54
 1.45 with sigma of 0.02
 O52-C52
 1.45 with sigma of 0.02
 C51-C52
 1.5 with sigma of 0.02
 C51-O64
 1.45 with sigma of 0.02
 C62-C63
 1.5 with sigma of 0.02
 C62-C61
 1.5 with sigma of 0.02
 C62-O62
 1.45 with sigma of 0.02
 C55-C56
 1.5 with sigma of 0.02
 O56-C56
 1.45 with sigma of 0.005
 O55-C51
 1.45 with sigma of 0.01
 O55-C55
 1.45 with sigma of 0.02
 C74-C75
 1.5 with sigma of 0.02
 C74-C73
 1.5 with sigma of 0.005
 C75-O75
 1.5 with sigma of 0.02
 O75-C71
 1.45 with sigma of 0.02
 C75-C76
 1.5 with sigma of 0.02
 O76-C76
 1.45 with sigma of 0.005
 C42-C44
 2.5 with sigma of 0.04
 C43-C45
 2.5 with sigma of 0.04
 C11-C13
 2.5 with sigma of 0.04
 C61-C65
 2.5 with sigma of 0.04
 C71-C75
 2.5 with sigma of 0.04
 C71-C73
 2.5 with sigma of 0.04
 C75-C73
 2.5 with sigma of 0.04
 O73-C72
 2.5 with sigma of 0.04
 O45-C44
 2.5 with sigma of 0.04
 O45-C42
 2.5 with sigma of 0.04
 O25-C24
 2.5 with sigma of 0.04
 O65-C64
 2.5 with sigma of 0.04
 O26-C25
 2.5 with sigma of 0.04
 C5-O4
 2.5 with sigma of 0.04
 O14-C2
 2.5 with sigma of 0.04
 O25-C22
 2.5 with sigma of 0.04
 C21-C25
 2.5 with sigma of 0.04
 C23-O24
 2.5 with sigma of 0.04
 C36-O35
 2.5 with sigma of 0.04
 C23-C25
 2.5 with sigma of 0.04
 C21-O22
 2.5 with sigma of 0.04
 C71-O72
 2.5 with sigma of 0.04
 C71-C4
 2.5 with sigma of 0.04
 O4-C3
 2.5 with sigma of 0.04
 O4-C5
 2.5 with sigma of 0.04
 O3-C2
 2.5 with sigma of 0.04
 C63-C65
 2.5 with sigma of 0.04
 C64-O65
 2.5 with sigma of 0.04
 C65-C61
 2.5 with sigma of 0.04
 C61-C63
 2.5 with sigma of 0.04
 C26-O25
 2.5 with sigma of 0.04
 C26-C24
 2.5 with sigma of 0.04
 C15-C11
 2.5 with sigma of 0.01
 C35-C31
 2.5 with sigma of 0.01
 C44-C31
 2.5 with sigma of 0.01
 C55-C51
 2.5 with sigma of 0.02
 C53-C55
 2.5 with sigma of 0.04
 C41-C45
 2.5 with sigma of 0.04
 C43-C41
 2.5 with sigma of 0.04
 C45-C41
 2.5 with sigma of 0.04
 C54-C41
 2.5 with sigma of 0.02
 C4-C71
 2.5 with sigma of 0.01
 C1-C14
 2.5 with sigma of 0.01
 O4-C72
 2.5 with sigma of 0.04
 C36-C34
 2.5 with sigma of 0.04
 C32-C34
 2.5 with sigma of 0.04
 C2-C4
 2.5 with sigma of 0.01
 C4-O5
 2.5 with sigma of 0.01
 O5-C4
 2.5 with sigma of 0.02
 O15-C12
 2.5 with sigma of 0.02
 O25-C26
 2.5 with sigma of 0.04
 C44-O45
 2.5 with sigma of 0.02
 C54-C52
 2.5 with sigma of 0.02
 C41-C54
 2.5 with sigma of 0.01
 O52-C51
 2.5 with sigma of 0.04
 C66-O65
 2.5 with sigma of 0.04
 C66-C64
 2.5 with sigma of 0.04
 C1-O2
 2.5 with sigma of 0.04
 C1-C3
 2.5 with sigma of 0.04
 C3-O2
 2.5 with sigma of 0.04
 C12-C14
 2.5 with sigma of 0.04
 O13-C14
 2.5 with sigma of 0.02
 O13-C12
 2.5 with sigma of 0.02
 C14-O15
 2.5 with sigma of 0.04
 O24-C23
 2.5 with sigma of 0.04
 O52-C53
 2.5 with sigma of 0.04
 C53-O52
 2.5 with sigma of 0.01
 O76-C75
 2.5 with sigma of 0.04
 C13-C15
 2.5 with sigma of 0.04
 O14-C13
 2.5 with sigma of 0.04
 O24-C25
 2.5 with sigma of 0.04
 C25-O24
 2.5 with sigma of 0.01
 C64-C62
 2.5 with sigma of 0.04
 C62-C64
 2.5 with sigma of 0.04
 O62-C61
 2.5 with sigma of 0.04
 O62-C63
 2.5 with sigma of 0.04
 C52-O55
 2.5 with sigma of 0.01
 C54-O55
 2.5 with sigma of 0.04
 O55-C56
 2.5 with sigma of 0.04
 C56-C54
 2.5 with sigma of 0.04
 O55-C54
 2.5 with sigma of 0.04
 C54-C56
 2.5 with sigma of 0.04
 C56-O55
 2.5 with sigma of 0.04
 C74-O73
 2.5 with sigma of 0.04
 O4-O75
 2.5 with sigma of 0.04
 O75-C76
 2.5 with sigma of 0.02
 O75-C74
 2.5 with sigma of 0.04
 C74-C76
 2.5 with sigma of 0.01
 C15-C13
 2.5 with sigma of 0.04
 C13-O14
 2.5 with sigma of 0.04
 O14-C15
 2.5 with sigma of 0.04
 C24-C11
 2.5 with sigma of 0.01
3. Rigid bond restraints
 C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
 O16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
: with sigma of 0.001 and sigma for terminal atoms of 0.00001
: with sigma of 0.001 and sigma for terminal atoms of 0.0001
: with sigma of 0.05 and sigma for terminal atoms of 0.01
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(K2) \\sim Ueq, Uanis(K1) \\sim Ueq, Uanis(K3) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Uiso(O2)=Uiso(O3)=Uiso(O4)=Uiso(O5)=Uiso(O6)=Uiso(O12)=Uiso(O13)=Uiso(O14)=
 Uiso(O15)=Uiso(O16)=Uiso(O22)=Uiso(O23)=Uiso(O24)=Uiso(O25)=Uiso(O26)=
 Uiso(O32)=Uiso(O33)=Uiso(O34)=Uiso(O35)=Uiso(O36)=Uiso(O42)=Uiso(O43)=
 Uiso(O44)=Uiso(O45)=Uiso(O46)=Uiso(O52)=Uiso(O53)=Uiso(O54)=Uiso(O55)=
 Uiso(O56)=Uiso(O62)=Uiso(O63)=Uiso(O64)=Uiso(O65)=Uiso(O66)=Uiso(O72)=
 Uiso(O73)=Uiso(O74)=Uiso(O75)=Uiso(O76)=FVAR(1)
 Uiso(OA)=Uiso(OB)=FVAR(2)
7.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), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C61(H61),
  C62(H62), C63(H63), C64(H64), C65(H65), C71(H71), C72(H72), C73(H73),
 C74(H74), C75(H75)
7.b Secondary CH2 refined with riding coordinates:
 C6(H6B,H6A), C16(H16A,H16B), C26(H26B,H26A), C36(H36A,H36B), C46(H46A,H46B),
 C56(H56A,H56B), C66(H66A,H66B), C76(H76A,H76B)
7.c Tetrahedral OH refined with riding coordinates:
 O2(H2A), O3(H3A), O6(H6), O12(H12A), O13(H13A), O16(H16), O22(H22A),
 O23(H23A), O26(H26), O32(H32A), O33(H33A), O36(H36), O42(H42A), O43(H43A),
 O46(H46), O52(H52A), O53(H53A), O56(H56), O62(H62A), O63(H63A), O66(H66),
 O72(H72A), O73(H73A), O76(H76)
;
_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 4.908
_oxdiff_exptl_absorpt_empirical_full_min 0.626