# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_1_76GPa
_database_code_depnum_ccdc_archive 'CCDC 1529143'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_cell_length_a                   30.56(3)
_cell_length_b                   30.56(3)
_cell_length_c                   30.56(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     28529(78)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    27
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      9.7810
_cell_measurement_theta_min      4.7860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
# EXPERIMENTAL DATA 

_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.1GPa and then 
compressed to 1.76GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8928
_exptl_crystal_recrystallization_method 
'Crystal grown in situ 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          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.6092
_diffrn_reflns_av_unetI/netI     0.2499
_diffrn_reflns_Laue_measured_fraction_full 0.852
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8391
_diffrn_reflns_point_group_measured_fraction_full 0.882
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        10.203
_diffrn_reflns_theta_max         10.203
_diffrn_reflns_theta_min         4.717
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1760000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.852
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   25.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   25.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   25.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   25.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   25.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   25.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   25.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   25.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   25.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   25.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0027124000
_diffrn_orient_matrix_UB_12      0.0016870000
_diffrn_orient_matrix_UB_13      0.0228740000
_diffrn_orient_matrix_UB_21      0.0191393000
_diffrn_orient_matrix_UB_22      0.0127984000
_diffrn_orient_matrix_UB_23      -0.0034447000
_diffrn_orient_matrix_UB_31      -0.0128240000
_diffrn_orient_matrix_UB_32      0.0194219000
_diffrn_orient_matrix_UB_33      0.0000762000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.543
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                251
_reflns_number_total             284
_reflns_odcompleteness_completeness 84.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     10.18
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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    ?
_computing_publication_material  ?
_computing_structure_refinement  ?
_computing_structure_solution    ?

# REFINEMENT DATA

_refine_diff_density_max         0.747
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.204
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     ?
_refine_ls_number_reflns         ?
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          ?
_refine_ls_R_factor_gt           ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          ?
_refine_ls_wR_factor_ref         ?
_refine_special_details          
;
Due to the low quality of collected data no structure refinement was performed
;

_shelx_SHELXL_version_number     2014/7


_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.000
_oxdiff_exptl_absorpt_empirical_full_min 1.000


##################################################################

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_0_26GPa
_database_code_depnum_ccdc_archive 'CCDC 1529142'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2016-10-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_cell_length_a                   31.17(2)
_cell_length_b                   31.17(2)
_cell_length_c                   31.17(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     30273(70)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    43
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      9.9800
_cell_measurement_theta_min      3.4730
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27454
_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_absorpt_special_details   ?
# EXPERIMENTAL DATA 

_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.26GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.928
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             8928
_exptl_crystal_recrystallization_method 
'Crystal grown in situ in the diamond-anvil cell from methanol:water mixture by heating and subsequent cooling of the cell'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.8770
_diffrn_reflns_av_unetI/netI     0.4272
_diffrn_reflns_Laue_measured_fraction_full 0.879
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9708
_diffrn_reflns_point_group_measured_fraction_full 0.908
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        10.260
_diffrn_reflns_theta_max         10.260
_diffrn_reflns_theta_min         3.202
_diffrn_ambient_temperature      295(2)
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         260000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0338
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.879
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0226469000
_diffrn_orient_matrix_UB_12      -0.0000835000
_diffrn_orient_matrix_UB_13      0.0026969000
_diffrn_orient_matrix_UB_21      0.0021042000
_diffrn_orient_matrix_UB_22      0.0045703000
_diffrn_orient_matrix_UB_23      0.0219158000
_diffrn_orient_matrix_UB_31      -0.0004600000
_diffrn_orient_matrix_UB_32      0.0223236000
_diffrn_orient_matrix_UB_33      -0.0045484000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.552
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                163
_reflns_number_total             315
_reflns_odcompleteness_completeness 87.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     10.21
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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    ?
_computing_publication_material  ?
_computing_structure_refinement  ?
_computing_structure_solution    ?

# REFINEMENT DATA
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.296
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     ?
_refine_ls_number_reflns         ?
_refine_ls_number_restraints     ?
_refine_ls_R_factor_all          ?
_refine_ls_R_factor_gt           ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          ?
_refine_ls_wR_factor_ref         ?
_refine_special_details          
;
Due to the low quality of collected data no structure refinement was performed
;

_shelx_SHELXL_version_number     2014/7


_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.470
_oxdiff_exptl_absorpt_empirical_full_min 0.640
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_0_16GPa
_database_code_depnum_ccdc_archive 'CCDC 1529144'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7


# start Validation Reply Form
_vrf_REFNR01_CDMOF_a_0_16GPa     
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_THETM01_CDMOF_a_0_16GPa     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT029_CDMOF_a_0_16GPa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.715 Note  
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT090_CDMOF_a_0_16GPa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       3.91 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT201_CDMOF_a_0_16GPa     
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT241_CDMOF_a_0_16GPa     
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         K1 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT306_CDMOF_a_0_16GPa     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_0_16GPa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.035 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_CDMOF_a_0_16GPa     
;
PROBLEM: D-H Without Acceptor       O6     --  H6     ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
# end Validation Reply Form

# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0030 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2030 0.2500 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   31.3469(11)
_cell_length_b                   31.3469(11)
_cell_length_c                   31.3469(11)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30802(2)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    2204
_cell_measurement_temperature    295
_cell_measurement_theta_max      10.7200
_cell_measurement_theta_min      1.7820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55803
_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_absorpt_special_details   ?

# EXPERIMENTAL DATA 

_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.16GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.912
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8928
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Crystal grown in situ 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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1007
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.715
_diffrn_reflns_Laue_measured_fraction_max 0.715
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4484
_diffrn_reflns_point_group_measured_fraction_full 0.739
_diffrn_reflns_point_group_measured_fraction_max 0.739
_diffrn_reflns_theta_full        11.009
_diffrn_reflns_theta_max         11.009
_diffrn_reflns_theta_min         1.991
_diffrn_ambient_temperature      295
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         160000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.715
_diffrn_measured_fraction_theta_max 0.715
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 155.77  155
  2  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 -24.23  155
  3  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00-155.77  200
  4  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00  24.23  200
  5  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 -24.23  280
  6  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 155.77  280
  7  ω    -96.00 -30.00   0.20    0.70    --   15.00 -70.00  24.23  330
  8  ω    -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       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0038201000
_diffrn_orient_matrix_UB_12      -0.0000686000
_diffrn_orient_matrix_UB_13      0.0217101000
_diffrn_orient_matrix_UB_21      -0.0110961000
_diffrn_orient_matrix_UB_22      0.0188536000
_diffrn_orient_matrix_UB_23      -0.0019012000
_diffrn_orient_matrix_UB_31      -0.0185345000
_diffrn_orient_matrix_UB_32      -0.0112572000
_diffrn_orient_matrix_UB_33      -0.0032504000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   synchrotron
_diffrn_special_details          
'high-pressure measurement with diamond-anvil cell at 0.16 GPa'
_reflns_Friedel_coverage         0.588
_reflns_Friedel_fraction_full    0.783
_reflns_Friedel_fraction_max     0.783
_reflns_number_gt                326
_reflns_number_total             351
_reflns_odcompleteness_completeness 74.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     11.01
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.119
_refine_diff_density_min         -0.128
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details 
;
 Flack x determined using 110 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         351
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0745
_refine_ls_restrained_S_all      1.542
_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/[σ²(Fo²)+(0.1818P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.2092
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
 resulting in a low data:parameter ratio.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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
 C16-O16
 1.45 with sigma of 0.002
 C6-C5
 1.5 with sigma of 0.002
 C6-O6
 1.45 with sigma of 0.002
 C16-C15
 1.5 with sigma of 0.002
 C14-C15
 1.5 with sigma of 0.002
 O14-C15
 2.4 with sigma of 0.02
 C14-O14
 1.45 with sigma of 0.002
 C14-C13
 1.5 with sigma of 0.02
 O13-C13
 1.45 with sigma of 0.002
 O2-C3
 2.2 with sigma of 0.02
 O3-C3
 1.45 with sigma of 0.002
 C2-C3
 1.5 with sigma of 0.002
 C2-O2
 1.45 with sigma of 0.002
 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
 C11-O4
 1.45 with sigma of 0.002
 C11-C14
 3 with sigma of 0.02
 C4-O4
 1.45 with sigma of 0.002
 C4-C5
 1.5 with sigma of 0.002
 C4-C3
 1.5 with sigma of 0.002
 C5-C1
 2.3 with sigma of 0.002
 C2-C1
 1.5 with sigma of 0.002
 C1-C4
 2.8 with sigma of 0.02
 C12-O4
 2 with sigma of 0.02
 C12-C15
 3 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.02
 C12-O12
 1.45 with sigma of 0.02
 C15-C12
 3 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.002
 O5-C6
 2.5 with sigma of 0.02
 O15-C16
 2.2 with sigma of 0.02
 O5-C5
 1.45 with sigma of 0.002
 O15-C15
 1.45 with sigma of 0.002
 O5-C3
 3 with sigma of 0.02
 O15-C13
 3 with sigma of 0.02
 O15-C11
 1.45 with sigma of 0.002
 O5-C1
 1.45 with sigma of 0.002
 C5-C3
 2.5 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
 C11-C13
 2.4 with sigma of 0.02
 C15-C11
 2.4 with sigma of 0.02
 C4-C2
 2.5 with sigma of 0.02
 C4-C11
 2.5 with sigma of 0.04
 C11-C4
 2.5 with sigma of 0.04
 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
 C2-O5
 2.5 with sigma of 0.02
 C14-O15
 2.4 with sigma of 0.02
 O5-C4
 2.5 with sigma of 0.02
 O15-C12
 2.4 with sigma of 0.02
3. 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)=FVAR(2)
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), O16(H16)
4.d Idealised tetrahedral OH refined as rotating group:
 O6(H6), O12(H12A), O13(H13A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?


# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8453(7) 0.6876(7) 0.6330(10) 0.156(8) Uiso 1 1 d D . . . .
H1 H 0.8411 0.7183 0.6284 0.188 Uiso 1 1 calc R . . . .
C2 C 0.8869(6) 0.6787(7) 0.6550(9) 0.156(8) Uiso 1 1 d D . . . .
H2 H 0.8865 0.6908 0.6838 0.188 Uiso 1 1 calc R . . . .
C3 C 0.8935(6) 0.6313(7) 0.6572(10) 0.156(8) Uiso 1 1 d D . . . .
H3 H 0.9046 0.6228 0.6292 0.188 Uiso 1 1 calc R . . . .
C4 C 0.8534(7) 0.6060(7) 0.6640(11) 0.156(8) Uiso 1 1 d D . . . .
H4 H 0.8465 0.6148 0.6932 0.188 Uiso 1 1 calc R . . . .
C5 C 0.8143(7) 0.6216(6) 0.6413(11) 0.156(8) Uiso 1 1 d D . . . .
H5 H 0.8284 0.6246 0.6135 0.188 Uiso 1 1 calc R . . . .
C6 C 0.7753(8) 0.6002(10) 0.6236(8) 0.156(8) Uiso 1 1 d D . . . .
H6A H 0.7599 0.6180 0.6036 0.188 Uiso 1 1 calc R . . . .
H6B H 0.7816 0.5727 0.6107 0.188 Uiso 1 1 calc R . . . .
C11 C 0.8570(7) 0.5378(6) 0.7048(10) 0.156(8) Uiso 1 1 d D . . . .
H11 H 0.8590 0.5561 0.7300 0.188 Uiso 1 1 calc R . . . .
C12 C 0.9003(6) 0.5174(8) 0.7054(12) 0.156(8) Uiso 1 1 d D . . . .
H12 H 0.8992 0.5063 0.7347 0.188 Uiso 1 1 calc R . . . .
C13 C 0.8994(7) 0.4746(10) 0.6822(14) 0.156(8) Uiso 1 1 d D . . . .
H13 H 0.8942 0.4826 0.6525 0.188 Uiso 1 1 calc R . . . .
C14 C 0.8629(8) 0.4472(7) 0.6925(11) 0.156(8) Uiso 1 1 d D . . . .
H14 H 0.8683 0.4351 0.7208 0.188 Uiso 1 1 calc R . . . .
C15 C 0.8205(7) 0.4693(8) 0.6949(10) 0.156(8) Uiso 1 1 d D . . . .
H15 H 0.8126 0.4761 0.6655 0.188 Uiso 1 1 calc R . . . .
C16 C 0.7803(8) 0.4543(9) 0.7162(8) 0.156(8) Uiso 1 1 d D . . . .
H16A H 0.7604 0.4779 0.7182 0.188 Uiso 1 1 calc R . . . .
H16B H 0.7673 0.4322 0.6989 0.188 Uiso 1 1 calc R . . . .
K1 K 0.8073(4) 0.5000 0.8073(4) 0.287(11) Uani 1 2 d S T P . .
O2 O 0.9257(8) 0.6910(8) 0.6332(9) 0.175(5) Uiso 1 1 d D . . . .
H2A H 0.9455 0.6759 0.6414 0.262 Uiso 1 1 calc R . . . .
O3 O 0.9287(8) 0.6271(8) 0.6868(8) 0.175(5) Uiso 1 1 d D . . . .
H3A H 0.9292 0.6028 0.6964 0.262 Uiso 1 1 calc R . . . .
O4 O 0.8748(8) 0.5659(7) 0.6726(8) 0.175(5) Uiso 1 1 d D . . . .
O5 O 0.8063(6) 0.6669(7) 0.6465(7) 0.175(5) Uiso 1 1 d D . . . .
O6 O 0.7539(11) 0.5963(9) 0.6644(9) 0.175(5) Uiso 1 1 d D . . . .
H6 H 0.7449 0.5719 0.6673 0.262 Uiso 1 1 calc GR . . . .
O12 O 0.9466(8) 0.5263(10) 0.7036(10) 0.175(5) Uiso 1 1 d D . . . .
H12A H 0.9598 0.5060 0.7136 0.262 Uiso 1 1 calc GR . . . .
O13 O 0.9387(8) 0.4502(10) 0.6798(9) 0.175(5) Uiso 1 1 d D . . . .
H13A H 0.9403 0.4342 0.7005 0.262 Uiso 1 1 calc GR . . . .
O14 O 0.8596(8) 0.4117(8) 0.6631(8) 0.175(5) Uiso 1 1 d D . . . .
O15 O 0.8224(6) 0.5099(7) 0.7172(7) 0.175(5) Uiso 1 1 d D . . . .
O16 O 0.7883(8) 0.4376(8) 0.7586(8) 0.175(5) Uiso 1 1 d D . . . .
H16 H 0.7814 0.4124 0.7595 0.262 Uiso 1 1 calc R . . . .
OA O 0.964(2) 0.464(2) 0.7500 0.46(5) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.500(3) . ?
C1 O5 1.450(3) . ?
C1 O14 1.66(4) 7_556 ?
C2 H2 0.9800 . ?
C2 C3 1.500(3) . ?
C2 O2 1.450(3) . ?
C3 H3 0.9800 . ?
C3 C4 1.500(3) . ?
C3 O3 1.450(3) . ?
C4 H4 0.9800 . ?
C4 C5 1.501(3) . ?
C4 O4 1.450(3) . ?
C5 H5 0.9800 . ?
C5 C6 1.500(3) . ?
C5 O5 1.451(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.450(3) . ?
C11 H11 0.9800 . ?
C11 C12 1.500(3) . ?
C11 O4 1.450(3) . ?
C11 O15 1.450(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.53(2) . ?
C12 O12 1.48(2) . ?
C13 H13 0.9800 . ?
C13 C14 1.47(2) . ?
C13 O13 1.450(3) . ?
C14 H14 0.9800 . ?
C14 C15 1.500(3) . ?
C14 O14 1.450(3) . ?
C15 H15 0.9800 . ?
C15 C16 1.500(3) . ?
C15 O15 1.450(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 K1 3.31(3) . ?
C16 O16 1.450(3) . ?
K1 C16 3.30(3) 23_565 ?
K1 O2 2.98(3) 44_666 ?
K1 O2 2.98(3) 41_646 ?
K1 O3 3.04(3) 44_666 ?
K1 O3 3.04(3) 41_646 ?
K1 O15 2.88(3) 23_565 ?
K1 O15 2.88(3) . ?
K1 O16 2.55(3) 23_565 ?
K1 O16 2.55(3) . ?
O2 K1 2.98(3) 42_566 ?
O2 H2A 0.8200 . ?
O3 K1 3.04(3) 42_566 ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O14 C1 1.66(4) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 111.6 . . ?
C2 C1 O14 94(2) . 7_556 ?
O5 C1 H1 111.6 . . ?
O5 C1 C2 120.9(15) . . ?
O5 C1 O14 105.4(17) . 7_556 ?
O14 C1 H1 111.6 7_556 . ?
C1 C2 H2 110.0 . . ?
C1 C2 C3 109.1(12) . . ?
C3 C2 H2 110.0 . . ?
O2 C2 C1 118(2) . . ?
O2 C2 H2 110.0 . . ?
O2 C2 C3 99.6(15) . . ?
C2 C3 H3 106.2 . . ?
C2 C3 C4 114.4(13) . . ?
C4 C3 H3 106.2 . . ?
O3 C3 C2 103.0(15) . . ?
O3 C3 H3 106.2 . . ?
O3 C3 C4 120(2) . . ?
C3 C4 H4 99.9 . . ?
C3 C4 C5 116.4(13) . . ?
C5 C4 H4 99.9 . . ?
O4 C4 C3 95.7(18) . . ?
O4 C4 H4 99.9 . . ?
O4 C4 C5 138(2) . . ?
C4 C5 H5 94.8 . . ?
C6 C5 C4 134.1(18) . . ?
C6 C5 H5 94.8 . . ?
O5 C5 C4 113.9(14) . . ?
O5 C5 H5 94.8 . . ?
O5 C5 C6 109.9(16) . . ?
C5 C6 H6A 112.7 . . ?
C5 C6 H6B 112.7 . . ?
H6A C6 H6B 110.2 . . ?
O6 C6 C5 95(2) . . ?
O6 C6 H6A 112.7 . . ?
O6 C6 H6B 112.7 . . ?
C12 C11 H11 100.6 . . ?
O4 C11 H11 100.6 . . ?
O4 C11 C12 85.5(12) . . ?
O4 C11 O15 147(3) . . ?
O15 C11 H11 100.6 . . ?
O15 C11 C12 114.5(14) . . ?
C11 C12 H12 97.7 . . ?
C11 C12 C13 110.7(15) . . ?
C13 C12 H12 97.7 . . ?
O12 C12 C11 144(2) . . ?
O12 C12 H12 97.7 . . ?
O12 C12 C13 100(3) . . ?
C12 C13 H13 103.2 . . ?
C14 C13 C12 115.0(17) . . ?
C14 C13 H13 103.2 . . ?
O13 C13 C12 118(3) . . ?
O13 C13 H13 103.2 . . ?
O13 C13 C14 112(3) . . ?
C13 C14 H14 106.7 . . ?
C13 C14 C15 115.7(16) . . ?
C15 C14 H14 106.7 . . ?
O14 C14 C13 111(3) . . ?
O14 C14 H14 106.7 . . ?
O14 C14 C15 108.9(15) . . ?
C14 C15 H15 106.0 . . ?
C14 C15 C16 128(3) . . ?
C16 C15 H15 106.0 . . ?
O15 C15 C14 113.2(13) . . ?
O15 C15 H15 106.0 . . ?
O15 C15 C16 95.5(14) . . ?
C15 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
C15 C16 K1 91.9(15) . . ?
H16A C16 H16B 107.9 . . ?
K1 C16 H16A 77.3 . . ?
K1 C16 H16B 154.3 . . ?
O16 C16 C15 112(3) . . ?
O16 C16 H16A 109.2 . . ?
O16 C16 H16B 109.2 . . ?
O16 C16 K1 47.2(14) . . ?
C16 K1 C16 75.3(11) 23_565 . ?
O2 K1 C16 152.0(8) 41_646 23_565 ?
O2 K1 C16 80.6(8) 41_646 . ?
O2 K1 C16 152.0(8) 44_666 . ?
O2 K1 C16 80.6(8) 44_666 23_565 ?
O2 K1 O2 125.9(12) 44_666 41_646 ?
O2 K1 O3 98.6(7) 44_666 41_646 ?
O2 K1 O3 51.5(6) 41_646 41_646 ?
O2 K1 O3 51.5(6) 44_666 44_666 ?
O2 K1 O3 98.6(7) 41_646 44_666 ?
O3 K1 C16 106.3(7) 41_646 . ?
O3 K1 C16 122.9(6) 44_666 . ?
O3 K1 C16 106.3(7) 44_666 23_565 ?
O3 K1 C16 122.9(6) 41_646 23_565 ?
O3 K1 O3 117.2(12) 44_666 41_646 ?
O15 K1 C16 40.6(5) 23_565 23_565 ?
O15 K1 C16 81.0(7) 23_565 . ?
O15 K1 C16 40.6(5) . . ?
O15 K1 C16 81.0(7) . 23_565 ?
O15 K1 O2 121.8(6) . 44_666 ?
O15 K1 O2 121.8(6) 23_565 41_646 ?
O15 K1 O2 89.9(6) . 41_646 ?
O15 K1 O2 89.9(6) 23_565 44_666 ?
O15 K1 O3 137.0(6) . 41_646 ?
O15 K1 O3 137.0(6) 23_565 44_666 ?
O15 K1 O3 82.5(6) 23_565 41_646 ?
O15 K1 O3 82.5(6) . 44_666 ?
O15 K1 O15 109.4(10) . 23_565 ?
O16 K1 C16 88.7(10) 23_565 . ?
O16 K1 C16 88.7(10) . 23_565 ?
O16 K1 C16 24.6(5) 23_565 23_565 ?
O16 K1 C16 24.6(5) . . ?
O16 K1 O2 63.8(7) 23_565 44_666 ?
O16 K1 O2 167.5(9) . 44_666 ?
O16 K1 O2 63.8(7) . 41_646 ?
O16 K1 O2 167.5(9) 23_565 41_646 ?
O16 K1 O3 139.2(7) 23_565 41_646 ?
O16 K1 O3 81.7(8) 23_565 44_666 ?
O16 K1 O3 139.2(7) . 44_666 ?
O16 K1 O3 81.7(8) . 41_646 ?
O16 K1 O15 77.7(8) 23_565 . ?
O16 K1 O15 62.2(8) . . ?
O16 K1 O15 62.2(8) 23_565 23_565 ?
O16 K1 O15 77.7(8) . 23_565 ?
O16 K1 O16 107.9(13) . 23_565 ?
C2 O2 K1 111.4(17) . 42_566 ?
C2 O2 H2A 109.5 . . ?
K1 O2 H2A 39.1 42_566 . ?
C3 O3 K1 122.5(15) . 42_566 ?
C3 O3 H3A 109.5 . . ?
K1 O3 H3A 126.4 42_566 . ?
C11 O4 C4 118.6(18) . . ?
C1 O5 C5 105.1(3) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12A 109.5 . . ?
C13 O13 H13A 109.5 . . ?
C14 O14 C1 112(2) . 5_565 ?
C11 O15 C15 115.5(15) . . ?
C11 O15 K1 116.8(18) . . ?
C15 O15 K1 111.8(16) . . ?
C16 O16 K1 108.1(19) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 141.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -36(3) . . . . ?
C1 C2 C3 O3 -168(3) . . . . ?
C1 C2 O2 K1 163.8(16) . . . 42_566 ?
C2 C1 O5 C5 -60(2) . . . . ?
C2 C3 C4 C5 38(4) . . . . ?
C2 C3 C4 O4 -169(2) . . . . ?
C2 C3 O3 K1 -34(2) . . . 42_566 ?
C3 C2 O2 K1 -78.7(16) . . . 42_566 ?
C3 C4 C5 C6 150(3) . . . . ?
C3 C4 C5 O5 -49(3) . . . . ?
C3 C4 O4 C11 143(3) . . . . ?
C4 C3 O3 K1 -162.0(19) . . . 42_566 ?
C4 C5 C6 O6 80(4) . . . . ?
C4 C5 O5 C1 55(2) . . . . ?
C5 C4 O4 C11 -76(5) . . . . ?
C6 C5 O5 C1 -140(3) . . . . ?
C11 C12 C13 C14 -45(4) . . . . ?
C11 C12 C13 O13 -180(3) . . . . ?
C12 C11 O4 C4 -161(3) . . . . ?
C12 C11 O15 C15 -52(4) . . . . ?
C12 C11 O15 K1 83(2) . . . . ?
C12 C13 C14 C15 43(4) . . . . ?
C12 C13 C14 O14 168(3) . . . . ?
C13 C14 C15 C16 -161(3) . . . . ?
C13 C14 C15 O15 -43(4) . . . . ?
C13 C14 O14 C1 141(2) . . . 5_565 ?
C14 C15 C16 K1 90(2) . . . . ?
C14 C15 C16 O16 46(3) . . . . ?
C14 C15 O15 C11 47(4) . . . . ?
C14 C15 O15 K1 -90(2) . . . . ?
C15 C14 O14 C1 -90(3) . . . 5_565 ?
C15 C16 O16 K1 71(2) . . . . ?
C16 C15 O15 C11 -177(3) . . . . ?
C16 C15 O15 K1 46(2) . . . . ?
O2 C2 C3 C4 -160(3) . . . . ?
O2 C2 C3 O3 69(2) . . . . ?
O3 C3 C4 C5 161(2) . . . . ?
O3 C3 C4 O4 -46(3) . . . . ?
O4 C4 C5 C6 13(6) . . . . ?
O4 C4 C5 O5 174(3) . . . . ?
O4 C11 C12 C13 -105(3) . . . . ?
O4 C11 C12 O12 40(6) . . . . ?
O4 C11 O15 C15 72(4) . . . . ?
O4 C11 O15 K1 -153(3) . . . . ?
O5 C1 C2 C3 51(3) . . . . ?
O5 C1 C2 O2 164(2) . . . . ?
O5 C5 C6 O6 -82(3) . . . . ?
O12 C12 C13 C14 156(3) . . . . ?
O12 C12 C13 O13 21(4) . . . . ?
O13 C13 C14 C15 -179(3) . . . . ?
O13 C13 C14 O14 -54(4) . . . . ?
O14 C1 C2 C3 -59(2) 7_556 . . . ?
O14 C1 C2 O2 53(2) 7_556 . . . ?
O14 C1 O5 C5 44(2) 7_556 . . . ?
O14 C14 C15 C16 73(4) . . . . ?
O14 C14 C15 O15 -169(2) . . . . ?
O15 C11 C12 C13 48(4) . . . . ?
O15 C11 C12 O12 -167(5) . . . . ?
O15 C11 O4 C4 68(5) . . . . ?
O15 C15 C16 K1 -35.6(19) . . . . ?
O15 C15 C16 O16 -80(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.767 -0.755 -0.506 13887.0 2416.9 ?


_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_olex2_submission_original_sample_id CDMOF_alpha_1_016
_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 1.452
_oxdiff_exptl_absorpt_empirical_full_min 0.832
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_b_295K
_database_code_depnum_ccdc_archive 'CCDC 1529141'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_REFNR01_CDMOF_b_295K        
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: 'Complexity of the molecular and crystal structures'
;
_vrf_THETM01_CDMOF_b_295K        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly diffracting sample crystal'
;
_vrf_PLAT090_CDMOF_b_295K        
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       3.27 Note  
RESPONSE: 'Data limited due to the poorly diffracting sample crystal; 
large number of parameters is the result of the complex molecular 
and crystal structures'
;
_vrf_PLAT084_CDMOF_b_295K        
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: 'Complexity of the molecular and crystal structures'
;
_vrf_PLAT306_CDMOF_b_295K        
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_b_295K        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04162 Ang.  
RESPONSE: 'The complexity of the molecular and crystal structures, 
along with low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT410_CDMOF_b_295K        
;
PROBLEM: Short Intra H...H Contact  H51    ..  H64     ..       1.89 Ang.  
RESPONSE: 'Result of the strained conformation'
;
_vrf_PLAT414_CDMOF_b_295K        
;
PROBLEM: Short Intra D-H..H-X       H32A   ..  H33     ..       1.82 Ang.  
RESPONSE: 'Result of the strained conformation'
;
_vrf_PLAT420_CDMOF_b_295K        
;
PROBLEM: D-H Without Acceptor       O6     --  H6     ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
# end Validation Reply Form
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2030 0.2500 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'



# CRYSTAL DATA

_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'


_cell_length_a                   43.6764(14)
_cell_length_b                   43.6764(14)
_cell_length_c                   28.1864(9)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_volume                     46565(3)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    21640
_cell_measurement_temperature    295
_cell_measurement_theta_max      15.4630
_cell_measurement_theta_min      2.2120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24881
_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    0.904
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             13392
_exptl_crystal_preparation       
'Crystallised from water solution by methanol vapour diffusion'
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40108
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        15.372
_diffrn_reflns_theta_max         15.372
_diffrn_reflns_theta_min         1.967
_diffrn_ambient_environment      'methanol:water mother liquor'
_diffrn_ambient_temperature      295.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -90.00  38.00   0.40    0.40    --   30.00  65.00 -80.00  320
  2  φ    -80.00  40.00   0.40    0.40  38.00  30.00  65.00    --   300
  3  ω    -90.00  38.00   0.40    0.40    --   30.00  65.00  40.00  320
  4  φ     40.00 160.00   0.40    0.40  38.00  30.00  65.00    --   300
  5  ω    -90.00  38.00   0.40    0.40    --   30.00  65.00 160.00  320
  6  ω    -90.00  38.00   0.40    0.40    --   30.00  30.00-160.00  320
  7  φ    -90.00 174.00   0.40    0.40  38.00  30.00   0.00    --   660
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Newport IS4CCD (4 circle), Pilatus 300K'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0111512000
_diffrn_orient_matrix_UB_12      0.0024165000
_diffrn_orient_matrix_UB_13      -0.0186823000
_diffrn_orient_matrix_UB_21      0.0117344000
_diffrn_orient_matrix_UB_22      0.0167165000
_diffrn_orient_matrix_UB_23      0.0082136000
_diffrn_orient_matrix_UB_31      0.0083647000
_diffrn_orient_matrix_UB_32      -0.0068265000
_diffrn_orient_matrix_UB_33      0.0134041000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   synchrotron
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                4688
_reflns_number_total             4856
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.549
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 
;
 Flack x determined using 1915 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.19(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         4856
_refine_ls_number_restraints     1229
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.1354
_refine_ls_restrained_S_all      3.052
_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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3715
_refine_ls_wR_factor_ref         0.3798
_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              

;
_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
 C41-C42
 1.5 with sigma of 0.02
 C65-C66
 1.5 with sigma of 0.02
 C54-C55
 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
 O14-C14
 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
 C21-C22
 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
 C26-C25
 1.5 with sigma of 0.02
 C31-O44
 1.45 with sigma of 0.02
 C44-C45
 1.5 with sigma of 0.02
 C55-C56
 1.5 with sigma of 0.02
 O56-C56
 1.45 with sigma of 0.005
 O63-C63
 1.45 with sigma of 0.005
 C62-C63
 1.5 with sigma of 0.02
 C62-C61
 1.5 with sigma of 0.02
 C74-C75
 1.5 with sigma of 0.02
 C72-C73
 1.5 with sigma of 0.02
 C74-C73
 1.5 with sigma of 0.005
 C13-C14
 1.5 with sigma of 0.02
 C13-C12
 1.5 with sigma of 0.02
 C75-C76
 1.5 with sigma of 0.02
 O76-C76
 1.45 with sigma of 0.005
 C12-K001
 3.7 with sigma of 0.02
 C72-O72
 1.45 with sigma of 0.02
 C73-O73
 1.45 with sigma of 0.02
 C42-C43
 1.5 with sigma of 0.02
 C44-C43
 1.5 with sigma of 0.02
 C26-O26
 1.45 with sigma of 0.005
 C11-C12
 1.5 with sigma of 0.02
 O15-C11
 1.45 with sigma of 0.02
 C12-O12
 1.45 with sigma of 0.02
 O34-C21
 1.45 with sigma of 0.02
 C15-O15
 1.45 with sigma of 0.02
 O24-C11
 1.45 with sigma of 0.02
 C1-O14
 1.45 with sigma of 0.02
 C41-C54
 2.5 with sigma of 0.02
 C71-C72
 1.5 with sigma of 0.02
 C71-O4
 1.45 with sigma of 0.02
 C65-C64
 1.5 with sigma of 0.02
 C65-O65
 1.45 with sigma of 0.02
 C6-C5
 1.5 with sigma of 0.005
 O65-C61
 1.45 with sigma of 0.02
 C63-C64
 1.5 with sigma of 0.01
 C64-C63
 1.5 with sigma of 0.02
 C24-C25
 1.5 with sigma of 0.02
 C14-C15
 1.5 with sigma of 0.02
 C4-C1
 3.5 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.005
 O44-C44
 1.45 with sigma of 0.02
 C53-C52
 1.5 with sigma of 0.02
 O24-C24
 1.45 with sigma of 0.02
 O74-C61
 1.45 with sigma of 0.02
 O14-C1
 1.45 with sigma of 0.02
 O2-C2
 1.45 with sigma of 0.02
 C6-O6
 1.45 with sigma of 0.02
 O16-C16
 1.45 with sigma of 0.01
 O43-C43
 1.45 with sigma of 0.02
 C43-O43
 1.45 with sigma of 0.01
 O22-C22
 1.45 with sigma of 0.02
 O25-C25
 1.45 with sigma of 0.02
 C21-O25
 1.45 with sigma of 0.02
 O66-C66
 1.45 with sigma of 0.02
 C45-C46
 1.5 with sigma of 0.02
 C46-O46
 1.45 with sigma of 0.02
 C31-O35
 1.45 with sigma of 0.005
 O42-C42
 1.45 with sigma of 0.02
 C36-O36
 1.45 with sigma of 0.02
 O62-C62
 1.45 with sigma of 0.02
 C4-O4
 1.45 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C4-C3
 1.5 with sigma of 0.005
 C5-C3
 2.5 with sigma of 0.02
 O3-C3
 1.45 with sigma of 0.02
 C35-O35
 1.45 with sigma of 0.01
 O23-C23
 1.45 with sigma of 0.02
 C35-C36
 1.5 with sigma of 0.02
 C53-C54
 1.5 with sigma of 0.02
 C71-O75
 1.45 with sigma of 0.02
 O75-C75
 1.45 with sigma of 0.01
 O15-C15
 1.45 with sigma of 0.01
 C51-O55
 1.45 with sigma of 0.02
 C64-O64
 1.45 with sigma of 0.02
 C74-O74
 1.5 with sigma of 0.02
 C64-C65
 1.5 with sigma of 0.02
 O64-C64
 1.45 with sigma of 0.02
 C51-C52
 1.5 with sigma of 0.02
 C31-C32
 1.5 with sigma of 0.02
 C34-O34
 1.45 with sigma of 0.02
 O34-C34
 1.45 with sigma of 0.02
 C35-C34
 1.5 with sigma of 0.01
 C33-O35
 3 with sigma of 0.02
 C33-C34
 1.5 with sigma of 0.02
 O33-C33
 1.45 with sigma of 0.01
 O33-O32
 2.4 with sigma of 0.02
 C33-C32
 1.5 with sigma of 0.01
 C11-C13
 2.5 with sigma of 0.04
 C12-O15
 2.5 with sigma of 0.04
 O24-O15
 2.5 with sigma of 0.04
 O24-C12
 2.5 with sigma of 0.04
 C56-O55
 2.5 with sigma of 0.04
 C56-C54
 2.5 with sigma of 0.04
 C73-C71
 2.5 with sigma of 0.04
 C61-O62
 2.5 with sigma of 0.04
 O62-C63
 2.5 with sigma of 0.04
 C24-C11
 2.5 with sigma of 0.04
 C5-C1
 2.5 with sigma of 0.04
 O5-C6
 2.5 with sigma of 0.04
 C6-C4
 2.5 with sigma of 0.04
 C16-O15
 2.5 with sigma of 0.04
 C16-C14
 2.5 with sigma of 0.04
 C44-O45
 2.5 with sigma of 0.04
 C44-C42
 2.5 with sigma of 0.04
 C45-C41
 2.5 with sigma of 0.04
 C45-C43
 2.5 with sigma of 0.04
 C66-C64
 2.5 with sigma of 0.04
 C66-O65
 2.5 with sigma of 0.04
 C65-C63
 2.5 with sigma of 0.04
 C65-C61
 2.5 with sigma of 0.04
 C75-O76
 2.5 with sigma of 0.04
 C76-O75
 2.5 with sigma of 0.04
 C76-C74
 2.5 with sigma of 0.04
 C72-O4
 2.5 with sigma of 0.04
 O4-O75
 2.5 with sigma of 0.04
 O72-C71
 2.5 with sigma of 0.04
 O72-C73
 2.5 with sigma of 0.04
 C72-O75
 2.5 with sigma of 0.04
 C72-C74
 2.5 with sigma of 0.04
 C11-C24
 2.6 with sigma of 0.04
 C71-C4
 2.5 with sigma of 0.01
 O44-C45
 2.5 with sigma of 0.04
 O44-C43
 2.5 with sigma of 0.04
 O32-C31
 2.5 with sigma of 0.04
 C64-C51
 2.3 with sigma of 0.04
 C51-C64
 2.4 with sigma of 0.04
 C1-C14
 2.6 with sigma of 0.04
 C74-C61
 2.6 with sigma of 0.04
 C5-O6
 2.5 with sigma of 0.04
 O16-C15
 2.5 with sigma of 0.04
 C14-C1
 2.6 with sigma of 0.02
 C21-C23
 2.5 with sigma of 0.04
 O43-C44
 2.5 with sigma of 0.04
 O43-C42
 2.5 with sigma of 0.04
 O22-C23
 2.5 with sigma of 0.04
 O25-C22
 2.5 with sigma of 0.04
 C2-O3
 2.5 with sigma of 0.04
 C25-C21
 2.5 with sigma of 0.04
 C25-C23
 2.5 with sigma of 0.04
 C46-O45
 2.5 with sigma of 0.04
 C46-C44
 2.5 with sigma of 0.04
 O46-C45
 2.5 with sigma of 0.04
 O44-O35
 2.5 with sigma of 0.04
 O22-C21
 2.5 with sigma of 0.04
 C23-C21
 2.5 with sigma of 0.04
 C4-C2
 2.5 with sigma of 0.04
 C4-C71
 2.6 with sigma of 0.02
 O3-C4
 2.5 with sigma of 0.04
 C5-C3
 2.5 with sigma of 0.04
 C3-C1
 2.4 with sigma of 0.04
 O34-C35
 2.5 with sigma of 0.04
 C31-C35
 2.5 with sigma of 0.04
 O36-C35
 2.4 with sigma of 0.01
 C35-C31
 2.4 with sigma of 0.01
 C35-O34
 2.4 with sigma of 0.01
 O23-C22
 2.5 with sigma of 0.04
 O23-C24
 2.5 with sigma of 0.04
 C36-O35
 2.5 with sigma of 0.04
 C75-C71
 2.5 with sigma of 0.04
 C15-C11
 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
 C71-C75
 2.5 with sigma of 0.04
 O75-C72
 2.5 with sigma of 0.04
 O75-C74
 2.5 with sigma of 0.04
 C51-C53
 2.5 with sigma of 0.04
 C52-O55
 2.5 with sigma of 0.04
 C51-C55
 2.5 with sigma of 0.04
 C64-C62
 2.5 with sigma of 0.04
 O44-C32
 2.5 with sigma of 0.04
 C32-O35
 2.5 with sigma of 0.04
 C21-C34
 2.5 with sigma of 0.04
 C32-C34
 2.5 with sigma of 0.04
 C34-C32
 2.5 with sigma of 0.04
 C34-O35
 2.5 with sigma of 0.04
 C34-C21
 2.4 with sigma of 0.04
 C36-C34
 2.5 with sigma of 0.04
 C32-O33
 2.5 with sigma of 0.04
 C34-O33
 2.5 with sigma of 0.04
 O33-C32
 2.6 with sigma of 0.01
 O33-C34
 2.6 with sigma of 0.01
 O34-C33
 2.5 with sigma of 0.04
 C33-C31
 2.5 with sigma of 0.04
 C33-O34
 2.5 with sigma of 0.04
 C31-C33
 2.5 with sigma of 0.04
 C33-O32
 2.5 with sigma of 0.04
 C33-C35
 2.5 with sigma of 0.04
 C35-C33
 2.4 with sigma of 0.02
3. Rigid bond restraints
 C44
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 OA, OB
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O4: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.005
C44: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.005
O52: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
O5 \\sim O6 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O22 \\sim
O23 \\sim O24 \\sim O25 \\sim O26 \\sim O32: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
O2 \\sim O3: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C45 \\sim C46 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C71 \\sim C72 \\sim
C73 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
OA \\sim OB: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O46: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O34 \\sim O35: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
O53 \\sim O54 \\sim O55 \\sim O56 \\sim O62 \\sim O63 \\sim O64 \\sim O65 \\sim
O66 \\sim O72 \\sim O73 \\sim O74 \\sim O75 \\sim O76: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C11 \\sim C12 \\sim C13
\\sim C14 \\sim C15 \\sim C16 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C41
\\sim C42 \\sim C43: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
Uanis(C44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of
0.00001
Uanis(C45) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.0001
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O46) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O36) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O33) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Uiso(OA)=Uiso(OB)=FVAR(1)
 Fixed U11: C44(0.204927)
 Fixed U13: C44(0.104258)
 Fixed U22: C44(0.2037)
 Fixed X: C3(0.72001) C35(0.90214)
 Fixed Y: C3(0.65503) C35(0.54048)
 Fixed Z: C3(0.48914) C35(0.53339)
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(H6A,H6B), C16(H16A,H16B), C26(H26A,H26B), 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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7486(7) 0.6695(7) 0.4011(9) 0.201(5) Uani 1 1 d D U . . .
H1 H 0.7593 0.6866 0.3752 0.241 Uiso 1 1 calc R . . . .
C2 C 0.7420(9) 0.6801(7) 0.4520(9) 0.203(5) Uani 1 1 d D U . . .
H2 H 0.7279 0.6911 0.4442 0.244 Uiso 1 1 calc R . . . .
C3 C 0.7200 0.6550 0.4891 0.213(6) Uani 1 1 d D U . . .
H3 H 0.7366 0.6501 0.5063 0.255 Uiso 1 1 calc R . . . .
C4 C 0.6893(6) 0.6187(4) 0.4783(8) 0.197(6) Uani 1 1 d D U . . .
H4 H 0.6698 0.6226 0.4702 0.236 Uiso 1 1 calc R . . . .
C5 C 0.6979(8) 0.6064(8) 0.4328(10) 0.207(5) Uani 1 1 d D U . . .
H5 H 0.7152 0.5995 0.4417 0.249 Uiso 1 1 calc R . . . .
C6 C 0.6668(8) 0.5733(8) 0.4138(14) 0.216(6) Uani 1 1 d D U . . .
H6A H 0.6743 0.5655 0.3861 0.259 Uiso 1 1 calc R . . . .
H6B H 0.6589 0.5549 0.4376 0.259 Uiso 1 1 calc R . . . .
C11 C 0.8627(8) 0.6720(8) 0.3744(11) 0.198(5) Uani 1 1 d D U . . .
H11 H 0.8845 0.6810 0.3558 0.238 Uiso 1 1 calc R . . . .
C12 C 0.8564(8) 0.7019(6) 0.3837(12) 0.195(5) Uani 1 1 d D U . . .
H12 H 0.8562 0.7139 0.3544 0.234 Uiso 1 1 calc R . . . .
C13 C 0.8243(9) 0.6917(8) 0.4138(14) 0.190(6) Uani 1 1 d D U . . .
H13 H 0.8328 0.6872 0.4437 0.228 Uiso 1 1 calc R . . . .
C14 C 0.7982(7) 0.6538(8) 0.4002(13) 0.191(6) Uani 1 1 d D U . . .
H14 H 0.7935 0.6607 0.3691 0.229 Uiso 1 1 calc R . . . .
C15 C 0.8042(7) 0.6251(7) 0.3790(10) 0.196(5) Uani 1 1 d D U . . .
H15 H 0.8115 0.6139 0.4030 0.235 Uiso 1 1 calc R . . . .
C16 C 0.7700(9) 0.5990(8) 0.3552(10) 0.197(7) Uani 1 1 d D U . . .
H16A H 0.7694 0.5768 0.3494 0.236 Uiso 1 1 calc R . . . .
H16B H 0.7499 0.5945 0.3748 0.236 Uiso 1 1 calc R . . . .
C21 C 0.9364(10) 0.6164(8) 0.4540(10) 0.236(5) Uani 1 1 d D U . . .
H21 H 0.9585 0.6157 0.4527 0.284 Uiso 1 1 calc R . . . .
C22 C 0.9455(11) 0.6537(10) 0.4642(13) 0.231(6) Uani 1 1 d D U . . .
H22 H 0.9677 0.6688 0.4474 0.277 Uiso 1 1 calc R . . . .
C23 C 0.9217(11) 0.6668(9) 0.4513(14) 0.220(7) Uani 1 1 d D U . . .
H23 H 0.9056 0.6560 0.4782 0.264 Uiso 1 1 calc R . . . .
C24 C 0.8957(9) 0.6459(9) 0.4147(14) 0.215(6) Uani 1 1 d D U . . .
H24 H 0.9080 0.6579 0.3855 0.257 Uiso 1 1 calc R . . . .
C25 C 0.8883(11) 0.6096(10) 0.4065(14) 0.228(5) Uani 1 1 d D U . . .
H25 H 0.8695 0.5936 0.4281 0.273 Uiso 1 1 calc R . . . .
C26 C 0.8756(11) 0.5995(13) 0.3555(12) 0.229(7) Uani 1 1 d D U . . .
H26A H 0.8561 0.5754 0.3564 0.275 Uiso 1 1 calc R . . . .
H26B H 0.8656 0.6141 0.3463 0.275 Uiso 1 1 calc R . . . .
C31 C 0.9282(7) 0.5424(8) 0.6087(6) 0.230(5) Uani 1 1 d D U . . .
H31 H 0.9356 0.5295 0.6298 0.276 Uiso 1 1 calc R . . . .
C32 C 0.9555(9) 0.5781(7) 0.6061(10) 0.237(6) Uani 1 1 d D U . . .
H32 H 0.9774 0.5779 0.5991 0.284 Uiso 1 1 calc R . . . .
C33 C 0.9511(9) 0.6001(5) 0.5668(10) 0.262(8) Uani 1 1 d D U . . .
H33 H 0.9345 0.6059 0.5822 0.314 Uiso 1 1 calc R . . . .
C34 C 0.9294(8) 0.5787(4) 0.5260(11) 0.264(8) Uani 1 1 d D U . . .
H34 H 0.9469 0.5772 0.5060 0.316 Uiso 1 1 calc R . . . .
C35 C 0.9021 0.5405 0.5334 0.266(7) Uani 1 1 d D U . . .
H35 H 0.8860 0.5423 0.5559 0.319 Uiso 1 1 calc R . . . .
C36 C 0.8778(10) 0.5180(12) 0.4969(12) 0.268(9) Uani 1 1 d D U . . .
H36A H 0.8602 0.4963 0.5120 0.321 Uiso 1 1 calc R . . . .
H36B H 0.8655 0.5297 0.4847 0.321 Uiso 1 1 calc R . . . .
C41 C 0.8336(7) 0.4904(8) 0.7570(11) 0.163(4) Uani 1 1 d D U . . .
H41 H 0.8285 0.4779 0.7874 0.195 Uiso 1 1 calc R . . . .
C42 C 0.8643(8) 0.5272(7) 0.7563(9) 0.162(4) Uani 1 1 d D U . . .
H42 H 0.8828 0.5235 0.7699 0.195 Uiso 1 1 calc R . . . .
C43 C 0.8829(7) 0.5485(7) 0.7125(9) 0.174(5) Uani 1 1 d D U . . .
H43 H 0.8688 0.5580 0.6989 0.209 Uiso 1 1 calc R . . . .
C44 C 0.8866(10) 0.5255(7) 0.6758(10) 0.2053(7) Uani 1 1 d D U . . .
H44 H 0.9061 0.5222 0.6864 0.246 Uiso 1 1 calc R . . . .
C45 C 0.8541(9) 0.4894(8) 0.6750(12) 0.191(3) Uani 1 1 d D U . . .
H45 H 0.8353 0.4946 0.6677 0.229 Uiso 1 1 calc R . . . .
C46 C 0.8514(11) 0.4653(10) 0.6343(11) 0.201(6) Uani 1 1 d D U . . .
H46A H 0.8279 0.4448 0.6325 0.241 Uiso 1 1 calc R . . . .
H46B H 0.8570 0.4777 0.6042 0.241 Uiso 1 1 calc R . . . .
C51 C 0.7066(6) 0.4687(7) 0.7753(10) 0.140(4) Uani 1 1 d D U . . .
H51 H 0.6830 0.4566 0.7896 0.168 Uiso 1 1 calc R . . . .
C52 C 0.7324(6) 0.4842(7) 0.8167(9) 0.138(4) Uani 1 1 d D U . . .
H52 H 0.7319 0.4664 0.8385 0.166 Uiso 1 1 calc R . . . .
C53 C 0.7666(6) 0.5044(7) 0.7894(10) 0.143(5) Uani 1 1 d D U . . .
H53 H 0.7640 0.5222 0.7715 0.172 Uiso 1 1 calc R . . . .
C54 C 0.7722(6) 0.4818(8) 0.7508(10) 0.149(5) Uani 1 1 d D U . . .
H54 H 0.7730 0.4644 0.7720 0.178 Uiso 1 1 calc R . . . .
C55 C 0.7419(7) 0.4565(7) 0.7201(11) 0.149(4) Uani 1 1 d D U . . .
H55 H 0.7379 0.4701 0.6957 0.179 Uiso 1 1 calc R . . . .
C56 C 0.7433(8) 0.4264(7) 0.6963(8) 0.155(5) Uani 1 1 d D U . . .
H56A H 0.7216 0.4110 0.6793 0.185 Uiso 1 1 calc R . . . .
H56B H 0.7633 0.4347 0.6750 0.185 Uiso 1 1 calc R . . . .
C61 C 0.6331(7) 0.5178(6) 0.6924(9) 0.150(4) Uani 1 1 d D U . . .
H61 H 0.6109 0.5182 0.6911 0.180 Uiso 1 1 calc R . . . .
C62 C 0.6505(7) 0.5378(8) 0.7363(11) 0.156(5) Uani 1 1 d D U . . .
H62 H 0.6342 0.5212 0.7599 0.188 Uiso 1 1 calc R . . . .
C63 C 0.6798(7) 0.5304(6) 0.7411(9) 0.155(5) Uani 1 1 d D U . . .
H63 H 0.6964 0.5440 0.7157 0.186 Uiso 1 1 calc R . . . .
C64 C 0.6746(6) 0.4940(6) 0.7368(10) 0.143(5) Uani 1 1 d D U . . .
H64 H 0.6626 0.4830 0.7666 0.172 Uiso 1 1 calc R . . . .
C65 C 0.6482(6) 0.4717(6) 0.7011(10) 0.134(5) Uani 1 1 d D U . . .
H65 H 0.6636 0.4815 0.6734 0.161 Uiso 1 1 calc R . . . .
C66 C 0.6387(6) 0.4350(6) 0.6932(10) 0.132(5) Uani 1 1 d D U . . .
H66A H 0.6593 0.4323 0.6977 0.158 Uiso 1 1 calc R . . . .
H66B H 0.6301 0.4279 0.6611 0.158 Uiso 1 1 calc R . . . .
C71 C 0.6389(6) 0.5839(6) 0.5349(9) 0.176(4) Uani 1 1 d D U . . .
H71 H 0.6288 0.5925 0.5109 0.211 Uiso 1 1 calc R . . . .
C72 C 0.6438(9) 0.6041(6) 0.5794(9) 0.172(5) Uani 1 1 d D U . . .
H72 H 0.6200 0.6008 0.5835 0.207 Uiso 1 1 calc R . . . .
C73 C 0.6476(8) 0.5882(6) 0.6243(9) 0.167(5) Uani 1 1 d D U . . .
H73 H 0.6730 0.5970 0.6265 0.200 Uiso 1 1 calc R . . . .
C74 C 0.6315(8) 0.5490(6) 0.6199(9) 0.163(5) Uani 1 1 d D U . . .
H74 H 0.6068 0.5373 0.6301 0.196 Uiso 1 1 calc R . . . .
C75 C 0.6342(9) 0.5340(7) 0.5727(9) 0.170(5) Uani 1 1 d D U . . .
H75 H 0.6593 0.5477 0.5645 0.204 Uiso 1 1 calc R . . . .
C76 C 0.6265(8) 0.4975(7) 0.5750(12) 0.171(7) Uani 1 1 d D U . . .
H76A H 0.6477 0.4973 0.5655 0.205 Uiso 1 1 calc R . . . .
H76B H 0.6221 0.4902 0.6079 0.205 Uiso 1 1 calc R . . . .
K001 K 0.8962(2) 0.7933(2) 0.4203(2) 0.155(2) Uani 1 1 d D U . . .
K002 K 0.6667 0.6390(4) 0.3333 0.216(4) Uani 1 2 d S TU P . .
K003 K 0.9749(5) 0.6416(5) 0.3333 0.257(6) Uani 1 2 d S TU P . .
O2 O 0.7732(7) 0.7097(7) 0.4716(10) 0.201(7) Uani 1 1 d D U . . .
H2A H 0.7758 0.7054 0.4991 0.302 Uiso 1 1 calc R . . . .
O3 O 0.7058(8) 0.6685(7) 0.5269(9) 0.215(8) Uani 1 1 d D U . . .
H3A H 0.7214 0.6801 0.5461 0.322 Uiso 1 1 calc R . . . .
O4 O 0.6760(6) 0.5936(6) 0.5191(9) 0.185(5) Uani 1 1 d D U . . .
O5 O 0.7153(7) 0.6335(6) 0.3946(9) 0.204(5) Uani 1 1 d D U . . .
O6 O 0.6378(8) 0.5783(8) 0.4008(10) 0.221(7) Uani 1 1 d D U . . .
H6 H 0.6199 0.5639 0.4149 0.332 Uiso 1 1 calc R . . . .
O12 O 0.8906(7) 0.7215(6) 0.4093(9) 0.193(6) Uani 1 1 d D U . . .
H12A H 0.8968 0.7077 0.4183 0.289 Uiso 1 1 calc R . . . .
O13 O 0.8260(6) 0.7281(6) 0.4279(7) 0.171(6) Uani 1 1 d . U . . .
H13A H 0.8088 0.7239 0.4442 0.257 Uiso 1 1 calc R . . . .
O14 O 0.7653(7) 0.6505(6) 0.4214(9) 0.193(5) Uani 1 1 d D U . . .
O15 O 0.8327(6) 0.6458(6) 0.3446(8) 0.200(5) Uani 1 1 d D U . . .
O16 O 0.7696(7) 0.6157(6) 0.3108(8) 0.194(7) Uani 1 1 d D U . . .
H16 H 0.7873 0.6203 0.2953 0.291 Uiso 1 1 calc R . . . .
O22 O 0.9544(10) 0.6581(10) 0.5145(11) 0.253(9) Uani 1 1 d D U . . .
H22A H 0.9616 0.6787 0.5222 0.379 Uiso 1 1 calc R . . . .
O23 O 0.9275(11) 0.7029(9) 0.4588(16) 0.292(15) Uani 1 1 d D U . . .
H23A H 0.9445 0.7139 0.4765 0.438 Uiso 1 1 calc R . . . .
O24 O 0.8653(7) 0.6528(7) 0.4156(9) 0.204(5) Uani 1 1 d D U . . .
O25 O 0.9180(9) 0.6029(9) 0.4098(11) 0.235(5) Uani 1 1 d D U . . .
O26 O 0.8984(9) 0.6014(9) 0.3169(11) 0.238(8) Uani 1 1 d D U . . .
H26 H 0.8966 0.6127 0.2949 0.357 Uiso 1 1 calc R . . . .
O32 O 0.9647(7) 0.6071(8) 0.6465(8) 0.222(7) Uani 1 1 d D U . . .
H32A H 0.9554 0.6188 0.6402 0.333 Uiso 1 1 calc R . . . .
O33 O 0.9821(9) 0.6358(6) 0.5611(9) 0.303(13) Uani 1 1 d D U . . .
H33A H 0.9881 0.6391 0.5332 0.455 Uiso 1 1 calc R . . . .
O34 O 0.9163(9) 0.5960(5) 0.4952(9) 0.255(6) Uani 1 1 d D U . . .
O35 O 0.9180(6) 0.5245(6) 0.5631(6) 0.238(6) Uani 1 1 d D U . . .
O36 O 0.8917(11) 0.5087(12) 0.4579(10) 0.295(16) Uani 1 1 d D U . . .
H36 H 0.8812 0.4872 0.4551 0.443 Uiso 1 1 calc R . . . .
O42 O 0.8603(5) 0.5480(6) 0.7937(8) 0.173(6) Uani 1 1 d D U . . .
H42A H 0.8698 0.5688 0.7855 0.259 Uiso 1 1 calc R . . . .
O43 O 0.9177(5) 0.5779(6) 0.7245(8) 0.171(5) Uani 1 1 d D U . . .
H43A H 0.9329 0.5757 0.7103 0.257 Uiso 1 1 calc R . . . .
O44 O 0.8966(7) 0.5421(7) 0.6295(8) 0.210(5) Uani 1 1 d D U . . .
O45 O 0.8453(5) 0.4751(6) 0.7163(8) 0.165(4) Uani 1 1 d D U . . .
O46 O 0.8770(6) 0.4551(5) 0.6459(8) 0.173(6) Uani 1 1 d D U . . .
H46 H 0.8852 0.4519 0.6215 0.260 Uiso 1 1 calc R . . . .
O52 O 0.7240(5) 0.5106(5) 0.8403(7) 0.136(5) Uani 1 1 d . U . . .
H52A H 0.7414 0.5253 0.8549 0.204 Uiso 1 1 calc R . . . .
O53 O 0.7904(5) 0.5239(5) 0.8283(7) 0.150(5) Uani 1 1 d . U . . .
H53A H 0.8105 0.5288 0.8214 0.225 Uiso 1 1 calc R . . . .
O54 O 0.8090(5) 0.5029(6) 0.7422(8) 0.158(4) Uani 1 1 d . U . . .
O55 O 0.7111(4) 0.4417(5) 0.7542(7) 0.144(4) Uani 1 1 d D U . . .
O56 O 0.7475(7) 0.4095(6) 0.7381(8) 0.180(7) Uani 1 1 d D U . . .
H56 H 0.7316 0.4054 0.7571 0.269 Uiso 1 1 calc R . . . .
O62 O 0.6545(8) 0.5679(8) 0.7543(11) 0.223(10) Uani 1 1 d D U . . .
H62A H 0.6720 0.5770 0.7715 0.334 Uiso 1 1 calc R . . . .
O63 O 0.6986(6) 0.5466(6) 0.7848(8) 0.182(7) Uani 1 1 d D U . . .
H63A H 0.7119 0.5390 0.7913 0.274 Uiso 1 1 calc R . . . .
O64 O 0.7057(4) 0.4920(5) 0.7398(7) 0.140(4) Uani 1 1 d D U . . .
O65 O 0.6221(5) 0.4803(5) 0.6860(7) 0.146(4) Uani 1 1 d D U . . .
O66 O 0.6109(5) 0.4127(5) 0.7276(7) 0.152(6) Uani 1 1 d D U . . .
H66 H 0.6005 0.3922 0.7183 0.228 Uiso 1 1 calc R . . . .
O72 O 0.6653(7) 0.6431(6) 0.5780(8) 0.191(7) Uani 1 1 d D U . . .
H72A H 0.6603 0.6514 0.6008 0.286 Uiso 1 1 calc R . . . .
O73 O 0.6391(6) 0.5987(5) 0.6689(8) 0.164(6) Uani 1 1 d D U . . .
H73A H 0.6435 0.5892 0.6908 0.245 Uiso 1 1 calc R . . . .
O74 O 0.6512(5) 0.5353(5) 0.6485(7) 0.153(4) Uani 1 1 d D U . . .
O75 O 0.6166(6) 0.5444(5) 0.5372(8) 0.174(4) Uani 1 1 d D U . . .
O76 O 0.5975(8) 0.4709(7) 0.5473(14) 0.256(15) Uani 1 1 d D U . . .
H76 H 0.5921 0.4805 0.5265 0.385 Uiso 1 1 calc R . . . .
OA O 0.9373(12) 0.7093(12) 0.5443(12) 0.274(11) Uiso 1 1 d . U . . .
OB O 0.7621(11) 0.6927(12) 0.5691(14) 0.274(11) Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.58(3) . ?
C1 O5 1.53(3) . ?
C1 O14 1.47(2) . ?
C2 H2 0.9800 . ?
C2 C3 1.47(2) . ?
C2 O2 1.44(3) . ?
C3 H3 0.9800 . ?
C3 C4 1.511(8) . ?
C3 O3 1.492(19) . ?
C4 H4 0.9800 . ?
C4 C5 1.507(8) . ?
C4 O4 1.49(2) . ?
C5 H5 0.9800 . ?
C5 C6 1.501(8) . ?
C5 O5 1.50(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.44(3) . ?
C11 H11 0.9800 . ?
C11 C12 1.48(2) . ?
C11 O15 1.50(3) . ?
C11 O24 1.47(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.50(3) . ?
C12 O12 1.48(3) . ?
C13 H13 0.9800 . ?
C13 C14 1.52(3) . ?
C13 O13 1.60(4) . ?
C14 H14 0.9800 . ?
C14 C15 1.53(3) . ?
C14 O14 1.50(2) . ?
C15 H15 0.9800 . ?
C15 C16 1.51(3) . ?
C15 O15 1.475(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 O16 1.455(15) . ?
C21 H21 0.9800 . ?
C21 C22 1.50(3) . ?
C21 O25 1.44(3) . ?
C21 O34 1.46(3) . ?
C22 H22 0.9800 . ?
C22 C23 1.46(3) . ?
C22 O22 1.46(3) . ?
C23 H23 0.9800 . ?
C23 C24 1.47(3) . ?
C23 O23 1.48(3) . ?
C24 H24 0.9800 . ?
C24 C25 1.47(3) . ?
C24 O24 1.50(3) . ?
C25 H25 0.9800 . ?
C25 C26 1.53(3) . ?
C25 O25 1.47(3) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 O26 1.449(8) . ?
C31 H31 0.9800 . ?
C31 C32 1.41(2) . ?
C31 O35 1.452(8) . ?
C31 O44 1.49(3) . ?
C32 H32 0.9800 . ?
C32 C33 1.540(15) . ?
C32 O32 1.60(4) . ?
C33 H33 0.9800 . ?
C33 C34 1.49(2) . ?
C33 O33 1.476(15) . ?
C34 H34 0.9800 . ?
C34 C35 1.504(14) . ?
C34 O34 1.44(2) . ?
C35 H35 0.9800 . ?
C35 C36 1.45(3) . ?
C35 O35 1.466(14) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 O36 1.41(3) . ?
C41 H41 0.9800 . ?
C41 C42 1.49(3) . ?
C41 O45 1.54(3) . ?
C41 O54 1.49(3) . ?
C42 H42 0.9800 . ?
C42 C43 1.51(3) . ?
C42 O42 1.46(2) . ?
C43 H43 0.9800 . ?
C43 C44 1.50(2) . ?
C43 O43 1.456(14) . ?
C44 H44 0.9800 . ?
C44 C45 1.50(3) . ?
C44 O44 1.45(3) . ?
C45 H45 0.9800 . ?
C45 C46 1.52(3) . ?
C45 O45 1.28(3) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 O46 1.43(3) . ?
C51 H51 0.9800 . ?
C51 C52 1.53(2) . ?
C51 O55 1.42(2) . ?
C51 O64 1.44(3) . ?
C52 H52 0.9800 . ?
C52 C53 1.51(2) . ?
C52 K001 3.46(3) 10_566 ?
C52 O52 1.53(3) . ?
C53 H53 0.9800 . ?
C53 C54 1.57(3) . ?
C53 O53 1.46(3) . ?
C54 H54 0.9800 . ?
C54 C55 1.50(2) . ?
C54 O54 1.42(3) . ?
C55 H55 0.9800 . ?
C55 C56 1.50(2) . ?
C55 O55 1.51(3) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 O56 1.450(8) . ?
C61 H61 0.9800 . ?
C61 C62 1.49(2) . ?
C61 O65 1.47(2) . ?
C61 O74 1.46(2) . ?
C62 H62 0.9800 . ?
C62 C63 1.48(2) . ?
C62 O62 1.34(2) . ?
C63 H63 0.9800 . ?
C63 C64 1.497(14) . ?
C63 O63 1.451(8) . ?
C64 H64 0.9800 . ?
C64 C65 1.473(19) . ?
C64 O64 1.404(18) . ?
C65 H65 0.9800 . ?
C65 C66 1.46(2) . ?
C65 K001 3.53(3) 9_565 ?
C65 O65 1.43(2) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C66 O66 1.48(2) . ?
C71 H71 0.9800 . ?
C71 C72 1.49(2) . ?
C71 O4 1.52(2) . ?
C71 O75 1.50(2) . ?
C72 H72 0.9800 . ?
C72 C73 1.49(2) . ?
C72 O72 1.48(2) . ?
C73 H73 0.9800 . ?
C73 C74 1.498(8) . ?
C73 O73 1.45(2) . ?
C74 H74 0.9800 . ?
C74 C75 1.51(3) . ?
C74 O74 1.50(2) . ?
C75 H75 0.9800 . ?
C75 C76 1.46(2) . ?
C75 O75 1.466(15) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C76 O76 1.447(8) . ?
K001 C52 3.46(3) 10_566 ?
K001 C65 3.53(3) 14_654 ?
K001 O12 3.04(2) . ?
K001 O13 2.97(2) . ?
K001 O45 2.75(2) 15_664 ?
K001 O46 3.13(2) 15_664 ?
K001 O52 2.69(2) 10_566 ?
K001 O53 2.77(2) 10_566 ?
K001 O65 2.98(2) 14_654 ?
K001 O66 2.847(18) 14_654 ?
K002 O5 2.84(3) 17_655 ?
K002 O5 2.84(3) . ?
K002 O6 2.98(3) 17_655 ?
K002 O6 2.98(3) . ?
K002 O72 3.13(2) 14_654 ?
K002 O72 3.13(2) 6_556 ?
K002 O73 2.97(2) 14_654 ?
K002 O73 2.97(2) 6_556 ?
K003 O25 3.08(4) 18_545 ?
K003 O25 3.08(4) . ?
K003 O26 2.93(4) . ?
K003 O26 2.93(4) 18_545 ?
K003 O32 2.68(3) 15_664 ?
K003 O32 2.68(3) 5_766 ?
K003 O33 3.41(3) 5_766 ?
K003 O33 3.41(3) 15_664 ?
O2 H2A 0.8200 . ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O16 H16 0.8200 . ?
O22 H22A 0.8200 . ?
O23 H23A 0.8200 . ?
O26 H26 0.8200 . ?
O32 K003 2.68(3) 8_655 ?
O32 H32A 0.8200 . ?
O33 K003 3.41(3) 8_655 ?
O33 H33A 0.8200 . ?
O36 H36 0.8200 . ?
O42 H42A 0.8200 . ?
O43 H43A 0.8200 . ?
O45 K001 2.75(2) 8_655 ?
O46 K001 3.13(2) 8_655 ?
O46 H46 0.8200 . ?
O52 K001 2.69(2) 10_566 ?
O52 H52A 0.8200 . ?
O53 K001 2.77(2) 10_566 ?
O53 H53A 0.8200 . ?
O56 H56 0.8200 . ?
O62 H62A 0.8200 . ?
O63 H63A 0.8200 . ?
O65 K001 2.98(2) 9_565 ?
O66 K001 2.847(18) 9_565 ?
O66 H66 0.8200 . ?
O72 K002 3.13(2) 9_565 ?
O72 H72A 0.8200 . ?
O73 K002 2.97(2) 9_565 ?
O73 H73A 0.8200 . ?
O76 H76 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 122.8 . . ?
O5 C1 H1 122.8 . . ?
O5 C1 C2 101.0(16) . . ?
O14 C1 H1 122.8 . . ?
O14 C1 C2 91(2) . . ?
O14 C1 O5 87(2) . . ?
C1 C2 H2 100.9 . . ?
C3 C2 C1 125.2(18) . . ?
C3 C2 H2 100.9 . . ?
O2 C2 C1 112(2) . . ?
O2 C2 H2 100.9 . . ?
O2 C2 C3 112(2) . . ?
C2 C3 H3 103.5 . . ?
C2 C3 C4 123.0(13) . . ?
C2 C3 O3 117.4(15) . . ?
C4 C3 H3 103.5 . . ?
O3 C3 H3 103.5 . . ?
O3 C3 C4 103.4(14) . . ?
C3 C4 H4 104.8 . . ?
C5 C4 C3 107.3(12) . . ?
C5 C4 H4 104.8 . . ?
O4 C4 C3 115.6(18) . . ?
O4 C4 H4 104.8 . . ?
O4 C4 C5 118(2) . . ?
C4 C5 H5 105.0 . . ?
C6 C5 C4 112(2) . . ?
C6 C5 H5 105.0 . . ?
O5 C5 C4 117(2) . . ?
O5 C5 H5 105.0 . . ?
O5 C5 C6 111(3) . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
O6 C6 C5 113(3) . . ?
O6 C6 H6A 109.1 . . ?
O6 C6 H6B 109.1 . . ?
C12 C11 H11 108.2 . . ?
C12 C11 O15 107(2) . . ?
O15 C11 H11 108.2 . . ?
O24 C11 H11 108.2 . . ?
O24 C11 C12 118(3) . . ?
O24 C11 O15 107(2) . . ?
C11 C12 H12 112.1 . . ?
C11 C12 C13 113(2) . . ?
C13 C12 H12 112.1 . . ?
O12 C12 C11 91(2) . . ?
O12 C12 H12 112.1 . . ?
O12 C12 C13 115(3) . . ?
C12 C13 H13 98.8 . . ?
C12 C13 C14 105(2) . . ?
C12 C13 O13 106(2) . . ?
C14 C13 H13 98.8 . . ?
C14 C13 O13 141(3) . . ?
O13 C13 H13 98.8 . . ?
C13 C14 H14 92.9 . . ?
C13 C14 C15 131(2) . . ?
C15 C14 H14 92.9 . . ?
O14 C14 C13 100(2) . . ?
O14 C14 H14 92.9 . . ?
O14 C14 C15 129(2) . . ?
C14 C15 H15 112.0 . . ?
C16 C15 C14 106(2) . . ?
C16 C15 H15 112.0 . . ?
O15 C15 C14 101(2) . . ?
O15 C15 H15 112.0 . . ?
O15 C15 C16 113(2) . . ?
C15 C16 H16A 110.8 . . ?
C15 C16 H16B 110.8 . . ?
H16A C16 H16B 108.8 . . ?
O16 C16 C15 105(2) . . ?
O16 C16 H16A 110.8 . . ?
O16 C16 H16B 110.8 . . ?
C22 C21 H21 108.1 . . ?
O25 C21 H21 108.1 . . ?
O25 C21 C22 114(2) . . ?
O25 C21 O34 113(3) . . ?
O34 C21 H21 108.1 . . ?
O34 C21 C22 105(3) . . ?
C21 C22 H22 105.9 . . ?
C23 C22 C21 122(3) . . ?
C23 C22 H22 105.9 . . ?
O22 C22 C21 104(3) . . ?
O22 C22 H22 105.9 . . ?
O22 C22 C23 113(3) . . ?
C22 C23 H23 95.7 . . ?
C22 C23 C24 114(2) . . ?
C22 C23 O23 127(3) . . ?
C24 C23 H23 95.7 . . ?
C24 C23 O23 115(3) . . ?
O23 C23 H23 95.7 . . ?
C23 C24 H24 102.2 . . ?
C23 C24 C25 118(3) . . ?
C23 C24 O24 111(3) . . ?
C25 C24 H24 102.2 . . ?
C25 C24 O24 119(3) . . ?
O24 C24 H24 102.2 . . ?
C24 C25 H25 109.1 . . ?
C24 C25 C26 108(3) . . ?
C26 C25 H25 109.1 . . ?
O25 C25 C24 118(3) . . ?
O25 C25 H25 109.1 . . ?
O25 C25 C26 103(3) . . ?
C25 C26 H26A 106.5 . . ?
C25 C26 H26B 106.5 . . ?
H26A C26 H26B 106.5 . . ?
O26 C26 C25 123(4) . . ?
O26 C26 H26A 106.5 . . ?
O26 C26 H26B 106.5 . . ?
C32 C31 H31 109.1 . . ?
C32 C31 O35 114(2) . . ?
C32 C31 O44 107(2) . . ?
O35 C31 H31 109.1 . . ?
O35 C31 O44 108.1(18) . . ?
O44 C31 H31 109.1 . . ?
C31 C32 H32 106.8 . . ?
C31 C32 C33 115(2) . . ?
C31 C32 O32 125(2) . . ?
C33 C32 H32 106.8 . . ?
O32 C32 H32 106.8 . . ?
O32 C32 C33 95(2) . . ?
C32 C33 H33 100.5 . . ?
C34 C33 C32 113.7(18) . . ?
C34 C33 H33 100.5 . . ?
O33 C33 C32 113.7(15) . . ?
O33 C33 H33 100.5 . . ?
O33 C33 C34 123(2) . . ?
C33 C34 H34 102.4 . . ?
C33 C34 C35 119.6(18) . . ?
C35 C34 H34 102.4 . . ?
O34 C34 C33 116(2) . . ?
O34 C34 H34 102.4 . . ?
O34 C34 C35 111.3(16) . . ?
C34 C35 H35 101.5 . . ?
C36 C35 C34 124(2) . . ?
C36 C35 H35 101.5 . . ?
C36 C35 O35 116(2) . . ?
O35 C35 C34 107.8(15) . . ?
O35 C35 H35 101.5 . . ?
C35 C36 H36A 107.8 . . ?
C35 C36 H36B 107.8 . . ?
H36A C36 H36B 107.1 . . ?
O36 C36 C35 118(3) . . ?
O36 C36 H36A 107.8 . . ?
O36 C36 H36B 107.8 . . ?
C42 C41 H41 116.3 . . ?
C42 C41 O45 98(2) . . ?
C42 C41 O54 91(2) . . ?
O45 C41 H41 116.3 . . ?
O54 C41 H41 116.3 . . ?
O54 C41 O45 114(2) . . ?
C41 C42 H42 100.7 . . ?
C41 C42 C43 126(2) . . ?
C43 C42 H42 100.7 . . ?
O42 C42 C41 110(2) . . ?
O42 C42 H42 100.7 . . ?
O42 C42 C43 114(2) . . ?
C42 C43 H43 108.5 . . ?
C44 C43 C42 111(2) . . ?
C44 C43 H43 108.5 . . ?
O43 C43 C42 111(2) . . ?
O43 C43 H43 108.5 . . ?
O43 C43 C44 110(2) . . ?
C43 C44 H44 106.3 . . ?
C45 C44 C43 111(2) . . ?
C45 C44 H44 106.3 . . ?
O44 C44 C43 113(2) . . ?
O44 C44 H44 106.3 . . ?
O44 C44 C45 114(3) . . ?
C44 C45 H45 102.7 . . ?
C44 C45 C46 116(3) . . ?
C46 C45 H45 102.7 . . ?
O45 C45 C44 113(3) . . ?
O45 C45 H45 102.7 . . ?
O45 C45 C46 116(3) . . ?
C45 C46 H46A 111.0 . . ?
C45 C46 H46B 111.0 . . ?
H46A C46 H46B 109.0 . . ?
O46 C46 C45 104(2) . . ?
O46 C46 H46A 111.0 . . ?
O46 C46 H46B 111.0 . . ?
C52 C51 H51 105.7 . . ?
O55 C51 H51 105.7 . . ?
O55 C51 C52 108.1(19) . . ?
O55 C51 O64 111(2) . . ?
O64 C51 H51 105.7 . . ?
O64 C51 C52 119(2) . . ?
C51 C52 H52 114.0 . . ?
C51 C52 K001 153.4(16) . 10_566 ?
C51 C52 O52 105.3(19) . . ?
C53 C52 C51 99.5(19) . . ?
C53 C52 H52 114.0 . . ?
C53 C52 K001 90.6(14) . 10_566 ?
C53 C52 O52 108.7(19) . . ?
K001 C52 H52 83.4 10_566 . ?
O52 C52 H52 114.0 . . ?
O52 C52 K001 48.0(10) . 10_566 ?
C52 C53 H53 104.9 . . ?
C52 C53 C54 114(2) . . ?
C54 C53 H53 104.9 . . ?
O53 C53 C52 99.6(19) . . ?
O53 C53 H53 104.9 . . ?
O53 C53 C54 127(2) . . ?
C53 C54 H54 98.1 . . ?
C55 C54 C53 120(2) . . ?
C55 C54 H54 98.1 . . ?
O54 C54 C53 101.1(19) . . ?
O54 C54 H54 98.1 . . ?
O54 C54 C55 133(2) . . ?
C54 C55 H55 108.4 . . ?
C54 C55 C56 120(2) . . ?
C54 C55 O55 102(2) . . ?
C56 C55 H55 108.4 . . ?
C56 C55 O55 109(2) . . ?
O55 C55 H55 108.4 . . ?
C55 C56 H56A 112.0 . . ?
C55 C56 H56B 112.0 . . ?
H56A C56 H56B 109.7 . . ?
O56 C56 C55 99(2) . . ?
O56 C56 H56A 112.0 . . ?
O56 C56 H56B 112.0 . . ?
C62 C61 H61 103.9 . . ?
O65 C61 H61 103.9 . . ?
O65 C61 C62 123(2) . . ?
O74 C61 H61 103.9 . . ?
O74 C61 C62 114(2) . . ?
O74 C61 O65 105.7(18) . . ?
C61 C62 H62 99.3 . . ?
C63 C62 C61 101(2) . . ?
C63 C62 H62 99.3 . . ?
O62 C62 C61 132(2) . . ?
O62 C62 H62 99.3 . . ?
O62 C62 C63 119(2) . . ?
C62 C63 H63 105.0 . . ?
C62 C63 C64 123(2) . . ?
C64 C63 H63 105.0 . . ?
O63 C63 C62 108.1(19) . . ?
O63 C63 H63 105.0 . . ?
O63 C63 C64 110(2) . . ?
C63 C64 H64 102.2 . . ?
C65 C64 C63 114.3(18) . . ?
C65 C64 H64 102.2 . . ?
O64 C64 C63 114.9(18) . . ?
O64 C64 H64 102.2 . . ?
O64 C64 C65 117.6(19) . . ?
C64 C65 H65 96.5 . . ?
C64 C65 K001 107.5(16) . 9_565 ?
C66 C65 C64 122(2) . . ?
C66 C65 H65 96.5 . . ?
C66 C65 K001 86.2(14) . 9_565 ?
K001 C65 H65 149.8 9_565 . ?
O65 C65 C64 119.6(18) . . ?
O65 C65 H65 96.5 . . ?
O65 C65 C66 114.8(19) . . ?
O65 C65 K001 55.9(11) . 9_565 ?
C65 C66 H66A 110.1 . . ?
C65 C66 H66B 110.1 . . ?
C65 C66 O66 108.1(19) . . ?
H66A C66 H66B 108.4 . . ?
O66 C66 H66A 110.1 . . ?
O66 C66 H66B 110.1 . . ?
C72 C71 H71 108.3 . . ?
C72 C71 O4 105(2) . . ?
C72 C71 O75 117.5(18) . . ?
O4 C71 H71 108.3 . . ?
O75 C71 H71 108.3 . . ?
O75 C71 O4 108.9(19) . . ?
C71 C72 H72 100.7 . . ?
C71 C72 C73 117(2) . . ?
C73 C72 H72 100.7 . . ?
O72 C72 C71 119(2) . . ?
O72 C72 H72 100.7 . . ?
O72 C72 C73 114(2) . . ?
C72 C73 H73 104.0 . . ?
C72 C73 C74 111(2) . . ?
C74 C73 H73 104.0 . . ?
O73 C73 C72 119(2) . . ?
O73 C73 H73 104.0 . . ?
O73 C73 C74 113(2) . . ?
C73 C74 H74 109.6 . . ?
C73 C74 C75 118(2) . . ?
C73 C74 O74 112(2) . . ?
C75 C74 H74 109.6 . . ?
O74 C74 H74 109.6 . . ?
O74 C74 C75 96.8(18) . . ?
C74 C75 H75 104.5 . . ?
C76 C75 C74 114(2) . . ?
C76 C75 H75 104.5 . . ?
C76 C75 O75 120(2) . . ?
O75 C75 C74 107.5(19) . . ?
O75 C75 H75 104.5 . . ?
C75 C76 H76A 107.6 . . ?
C75 C76 H76B 107.6 . . ?
H76A C76 H76B 107.0 . . ?
O76 C76 C75 119(2) . . ?
O76 C76 H76A 107.6 . . ?
O76 C76 H76B 107.6 . . ?
C52 K001 C65 85.3(6) 10_566 14_654 ?
O12 K001 C52 132.5(7) . 10_566 ?
O12 K001 C65 139.0(7) . 14_654 ?
O12 K001 O46 76.0(6) . 15_664 ?
O13 K001 C52 112.7(6) . 10_566 ?
O13 K001 C65 93.9(6) . 14_654 ?
O13 K001 O12 60.3(6) . . ?
O13 K001 O46 99.5(6) . 15_664 ?
O13 K001 O65 78.2(6) . 14_654 ?
O45 K001 C52 99.3(7) 15_664 10_566 ?
O45 K001 C65 104.6(6) 15_664 14_654 ?
O45 K001 O12 86.5(7) 15_664 . ?
O45 K001 O13 144.2(6) 15_664 . ?
O45 K001 O46 56.3(6) 15_664 15_664 ?
O45 K001 O53 82.1(6) 15_664 10_566 ?
O45 K001 O65 107.8(6) 15_664 14_654 ?
O45 K001 O66 71.4(6) 15_664 14_654 ?
O46 K001 C52 144.6(7) 15_664 10_566 ?
O46 K001 C65 78.0(6) 15_664 14_654 ?
O52 K001 C52 24.9(6) 10_566 10_566 ?
O52 K001 C65 74.5(6) 10_566 14_654 ?
O52 K001 O12 131.7(7) 10_566 . ?
O52 K001 O13 90.7(6) 10_566 . ?
O52 K001 O45 123.5(6) 10_566 15_664 ?
O52 K001 O46 151.2(6) 10_566 15_664 ?
O52 K001 O53 58.7(5) 10_566 10_566 ?
O52 K001 O65 92.1(6) 10_566 14_654 ?
O52 K001 O66 73.5(6) 10_566 14_654 ?
O53 K001 C52 40.8(5) 10_566 10_566 ?
O53 K001 C65 125.4(6) 10_566 14_654 ?
O53 K001 O12 94.9(7) 10_566 . ?
O53 K001 O13 111.8(6) 10_566 . ?
O53 K001 O46 137.5(6) 10_566 15_664 ?
O53 K001 O65 148.1(6) 10_566 14_654 ?
O53 K001 O66 95.3(6) 10_566 14_654 ?
O65 K001 C52 107.4(5) 14_654 10_566 ?
O65 K001 C65 23.5(4) 14_654 14_654 ?
O65 K001 O12 115.5(7) 14_654 . ?
O65 K001 O46 64.2(6) 14_654 15_664 ?
O66 K001 C52 66.6(6) 14_654 10_566 ?
O66 K001 C65 42.1(5) 14_654 14_654 ?
O66 K001 O12 154.1(7) 14_654 . ?
O66 K001 O13 135.5(6) 14_654 . ?
O66 K001 O46 80.4(6) 14_654 15_664 ?
O66 K001 O65 61.5(5) 14_654 14_654 ?
O5 K002 O5 125.4(11) . 17_655 ?
O5 K002 O6 80.7(8) 17_655 . ?
O5 K002 O6 80.7(8) . 17_655 ?
O5 K002 O6 62.6(8) 17_655 17_655 ?
O5 K002 O6 62.6(8) . . ?
O5 K002 O72 123.0(7) . 14_654 ?
O5 K002 O72 123.0(7) 17_655 6_556 ?
O5 K002 O72 86.7(6) 17_655 14_654 ?
O5 K002 O72 86.7(6) . 6_556 ?
O5 K002 O73 143.4(6) 17_655 14_654 ?
O5 K002 O73 69.9(6) 17_655 6_556 ?
O5 K002 O73 143.5(6) . 6_556 ?
O5 K002 O73 69.9(6) . 14_654 ?
O6 K002 O6 94.7(12) 17_655 . ?
O6 K002 O72 166.6(8) 17_655 6_556 ?
O6 K002 O72 75.3(8) . 6_556 ?
O6 K002 O72 166.6(8) . 14_654 ?
O6 K002 O72 75.3(8) 17_655 14_654 ?
O72 K002 O72 116.0(11) 14_654 6_556 ?
O73 K002 O6 130.0(7) 6_556 17_655 ?
O73 K002 O6 92.0(8) 6_556 . ?
O73 K002 O6 92.0(8) 14_654 17_655 ?
O73 K002 O6 130.0(7) 14_654 . ?
O73 K002 O72 88.0(7) 6_556 14_654 ?
O73 K002 O72 60.3(6) 14_654 14_654 ?
O73 K002 O72 60.3(6) 6_556 6_556 ?
O73 K002 O72 88.0(7) 14_654 6_556 ?
O73 K002 O73 120.0(10) 14_654 6_556 ?
O25 K003 O25 94.6(13) . 18_545 ?
O25 K003 O33 140.6(10) 18_545 5_766 ?
O25 K003 O33 72.9(9) . 5_766 ?
O25 K003 O33 72.9(9) 18_545 15_664 ?
O25 K003 O33 140.6(10) . 15_664 ?
O26 K003 O25 54.3(9) 18_545 18_545 ?
O26 K003 O25 53.5(8) 18_545 . ?
O26 K003 O25 53.5(8) . 18_545 ?
O26 K003 O25 54.3(9) . . ?
O26 K003 O26 59.4(14) . 18_545 ?
O26 K003 O33 90.5(11) . 15_664 ?
O26 K003 O33 127.2(10) . 5_766 ?
O26 K003 O33 127.2(10) 18_545 15_664 ?
O26 K003 O33 90.5(11) 18_545 5_766 ?
O32 K003 O25 112.2(8) 15_664 18_545 ?
O32 K003 O25 112.2(8) 5_766 . ?
O32 K003 O25 107.3(8) 5_766 18_545 ?
O32 K003 O25 107.3(8) 15_664 . ?
O32 K003 O26 149.4(11) 15_664 18_545 ?
O32 K003 O26 149.4(11) 5_766 . ?
O32 K003 O26 90.3(9) 5_766 18_545 ?
O32 K003 O26 90.3(9) 15_664 . ?
O32 K003 O32 120.2(15) 15_664 5_766 ?
O32 K003 O33 107.2(10) 5_766 15_664 ?
O32 K003 O33 49.7(5) 15_664 15_664 ?
O32 K003 O33 107.2(10) 15_664 5_766 ?
O32 K003 O33 49.7(5) 5_766 5_766 ?
O33 K003 O33 138.7(18) 15_664 5_766 ?
C2 O2 H2A 109.5 . . ?
C3 O3 H3A 109.5 . . ?
C4 O4 C71 113.6(18) . . ?
C1 O5 K002 110.7(17) . . ?
C5 O5 C1 125(2) . . ?
C5 O5 K002 113(2) . . ?
C6 O6 K002 106(2) . . ?
C6 O6 H6 109.5 . . ?
K002 O6 H6 144.1 . . ?
C12 O12 K001 100.7(14) . . ?
C12 O12 H12A 109.5 . . ?
K001 O12 H12A 147.9 . . ?
C13 O13 K001 116.6(15) . . ?
C13 O13 H13A 109.5 . . ?
K001 O13 H13A 130.3 . . ?
C1 O14 C14 121(2) . . ?
C15 O15 C11 104(2) . . ?
C16 O16 H16 109.5 . . ?
C22 O22 H22A 109.5 . . ?
C23 O23 H23A 109.5 . . ?
C11 O24 C24 115(2) . . ?
C21 O25 C25 110(2) . . ?
C21 O25 K003 104(2) . . ?
C25 O25 K003 113(3) . . ?
C26 O26 K003 117(2) . . ?
C26 O26 H26 109.5 . . ?
K003 O26 H26 100.6 . . ?
C32 O32 K003 130.9(15) . 8_655 ?
C32 O32 H32A 109.5 . . ?
K003 O32 H32A 89.6 8_655 . ?
C33 O33 K003 110.8(13) . 8_655 ?
C33 O33 H33A 109.5 . . ?
K003 O33 H33A 134.6 8_655 . ?
C34 O34 C21 122(3) . . ?
C31 O35 C35 109.8(12) . . ?
C36 O36 H36 109.5 . . ?
C42 O42 H42A 109.5 . . ?
C43 O43 H43A 109.5 . . ?
C44 O44 C31 114(2) . . ?
C41 O45 K001 109.3(15) . 8_655 ?
C45 O45 C41 123(2) . . ?
C45 O45 K001 122(2) . 8_655 ?
C46 O46 K001 111.1(18) . 8_655 ?
C46 O46 H46 109.5 . . ?
K001 O46 H46 137.7 8_655 . ?
C52 O52 K001 107.0(13) . 10_566 ?
C52 O52 H52A 109.5 . . ?
K001 O52 H52A 21.5 10_566 . ?
C53 O53 K001 124.6(13) . 10_566 ?
C53 O53 H53A 109.5 . . ?
K001 O53 H53A 125.9 10_566 . ?
C54 O54 C41 120(2) . . ?
C51 O55 C55 112.1(19) . . ?
C56 O56 H56 109.5 . . ?
C62 O62 H62A 109.5 . . ?
C63 O63 H63A 109.5 . . ?
C64 O64 C51 117.1(19) . . ?
C61 O65 K001 109.0(13) . 9_565 ?
C65 O65 C61 113.3(19) . . ?
C65 O65 K001 100.6(14) . 9_565 ?
C66 O66 K001 115.6(13) . 9_565 ?
C66 O66 H66 109.5 . . ?
K001 O66 H66 112.6 9_565 . ?
C72 O72 K002 103.5(15) . 9_565 ?
C72 O72 H72A 109.5 . . ?
K002 O72 H72A 6.2 9_565 . ?
C73 O73 K002 115.2(14) . 9_565 ?
C73 O73 H73A 109.5 . . ?
K002 O73 H73A 129.7 9_565 . ?
C61 O74 C74 113.3(19) . . ?
C75 O75 C71 104.3(18) . . ?
C76 O76 H76 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -27(4) . . . . ?
C1 C2 C3 O3 -158(3) . . . . ?
C2 C1 O5 C5 -39(4) . . . . ?
C2 C1 O5 K002 103(2) . . . . ?
C2 C1 O14 C14 -137(2) . . . . ?
C2 C3 C4 C5 30(4) . . . . ?
C2 C3 C4 O4 165(2) . . . . ?
C3 C4 C5 C6 -170(3) . . . . ?
C3 C4 C5 O5 -40(4) . . . . ?
C3 C4 O4 C71 113(2) . . . . ?
C4 C5 C6 O6 64(5) . . . . ?
C4 C5 O5 C1 52(4) . . . . ?
C4 C5 O5 K002 -89(3) . . . . ?
C5 C4 O4 C71 -118(3) . . . . ?
C5 C6 O6 K002 54(3) . . . . ?
C6 C5 O5 C1 -177(2) . . . . ?
C6 C5 O5 K002 42(3) . . . . ?
C11 C12 C13 C14 -34(4) . . . . ?
C11 C12 C13 O13 170(3) . . . . ?
C11 C12 O12 K001 169.7(17) . . . . ?
C12 C11 O15 C15 -82(3) . . . . ?
C12 C11 O24 C24 -134(3) . . . . ?
C12 C13 C14 C15 25(6) . . . . ?
C12 C13 C14 O14 -165(3) . . . . ?
C12 C13 O13 K001 -20(3) . . . . ?
C13 C12 O12 K001 -74(2) . . . . ?
C13 C14 C15 C16 -158(4) . . . . ?
C13 C14 C15 O15 -40(5) . . . . ?
C13 C14 O14 C1 70(4) . . . . ?
C14 C13 O13 K001 -162(4) . . . . ?
C14 C15 C16 O16 78(3) . . . . ?
C14 C15 O15 C11 62(3) . . . . ?
C15 C14 O14 C1 -119(4) . . . . ?
C16 C15 O15 C11 175(2) . . . . ?
C21 C22 C23 C24 -20(6) . . . . ?
C21 C22 C23 O23 -179(4) . . . . ?
C22 C21 O25 C25 -49(4) . . . . ?
C22 C21 O25 K003 73(3) . . . . ?
C22 C21 O34 C34 -116(3) . . . . ?
C22 C23 C24 C25 19(6) . . . . ?
C22 C23 C24 O24 160(3) . . . . ?
C23 C24 C25 C26 -154(4) . . . . ?
C23 C24 C25 O25 -37(6) . . . . ?
C23 C24 O24 C11 111(3) . . . . ?
C24 C25 C26 O26 98(4) . . . . ?
C24 C25 O25 C21 52(5) . . . . ?
C24 C25 O25 K003 -64(4) . . . . ?
C25 C24 O24 C11 -108(4) . . . . ?
C25 C26 O26 K003 -15(5) . . . . ?
C26 C25 O25 C21 171(3) . . . . ?
C26 C25 O25 K003 55(3) . . . . ?
C31 C32 C33 C34 -26(5) . . . . ?
C31 C32 C33 O33 -173(3) . . . . ?
C31 C32 O32 K003 155(2) . . . 8_655 ?
C32 C31 O35 C35 -66(3) . . . . ?
C32 C31 O44 C44 -114(2) . . . . ?
C32 C33 C34 C35 26(5) . . . . ?
C32 C33 C34 O34 163(3) . . . . ?
C32 C33 O33 K003 -30(4) . . . 8_655 ?
C33 C32 O32 K003 -80(3) . . . 8_655 ?
C33 C34 C35 C36 175(3) . . . . ?
C33 C34 C35 O35 -44(4) . . . . ?
C33 C34 O34 C21 90(4) . . . . ?
C34 C33 O33 K003 -174(3) . . . 8_655 ?
C34 C35 C36 O36 68(5) . . . . ?
C34 C35 O35 C31 61(3) . . . . ?
C35 C34 O34 C21 -129(3) . . . . ?
C36 C35 O35 C31 -155(2) . . . . ?
C41 C42 C43 C44 -39(4) . . . . ?
C41 C42 C43 O43 -161(3) . . . . ?
C42 C41 O45 C45 -52(3) . . . . ?
C42 C41 O45 K001 102(2) . . . 8_655 ?
C42 C41 O54 C54 -159(2) . . . . ?
C42 C43 C44 C45 38(4) . . . . ?
C42 C43 C44 O44 166(3) . . . . ?
C43 C44 C45 C46 170(3) . . . . ?
C43 C44 C45 O45 -51(4) . . . . ?
C43 C44 O44 C31 127(3) . . . . ?
C44 C45 C46 O46 73(4) . . . . ?
C44 C45 O45 C41 64(4) . . . . ?
C44 C45 O45 K001 -87(3) . . . 8_655 ?
C45 C44 O44 C31 -105(3) . . . . ?
C45 C46 O46 K001 43(3) . . . 8_655 ?
C46 C45 O45 C41 -157(3) . . . . ?
C46 C45 O45 K001 52(4) . . . 8_655 ?
C51 C52 C53 C54 -51(3) . . . . ?
C51 C52 C53 O53 171(2) . . . . ?
C51 C52 O52 K001 -179.0(15) . . . 10_566 ?
C52 C51 O55 C55 -82(2) . . . . ?
C52 C51 O64 C64 -114(2) . . . . ?
C52 C53 C54 C55 42(4) . . . . ?
C52 C53 C54 O54 -163(2) . . . . ?
C52 C53 O53 K001 -24(3) . . . 10_566 ?
C53 C52 O52 K001 -73.2(19) . . . 10_566 ?
C53 C54 C55 C56 -158(3) . . . . ?
C53 C54 C55 O55 -38(3) . . . . ?
C53 C54 O54 C41 112(3) . . . . ?
C54 C53 O53 K001 -154(2) . . . 10_566 ?
C54 C55 C56 O56 58(3) . . . . ?
C54 C55 O55 C51 57(3) . . . . ?
C55 C54 O54 C41 -97(4) . . . . ?
C56 C55 O55 C51 -176(2) . . . . ?
C61 C62 C63 C64 -47(3) . . . . ?
C61 C62 C63 O63 -176(2) . . . . ?
C62 C61 O65 C65 -45(3) . . . . ?
C62 C61 O65 K001 67(3) . . . 9_565 ?
C62 C61 O74 C74 -109(2) . . . . ?
C62 C63 C64 C65 36(4) . . . . ?
C62 C63 C64 O64 177(3) . . . . ?
C63 C64 C65 C66 -178(2) . . . . ?
C63 C64 C65 K001 -81(2) . . . 9_565 ?
C63 C64 C65 O65 -21(4) . . . . ?
C63 C64 O64 C51 125(2) . . . . ?
C64 C65 C66 O66 86(3) . . . . ?
C64 C65 O65 C61 24(3) . . . . ?
C64 C65 O65 K001 -92(2) . . . 9_565 ?
C65 C64 O64 C51 -96(3) . . . . ?
C65 C66 O66 K001 32(2) . . . 9_565 ?
C66 C65 O65 C61 -177(2) . . . . ?
C66 C65 O65 K001 66(2) . . . 9_565 ?
C71 C72 C73 C74 -23(4) . . . . ?
C71 C72 C73 O73 -157(2) . . . . ?
C71 C72 O72 K002 158(2) . . . 9_565 ?
C72 C71 O4 C4 -105(2) . . . . ?
C72 C71 O75 C75 -59(3) . . . . ?
C72 C73 C74 C75 35(4) . . . . ?
C72 C73 C74 O74 147(2) . . . . ?
C72 C73 O73 K002 -20(3) . . . 9_565 ?
C73 C72 O72 K002 -58(3) . . . 9_565 ?
C73 C74 C75 C76 165(3) . . . . ?
C73 C74 C75 O75 -60(3) . . . . ?
C73 C74 O74 C61 104(2) . . . . ?
C74 C73 O73 K002 -153.0(18) . . . 9_565 ?
C74 C75 C76 O76 120(3) . . . . ?
C74 C75 O75 C71 65(3) . . . . ?
C75 C74 O74 C61 -132(2) . . . . ?
C76 C75 O75 C71 -162(3) . . . . ?
K001 C52 C53 C54 153(2) 10_566 . . . ?
K001 C52 C53 O53 15.7(17) 10_566 . . . ?
K001 C65 C66 O66 -22.7(17) 9_565 . . . ?
K001 C65 O65 C61 116.3(19) 9_565 . . . ?
O2 C2 C3 C4 -169(2) . . . . ?
O2 C2 C3 O3 61(3) . . . . ?
O3 C3 C4 C5 167(3) . . . . ?
O3 C3 C4 O4 -59(3) . . . . ?
O4 C4 C5 C6 57(4) . . . . ?
O4 C4 C5 O5 -173(3) . . . . ?
O4 C71 C72 C73 -84(3) . . . . ?
O4 C71 C72 O72 60(3) . . . . ?
O4 C71 O75 C75 61(3) . . . . ?
O5 C1 C2 C3 26(4) . . . . ?
O5 C1 C2 O2 167(3) . . . . ?
O5 C1 O14 C14 122(3) . . . . ?
O5 C5 C6 O6 -69(4) . . . . ?
O12 C12 C13 C14 -136(3) . . . . ?
O12 C12 C13 O13 67(3) . . . . ?
O13 C13 C14 C15 167(4) . . . . ?
O13 C13 C14 O14 -23(6) . . . . ?
O14 C1 C2 C3 -62(3) . . . . ?
O14 C1 C2 O2 80(3) . . . . ?
O14 C1 O5 C5 52(3) . . . . ?
O14 C1 O5 K002 -166.1(14) . . . . ?
O14 C14 C15 C16 35(4) . . . . ?
O14 C14 C15 O15 152(3) . . . . ?
O15 C11 C12 C13 66(3) . . . . ?
O15 C11 C12 O12 -177(2) . . . . ?
O15 C11 O24 C24 106(3) . . . . ?
O15 C15 C16 O16 -32(3) . . . . ?
O22 C22 C23 C24 -144(4) . . . . ?
O22 C22 C23 O23 57(6) . . . . ?
O23 C23 C24 C25 -179(4) . . . . ?
O23 C23 C24 O24 -38(5) . . . . ?
O24 C11 C12 C13 -55(4) . . . . ?
O24 C11 C12 O12 63(3) . . . . ?
O24 C11 O15 C15 45(3) . . . . ?
O24 C24 C25 C26 69(5) . . . . ?
O24 C24 C25 O25 -175(3) . . . . ?
O25 C21 C22 C23 37(5) . . . . ?
O25 C21 C22 O22 165(3) . . . . ?
O25 C21 O34 C34 119(3) . . . . ?
O25 C25 C26 O26 -27(5) . . . . ?
O32 C32 C33 C34 -158(3) . . . . ?
O32 C32 C33 O33 55(3) . . . . ?
O33 C33 C34 C35 170(3) . . . . ?
O33 C33 C34 O34 -53(5) . . . . ?
O34 C21 C22 C23 -88(4) . . . . ?
O34 C21 C22 O22 40(4) . . . . ?
O34 C21 O25 C25 71(4) . . . . ?
O34 C21 O25 K003 -167.2(19) . . . . ?
O34 C34 C35 C36 36(4) . . . . ?
O34 C34 C35 O35 177(2) . . . . ?
O35 C31 C32 C33 46(4) . . . . ?
O35 C31 C32 O32 162(2) . . . . ?
O35 C31 O44 C44 123(2) . . . . ?
O35 C35 C36 O36 -70(5) . . . . ?
O42 C42 C43 C44 179(3) . . . . ?
O42 C42 C43 O43 57(3) . . . . ?
O43 C43 C44 C45 160(3) . . . . ?
O43 C43 C44 O44 -71(4) . . . . ?
O44 C31 C32 C33 -74(3) . . . . ?
O44 C31 C32 O32 42(3) . . . . ?
O44 C31 O35 C35 54(2) . . . . ?
O44 C44 C45 C46 42(4) . . . . ?
O44 C44 C45 O45 -179(3) . . . . ?
O45 C41 C42 C43 39(4) . . . . ?
O45 C41 C42 O42 -178(2) . . . . ?
O45 C41 O54 C54 101(3) . . . . ?
O45 C45 C46 O46 -65(4) . . . . ?
O52 C52 C53 C54 -161(2) . . . . ?
O52 C52 C53 O53 61(2) . . . . ?
O53 C53 C54 C55 166(3) . . . . ?
O53 C53 C54 O54 -39(3) . . . . ?
O54 C41 C42 C43 -76(3) . . . . ?
O54 C41 C42 O42 67(3) . . . . ?
O54 C41 O45 C45 43(4) . . . . ?
O54 C41 O45 K001 -163.1(17) . . . 8_655 ?
O54 C54 C55 C56 55(5) . . . . ?
O54 C54 C55 O55 176(3) . . . . ?
O55 C51 C52 C53 72(2) . . . . ?
O55 C51 C52 K001 -177(3) . . . 10_566 ?
O55 C51 C52 O52 -175.2(19) . . . . ?
O55 C51 O64 C64 119(2) . . . . ?
O55 C55 C56 O56 -60(3) . . . . ?
O62 C62 C63 C64 160(3) . . . . ?
O62 C62 C63 O63 31(4) . . . . ?
O63 C63 C64 C65 165(2) . . . . ?
O63 C63 C64 O64 -55(3) . . . . ?
O64 C51 C52 C53 -56(3) . . . . ?
O64 C51 C52 K001 55(4) . . . 10_566 ?
O64 C51 C52 O52 56(2) . . . . ?
O64 C51 O55 C55 51(2) . . . . ?
O64 C64 C65 C66 43(4) . . . . ?
O64 C64 C65 K001 139.4(19) . . . 9_565 ?
O64 C64 C65 O65 -160(2) . . . . ?
O65 C61 C62 C63 53(3) . . . . ?
O65 C61 C62 O62 -161(3) . . . . ?
O65 C61 O74 C74 112(2) . . . . ?
O65 C65 C66 O66 -72(3) . . . . ?
O72 C72 C73 C74 -168(2) . . . . ?
O72 C72 C73 O73 58(4) . . . . ?
O73 C73 C74 C75 172(2) . . . . ?
O73 C73 C74 O74 -77(3) . . . . ?
O74 C61 C62 C63 -78(3) . . . . ?
O74 C61 C62 O62 69(4) . . . . ?
O74 C61 O65 C65 89(2) . . . . ?
O74 C61 O65 K001 -159.5(14) . . . 9_565 ?
O74 C74 C75 C76 45(3) . . . . ?
O74 C74 C75 O75 -179(2) . . . . ?
O75 C71 C72 C73 38(4) . . . . ?
O75 C71 C72 O72 -179(2) . . . . ?
O75 C71 O4 C4 128(2) . . . . ?
O75 C75 C76 O76 -10(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.089 -0.005 -0.902 21908.4 4657.8 ?


_olex2_exptl_crystal_mounting_method 
'Coated in a mother liquor and mounted in a quartx 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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.333
_oxdiff_exptl_absorpt_empirical_full_min 0.191
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_295K_MeOH
_database_code_depnum_ccdc_archive 'CCDC 1529165'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2016-11-21
_audit_creation_method           'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_cell_length_a                   31.255(9)
_cell_length_b                   31.255(9)
_cell_length_c                   31.255(9)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30531(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    295.00(14)
_cell_measurement_reflns_used    59
_cell_measurement_theta_min      3.6560
_cell_measurement_theta_max      5.3000
_cell_oxdiff_length_a            31.280(15)
_cell_oxdiff_length_b            31.251(14)
_cell_oxdiff_length_c            31.234(16)
_cell_oxdiff_angle_alpha         89.99(4)
_cell_oxdiff_angle_beta          89.97(4)
_cell_oxdiff_angle_gamma         89.99(4)
_cell_oxdiff_volume              30531(20)
_cell_oxdiff_measurement_reflns_used 59
_exptl_absorpt_correction_type   none
_oxdiff_exptl_absorpt_empirical_full_min 1.000
_oxdiff_exptl_absorpt_empirical_full_max 1.000
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_diffrn_ambient_temperature      295.00(14)
_diffrn_ambient_environment      air
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.0169
_diffrn_reflns_number            3788
_diffrn_reflns_av_R_equivalents  0.2399
_diffrn_reflns_av_sigmaI/netI    0.3112
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.3236
_diffrn_reflns_theta_max         8.1114
_diffrn_measured_fraction_theta_max 0.9227
_diffrn_reflns_theta_full        8.0949
_diffrn_measured_fraction_theta_full 0.8828
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0128796000
_diffrn_orient_matrix_UB_12      0.0186758000
_diffrn_orient_matrix_UB_13      -0.0003420000
_diffrn_orient_matrix_UB_21      -0.0186606000
_diffrn_orient_matrix_UB_22      0.0128970000
_diffrn_orient_matrix_UB_23      0.0001748000
_diffrn_orient_matrix_UB_31      0.0003260000
_diffrn_orient_matrix_UB_32      0.0001778000
_diffrn_orient_matrix_UB_33      0.0227062000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00  84.00   1.00   25.00    --    0.71  19.00 -90.00  167
  2  ω    -79.00 -54.00   1.00   25.00    --    0.71  19.00  30.00   25
;
_diffrn_measurement_method       'ω scans'
_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_symmetry_space_group_name_H-M   'I 4 3 2'
_symmetry_cell_setting           cubic
_space_group_IT_number           211
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I 4 3 2'
_reflns_odcompleteness_completeness 88.28
_reflns_odcompleteness_theta     8.09
_reflns_odcompleteness_iscentric 1

##################################################################



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_0_86GPa
_database_code_depnum_ccdc_archive 'CCDC 1529150'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_REFNR01_a_0_86GPa           
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_THETM01_a_0_86GPa           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT029_a_0_86GPa           
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.849 Note  
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT090_a_0_86GPa           
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.55 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT201_a_0_86GPa           
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT241_a_0_86GPa           
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O4 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT242_a_0_86GPa           
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C1 Check 
RESPONSE: 'Poor data quality'
;
_vrf_PLAT306_a_0_86GPa           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_a_0_86GPa           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.04 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_a_0_86GPa           
;
PROBLEM: D-H Without Acceptor       O16    --  H16    ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
_vrf_PLAT910_a_0_86GPa           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          12 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample limiting the range of 
collected reflections'
;
_vrf_PLAT911_a_0_86GPa           
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.249         22 Report
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample limiting the range of 
collected reflections'
;
# end Validation Reply Form
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   30.988(3)
_cell_length_b                   30.988(3)
_cell_length_c                   30.988(3)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     29758(6)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    2310
_cell_measurement_temperature    295
_cell_measurement_theta_max      10.1810
_cell_measurement_theta_min      3.6480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20429
_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_absorpt_special_details   ?
# EXPERIMENTAL DATA 

_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.1GPa and 
then compressed to 0.86GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.944
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             8928
_exptl_crystal_recrystallization_method 
'Compressed crystal that was grown in situ from methano:water solution in the diamond-anvil cell at 0.2 GPa.'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1133
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.849
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9256
_diffrn_reflns_point_group_measured_fraction_full 0.885
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        10.190
_diffrn_reflns_theta_max         10.190
_diffrn_reflns_theta_min         3.221
_diffrn_ambient_temperature      295
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         860000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0338
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.849
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0028009000
_diffrn_orient_matrix_UB_12      -0.0000220000
_diffrn_orient_matrix_UB_13      -0.0227393000
_diffrn_orient_matrix_UB_21      0.0222972000
_diffrn_orient_matrix_UB_22      -0.0047643000
_diffrn_orient_matrix_UB_23      0.0024687000
_diffrn_orient_matrix_UB_31      -0.0048939000
_diffrn_orient_matrix_UB_32      -0.0223478000
_diffrn_orient_matrix_UB_33      -0.0003526000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          
'high-pressure measurement in diamond-anvil cell at 0.86 GPa'
_reflns_Friedel_coverage         0.565
_reflns_Friedel_fraction_full    0.956
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                297
_reflns_number_total             299
_reflns_odcompleteness_completeness 89.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     10.18
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.115
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details 
;
 Flack x determined using 103 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         299
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0863
_refine_ls_restrained_S_all      1.808
_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/[σ²(Fo²)+(0.1319P)²+337.3702P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2187
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
 resulting in a low data:parameter ratio.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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
 C16-C15
 1.5 with sigma of 0.002
 C14-C15
 1.5 with sigma of 0.002
 C14-C13
 1.5 with sigma of 0.02
 C11-C14
 3 with sigma of 0.02
 C4-C3
 1.5 with sigma of 0.002
 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
 C12-C11
 1.5 with sigma of 0.002
 C2-C3
 1.5 with sigma of 0.002
 C1-C4
 2.8 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.002
 C6-C5
 1.5 with sigma of 0.002
 C4-C5
 1.5 with sigma of 0.002
 C2-C5
 3 with sigma of 0.02
 C5-C2
 3 with sigma of 0.02
 C5-C1
 2.3 with sigma of 0.002
 C16-O16
 1.45 with sigma of 0.002
 O14-C15
 2.4 with sigma of 0.02
 C14-O14
 1.45 with sigma of 0.002
 O2-C3
 2.2 with sigma of 0.02
 O3-C3
 1.45 with sigma of 0.002
 C11-O4
 1.45 with sigma of 0.002
 C4-O4
 1.45 with sigma of 0.002
 C12-O4
 2 with sigma of 0.02
 C12-O12
 1.45 with sigma of 0.02
 C2-O2
 1.45 with sigma of 0.002
 C2-O3
 2.3 with sigma of 0.02
 C6-O6
 1.45 with sigma of 0.002
 O5-C6
 2.5 with sigma of 0.02
 O15-C16
 2.2 with sigma of 0.02
 O15-C15
 1.45 with sigma of 0.002
 O5-C3
 3 with sigma of 0.02
 O15-C13
 3 with sigma of 0.02
 O15-C11
 1.45 with sigma of 0.002
 O5-C1
 1.45 with sigma of 0.002
 O5-C5
 1.45 with sigma of 0.002
 O13-C13
 1.45 with sigma of 0.002
 C13-C15
 2.4 with sigma of 0.02
 C11-C13
 2.4 with sigma of 0.02
 C15-C11
 2.4 with sigma of 0.02
 C11-C4
 2.5 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.02
 C4-C2
 2.5 with sigma of 0.02
 C4-C11
 2.5 with sigma of 0.04
 C3-C1
 2.5 with sigma of 0.02
 C14-C16
 2.5 with sigma of 0.04
 C5-C3
 2.5 with sigma of 0.02
 C1-C5
 2.5 with sigma of 0.02
 O14-C15
 2.5 with sigma of 0.04
 C13-O14
 2.5 with sigma of 0.04
 O2-C3
 2.5 with sigma of 0.04
 O4-C3
 2.5 with sigma of 0.04
 O4-C12
 2.5 with sigma of 0.04
 O2-C1
 2.5 with sigma of 0.04
 C3-O4
 2.1 with sigma of 0.04
 O3-C4
 2.5 with sigma of 0.04
 O3-C2
 2.5 with sigma of 0.04
 O4-C5
 2.5 with sigma of 0.04
 C14-O15
 2.4 with sigma of 0.02
 O5-C4
 2.5 with sigma of 0.02
 O15-C12
 2.4 with sigma of 0.02
 C2-O5
 2.5 with sigma of 0.02
 O4-O15
 2.5 with sigma of 0.04
 O15-C16
 2.5 with sigma of 0.04
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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8541(10) 0.6859(9) 0.6237(11) 0.169(10) Uiso 1 1 d D . . . .
H1 H 0.8509 0.7172 0.6210 0.203 Uiso 1 1 calc R . . . .
C2 C 0.8912(8) 0.6790(7) 0.6540(11) 0.169(10) Uiso 1 1 d D . . . .
H2 H 0.8864 0.6952 0.6807 0.203 Uiso 1 1 calc R . . . .
C3 C 0.8944(8) 0.6316(8) 0.6638(11) 0.169(10) Uiso 1 1 d D . . . .
H3 H 0.9085 0.6184 0.6388 0.203 Uiso 1 1 calc R . . . .
C4 C 0.8517(9) 0.6094(8) 0.6685(11) 0.169(10) Uiso 1 1 d D . . . .
H4 H 0.8411 0.6173 0.6972 0.203 Uiso 1 1 calc R . . . .
C5 C 0.8169(8) 0.6231(8) 0.6377(12) 0.169(10) Uiso 1 1 d D . . . .
H5 H 0.8272 0.6144 0.6091 0.203 Uiso 1 1 calc R . . . .
C6 C 0.7755(9) 0.5989(12) 0.6442(13) 0.169(10) Uiso 1 1 d D . . . .
H6A H 0.7504 0.6134 0.6323 0.203 Uiso 1 1 calc R . . . .
H6B H 0.7767 0.5691 0.6347 0.203 Uiso 1 1 calc R . . . .
C11 C 0.8582(11) 0.5453(8) 0.7139(10) 0.169(10) Uiso 1 1 d D . . . .
H11 H 0.8603 0.5682 0.7356 0.203 Uiso 1 1 calc R . . . .
C12 C 0.9010(8) 0.5233(11) 0.7085(14) 0.169(10) Uiso 1 1 d D . . . .
H12 H 0.9027 0.5101 0.7372 0.203 Uiso 1 1 calc R . . . .
C13 C 0.8976(9) 0.4825(12) 0.6828(14) 0.169(10) Uiso 1 1 d D . . . .
H13 H 0.9019 0.4861 0.6517 0.203 Uiso 1 1 calc R . . . .
C14 C 0.8595(9) 0.4551(9) 0.6949(13) 0.169(10) Uiso 1 1 d D . . . .
H14 H 0.8640 0.4465 0.7250 0.203 Uiso 1 1 calc R . . . .
C15 C 0.8186(7) 0.4809(10) 0.6939(10) 0.169(10) Uiso 1 1 d D . . . .
H15 H 0.8149 0.4925 0.6648 0.203 Uiso 1 1 calc R . . . .
C16 C 0.7764(10) 0.4617(12) 0.7080(12) 0.169(10) Uiso 1 1 d D . . . .
H16A H 0.7557 0.4847 0.7126 0.203 Uiso 1 1 calc R . . . .
H16B H 0.7654 0.4432 0.6853 0.203 Uiso 1 1 calc R . . . .
K1 K 0.8051(6) 0.5000 0.8051(6) 0.284(15) Uani 1 2 d S TU P . .
O2 O 0.9337(10) 0.6886(12) 0.6370(14) 0.297(10) Uiso 1 1 d D . . . .
H2A H 0.9482 0.6665 0.6362 0.446 Uiso 1 1 calc R . . . .
O3 O 0.9250(12) 0.6283(13) 0.6991(12) 0.297(10) Uiso 1 1 d D . . . .
H3A H 0.9252 0.6035 0.7083 0.446 Uiso 1 1 calc R . . . .
O4 O 0.8606(12) 0.5635(8) 0.6708(10) 0.297(10) Uiso 1 1 d D . . . .
O5 O 0.8118(8) 0.6696(9) 0.6354(11) 0.297(10) Uiso 1 1 d D . . . .
O6 O 0.7797(15) 0.6039(15) 0.6906(13) 0.297(10) Uiso 1 1 d D . . . .
H6 H 0.7909 0.5822 0.7008 0.446 Uiso 1 1 calc R . . . .
O12 O 0.9432(12) 0.5416(15) 0.7076(13) 0.297(10) Uiso 1 1 d D . . . .
H12A H 0.9611 0.5223 0.7043 0.446 Uiso 1 1 calc R . . . .
O13 O 0.9227(13) 0.4481(13) 0.7021(13) 0.297(10) Uiso 1 1 d D . . . .
H13A H 0.9127 0.4247 0.6948 0.446 Uiso 1 1 calc R . . . .
O14 O 0.8534(13) 0.4154(11) 0.6708(14) 0.297(10) Uiso 1 1 d D . . . .
O15 O 0.8224(9) 0.5168(10) 0.7236(11) 0.297(10) Uiso 1 1 d D . . . .
O16 O 0.7809(14) 0.4368(14) 0.7474(12) 0.297(10) Uiso 1 1 d D . . . .
H16 H 0.7684 0.4137 0.7448 0.446 Uiso 1 1 calc R . . . .
OA O 1.0000 0.5000 0.671(2) 0.297(10) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.500(3) . ?
C1 O5 1.450(3) . ?
C1 O14 1.30(5) 7_556 ?
C2 H2 0.9800 . ?
C2 C3 1.501(3) . ?
C2 O2 1.450(3) . ?
C3 H3 0.9800 . ?
C3 C4 1.500(3) . ?
C3 O3 1.450(3) . ?
C4 H4 0.9800 . ?
C4 C5 1.500(3) . ?
C4 O4 1.450(3) . ?
C5 H5 0.9800 . ?
C5 C6 1.500(3) . ?
C5 O5 1.450(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.450(3) . ?
C11 H11 0.9800 . ?
C11 C12 1.500(3) . ?
C11 O4 1.450(3) . ?
C11 O15 1.450(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.50(2) . ?
C12 O12 1.43(3) . ?
C13 H13 0.9800 . ?
C13 C14 1.50(2) . ?
C13 O13 1.450(3) . ?
C14 H14 0.9800 . ?
C14 C15 1.500(3) . ?
C14 O14 1.450(3) . ?
C15 H15 0.9800 . ?
C15 C16 1.500(3) . ?
C15 K1 3.52(3) . ?
C15 O15 1.451(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 K1 3.35(4) . ?
C16 O16 1.450(3) . ?
K1 C15 3.52(3) 23_565 ?
K1 C16 3.35(4) 23_565 ?
K1 O2 2.73(4) 41_646 ?
K1 O2 2.73(4) 44_666 ?
K1 O3 3.11(4) 44_666 ?
K1 O3 3.11(4) 41_646 ?
K1 O15 2.63(4) . ?
K1 O15 2.63(4) 23_565 ?
K1 O16 2.75(4) 23_565 ?
K1 O16 2.75(4) . ?
O2 K1 2.73(4) 42_566 ?
O2 H2A 0.8200 . ?
O3 K1 3.11(4) 42_566 ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O14 C1 1.30(5) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 105.9 . . ?
O5 C1 H1 105.9 . . ?
O5 C1 C2 119.2(16) . . ?
O14 C1 H1 105.9 7_556 . ?
O14 C1 C2 123(3) 7_556 . ?
O14 C1 O5 95(3) 7_556 . ?
C1 C2 H2 109.8 . . ?
C1 C2 C3 108.5(13) . . ?
C3 C2 H2 109.8 . . ?
O2 C2 C1 116(3) . . ?
O2 C2 H2 109.8 . . ?
O2 C2 C3 102.5(15) . . ?
C2 C3 H3 106.0 . . ?
C4 C3 C2 114.3(13) . . ?
C4 C3 H3 106.0 . . ?
O3 C3 C2 105.4(16) . . ?
O3 C3 H3 106.0 . . ?
O3 C3 C4 118(3) . . ?
C3 C4 H4 105.4 . . ?
C5 C4 C3 116.3(13) . . ?
C5 C4 H4 105.4 . . ?
O4 C4 C3 107(2) . . ?
O4 C4 H4 105.4 . . ?
O4 C4 C5 117(2) . . ?
C4 C5 H5 105.2 . . ?
C4 C5 C6 113(3) . . ?
C6 C5 H5 105.2 . . ?
O5 C5 C4 113.1(15) . . ?
O5 C5 H5 105.2 . . ?
O5 C5 C6 114.3(19) . . ?
C5 C6 H6A 113.6 . . ?
C5 C6 H6B 113.6 . . ?
H6A C6 H6B 110.9 . . ?
O6 C6 C5 90(3) . . ?
O6 C6 H6A 113.6 . . ?
O6 C6 H6B 113.6 . . ?
C12 C11 H11 110.3 . . ?
O4 C11 H11 110.3 . . ?
O4 C11 C12 91.7(14) . . ?
O4 C11 O15 118(3) . . ?
O15 C11 H11 110.3 . . ?
O15 C11 C12 115.0(14) . . ?
C11 C12 H12 97.8 . . ?
C13 C12 C11 112.3(15) . . ?
C13 C12 H12 97.8 . . ?
O12 C12 C11 129(3) . . ?
O12 C12 H12 97.8 . . ?
O12 C12 C13 113(3) . . ?
C12 C13 H13 114.7 . . ?
C12 C13 C14 114(2) . . ?
C14 C13 H13 114.7 . . ?
O13 C13 C12 111(4) . . ?
O13 C13 H13 114.7 . . ?
O13 C13 C14 84(3) . . ?
C13 C14 H14 106.3 . . ?
C15 C14 C13 111.0(18) . . ?
C15 C14 H14 106.3 . . ?
O14 C14 C13 117(3) . . ?
O14 C14 H14 106.3 . . ?
O14 C14 C15 109.3(17) . . ?
C14 C15 H15 108.2 . . ?
C14 C15 K1 99.9(19) . . ?
C16 C15 C14 121(3) . . ?
C16 C15 H15 108.2 . . ?
C16 C15 K1 71.3(16) . . ?
K1 C15 H15 145.8 . . ?
O15 C15 C14 109.2(15) . . ?
O15 C15 H15 108.2 . . ?
O15 C15 C16 101.0(15) . . ?
O15 C15 K1 42.2(14) . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
C15 C16 K1 83.7(16) . . ?
H16A C16 H16B 107.9 . . ?
K1 C16 H16A 77.5 . . ?
K1 C16 H16B 162.4 . . ?
O16 C16 C15 112(3) . . ?
O16 C16 H16A 109.3 . . ?
O16 C16 H16B 109.3 . . ?
O16 C16 K1 54(2) . . ?
C15 K1 C15 105.1(10) 23_565 . ?
C16 K1 C15 25.1(2) . . ?
C16 K1 C15 25.0(2) 23_565 23_565 ?
C16 K1 C15 84.6(10) . 23_565 ?
C16 K1 C15 84.6(10) 23_565 . ?
C16 K1 C16 69.5(14) . 23_565 ?
O2 K1 C15 139.5(8) 44_666 . ?
O2 K1 C15 139.5(8) 41_646 23_565 ?
O2 K1 C15 82.2(9) 44_666 23_565 ?
O2 K1 C15 82.2(9) 41_646 . ?
O2 K1 C16 88.4(11) 41_646 . ?
O2 K1 C16 150.8(12) 44_666 . ?
O2 K1 C16 88.4(11) 44_666 23_565 ?
O2 K1 C16 150.8(12) 41_646 23_565 ?
O2 K1 O2 118.1(19) 44_666 41_646 ?
O2 K1 O3 54.5(8) 41_646 41_646 ?
O2 K1 O3 97.4(11) 41_646 44_666 ?
O2 K1 O3 54.5(8) 44_666 44_666 ?
O2 K1 O3 97.4(11) 44_666 41_646 ?
O2 K1 O16 72.0(12) 41_646 . ?
O2 K1 O16 168.2(14) 41_646 23_565 ?
O2 K1 O16 72.0(12) 44_666 23_565 ?
O2 K1 O16 168.2(14) 44_666 . ?
O3 K1 C15 121.9(9) 44_666 23_565 ?
O3 K1 C15 90.4(8) 44_666 . ?
O3 K1 C15 121.9(9) 41_646 . ?
O3 K1 C15 90.4(8) 41_646 23_565 ?
O3 K1 C16 108.6(10) 41_646 . ?
O3 K1 C16 108.6(10) 44_666 23_565 ?
O3 K1 C16 113.7(8) 41_646 23_565 ?
O3 K1 C16 113.7(8) 44_666 . ?
O3 K1 O3 127.9(18) 44_666 41_646 ?
O15 K1 C15 21.7(5) 23_565 23_565 ?
O15 K1 C15 21.7(5) . . ?
O15 K1 C15 106.2(12) 23_565 . ?
O15 K1 C15 106.2(12) . 23_565 ?
O15 K1 C16 81.8(11) 23_565 . ?
O15 K1 C16 81.8(11) . 23_565 ?
O15 K1 C16 42.6(7) 23_565 23_565 ?
O15 K1 C16 42.6(7) . . ?
O15 K1 O2 117.8(9) 23_565 41_646 ?
O15 K1 O2 117.8(9) . 44_666 ?
O15 K1 O2 94.8(9) . 41_646 ?
O15 K1 O2 94.8(9) 23_565 44_666 ?
O15 K1 O3 142.4(9) 23_565 44_666 ?
O15 K1 O3 142.4(9) . 41_646 ?
O15 K1 O3 71.1(10) 23_565 41_646 ?
O15 K1 O3 71.1(10) . 44_666 ?
O15 K1 O15 115.4(17) 23_565 . ?
O15 K1 O16 64.8(11) 23_565 23_565 ?
O15 K1 O16 64.8(11) . . ?
O15 K1 O16 74.4(12) . 23_565 ?
O15 K1 O16 74.4(12) 23_565 . ?
O16 K1 C15 86.0(11) 23_565 . ?
O16 K1 C15 43.7(10) 23_565 23_565 ?
O16 K1 C15 43.7(10) . . ?
O16 K1 C15 86.0(12) . 23_565 ?
O16 K1 C16 80.5(14) . 23_565 ?
O16 K1 C16 80.5(14) 23_565 . ?
O16 K1 C16 25.1(5) . . ?
O16 K1 C16 25.1(5) 23_565 23_565 ?
O16 K1 O3 133.2(11) 23_565 41_646 ?
O16 K1 O3 83.6(11) . 41_646 ?
O16 K1 O3 83.6(11) 23_565 44_666 ?
O16 K1 O3 133.2(11) . 44_666 ?
O16 K1 O16 98.7(19) 23_565 . ?
C2 O2 K1 117(2) . 42_566 ?
C2 O2 H2A 109.5 . . ?
K1 O2 H2A 70.6 42_566 . ?
C3 O3 K1 114.2(19) . 42_566 ?
C3 O3 H3A 109.5 . . ?
K1 O3 H3A 129.1 42_566 . ?
C11 O4 C4 115(2) . . ?
C1 O5 C5 105.1(3) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12A 109.5 . . ?
C13 O13 H13A 109.5 . . ?
C1 O14 C14 127(4) 5_565 . ?
C11 O15 C15 113.5(15) . . ?
C11 O15 K1 118(2) . . ?
C15 O15 K1 116.1(18) . . ?
C16 O16 K1 101(3) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 144.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -38(3) . . . . ?
C1 C2 C3 O3 -169(3) . . . . ?
C1 C2 O2 K1 166(2) . . . 42_566 ?
C2 C1 O5 C5 -63(3) . . . . ?
C2 C3 C4 C5 39(4) . . . . ?
C2 C3 C4 O4 171(3) . . . . ?
C2 C3 O3 K1 -36(3) . . . 42_566 ?
C3 C2 O2 K1 -76(2) . . . 42_566 ?
C3 C4 C5 C6 179(3) . . . . ?
C3 C4 C5 O5 -49(3) . . . . ?
C3 C4 O4 C11 103(3) . . . . ?
C4 C3 O3 K1 -165(2) . . . 42_566 ?
C4 C5 C6 O6 44(3) . . . . ?
C4 C5 O5 C1 56(3) . . . . ?
C5 C4 O4 C11 -125(3) . . . . ?
C6 C5 O5 C1 -173(3) . . . . ?
C11 C12 C13 C14 -43(4) . . . . ?
C11 C12 C13 O13 -137(3) . . . . ?
C12 C11 O4 C4 -131(3) . . . . ?
C12 C11 O15 C15 -52(4) . . . . ?
C12 C11 O15 K1 90(2) . . . . ?
C12 C13 C14 C15 52(4) . . . . ?
C12 C13 C14 O14 179(3) . . . . ?
C13 C14 C15 C16 -175(3) . . . . ?
C13 C14 C15 K1 -101(3) . . . . ?
C13 C14 C15 O15 -59(3) . . . . ?
C13 C14 O14 C1 118(5) . . . 5_565 ?
C14 C15 C16 K1 90(2) . . . . ?
C14 C15 C16 O16 44(4) . . . . ?
C14 C15 O15 C11 59(3) . . . . ?
C14 C15 O15 K1 -84(2) . . . . ?
C15 C14 O14 C1 -115(4) . . . 5_565 ?
C15 C16 O16 K1 64(3) . . . . ?
C16 C15 O15 C11 -172(3) . . . . ?
C16 C15 O15 K1 45(3) . . . . ?
K1 C15 C16 O16 -47(3) . . . . ?
K1 C15 O15 C11 142(3) . . . . ?
O2 C2 C3 C4 -161(3) . . . . ?
O2 C2 C3 O3 67(4) . . . . ?
O3 C3 C4 C5 164(3) . . . . ?
O3 C3 C4 O4 -64(3) . . . . ?
O4 C4 C5 C6 52(3) . . . . ?
O4 C4 C5 O5 -176(3) . . . . ?
O4 C11 C12 C13 -79(3) . . . . ?
O4 C11 C12 O12 72(5) . . . . ?
O4 C11 O15 C15 55(3) . . . . ?
O4 C11 O15 K1 -164(2) . . . . ?
O5 C1 C2 C3 54(3) . . . . ?
O5 C1 C2 O2 169(3) . . . . ?
O5 C5 C6 O6 -87(4) . . . . ?
O12 C12 C13 C14 160(3) . . . . ?
O12 C12 C13 O13 67(5) . . . . ?
O13 C13 C14 C15 163(3) . . . . ?
O13 C13 C14 O14 -70(4) . . . . ?
O14 C1 C2 C3 -65(3) 7_556 . . . ?
O14 C1 C2 O2 50(3) 7_556 . . . ?
O14 C1 O5 C5 70(3) 7_556 . . . ?
O14 C14 C15 C16 54(4) . . . . ?
O14 C14 C15 K1 128(3) . . . . ?
O14 C14 C15 O15 171(3) . . . . ?
O15 C11 C12 C13 43(4) . . . . ?
O15 C11 C12 O12 -166(4) . . . . ?
O15 C11 O4 C4 109(3) . . . . ?
O15 C15 C16 K1 -30(2) . . . . ?
O15 C15 C16 O16 -77(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.006 -0.939 -0.888 14121.1 1750.1 ?


_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_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 3.886
_oxdiff_exptl_absorpt_empirical_full_min 0.766
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_290K_MeOH_H2O
_database_code_depnum_ccdc_archive 'CCDC 1529160'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2016-11-21
_audit_creation_method           'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_cell_length_a                   31.42(2)
_cell_length_b                   31.42(2)
_cell_length_c                   31.42(2)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     31029(30)
_cell_formula_units_Z            1
_cell_measurement_temperature    289.4(9)
_cell_measurement_reflns_used    85
_cell_measurement_theta_min      3.6570
_cell_measurement_theta_max      7.8420
_cell_oxdiff_length_a            31.51(4)
_cell_oxdiff_length_b            31.31(4)
_cell_oxdiff_length_c            31.46(4)
_cell_oxdiff_angle_alpha         89.23(11)
_cell_oxdiff_angle_beta          89.10(10)
_cell_oxdiff_angle_gamma         89.63(11)
_cell_oxdiff_volume              31029(70)
_cell_oxdiff_measurement_reflns_used 85
_exptl_absorpt_correction_type   none
_oxdiff_exptl_absorpt_empirical_full_min 1.000
_oxdiff_exptl_absorpt_empirical_full_max 1.000
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_diffrn_ambient_temperature      289.4(9)
_diffrn_ambient_environment      methanol:water
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.0169
_diffrn_reflns_number            3362
_diffrn_reflns_av_R_equivalents  0.2803
_diffrn_reflns_av_sigmaI/netI    0.3481
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.3058
_diffrn_reflns_theta_max         8.0675
_diffrn_measured_fraction_theta_max 0.9227
_diffrn_reflns_theta_full        8.0512
_diffrn_measured_fraction_theta_full 0.8984
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0002694000
_diffrn_orient_matrix_UB_12      0.0219885000
_diffrn_orient_matrix_UB_13      0.0051443000
_diffrn_orient_matrix_UB_21      0.0004013000
_diffrn_orient_matrix_UB_22      0.0054644000
_diffrn_orient_matrix_UB_23      -0.0219552000
_diffrn_orient_matrix_UB_31      -0.0225097000
_diffrn_orient_matrix_UB_32      -0.0000224000
_diffrn_orient_matrix_UB_33      -0.0001014000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  75.00   1.00   20.00    --    0.72  57.00 -90.00  109
  2  ω    -73.00 -48.00   1.00   20.00    --    0.72 -57.00 150.00   25
  3  ω    -20.00  54.00   1.00   20.00    --    0.72 -99.00  90.00   74
;
_diffrn_measurement_method       'ω scans'
_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_symmetry_space_group_name_H-M   'I 4 3 2'
_symmetry_cell_setting           cubic
_space_group_IT_number           211
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I 4 3 2'
_reflns_odcompleteness_completeness 89.84
_reflns_odcompleteness_theta     8.05
_reflns_odcompleteness_iscentric 1
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_250K_MeOH
_database_code_depnum_ccdc_archive 'CCDC 1529164'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2016-12-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;

# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_cell_length_a                   31.247(12)
_cell_length_b                   31.247(12)
_cell_length_c                   31.247(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     30508(36)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    63
_cell_measurement_temperature    249.9(2)
_cell_measurement_theta_max      5.2980
_cell_measurement_theta_min      3.6560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?

# EXPERIMENTAL DATA 

_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.920
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             8928
_exptl_crystal_recrystallization_method 
'Crystal grown from water solution by methanol vapour diffusion'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2630
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.898
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3798
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        8.113
_diffrn_reflns_theta_max         8.113
_diffrn_reflns_theta_min         3.324
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      249.9(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.898
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00  84.00   1.00   25.00    --    0.71  19.00 -90.00  167
  2  ω    -79.00 -54.00   1.00   25.00    --    0.71  19.00  30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0002963000
_diffrn_orient_matrix_UB_12      0.0187405000
_diffrn_orient_matrix_UB_13      0.0128365000
_diffrn_orient_matrix_UB_21      -0.0001720000
_diffrn_orient_matrix_UB_22      0.0128995000
_diffrn_orient_matrix_UB_23      -0.0186696000
_diffrn_orient_matrix_UB_31      -0.0226866000
_diffrn_orient_matrix_UB_32      0.0001382000
_diffrn_orient_matrix_UB_33      0.0003616000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.465
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                132
_reflns_number_total             167
_reflns_odcompleteness_completeness 88.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     8.10
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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    ?
_computing_publication_material  ?
_computing_structure_refinement  ?
_computing_structure_solution    ?


# REFINEMENT DATA

_refine_diff_density_max         0.677
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     ?
_refine_ls_number_reflns         ?
_refine_ls_number_restraints     ?
_refine_ls_R_factor_all          ?
_refine_ls_R_factor_gt           ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          ?
_refine_ls_wR_factor_ref         ?
_refine_special_details          
;
Due to the low quality of collected data no structure refinement was performed
;

_shelx_SHELXL_version_number     2014/7

_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.000
_oxdiff_exptl_absorpt_empirical_full_min 1.000
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_270K_MeOH_H2O
_database_code_depnum_ccdc_archive 'CCDC 1529158'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2016-11-21
_audit_creation_method           'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_cell_length_a                   31.415(13)
_cell_length_b                   31.415(13)
_cell_length_c                   31.415(13)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     31003(20)
_cell_formula_units_Z            1
_cell_measurement_temperature    269.4(9)
_cell_measurement_reflns_used    96
_cell_measurement_theta_min      3.6520
_cell_measurement_theta_max      5.2860
_cell_oxdiff_length_a            31.408(19)
_cell_oxdiff_length_b            31.42(3)
_cell_oxdiff_length_c            31.413(17)
_cell_oxdiff_angle_alpha         89.92(6)
_cell_oxdiff_angle_beta          89.89(5)
_cell_oxdiff_angle_gamma         90.03(6)
_cell_oxdiff_volume              31003(30)
_cell_oxdiff_measurement_reflns_used 96
_exptl_absorpt_correction_type   none
_oxdiff_exptl_absorpt_empirical_full_min 1.000
_oxdiff_exptl_absorpt_empirical_full_max 1.000
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_diffrn_ambient_temperature      269.4(9)
_diffrn_ambient_environment      methanol:water
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.0169
_diffrn_reflns_number            1090
_diffrn_reflns_av_R_equivalents  0.1082
_diffrn_reflns_av_sigmaI/netI    0.1353
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.3067
_diffrn_reflns_theta_max         5.8070
_diffrn_measured_fraction_theta_max 0.8000
_diffrn_reflns_theta_full        5.7953
_diffrn_measured_fraction_theta_full 0.7455
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0003027000
_diffrn_orient_matrix_UB_12      -0.0051485000
_diffrn_orient_matrix_UB_13      -0.0219757000
_diffrn_orient_matrix_UB_21      -0.0000973000
_diffrn_orient_matrix_UB_22      0.0219771000
_diffrn_orient_matrix_UB_23      -0.0051822000
_diffrn_orient_matrix_UB_31      0.0225811000
_diffrn_orient_matrix_UB_32      0.0001757000
_diffrn_orient_matrix_UB_33      0.0002298000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  75.00   1.00   20.00    --    0.72  57.00 -90.00  109
  2  ω    -73.00 -48.00   1.00   20.00    --    0.72 -57.00 150.00   25
  3  ω    -20.00  54.00   1.00   20.00    --    0.72 -99.00  90.00   74
;
_diffrn_measurement_method       'ω scans'
_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_symmetry_space_group_name_H-M   'I 4 3 2'
_symmetry_cell_setting           cubic
_space_group_IT_number           211
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I 4 3 2'
_reflns_odcompleteness_completeness 74.55
_reflns_odcompleteness_theta     5.80
_reflns_odcompleteness_iscentric 1
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_200K_MeOH
_database_code_depnum_ccdc_archive 'CCDC 1529163'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2016-12-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
# CRYSTAL DATA
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_cell_length_a                   31.255(9)
_cell_length_b                   31.255(9)
_cell_length_c                   31.255(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     30531(26)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    41
_cell_measurement_temperature    199.90(14)
_cell_measurement_theta_max      5.2960
_cell_measurement_theta_min      3.6610
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?

# EXPERIMENTAL DATA 

_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.920
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       ?
_exptl_crystal_F_000             8928
_exptl_crystal_recrystallization_method 
'Crystal grown from water solution by methanol vapour diffusion'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2139
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.837
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1660
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        6.786
_diffrn_reflns_theta_max         6.786
_diffrn_reflns_theta_min         3.324
_diffrn_ambient_environment      Methanol
_diffrn_ambient_temperature      199.90(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.837
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00  71.00   1.00   25.00    --    0.71  19.00 -90.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0003127000
_diffrn_orient_matrix_UB_12      0.0187785000
_diffrn_orient_matrix_UB_13      -0.0127504000
_diffrn_orient_matrix_UB_21      0.0001682000
_diffrn_orient_matrix_UB_22      0.0127503000
_diffrn_orient_matrix_UB_23      0.0187580000
_diffrn_orient_matrix_UB_31      0.0226976000
_diffrn_orient_matrix_UB_32      0.0001644000
_diffrn_orient_matrix_UB_33      -0.0003333000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.388
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                78
_reflns_number_total             93
_reflns_odcompleteness_completeness 83.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     6.77
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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    ?
_computing_publication_material  ?
_computing_structure_refinement  ?
_computing_structure_solution    ?
# REFINEMENT DATA
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   ?
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     ?
_refine_ls_number_reflns         ?
_refine_ls_number_restraints     ?
_refine_ls_R_factor_all          ?
_refine_ls_R_factor_gt           ?
_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          ?
_refine_ls_wR_factor_ref         ?
_refine_special_details          
;
Due to the low quality of collected data no structure refinement was performed
;

_shelx_SHELXL_version_number     2014/7

_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.000
_oxdiff_exptl_absorpt_empirical_full_min 1.000
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_0_49GPa
_database_code_depnum_ccdc_archive 'CCDC 1529148'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_ATOM007_CDMOF_a_0_49GPa     
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_THETM01_CDMOF_a_0_49GPa     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_REFNR01_CDMOF_a_0_49GPa     
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT029_CDMOF_a_0_49GPa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.664 Note  
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT201_CDMOF_a_0_49GPa     
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         23 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT410_CDMOF_a_0_49GPa     
;
PROBLEM: Short Intra H...H Contact  H1     ..  H1      ..       1.77 Ang.  
RESPONSE: ...
;
_vrf_PLAT026_CDMOF_a_0_49GPa     
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         33 %     
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections; moreover crystal was destoyed during 
the measurment influencing the number of collected data'
;
_vrf_PLAT241_CDMOF_a_0_49GPa     
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O4 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT242_CDMOF_a_0_49GPa     
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         K1 Check 
RESPONSE: 'Poor data quality'
;
_vrf_PLAT306_CDMOF_a_0_49GPa     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_0_49GPa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.049 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_CDMOF_a_0_49GPa     
;
PROBLEM: D-H Without Acceptor       O16    --  H16    ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
# end Validation Reply Form
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2030 0.2500 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   31.223(3)
_cell_length_b                   31.223(3)
_cell_length_c                   31.223(3)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30438(5)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    544
_cell_measurement_temperature    295
_cell_measurement_theta_max      11.3480
_cell_measurement_theta_min      1.7850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74506
_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_absorpt_special_details   ?
# EXPERIMENTAL DATA 
_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.16GPa and then
compressed to 0.49GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.922
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8928
_exptl_crystal_preparation       ?
_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          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1225
_diffrn_reflns_av_unetI/netI     0.2244
_diffrn_reflns_Laue_measured_fraction_full 0.664
_diffrn_reflns_Laue_measured_fraction_max 0.664
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2461
_diffrn_reflns_point_group_measured_fraction_full 0.654
_diffrn_reflns_point_group_measured_fraction_max 0.654
_diffrn_reflns_theta_full        13.256
_diffrn_reflns_theta_max         13.256
_diffrn_reflns_theta_min         1.788
_diffrn_ambient_temperature      295
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         490000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.664
_diffrn_measured_fraction_theta_max 0.664
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 155.77  155
  2  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 -24.23  155
  3  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00-155.77  200
  4  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00  24.23  200
  5  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 -24.23  280
  6  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 155.77  280
  7  ω    -96.00 -30.00   0.20    0.70    --   15.00 -70.00  24.23  330
  8  ω    -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       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0037334000
_diffrn_orient_matrix_UB_12      -0.0217490000
_diffrn_orient_matrix_UB_13      -0.0001980000
_diffrn_orient_matrix_UB_21      -0.0111740000
_diffrn_orient_matrix_UB_22      0.0017036000
_diffrn_orient_matrix_UB_23      0.0189860000
_diffrn_orient_matrix_UB_31      -0.0186399000
_diffrn_orient_matrix_UB_32      0.0033240000
_diffrn_orient_matrix_UB_33      -0.0112572000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   synchrotron
_diffrn_special_details          
'high-pressure measurement with diamond-anvil cell at 0.41 GPa'
_reflns_Friedel_coverage         0.569
_reflns_Friedel_fraction_full    0.638
_reflns_Friedel_fraction_max     0.638
_reflns_number_gt                173
_reflns_number_total             524
_reflns_odcompleteness_completeness 72.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.26
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.112
_refine_diff_density_min         -0.124
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details 
;
 Flack x determined using 50 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.27(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         524
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.2266
_refine_ls_R_factor_gt           0.0670
_refine_ls_restrained_S_all      1.332
_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/[σ²(Fo²)+(0.1518P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1871
_refine_ls_wR_factor_ref         0.2693
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
 resulting in a low data:parameter ratio.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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
 C6-O6
 1.45 with sigma of 0.005
 C2-O2
 1.45 with sigma of 0.005
 O14-C15
 2.4 with sigma of 0.02
 C16-C15
 1.5 with sigma of 0.005
 O4-C12
 2.2 with sigma of 0.02
 C12-C15
 3 with sigma of 0.02
 C11-O4
 1.45 with sigma of 0.005
 C12-C11
 1.5 with sigma of 0.005
 C6-C5
 1.5 with sigma of 0.005
 C2-C5
 3 with sigma of 0.02
 C5-O6
 2 with sigma of 0.02
 O4-C4
 1.45 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.02
 O14-C14
 1.5 with sigma of 0.01
 C15-C14
 1.5 with sigma of 0.005
 C14-C15
 1.5 with sigma of 0.005
 C11-C14
 3 with sigma of 0.02
 O14-C13
 2.4 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.005
 C14-C13
 1.5 with sigma of 0.005
 C12-O12
 1.45 with sigma of 0.005
 O13-C14
 2.5 with sigma of 0.02
 O13-C13
 1.45 with sigma of 0.02
 C13-O13
 1.45 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.005
 C5-C1
 2.3 with sigma of 0.005
 C15-K1
 3.5 with sigma of 0.02
 C16-O16
 1.45 with sigma of 0.005
 O16-K1
 3 with sigma of 0.02
 O5-C6
 2.5 with sigma of 0.02
 O15-C16
 2.2 with sigma of 0.02
 O15-C15
 1.45 with sigma of 0.005
 O15-C11
 1.45 with sigma of 0.005
 O5-C5
 1.45 with sigma of 0.005
 O15-C13
 3 with sigma of 0.02
 O5-C1
 1.45 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.005
 O2-C3
 2.2 with sigma of 0.02
 C4-C3
 1.45 with sigma of 0.02
 C2-O3
 2.3 with sigma of 0.02
 O3-C3
 1.45 with sigma of 0.005
 O14-C15
 2.5 with sigma of 0.04
 O4-C12
 2.5 with sigma of 0.04
 C15-C11
 2.4 with sigma of 0.02
 O6-C5
 2.7 with sigma of 0.04
 C11-C4
 2.5 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.02
 C13-O14
 2.5 with sigma of 0.04
 C13-C15
 2.4 with sigma of 0.02
 C11-C13
 2.4 with sigma of 0.02
 O12-C11
 2.5 with sigma of 0.04
 O12-C13
 2.5 with sigma of 0.04
 O13-C12
 2.5 with sigma of 0.04
 O13-C14
 2.5 with sigma of 0.04
 O2-C1
 2.5 with sigma of 0.04
 C1-O2
 2.5 with sigma of 0.04
 C1-C5
 2.5 with sigma of 0.02
 C1-C4
 3 with sigma of 0.04
 C15-O16
 2.5 with sigma of 0.04
 O16-C15
 2.5 with sigma of 0.04
 O15-C12
 2.4 with sigma of 0.02
 C2-O5
 2.5 with sigma of 0.04
 C14-O15
 2.4 with sigma of 0.02
 C5-C3
 2.5 with sigma of 0.02
 C3-C1
 2.5 with sigma of 0.04
 O3-C2
 2.5 with sigma of 0.04
 O3-C4
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
: 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(H2A), C3(H3A), C4(H4), C5(H5), C11(H11), C12(H12A), C13(H13A),
 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(H2), O3(H3), O6(H6), O12(H12), O16(H16)
5.d Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8573(12) 0.6910(10) 0.6434(16) 0.266(15) Uiso 1 1 d D . . . .
H1 H 0.8519 0.7219 0.6425 0.319 Uiso 1 1 calc R . . . .
C2 C 0.8980(12) 0.6823(11) 0.6675(11) 0.266(15) Uiso 1 1 d D . . . .
H2A H 0.8982 0.6954 0.6960 0.319 Uiso 1 1 calc R . . . .
C3 C 0.9017(13) 0.6343(11) 0.6691(17) 0.266(15) Uiso 1 1 d D . . . .
H3A H 0.9094 0.6286 0.6393 0.319 Uiso 1 1 calc R . . . .
C4 C 0.8651(15) 0.6039(12) 0.6740(16) 0.266(15) Uiso 1 1 d D . . . .
H4 H 0.8568 0.6092 0.7038 0.319 Uiso 1 1 calc R . . . .
C5 C 0.8260(11) 0.6240(11) 0.6494(15) 0.266(15) Uiso 1 1 d D . . . .
H5 H 0.8341 0.6222 0.6191 0.319 Uiso 1 1 calc R . . . .
C6 C 0.7862(13) 0.5973(13) 0.6527(14) 0.266(15) Uiso 1 1 d D . . . .
H6A H 0.7624 0.6088 0.6363 0.319 Uiso 1 1 calc R . . . .
H6B H 0.7909 0.5674 0.6456 0.319 Uiso 1 1 calc R . . . .
C11 C 0.8663(12) 0.5337(9) 0.7144(15) 0.266(15) Uiso 1 1 d D . . . .
H11 H 0.8694 0.5546 0.7377 0.319 Uiso 1 1 calc R . . . .
C12 C 0.9058(11) 0.5064(10) 0.7153(13) 0.266(15) Uiso 1 1 d D . . . .
H12A H 0.9097 0.4966 0.7449 0.319 Uiso 1 1 calc R . . . .
C13 C 0.8999(9) 0.4672(9) 0.6880(13) 0.266(15) Uiso 1 1 d D . . . .
H13A H 0.8912 0.4795 0.6605 0.319 Uiso 1 1 calc R . . . .
C14 C 0.8606(10) 0.4428(9) 0.7011(10) 0.266(15) Uiso 1 1 d D . . . .
H14 H 0.8635 0.4320 0.7304 0.319 Uiso 1 1 calc R . . . .
C15 C 0.8223(9) 0.4715(12) 0.6972(8) 0.266(15) Uiso 1 1 d D . . . .
H15 H 0.8251 0.4827 0.6680 0.319 Uiso 1 1 calc R . . . .
C16 C 0.7745(9) 0.4688(14) 0.7027(14) 0.266(15) Uiso 1 1 d D . . . .
H16A H 0.7637 0.4974 0.7079 0.319 Uiso 1 1 calc R . . . .
H16B H 0.7623 0.4590 0.6758 0.319 Uiso 1 1 calc R . . . .
K1 K 0.8023(5) 0.5000 0.8023(5) 0.221(11) Uiso 1 2 d DS TU P . .
O2 O 0.9364(11) 0.6918(15) 0.6432(17) 0.365(12) Uiso 1 1 d D . . . .
H2 H 0.9555 0.6752 0.6502 0.547 Uiso 1 1 calc R . . . .
O3 O 0.9421(12) 0.6244(15) 0.6897(16) 0.365(12) Uiso 1 1 d D . . . .
H3 H 0.9412 0.6000 0.6994 0.547 Uiso 1 1 calc R . . . .
O4 O 0.8724(15) 0.5572(13) 0.6749(13) 0.365(12) Uiso 1 1 d D . . . .
O5 O 0.8199(11) 0.6694(11) 0.6570(15) 0.365(12) Uiso 1 1 d D . . . .
O6 O 0.7821(15) 0.6048(15) 0.6983(14) 0.365(12) Uiso 1 1 d D . . . .
H6 H 0.7798 0.5818 0.7108 0.547 Uiso 1 1 calc R . . . .
O12 O 0.9438(12) 0.5306(12) 0.7037(14) 0.365(12) Uiso 1 1 d D . . . .
H12 H 0.9641 0.5143 0.7010 0.547 Uiso 1 1 calc R . . . .
O13 O 0.9375(12) 0.4432(15) 0.6766(15) 0.365(12) Uiso 1 1 d D . . . .
H13 H 0.9471 0.4313 0.6979 0.547 Uiso 1 1 calc GR . . . .
O14 O 0.8540(13) 0.4068(12) 0.6702(13) 0.365(12) Uiso 1 1 d D . . . .
O15 O 0.8274(11) 0.5098(11) 0.7231(12) 0.365(12) Uiso 1 1 d D . . . .
O16 O 0.7591(12) 0.4411(12) 0.7365(12) 0.365(12) Uiso 1 1 d D . . . .
H16 H 0.7590 0.4162 0.7281 0.547 Uiso 1 1 calc R . . . .
OA O 1.0000 0.5000 0.647(2) 0.365(12) Uiso 1 2 d S T P . .

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.501(7) . ?
C1 O5 1.41(2) . ?
C1 O14 1.70(5) 7_556 ?
C2 H2A 0.9800 . ?
C2 C3 1.502(7) . ?
C2 K1 3.36(4) 42_566 ?
C2 O2 1.450(7) . ?
C3 H3A 0.9800 . ?
C3 C4 1.49(2) . ?
C3 O3 1.449(7) . ?
C4 H4 0.9800 . ?
C4 C5 1.57(2) . ?
C4 O4 1.47(2) . ?
C5 H5 0.9800 . ?
C5 C6 1.500(7) . ?
C5 O5 1.451(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.450(7) . ?
C11 H11 0.9800 . ?
C11 C12 1.501(7) . ?
C11 O4 1.449(7) . ?
C11 O15 1.451(7) . ?
C12 H12A 0.9800 . ?
C12 C13 1.502(7) . ?
C12 O12 1.451(7) . ?
C13 H13A 0.9800 . ?
C13 C14 1.499(7) . ?
C13 O13 1.440(18) . ?
C14 H14 0.9800 . ?
C14 C15 1.501(5) . ?
C14 O14 1.496(13) . ?
C15 H15 0.9800 . ?
C15 C16 1.502(7) . ?
C15 K1 3.46(2) . ?
C15 O15 1.452(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 K1 3.37(5) . ?
C16 O16 1.448(7) . ?
K1 C2 3.36(4) 41_646 ?
K1 C2 3.36(4) 44_666 ?
K1 C16 3.37(5) 23_565 ?
K1 O2 2.62(5) 44_666 ?
K1 O2 2.62(5) 41_646 ?
K1 O3 2.93(5) 44_666 ?
K1 O3 2.93(5) 41_646 ?
K1 O15 2.61(4) 23_565 ?
K1 O15 2.61(4) . ?
K1 O16 3.07(2) . ?
K1 O16 3.07(2) 23_565 ?
O2 K1 2.62(5) 42_566 ?
O2 H2 0.8200 . ?
O3 K1 2.93(5) 42_566 ?
O3 H3 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12 0.8200 . ?
O13 H13 0.8200 . ?
O14 C1 1.70(5) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 109.7 . . ?
C2 C1 O14 116(3) . 7_556 ?
O5 C1 H1 109.7 . . ?
O5 C1 C2 118(3) . . ?
O5 C1 O14 93(3) . 7_556 ?
O14 C1 H1 109.7 7_556 . ?
C1 C2 H2A 112.6 . . ?
C1 C2 C3 105.3(17) . . ?
C1 C2 K1 156.7(17) . 42_566 ?
C3 C2 H2A 112.6 . . ?
C3 C2 K1 93.4(14) . 42_566 ?
K1 C2 H2A 71.3 42_566 . ?
O2 C2 C1 114(3) . . ?
O2 C2 H2A 112.6 . . ?
O2 C2 C3 99.1(16) . . ?
O2 C2 K1 48(2) . 42_566 ?
C2 C3 H3A 99.7 . . ?
C4 C3 C2 125(3) . . ?
C4 C3 H3A 99.7 . . ?
O3 C3 C2 107.2(16) . . ?
O3 C3 H3A 99.7 . . ?
O3 C3 C4 119(3) . . ?
C3 C4 H4 101.0 . . ?
C3 C4 C5 106.9(19) . . ?
C5 C4 H4 101.0 . . ?
O4 C4 C3 121(4) . . ?
O4 C4 H4 101.0 . . ?
O4 C4 C5 122(3) . . ?
C4 C5 H5 104.3 . . ?
C6 C5 C4 113(3) . . ?
C6 C5 H5 104.3 . . ?
O5 C5 C4 114(3) . . ?
O5 C5 H5 104.3 . . ?
O5 C5 C6 115.1(19) . . ?
C5 C6 H6A 113.1 . . ?
C5 C6 H6B 113.1 . . ?
H6A C6 H6B 110.5 . . ?
O6 C6 C5 92.8(14) . . ?
O6 C6 H6A 113.1 . . ?
O6 C6 H6B 113.1 . . ?
C12 C11 H11 106.5 . . ?
O4 C11 H11 106.5 . . ?
O4 C11 C12 101.2(14) . . ?
O4 C11 O15 122(4) . . ?
O15 C11 H11 106.5 . . ?
O15 C11 C12 113.1(14) . . ?
C11 C12 H12A 107.2 . . ?
C11 C12 C13 110.6(14) . . ?
C13 C12 H12A 107.2 . . ?
O12 C12 C11 112(2) . . ?
O12 C12 H12A 107.2 . . ?
O12 C12 C13 113(3) . . ?
C12 C13 H13A 102.3 . . ?
C14 C13 C12 111.2(14) . . ?
C14 C13 H13A 102.3 . . ?
O13 C13 C12 118(3) . . ?
O13 C13 H13A 102.3 . . ?
O13 C13 C14 118(2) . . ?
C13 C14 H14 110.8 . . ?
C13 C14 C15 109.1(14) . . ?
C15 C14 H14 110.8 . . ?
O14 C14 C13 108.7(16) . . ?
O14 C14 H14 110.8 . . ?
O14 C14 C15 106.6(16) . . ?
C14 C15 H15 102.4 . . ?
C14 C15 C16 138(3) . . ?
C14 C15 K1 102.7(16) . . ?
C16 C15 H15 102.4 . . ?
C16 C15 K1 74.2(18) . . ?
K1 C15 H15 143.9 . . ?
O15 C15 C14 111.0(14) . . ?
O15 C15 H15 102.4 . . ?
O15 C15 C16 95.3(15) . . ?
O15 C15 K1 43.9(16) . . ?
C15 C16 H16A 108.1 . . ?
C15 C16 H16B 108.1 . . ?
C15 C16 K1 80.4(17) . . ?
H16A C16 H16B 107.3 . . ?
K1 C16 H16A 70.6 . . ?
K1 C16 H16B 171.3 . . ?
O16 C16 C15 117(3) . . ?
O16 C16 H16A 108.1 . . ?
O16 C16 H16B 108.1 . . ?
O16 C16 K1 65.5(19) . . ?
C2 K1 C2 145.1(14) 44_666 41_646 ?
C2 K1 C16 86.0(9) 41_646 . ?
C2 K1 C16 124.8(10) 41_646 23_565 ?
C2 K1 C16 86.0(9) 44_666 23_565 ?
C2 K1 C16 124.8(10) 44_666 . ?
C16 K1 C16 67.0(11) . 23_565 ?
O2 K1 C2 24.3(7) 44_666 44_666 ?
O2 K1 C2 127.3(15) 41_646 44_666 ?
O2 K1 C2 24.3(7) 41_646 41_646 ?
O2 K1 C2 127.3(15) 44_666 41_646 ?
O2 K1 C16 146.7(14) 41_646 23_565 ?
O2 K1 C16 90.7(13) 41_646 . ?
O2 K1 C16 146.7(14) 44_666 . ?
O2 K1 C16 90.7(13) 44_666 23_565 ?
O2 K1 O2 119(2) 44_666 41_646 ?
O2 K1 O3 54.7(12) 41_646 41_646 ?
O2 K1 O3 87.4(14) 44_666 41_646 ?
O2 K1 O3 87.4(14) 41_646 44_666 ?
O2 K1 O3 54.7(12) 44_666 44_666 ?
O2 K1 O16 83.1(14) 41_646 . ?
O2 K1 O16 156.8(15) 44_666 . ?
O2 K1 O16 83.1(14) 44_666 23_565 ?
O2 K1 O16 156.8(15) 41_646 23_565 ?
O3 K1 C2 43.8(6) 44_666 44_666 ?
O3 K1 C2 110.8(10) 44_666 41_646 ?
O3 K1 C2 43.8(6) 41_646 41_646 ?
O3 K1 C2 110.8(10) 41_646 44_666 ?
O3 K1 C16 124.3(10) 41_646 . ?
O3 K1 C16 124.3(10) 44_666 23_565 ?
O3 K1 C16 117.2(12) 41_646 23_565 ?
O3 K1 C16 117.2(12) 44_666 . ?
O3 K1 O3 104(2) 44_666 41_646 ?
O3 K1 O16 101.0(11) 44_666 23_565 ?
O3 K1 O16 140.4(12) 41_646 23_565 ?
O3 K1 O16 140.4(12) 44_666 . ?
O3 K1 O16 101.0(11) 41_646 . ?
O15 K1 C2 99.4(9) . 41_646 ?
O15 K1 C2 99.4(9) 23_565 44_666 ?
O15 K1 C2 96.4(10) . 44_666 ?
O15 K1 C2 96.4(10) 23_565 41_646 ?
O15 K1 C16 40.3(7) 23_565 23_565 ?
O15 K1 C16 89.9(14) . 23_565 ?
O15 K1 C16 40.3(7) . . ?
O15 K1 C16 90.0(14) 23_565 . ?
O15 K1 O2 87.8(12) . 41_646 ?
O15 K1 O2 87.8(12) 23_565 44_666 ?
O15 K1 O2 120.3(13) . 44_666 ?
O15 K1 O2 120.3(13) 23_565 41_646 ?
O15 K1 O3 76.9(12) 23_565 41_646 ?
O15 K1 O3 141.9(10) 23_565 44_666 ?
O15 K1 O3 141.9(10) . 41_646 ?
O15 K1 O3 76.9(12) . 44_666 ?
O15 K1 O15 126(2) . 23_565 ?
O15 K1 O16 73.4(13) 23_565 . ?
O15 K1 O16 64.4(9) 23_565 23_565 ?
O15 K1 O16 64.4(9) . . ?
O15 K1 O16 73.4(13) . 23_565 ?
O16 K1 C2 69.6(11) . 41_646 ?
O16 K1 C2 145.0(12) . 44_666 ?
O16 K1 C2 145.0(12) 23_565 41_646 ?
O16 K1 C2 69.6(11) 23_565 44_666 ?
O16 K1 C16 25.4(4) . . ?
O16 K1 C16 66.1(11) 23_565 . ?
O16 K1 C16 66.1(11) . 23_565 ?
O16 K1 C16 25.4(4) 23_565 23_565 ?
O16 K1 O16 76.7(18) . 23_565 ?
C2 O2 K1 108(3) . 42_566 ?
C2 O2 H2 109.5 . . ?
K1 O2 H2 47.1 42_566 . ?
C3 O3 K1 114.1(19) . 42_566 ?
C3 O3 H3 109.5 . . ?
K1 O3 H3 135.7 42_566 . ?
C11 O4 C4 120(3) . . ?
C1 O5 C5 107.9(15) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12 109.5 . . ?
C13 O13 H13 109.5 . . ?
C14 O14 C1 116(3) . 5_565 ?
C11 O15 C15 114.3(16) . . ?
C11 O15 K1 119(2) . . ?
C15 O15 K1 113(2) . . ?
C16 O16 K1 89(2) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 141.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -36(6) . . . . ?
C1 C2 C3 O3 176(5) . . . . ?
C1 C2 O2 K1 162(2) . . . 42_566 ?
C2 C1 O5 C5 -65(5) . . . . ?
C2 C3 C4 C5 35(7) . . . . ?
C2 C3 C4 O4 179(4) . . . . ?
C2 C3 O3 K1 -13(5) . . . 42_566 ?
C3 C2 O2 K1 -86(2) . . . 42_566 ?
C3 C4 C5 C6 -178(4) . . . . ?
C3 C4 C5 O5 -44(6) . . . . ?
C3 C4 O4 C11 110(6) . . . . ?
C4 C3 O3 K1 -163(4) . . . 42_566 ?
C4 C5 C6 O6 67(4) . . . . ?
C4 C5 O5 C1 60(5) . . . . ?
C5 C4 O4 C11 -110(4) . . . . ?
C6 C5 O5 C1 -167(3) . . . . ?
C11 C12 C13 C14 -55(3) . . . . ?
C11 C12 C13 O13 165(4) . . . . ?
C12 C11 O4 C4 -134(4) . . . . ?
C12 C11 O15 C15 -51(4) . . . . ?
C12 C11 O15 K1 88(3) . . . . ?
C12 C13 C14 C15 59(3) . . . . ?
C12 C13 C14 O14 174(3) . . . . ?
C13 C14 C15 C16 177(3) . . . . ?
C13 C14 C15 K1 -102.7(19) . . . . ?
C13 C14 C15 O15 -57(3) . . . . ?
C13 C14 O14 C1 117(3) . . . 5_565 ?
C14 C15 C16 K1 92(3) . . . . ?
C14 C15 C16 O16 35(5) . . . . ?
C14 C15 O15 C11 55(4) . . . . ?
C14 C15 O15 K1 -87(2) . . . . ?
C15 C14 O14 C1 -126(3) . . . 5_565 ?
C15 C16 O16 K1 64(3) . . . . ?
C16 C15 O15 C11 -158(3) . . . . ?
C16 C15 O15 K1 61(3) . . . . ?
K1 C2 C3 C4 158(5) 42_566 . . . ?
K1 C2 C3 O3 11(4) 42_566 . . . ?
K1 C15 C16 O16 -56(3) . . . . ?
K1 C15 O15 C11 141(4) . . . . ?
O2 C2 C3 C4 -154(5) . . . . ?
O2 C2 C3 O3 59(5) . . . . ?
O3 C3 C4 C5 178(5) . . . . ?
O3 C3 C4 O4 -37(8) . . . . ?
O4 C4 C5 C6 37(6) . . . . ?
O4 C4 C5 O5 171(4) . . . . ?
O4 C11 C12 C13 -82(4) . . . . ?
O4 C11 C12 O12 44(4) . . . . ?
O4 C11 O15 C15 70(4) . . . . ?
O4 C11 O15 K1 -151(3) . . . . ?
O5 C1 C2 C3 50(4) . . . . ?
O5 C1 C2 K1 -167(4) . . . 42_566 ?
O5 C1 C2 O2 158(3) . . . . ?
O5 C5 C6 O6 -67(5) . . . . ?
O12 C12 C13 C14 180(3) . . . . ?
O12 C12 C13 O13 39(5) . . . . ?
O13 C13 C14 C15 -161(4) . . . . ?
O13 C13 C14 O14 -45(4) . . . . ?
O14 C1 C2 C3 -58(3) 7_556 . . . ?
O14 C1 C2 K1 84(6) 7_556 . . 42_566 ?
O14 C1 C2 O2 50(3) 7_556 . . . ?
O14 C1 O5 C5 56(4) 7_556 . . . ?
O14 C14 C15 C16 60(4) . . . . ?
O14 C14 C15 K1 140(2) . . . . ?
O14 C14 C15 O15 -175(3) . . . . ?
O15 C11 C12 C13 50(3) . . . . ?
O15 C11 C12 O12 176(4) . . . . ?
O15 C11 O4 C4 99(5) . . . . ?
O15 C15 C16 K1 -39(2) . . . . ?
O15 C15 C16 O16 -95(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.360 -0.298 -0.350 14183.3 2153.6 ?


_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_olex2_submission_original_sample_id CDMOF_alpha_5_049
_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 1.829
_oxdiff_exptl_absorpt_empirical_full_min 0.599
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_310K_MeOH_H2O
_database_code_depnum_ccdc_archive 'CCDC 1529162'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2016-11-21
_audit_creation_method           'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'

_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_cell_length_a                   31.383(13)
_cell_length_b                   31.383(13)
_cell_length_c                   31.383(13)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30910(20)
_cell_formula_units_Z            1
_cell_measurement_temperature    279.3(10)
_cell_measurement_reflns_used    112
_cell_measurement_theta_min      3.6630
_cell_measurement_theta_max      5.8550
_cell_oxdiff_length_a            31.39(2)
_cell_oxdiff_length_b            31.379(17)
_cell_oxdiff_length_c            31.380(15)
_cell_oxdiff_angle_alpha         89.98(4)
_cell_oxdiff_angle_beta          89.93(5)
_cell_oxdiff_angle_gamma         90.04(5)
_cell_oxdiff_volume              30910(30)
_cell_oxdiff_measurement_reflns_used 112
_exptl_absorpt_correction_type   none
_oxdiff_exptl_absorpt_empirical_full_min 1.000
_oxdiff_exptl_absorpt_empirical_full_max 1.000
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_diffrn_ambient_temperature      279.3(10)
_diffrn_ambient_environment      methanol:water
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.0169
_diffrn_reflns_number            1865
_diffrn_reflns_av_R_equivalents  0.1429
_diffrn_reflns_av_sigmaI/netI    0.1821
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.3097
_diffrn_reflns_theta_max         6.7573
_diffrn_measured_fraction_theta_max 0.8692
_diffrn_reflns_theta_full        6.7436
_diffrn_measured_fraction_theta_full 0.8395
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0051549000
_diffrn_orient_matrix_UB_12      -0.0003020000
_diffrn_orient_matrix_UB_13      0.0219981000
_diffrn_orient_matrix_UB_21      -0.0219983000
_diffrn_orient_matrix_UB_22      0.0001072000
_diffrn_orient_matrix_UB_23      0.0051863000
_diffrn_orient_matrix_UB_31      -0.0001757000
_diffrn_orient_matrix_UB_32      -0.0225968000
_diffrn_orient_matrix_UB_33      -0.0002601000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  75.00   1.00   20.00    --    0.72  57.00 -90.00  109
  2  ω    -73.00 -48.00   1.00   20.00    --    0.72 -57.00 150.00   25
  3  ω    -20.00  54.00   1.00   20.00    --    0.72 -99.00  90.00   74
;
_diffrn_measurement_method       'ω scans'
_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_symmetry_space_group_name_H-M   'I 4 3 2'
_symmetry_cell_setting           cubic
_space_group_IT_number           211
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I 4 3 2'
_reflns_odcompleteness_completeness 83.95
_reflns_odcompleteness_theta     6.74
_reflns_odcompleteness_iscentric 1



##################################################################

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_280K_MeOH_H2O
_database_code_depnum_ccdc_archive 'CCDC 1529159'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2016-12-16
_audit_creation_method           'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_cell_length_a                   44.34(4)
_cell_length_b                   44.34(4)
_cell_length_c                   27.20(3)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_volume                     46323(70)
_cell_formula_units_Z            12
_cell_measurement_temperature    310.00(14)
_cell_measurement_reflns_used    56
_cell_measurement_theta_min      3.6680
_cell_measurement_theta_max      7.8830
_cell_oxdiff_length_a            44.25(5)
_cell_oxdiff_length_b            44.35(5)
_cell_oxdiff_length_c            27.24(2)
_cell_oxdiff_angle_alpha         90.02(8)
_cell_oxdiff_angle_beta          90.03(8)
_cell_oxdiff_angle_gamma         119.95(11)
_cell_oxdiff_volume              46323(70)
_cell_oxdiff_measurement_reflns_used 60
_exptl_absorpt_correction_T_min  0.67385
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.871
_oxdiff_exptl_absorpt_empirical_full_max 1.292
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      310.00(14)
_diffrn_ambient_environment      methanol:water
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.0169
_diffrn_reflns_number            4045
_diffrn_reflns_av_R_equivalents  0.7964
_diffrn_reflns_av_sigmaI/netI    0.8330
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.1816
_diffrn_reflns_theta_max         8.0852
_diffrn_measured_fraction_theta_max 0.9364
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0033707667
_diffrn_orient_matrix_UB_12      -0.0116199333
_diffrn_orient_matrix_UB_13      -0.0198637333
_diffrn_orient_matrix_UB_21      -0.0163709000
_diffrn_orient_matrix_UB_22      -0.0118876000
_diffrn_orient_matrix_UB_23      0.0104648000
_diffrn_orient_matrix_UB_31      -0.0079164333
_diffrn_orient_matrix_UB_32      0.0080209333
_diffrn_orient_matrix_UB_33      -0.0132124667
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  75.00   1.00   20.00    --    0.72  57.00 -90.00  109
  2  ω    -73.00 -48.00   1.00   20.00    --    0.72 -57.00 150.00   25
  3  ω    -20.00  54.00   1.00   20.00    --    0.72 -99.00  90.00   74
;
_diffrn_measurement_method       'ω scans'
_symmetry_space_group_name_H-M_alt 'R 3 2'
_symmetry_space_group_name_H-M   'R 3 2'
_symmetry_cell_setting           TRIGONAL
_space_group_IT_number           155
_space_group_crystal_system      TRIGONAL
_space_group_name_H-M_alt        'R 3 2'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_300K_MeOH_H2O
_database_code_depnum_ccdc_archive 'CCDC 1529161'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-20
_audit_creation_method           'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_cell_length_a                   31.325(9)
_cell_length_b                   31.325(9)
_cell_length_c                   31.325(9)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30736(16)
_cell_formula_units_Z            12
_cell_measurement_temperature    299.5(8)
_cell_measurement_reflns_used    143
_cell_measurement_theta_min      3.6570
_cell_measurement_theta_max      9.0860
_cell_oxdiff_length_a            31.360(15)
_cell_oxdiff_length_b            31.293(17)
_cell_oxdiff_length_c            31.320(15)
_cell_oxdiff_angle_alpha         89.96(4)
_cell_oxdiff_angle_beta          89.92(4)
_cell_oxdiff_angle_gamma         89.90(4)
_cell_oxdiff_volume              30736(20)
_cell_oxdiff_measurement_reflns_used 143
_exptl_absorpt_correction_T_min  0.80067
_exptl_absorpt_correction_T_max  1.00000
_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.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.869
_oxdiff_exptl_absorpt_empirical_full_max 1.231
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      299.5(8)
_diffrn_ambient_environment      methanol:water
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.0169
_diffrn_reflns_number            8324
_diffrn_reflns_av_R_equivalents  0.2781
_diffrn_reflns_av_sigmaI/netI    0.3863
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.1860
_diffrn_reflns_theta_max         10.2072
_diffrn_measured_fraction_theta_max 0.9625
_diffrn_reflns_theta_full        10.1865
_diffrn_measured_fraction_theta_full 0.9397
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0219111000
_diffrn_orient_matrix_UB_12      0.0056609000
_diffrn_orient_matrix_UB_13      -0.0001887000
_diffrn_orient_matrix_UB_21      -0.0056102000
_diffrn_orient_matrix_UB_22      -0.0219458000
_diffrn_orient_matrix_UB_23      -0.0009626000
_diffrn_orient_matrix_UB_31      -0.0004562000
_diffrn_orient_matrix_UB_32      -0.0009102000
_diffrn_orient_matrix_UB_33      0.0226237000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  75.00   1.00   20.00    --    0.72  57.00 -90.00  109
  2  ω    -73.00 -48.00   1.00   20.00    --    0.72 -57.00 150.00   25
  3  ω    -20.00  54.00   1.00   20.00    --    0.72 -99.00  90.00   74
;
_diffrn_measurement_method       'ω scans'
_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_symmetry_space_group_name_H-M   'I 4 3 2'
_symmetry_cell_setting           cubic
_space_group_IT_number           211
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        'I 4 3 2'
_reflns_odcompleteness_completeness 93.97
_reflns_odcompleteness_theta     10.19
_reflns_odcompleteness_iscentric 1
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_1_36GPa
_database_code_depnum_ccdc_archive 'CCDC 1529152'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_REFNR01_CDMOF_a_1_36GPa     
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_THETM01_CDMOF_a_1_36GPa     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT029_CDMOF_a_1_36GPa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.791 Note  
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT090_CDMOF_a_1_36GPa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.37 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT201_CDMOF_a_1_36GPa     
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT241_CDMOF_a_1_36GPa     
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O4 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT242_CDMOF_a_1_36GPa     
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C1 Check 
RESPONSE: 'Poor data quality'
;
_vrf_PLAT306_CDMOF_a_1_36GPa     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_1_36GPa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.039 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT410_CDMOF_a_1_36GPa     
;
PROBLEM: Short Intra H...H Contact  H1     ..  H14     ..       1.85 Ang.  
RESPONSE: 'Strained conformation'
;
_vrf_PLAT420_CDMOF_a_1_36GPa     
;
PROBLEM: D-H Without Acceptor       O16    --  H16    ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
_vrf_PLAT910_CDMOF_a_1_36GPa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          12 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample limiting the range of 
collected reflections'
;
_vrf_PLAT911_CDMOF_a_1_36GPa     
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.250         35 Report
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample limiting the range of 
collected reflections'
;
# end Validation Reply Form
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   30.898(3)
_cell_length_b                   30.898(3)
_cell_length_c                   30.898(3)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     29499(5)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    2119
_cell_measurement_temperature    295
_cell_measurement_theta_max      10.0680
_cell_measurement_theta_min      3.6860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32866
_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_absorpt_special_details   ?

# EXPERIMENTAL DATA 
_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.26GPa and then
compressed to 1.36GPa
;

_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.952
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             8928
_exptl_crystal_recrystallization_method 
'Compressed crystal that was grown in situ from methano:water solution in the diamond-anvil cell at 0.2 GPa.'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1072
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.791
_diffrn_reflns_Laue_measured_fraction_max 0.791
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9046
_diffrn_reflns_point_group_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        10.220
_diffrn_reflns_theta_max         10.220
_diffrn_reflns_theta_min         3.230
_diffrn_ambient_temperature      295
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         1360000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0338
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.791
_diffrn_measured_fraction_theta_max 0.791
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   35.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   35.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   35.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   35.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   35.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   35.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   35.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   35.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   35.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   35.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0001905000
_diffrn_orient_matrix_UB_12      -0.0028041000
_diffrn_orient_matrix_UB_13      0.0227885000
_diffrn_orient_matrix_UB_21      0.0049426000
_diffrn_orient_matrix_UB_22      -0.0222873000
_diffrn_orient_matrix_UB_23      -0.0026850000
_diffrn_orient_matrix_UB_31      0.0223866000
_diffrn_orient_matrix_UB_32      0.0050083000
_diffrn_orient_matrix_UB_33      0.0002623000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          
'high-pressure measurement in diamond-anvil cell at 1.36 GPa'
_reflns_Friedel_coverage         0.590
_reflns_Friedel_fraction_full    0.929
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                275
_reflns_number_total             283
_reflns_odcompleteness_completeness 88.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     10.20
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.162
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 
;
 Flack x determined using 99 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         283
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0907
_refine_ls_restrained_S_all      2.078
_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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2341
_refine_ls_wR_factor_ref         0.2350
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
 resulting in a low data:parameter ratio.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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
 C16-C15
 1.5 with sigma of 0.002
 C14-C15
 1.5 with sigma of 0.002
 O14-C15
 2.4 with sigma of 0.02
 C14-O14
 1.45 with sigma of 0.002
 C14-C13
 1.5 with sigma of 0.02
 O2-C3
 2.2 with sigma of 0.02
 O3-C3
 1.45 with sigma of 0.002
 C11-O4
 1.45 with sigma of 0.002
 C11-C14
 3 with sigma of 0.02
 C4-O4
 1.45 with sigma of 0.002
 C4-C3
 1.5 with sigma of 0.002
 C12-O4
 2 with sigma of 0.02
 C12-C15
 3 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.02
 C12-O12
 1.45 with sigma of 0.02
 C15-C12
 3 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.002
 C2-C3
 1.5 with sigma of 0.002
 C2-O2
 1.45 with sigma of 0.002
 C2-O3
 2.3 with sigma of 0.02
 C1-C4
 2.8 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.002
 O13-C13
 1.45 with sigma of 0.002
 C6-C5
 1.5 with sigma of 0.002
 C4-C5
 1.5 with sigma of 0.002
 C2-C5
 3 with sigma of 0.02
 C5-C2
 3 with sigma of 0.02
 C5-C1
 2.3 with sigma of 0.002
 O5-C6
 2.5 with sigma of 0.02
 O15-C16
 2.2 with sigma of 0.02
 O15-C15
 1.45 with sigma of 0.002
 O5-C3
 3 with sigma of 0.02
 O15-C13
 3 with sigma of 0.02
 O15-C11
 1.45 with sigma of 0.002
 O5-C1
 1.45 with sigma of 0.002
 O5-C5
 1.45 with sigma of 0.002
 C16-O16
 1.45 with sigma of 0.002
 C6-O6
 1.45 with sigma of 0.002
 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
 C11-C13
 2.4 with sigma of 0.02
 C15-C11
 2.4 with sigma of 0.02
 C11-C4
 2.5 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.02
 O2-C3
 2.5 with sigma of 0.04
 C4-C2
 2.5 with sigma of 0.02
 C4-C11
 2.5 with sigma of 0.04
 O4-C3
 2.5 with sigma of 0.04
 O4-C12
 2.5 with sigma of 0.04
 C3-C1
 2.5 with sigma of 0.02
 O2-C1
 2.5 with sigma of 0.04
 C3-O4
 2.1 with sigma of 0.04
 O3-C4
 2.5 with sigma of 0.04
 O3-C2
 2.5 with sigma of 0.04
 C14-C16
 2.5 with sigma of 0.04
 C5-C3
 2.5 with sigma of 0.02
 O4-C5
 2.5 with sigma of 0.04
 C6-C4
 2.5 with sigma of 0.04
 C14-O15
 2.4 with sigma of 0.02
 O5-C4
 2.5 with sigma of 0.02
 O15-C12
 2.4 with sigma of 0.02
 C2-O5
 2.5 with sigma of 0.02
 O4-O15
 2.5 with sigma of 0.04
 O15-C16
 2.5 with sigma of 0.04
 C6-O5
 2.5 with sigma of 0.04
 C1-C5
 2.5 with sigma of 0.04
 C1-C3
 2.5 with sigma of 0.04
 O6-C5
 2.7 with sigma of 0.04
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(H16B,H16A)
5.c Tetrahedral OH refined with riding coordinates:
 O2(H2A), O3(H3A), O6(H6), O12(H12A), O13(H13A), O16(H16)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8484(9) 0.6850(8) 0.6271(10) 0.157(10) Uiso 1 1 d D . . . .
H1 H 0.8441 0.7159 0.6215 0.188 Uiso 1 1 calc R . . . .
C2 C 0.8871(8) 0.6801(7) 0.6560(11) 0.157(10) Uiso 1 1 d D . . . .
H2 H 0.8832 0.6958 0.6832 0.188 Uiso 1 1 calc R . . . .
C3 C 0.8941(7) 0.6327(7) 0.6640(12) 0.157(10) Uiso 1 1 d D . . . .
H3 H 0.9066 0.6222 0.6368 0.188 Uiso 1 1 calc R . . . .
C4 C 0.8535(8) 0.6065(8) 0.6690(12) 0.157(10) Uiso 1 1 d D . . . .
H4 H 0.8447 0.6143 0.6984 0.188 Uiso 1 1 calc R . . . .
C5 C 0.8147(8) 0.6206(8) 0.6434(10) 0.157(10) Uiso 1 1 d D . . . .
H5 H 0.8167 0.6089 0.6140 0.188 Uiso 1 1 calc R . . . .
C6 C 0.7786(11) 0.5982(12) 0.6671(12) 0.157(10) Uiso 1 1 d D . . . .
H6A H 0.7511 0.6062 0.6543 0.188 Uiso 1 1 calc R . . . .
H6B H 0.7820 0.5671 0.6645 0.188 Uiso 1 1 calc R . . . .
C11 C 0.8541(9) 0.5372(8) 0.7132(10) 0.157(10) Uiso 1 1 d D . . . .
H11 H 0.8560 0.5576 0.7374 0.188 Uiso 1 1 calc R . . . .
C12 C 0.8963(8) 0.5134(10) 0.7120(14) 0.157(10) Uiso 1 1 d D . . . .
H12 H 0.9023 0.5019 0.7410 0.188 Uiso 1 1 calc R . . . .
C13 C 0.8928(9) 0.4756(11) 0.6807(13) 0.157(10) Uiso 1 1 d D . . . .
H13 H 0.8983 0.4804 0.6498 0.188 Uiso 1 1 calc R . . . .
C14 C 0.8548(9) 0.4461(9) 0.6944(12) 0.157(10) Uiso 1 1 d D . . . .
H14 H 0.8602 0.4355 0.7238 0.188 Uiso 1 1 calc R . . . .
C15 C 0.8135(7) 0.4717(10) 0.6942(10) 0.157(10) Uiso 1 1 d D . . . .
H15 H 0.8080 0.4818 0.6647 0.188 Uiso 1 1 calc R . . . .
C16 C 0.7727(10) 0.4522(12) 0.7119(12) 0.157(10) Uiso 1 1 d D . . . .
H16B H 0.7492 0.4726 0.7080 0.188 Uiso 1 1 calc R . . . .
H16A H 0.7659 0.4264 0.6953 0.188 Uiso 1 1 calc R . . . .
K1 K 0.8043(5) 0.5000 0.8043(5) 0.247(15) Uani 1 2 d S TU P . .
O2 O 0.9270(10) 0.6927(12) 0.6347(13) 0.269(10) Uiso 1 1 d D . . . .
H2A H 0.9432 0.6717 0.6331 0.403 Uiso 1 1 calc R . . . .
O3 O 0.9297(11) 0.6302(10) 0.6944(12) 0.269(10) Uiso 1 1 d D . . . .
H3A H 0.9310 0.6058 0.7046 0.403 Uiso 1 1 calc R . . . .
O4 O 0.8653(11) 0.5614(8) 0.6746(10) 0.269(10) Uiso 1 1 d D . . . .
O5 O 0.8075(8) 0.6669(9) 0.6413(11) 0.269(10) Uiso 1 1 d D . . . .
O6 O 0.7789(14) 0.6102(15) 0.7125(12) 0.269(10) Uiso 1 1 d D . . . .
H6 H 0.7834 0.5887 0.7274 0.403 Uiso 1 1 calc R . . . .
O12 O 0.9330(13) 0.5382(13) 0.6981(12) 0.269(10) Uiso 1 1 d D . . . .
H12A H 0.9534 0.5219 0.6932 0.403 Uiso 1 1 calc R . . . .
O13 O 0.9176(12) 0.4430(14) 0.7036(13) 0.269(10) Uiso 1 1 d D . . . .
H13A H 0.9228 0.4227 0.6873 0.403 Uiso 1 1 calc R . . . .
O14 O 0.8514(12) 0.4094(11) 0.6654(11) 0.269(10) Uiso 1 1 d D . . . .
O15 O 0.8177(8) 0.5090(9) 0.7225(10) 0.269(10) Uiso 1 1 d D . . . .
O16 O 0.7754(14) 0.4407(13) 0.7573(12) 0.269(10) Uiso 1 1 d D . . . .
H16 H 0.7856 0.4163 0.7597 0.403 Uiso 1 1 calc R . . . .
OA O 1.0000 0.5000 0.6516(19) 0.269(10) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.501(3) . ?
C1 O5 1.449(3) . ?
C1 O14 1.29(4) 7_556 ?
C2 H2 0.9800 . ?
C2 C3 1.501(3) . ?
C2 O2 1.450(3) . ?
C3 H3 0.9800 . ?
C3 C4 1.500(3) . ?
C3 O3 1.450(3) . ?
C4 H4 0.9800 . ?
C4 C5 1.501(3) . ?
C4 O4 1.450(3) . ?
C5 H5 0.9800 . ?
C5 C6 1.501(3) . ?
C5 O5 1.451(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.451(3) . ?
C11 H11 0.9800 . ?
C11 C12 1.500(3) . ?
C11 K1 3.41(3) . ?
C11 O4 1.450(3) . ?
C11 O15 1.450(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.52(2) . ?
C12 O12 1.43(3) . ?
C13 H13 0.9800 . ?
C13 C14 1.55(2) . ?
C13 O13 1.450(3) . ?
C14 H14 0.9800 . ?
C14 C15 1.500(3) . ?
C14 O14 1.450(3) . ?
C15 H15 0.9800 . ?
C15 C16 1.500(3) . ?
C15 K1 3.52(3) . ?
C15 O15 1.451(3) . ?
C16 H16B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 K1 3.36(4) . ?
C16 O16 1.450(3) . ?
K1 C11 3.41(3) 23_565 ?
K1 C16 3.36(4) 23_565 ?
K1 O2 2.94(4) 44_666 ?
K1 O2 2.94(4) 41_646 ?
K1 O3 2.97(3) 41_646 ?
K1 O3 2.97(3) 44_666 ?
K1 O15 2.58(3) . ?
K1 O15 2.58(3) 23_565 ?
K1 O16 2.50(4) . ?
K1 O16 2.50(4) 23_565 ?
O2 K1 2.94(4) 42_566 ?
O2 H2A 0.8200 . ?
O3 K1 2.97(3) 42_566 ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O14 C1 1.29(4) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 108.2 . . ?
O5 C1 H1 108.2 . . ?
O5 C1 C2 118.5(17) . . ?
O14 C1 H1 108.2 7_556 . ?
O14 C1 C2 115(3) 7_556 . ?
O14 C1 O5 98(3) 7_556 . ?
C1 C2 H2 111.2 . . ?
C1 C2 C3 108.1(12) . . ?
C3 C2 H2 111.2 . . ?
O2 C2 C1 112(3) . . ?
O2 C2 H2 111.2 . . ?
O2 C2 C3 102.5(16) . . ?
C2 C3 H3 103.8 . . ?
C4 C3 C2 115.1(13) . . ?
C4 C3 H3 103.8 . . ?
O3 C3 C2 105.5(16) . . ?
O3 C3 H3 103.8 . . ?
O3 C3 C4 123(3) . . ?
C3 C4 H4 101.2 . . ?
C3 C4 C5 117.3(13) . . ?
C5 C4 H4 101.2 . . ?
O4 C4 C3 108.6(19) . . ?
O4 C4 H4 101.2 . . ?
O4 C4 C5 123(2) . . ?
C4 C5 H5 109.3 . . ?
C4 C5 C6 102(2) . . ?
C6 C5 H5 109.3 . . ?
O5 C5 C4 115.6(15) . . ?
O5 C5 H5 109.3 . . ?
O5 C5 C6 111.2(17) . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
O6 C6 C5 110(3) . . ?
O6 C6 H6A 109.6 . . ?
O6 C6 H6B 109.6 . . ?
C12 C11 H11 106.4 . . ?
C12 C11 K1 104.3(17) . . ?
K1 C11 H11 67.2 . . ?
O4 C11 H11 106.4 . . ?
O4 C11 C12 91.4(14) . . ?
O4 C11 K1 164.1(17) . . ?
O4 C11 O15 131(3) . . ?
O15 C11 H11 106.4 . . ?
O15 C11 C12 112.5(15) . . ?
O15 C11 K1 44.3(15) . . ?
C11 C12 H12 108.6 . . ?
C11 C12 C13 109.3(17) . . ?
C13 C12 H12 108.6 . . ?
O12 C12 C11 116(3) . . ?
O12 C12 H12 108.6 . . ?
O12 C12 C13 106(3) . . ?
C12 C13 H13 119.3 . . ?
C12 C13 C14 109.3(19) . . ?
C14 C13 H13 119.3 . . ?
O13 C13 C12 101(3) . . ?
O13 C13 H13 119.3 . . ?
O13 C13 C14 82(2) . . ?
C13 C14 H14 108.9 . . ?
C15 C14 C13 109.6(17) . . ?
C15 C14 H14 108.9 . . ?
O14 C14 C13 110(3) . . ?
O14 C14 H14 108.9 . . ?
O14 C14 C15 110.3(17) . . ?
C14 C15 H15 108.7 . . ?
C14 C15 K1 101.3(17) . . ?
C16 C15 C14 120(3) . . ?
C16 C15 H15 108.7 . . ?
C16 C15 K1 71.4(14) . . ?
K1 C15 H15 143.6 . . ?
O15 C15 C14 109.8(15) . . ?
O15 C15 H15 108.7 . . ?
O15 C15 C16 100.1(15) . . ?
O15 C15 K1 39.6(13) . . ?
C15 C16 H16B 108.8 . . ?
C15 C16 H16A 108.8 . . ?
C15 C16 K1 83.6(15) . . ?
H16B C16 H16A 107.7 . . ?
K1 C16 H16B 92.2 . . ?
K1 C16 H16A 150.8 . . ?
O16 C16 C15 114(3) . . ?
O16 C16 H16B 108.8 . . ?
O16 C16 H16A 108.8 . . ?
O16 C16 K1 43(2) . . ?
C11 K1 C11 149.2(12) . 23_565 ?
C16 K1 C11 65.0(6) 23_565 23_565 ?
C16 K1 C11 89.7(8) 23_565 . ?
C16 K1 C11 89.7(8) . 23_565 ?
C16 K1 C11 65.0(6) . . ?
C16 K1 C16 72.5(14) . 23_565 ?
O2 K1 C11 104.9(7) 41_646 23_565 ?
O2 K1 C11 104.9(7) 44_666 . ?
O2 K1 C11 89.7(7) 44_666 23_565 ?
O2 K1 C11 89.7(7) 41_646 . ?
O2 K1 C16 82.8(11) 44_666 23_565 ?
O2 K1 C16 82.8(11) 41_646 . ?
O2 K1 C16 153.0(13) 44_666 . ?
O2 K1 C16 153.0(13) 41_646 23_565 ?
O2 K1 O2 123.3(19) 44_666 41_646 ?
O2 K1 O3 53.8(7) 41_646 41_646 ?
O2 K1 O3 97.1(10) 41_646 44_666 ?
O2 K1 O3 53.8(7) 44_666 44_666 ?
O2 K1 O3 97.1(10) 44_666 41_646 ?
O3 K1 C11 57.1(8) 44_666 . ?
O3 K1 C11 143.5(7) 44_666 23_565 ?
O3 K1 C11 57.1(8) 41_646 23_565 ?
O3 K1 C11 143.5(7) 41_646 . ?
O3 K1 C16 122.1(8) 41_646 23_565 ?
O3 K1 C16 105.1(9) 41_646 . ?
O3 K1 C16 105.1(9) 44_666 23_565 ?
O3 K1 C16 122.1(8) 44_666 . ?
O3 K1 O3 121.2(17) 44_666 41_646 ?
O15 K1 C11 127.7(12) . 23_565 ?
O15 K1 C11 23.1(5) . . ?
O15 K1 C11 127.7(12) 23_565 . ?
O15 K1 C11 23.1(5) 23_565 23_565 ?
O15 K1 C16 78.7(11) . 23_565 ?
O15 K1 C16 42.3(7) . . ?
O15 K1 C16 78.7(11) 23_565 . ?
O15 K1 C16 42.3(7) 23_565 23_565 ?
O15 K1 O2 122.8(9) 23_565 41_646 ?
O15 K1 O2 90.6(9) 23_565 44_666 ?
O15 K1 O2 90.6(9) . 41_646 ?
O15 K1 O2 122.8(9) . 44_666 ?
O15 K1 O3 79.9(9) 23_565 41_646 ?
O15 K1 O3 138.2(9) 23_565 44_666 ?
O15 K1 O3 138.2(9) . 41_646 ?
O15 K1 O3 79.9(9) . 44_666 ?
O15 K1 O15 109.1(15) 23_565 . ?
O16 K1 C11 85.9(11) . . ?
O16 K1 C11 73.7(11) 23_565 . ?
O16 K1 C11 73.7(11) . 23_565 ?
O16 K1 C11 85.9(11) 23_565 23_565 ?
O16 K1 C16 81.4(13) . 23_565 ?
O16 K1 C16 81.3(13) 23_565 . ?
O16 K1 C16 23.3(8) 23_565 23_565 ?
O16 K1 C16 23.3(8) . . ?
O16 K1 O2 160.8(14) 23_565 41_646 ?
O16 K1 O2 71.7(12) 23_565 44_666 ?
O16 K1 O2 160.8(14) . 44_666 ?
O16 K1 O2 71.7(12) . 41_646 ?
O16 K1 O3 141.9(11) 23_565 41_646 ?
O16 K1 O3 82.2(12) . 41_646 ?
O16 K1 O3 82.2(12) 23_565 44_666 ?
O16 K1 O3 141.9(11) . 44_666 ?
O16 K1 O15 70.4(13) 23_565 . ?
O16 K1 O15 64.3(12) . . ?
O16 K1 O15 64.3(12) 23_565 23_565 ?
O16 K1 O15 70.4(13) . 23_565 ?
O16 K1 O16 97(2) . 23_565 ?
C2 O2 K1 112(2) . 42_566 ?
C2 O2 H2A 109.5 . . ?
K1 O2 H2A 66.0 42_566 . ?
C3 O3 K1 121.9(18) . 42_566 ?
C3 O3 H3A 109.5 . . ?
K1 O3 H3A 126.0 42_566 . ?
C11 O4 C4 122(2) . . ?
C1 O5 C5 105.1(3) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12A 109.5 . . ?
C13 O13 H13A 109.5 . . ?
C1 O14 C14 114(3) 5_565 . ?
C11 O15 C15 115.4(16) . . ?
C11 O15 K1 113(2) . . ?
C15 O15 K1 119.3(18) . . ?
C16 O16 K1 114(3) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 118.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -37(3) . . . . ?
C1 C2 C3 O3 -176(3) . . . . ?
C1 C2 O2 K1 171.1(18) . . . 42_566 ?
C2 C1 O5 C5 -64(3) . . . . ?
C2 C3 C4 C5 33(4) . . . . ?
C2 C3 C4 O4 178(3) . . . . ?
C2 C3 O3 K1 -31(3) . . . 42_566 ?
C3 C2 O2 K1 -73(2) . . . 42_566 ?
C3 C4 C5 C6 -161(3) . . . . ?
C3 C4 C5 O5 -41(4) . . . . ?
C3 C4 O4 C11 119(4) . . . . ?
C4 C3 O3 K1 -166(2) . . . 42_566 ?
C4 C5 C6 O6 56(4) . . . . ?
C4 C5 O5 C1 52(3) . . . . ?
C5 C4 O4 C11 -98(4) . . . . ?
C6 C5 O5 C1 167(2) . . . . ?
C11 C12 C13 C14 -57(3) . . . . ?
C11 C12 C13 O13 -142(2) . . . . ?
C12 C11 O4 C4 -143(3) . . . . ?
C12 C11 O15 C15 -54(4) . . . . ?
C12 C11 O15 K1 88(2) . . . . ?
C12 C13 C14 C15 59(3) . . . . ?
C12 C13 C14 O14 -179(2) . . . . ?
C13 C14 C15 C16 -172(3) . . . . ?
C13 C14 C15 K1 -97(2) . . . . ?
C13 C14 C15 O15 -57(3) . . . . ?
C13 C14 O14 C1 131(4) . . . 5_565 ?
C14 C15 C16 K1 92(2) . . . . ?
C14 C15 C16 O16 61(4) . . . . ?
C14 C15 O15 C11 55(3) . . . . ?
C14 C15 O15 K1 -84(2) . . . . ?
C15 C14 O14 C1 -108(3) . . . 5_565 ?
C15 C16 O16 K1 49(4) . . . . ?
C16 C15 O15 C11 -178(3) . . . . ?
C16 C15 O15 K1 44(3) . . . . ?
K1 C11 C12 C13 100(2) . . . . ?
K1 C11 C12 O12 -141(3) . . . . ?
K1 C11 O4 C4 28(10) . . . . ?
K1 C11 O15 C15 -142(3) . . . . ?
K1 C15 C16 O16 -31(3) . . . . ?
K1 C15 O15 C11 139(3) . . . . ?
O2 C2 C3 C4 -156(3) . . . . ?
O2 C2 C3 O3 65(4) . . . . ?
O3 C3 C4 C5 163(3) . . . . ?
O3 C3 C4 O4 -52(4) . . . . ?
O4 C4 C5 C6 59(3) . . . . ?
O4 C4 C5 O5 180(3) . . . . ?
O4 C11 C12 C13 -83(3) . . . . ?
O4 C11 C12 O12 37(4) . . . . ?
O4 C11 O15 C15 60(4) . . . . ?
O4 C11 O15 K1 -159(2) . . . . ?
O5 C1 C2 C3 57(3) . . . . ?
O5 C1 C2 O2 170(2) . . . . ?
O5 C5 C6 O6 -67(4) . . . . ?
O12 C12 C13 C14 178(3) . . . . ?
O12 C12 C13 O13 93(3) . . . . ?
O13 C13 C14 C15 158(3) . . . . ?
O13 C13 C14 O14 -81(3) . . . . ?
O14 C1 C2 C3 -58(3) 7_556 . . . ?
O14 C1 C2 O2 54(3) 7_556 . . . ?
O14 C1 O5 C5 60(3) 7_556 . . . ?
O14 C14 C15 C16 66(4) . . . . ?
O14 C14 C15 K1 141(3) . . . . ?
O14 C14 C15 O15 -178(3) . . . . ?
O15 C11 C12 C13 54(3) . . . . ?
O15 C11 C12 O12 173(3) . . . . ?
O15 C11 O4 C4 95(3) . . . . ?
O15 C15 C16 K1 -28(2) . . . . ?
O15 C15 C16 O16 -59(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.330 -0.859 -0.733 13801.1 1602.4 ?
2 0.000 0.250 0.500 9.1 0.0 ?
3 0.000 0.500 0.250 9.1 0.0 ?
4 0.000 0.500 0.750 9.1 0.0 ?
5 0.000 0.750 0.500 9.1 0.0 ?
6 0.250 0.000 0.500 9.1 0.0 ?
7 0.250 0.500 0.000 9.1 0.0 ?
8 0.500 0.000 0.250 9.1 0.0 ?
9 0.500 0.000 0.750 9.1 0.0 ?
10 0.500 0.250 0.000 9.1 0.0 ?
11 0.500 0.750 0.000 9.1 0.0 ?
12 0.750 0.000 0.500 9.1 0.0 ?
13 0.750 0.500 0.000 9.1 0.0 ?


_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_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 2.197
_oxdiff_exptl_absorpt_empirical_full_min 0.750


##################################################################



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_270K
_database_code_depnum_ccdc_archive 'CCDC 1529156'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_THETM01_CDMOF_a_270K        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly diffracting sample crystal'
;
_vrf_PLAT029_CDMOF_a_270K        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.938 Note  
RESPONSE: 'Theta angle was limited due to the poorly diffracting sample crystal'
;
_vrf_PLAT201_CDMOF_a_270K        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT090_CDMOF_a_270K        
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.08 Note  
RESPONSE: 'Data limited due to the poorly diffracting sample crystal'
;
_vrf_PLAT242_CDMOF_a_270K        
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C1 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT306_CDMOF_a_270K        
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_270K        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.025 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_CDMOF_a_270K        
;
PROBLEM: D-H Without Acceptor       O16    --  H16    ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
# end Validation Reply Form

# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;


_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   31.2093(16)
_cell_length_b                   31.2093(16)
_cell_length_c                   31.2093(16)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30399(3)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    1891
_cell_measurement_temperature    269.99(10)
_cell_measurement_theta_max      12.9810
_cell_measurement_theta_min      3.1560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  54.00   1.00   15.00    --  -18.72   0.00-150.00  122
  2  ω    -73.00  20.00   1.00   15.00    --  -18.72 -19.00  60.00   93
  3  ω    -40.00   8.00   1.00   15.00    --  -18.72  57.00  60.00   48
  4  ω    -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       'ω 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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_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_odcompleteness_completeness 97.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.66
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_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_coef       .
_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_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0594
_refine_ls_restrained_S_all      1.177
_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/[σ²(Fo²)+(0.0986P)²+25.3536P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1534
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8512(5) 0.6780(5) 0.6275(5) 0.089(6) Uiso 1 1 d D . . . .
H1 H 0.8458 0.7089 0.6261 0.107 Uiso 1 1 calc R . . . .
C2 C 0.8881(6) 0.6752(6) 0.6548(6) 0.121(7) Uiso 1 1 d D . . . .
H2 H 0.8823 0.6899 0.6819 0.145 Uiso 1 1 calc R . . . .
C3 C 0.8947(5) 0.6273(5) 0.6631(5) 0.083(6) Uiso 1 1 d D . . . .
H3 H 0.9024 0.6169 0.6345 0.100 Uiso 1 1 calc R . . . .
C4 C 0.8563(5) 0.6027(6) 0.6723(5) 0.092(6) Uiso 1 1 d D . . . .
H4 H 0.8494 0.6120 0.7014 0.110 Uiso 1 1 calc R . . . .
C5 C 0.8142(6) 0.6151(7) 0.6468(7) 0.139(8) Uiso 1 1 d D . . . .
H5 H 0.8195 0.6055 0.6174 0.167 Uiso 1 1 calc R . . . .
C6 C 0.7709(7) 0.5958(7) 0.6585(7) 0.161(9) Uiso 1 1 d D . . . .
H6A H 0.7485 0.6061 0.6395 0.193 Uiso 1 1 calc R . . . .
H6B H 0.7717 0.5648 0.6573 0.193 Uiso 1 1 calc R . . . .
C11 C 0.8599(6) 0.5395(6) 0.7201(7) 0.162(9) Uiso 1 1 d D . . . .
H11 H 0.8608 0.5612 0.7428 0.194 Uiso 1 1 calc R . . . .
C12 C 0.8968(5) 0.5124(6) 0.7202(6) 0.106(7) Uiso 1 1 d D . . . .
H12 H 0.8977 0.4998 0.7489 0.127 Uiso 1 1 calc R . . . .
C13 C 0.8976(5) 0.4760(5) 0.6909(6) 0.108(7) Uiso 1 1 d D . . . .
H13 H 0.8985 0.4861 0.6612 0.130 Uiso 1 1 calc R . . . .
C14 C 0.8559(5) 0.4508(5) 0.6990(6) 0.090(6) Uiso 1 1 d D . . . .
H14 H 0.8551 0.4388 0.7280 0.108 Uiso 1 1 calc R . . . .
C15 C 0.8183(6) 0.4800(6) 0.6906(7) 0.132(8) Uiso 1 1 d D . . . .
H15 H 0.8168 0.4914 0.6615 0.159 Uiso 1 1 calc R . . . .
C16 C 0.7799(6) 0.4555(6) 0.7047(6) 0.130(8) Uiso 1 1 d D . . . .
H16A H 0.7550 0.4730 0.6989 0.156 Uiso 1 1 calc R . . . .
H16B H 0.7778 0.4303 0.6866 0.156 Uiso 1 1 calc R . . . .
K1 K 0.81029(13) 0.5000 0.81029(13) 0.138(3) Uani 1 2 d S T P . .
O2 O 0.9240(5) 0.6949(4) 0.6340(4) 0.163(3) Uiso 1 1 d . . . . .
H2A H 0.9429 0.6770 0.6305 0.245 Uiso 1 1 calc R . . . .
O3 O 0.9345(5) 0.6203(4) 0.6869(4) 0.163(3) Uiso 1 1 d . . . . .
H3A H 0.9349 0.5957 0.6962 0.245 Uiso 1 1 calc R . . . .
O4 O 0.8625(4) 0.5579(5) 0.6779(5) 0.142(6) Uiso 1 1 d D . . . .
O5 O 0.8141(4) 0.6623(5) 0.6442(5) 0.163(3) Uiso 1 1 d D . . . .
O6 O 0.7641(4) 0.6107(4) 0.7020(5) 0.163(3) Uiso 1 1 d . . . . .
H6 H 0.7630 0.5900 0.7182 0.245 Uiso 1 1 calc R . . . .
O12 O 0.9376(4) 0.5366(4) 0.7161(4) 0.147(5) Uiso 1 1 d . . . . .
H12A H 0.9573 0.5198 0.7113 0.221 Uiso 1 1 calc R . . . .
O13 O 0.9354(4) 0.4494(4) 0.7002(3) 0.125(5) Uiso 1 1 d D . . . .
H13A H 0.9276 0.4258 0.7086 0.187 Uiso 1 1 calc R . . . .
O14 O 0.8576(3) 0.4172(4) 0.6665(3) 0.093(4) Uiso 1 1 d . . . . .
O15 O 0.8226(3) 0.5115(4) 0.7235(3) 0.097(4) Uiso 1 1 d D . . . .
O16 O 0.7773(4) 0.4420(4) 0.7467(4) 0.141(5) Uiso 1 1 d . . . . .
H16 H 0.7833 0.4165 0.7481 0.211 Uiso 1 1 calc R . . . .
OA O 1.0000 0.5000 0.6626(10) 0.292(13) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.436(16) . ?
C1 O5 1.362(14) . ?
C1 O14 1.454(15) 7_556 ?
C2 H2 0.9800 . ?
C2 C3 1.531(16) . ?
C2 O2 1.432(17) . ?
C3 H3 0.9800 . ?
C3 C4 1.452(15) . ?
C3 O3 1.464(16) . ?
C4 H4 0.9800 . ?
C4 C5 1.585(19) . ?
C4 O4 1.421(14) . ?
C5 H5 0.9800 . ?
C5 C6 1.524(17) . ?
C5 O5 1.48(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.450(18) . ?
C11 H11 0.9800 . ?
C11 C12 1.430(17) . ?
C11 K1 3.44(2) . ?
C11 O4 1.439(17) . ?
C11 O15 1.462(16) . ?
C12 H12 0.9800 . ?
C12 C13 1.458(18) . ?
C12 O12 1.484(17) . ?
C13 H13 0.9800 . ?
C13 C14 1.542(19) . ?
C13 O13 1.471(9) . ?
C14 H14 0.9800 . ?
C14 C15 1.509(19) . ?
C14 O14 1.459(15) . ?
C15 H15 0.9800 . ?
C15 C16 1.488(9) . ?
C15 O15 1.427(15) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 O16 1.378(18) . ?
K1 C11 3.44(2) 23_565 ?
K1 O2 2.945(14) 41_646 ?
K1 O2 2.945(14) 44_666 ?
K1 O3 2.980(14) 41_646 ?
K1 O3 2.980(14) 44_666 ?
K1 O15 2.760(11) . ?
K1 O15 2.760(11) 23_565 ?
K1 O16 2.878(13) 23_565 ?
K1 O16 2.878(13) . ?
O2 K1 2.945(14) 42_566 ?
O2 H2A 0.8200 . ?
O3 K1 2.981(14) 42_566 ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O14 C1 1.454(15) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 103.0 . . ?
C2 C1 O14 116.4(16) . 7_556 ?
O5 C1 H1 103.0 . . ?
O5 C1 C2 115.6(16) . . ?
O5 C1 O14 113.3(14) . 7_556 ?
O14 C1 H1 103.0 7_556 . ?
C1 C2 H2 109.6 . . ?
C1 C2 C3 105.5(16) . . ?
C3 C2 H2 109.6 . . ?
O2 C2 C1 109.4(16) . . ?
O2 C2 H2 109.6 . . ?
O2 C2 C3 112.9(15) . . ?
C2 C3 H3 101.8 . . ?
C4 C3 C2 116.1(16) . . ?
C4 C3 H3 101.8 . . ?
C4 C3 O3 121.3(14) . . ?
O3 C3 C2 110.3(13) . . ?
O3 C3 H3 101.8 . . ?
C3 C4 H4 102.0 . . ?
C3 C4 C5 117.1(15) . . ?
C5 C4 H4 102.0 . . ?
O4 C4 C3 115.7(15) . . ?
O4 C4 H4 102.0 . . ?
O4 C4 C5 114.5(16) . . ?
C4 C5 H5 104.7 . . ?
C6 C5 C4 121.3(17) . . ?
C6 C5 H5 104.7 . . ?
O5 C5 C4 105.9(15) . . ?
O5 C5 H5 104.7 . . ?
O5 C5 C6 113.9(17) . . ?
C5 C6 H6A 111.1 . . ?
C5 C6 H6B 111.1 . . ?
H6A C6 H6B 109.1 . . ?
O6 C6 C5 103.2(16) . . ?
O6 C6 H6A 111.1 . . ?
O6 C6 H6B 111.1 . . ?
C12 C11 H11 112.6 . . ?
C12 C11 K1 98.6(12) . . ?
C12 C11 O4 101.1(17) . . ?
C12 C11 O15 106.8(15) . . ?
K1 C11 H11 70.7 . . ?
O4 C11 H11 112.6 . . ?
O4 C11 K1 156.4(12) . . ?
O4 C11 O15 110.4(16) . . ?
O15 C11 H11 112.6 . . ?
O15 C11 K1 50.8(8) . . ?
C11 C12 H12 105.1 . . ?
C11 C12 C13 118.2(16) . . ?
C11 C12 O12 113.0(16) . . ?
C13 C12 H12 105.1 . . ?
C13 C12 O12 109.1(15) . . ?
O12 C12 H12 105.1 . . ?
C12 C13 H13 110.1 . . ?
C12 C13 C14 106.3(14) . . ?
C12 C13 O13 109.2(15) . . ?
C14 C13 H13 110.1 . . ?
O13 C13 H13 110.1 . . ?
O13 C13 C14 110.8(13) . . ?
C13 C14 H14 111.7 . . ?
C15 C14 C13 108.6(13) . . ?
C15 C14 H14 111.7 . . ?
O14 C14 C13 102.9(13) . . ?
O14 C14 H14 111.7 . . ?
O14 C14 C15 109.9(14) . . ?
C14 C15 H15 114.9 . . ?
C16 C15 C14 105.4(16) . . ?
C16 C15 H15 114.9 . . ?
O15 C15 C14 102.7(15) . . ?
O15 C15 H15 114.9 . . ?
O15 C15 C16 102.6(15) . . ?
C15 C16 H16A 107.6 . . ?
C15 C16 H16B 107.6 . . ?
H16A C16 H16B 107.0 . . ?
O16 C16 C15 119.0(17) . . ?
O16 C16 H16A 107.6 . . ?
O16 C16 H16B 107.6 . . ?
C11 K1 C11 149.9(7) . 23_565 ?
O2 K1 C11 88.8(4) 44_666 23_565 ?
O2 K1 C11 88.8(4) 41_646 . ?
O2 K1 C11 102.6(4) 44_666 . ?
O2 K1 C11 102.6(4) 41_646 23_565 ?
O2 K1 O2 135.5(6) 44_666 41_646 ?
O2 K1 O3 97.2(4) 41_646 44_666 ?
O2 K1 O3 58.0(4) 44_666 44_666 ?
O2 K1 O3 58.0(4) 41_646 41_646 ?
O2 K1 O3 97.2(4) 44_666 41_646 ?
O3 K1 C11 56.7(4) 41_646 23_565 ?
O3 K1 C11 145.8(5) 41_646 . ?
O3 K1 C11 145.8(4) 44_666 23_565 ?
O3 K1 C11 56.7(4) 44_666 . ?
O3 K1 O3 115.3(5) 44_666 41_646 ?
O15 K1 C11 127.0(5) . 23_565 ?
O15 K1 C11 127.0(5) 23_565 . ?
O15 K1 C11 24.2(3) 23_565 23_565 ?
O15 K1 C11 24.2(3) . . ?
O15 K1 O2 118.8(4) 23_565 41_646 ?
O15 K1 O2 88.2(3) 23_565 44_666 ?
O15 K1 O2 88.2(3) . 41_646 ?
O15 K1 O2 118.8(4) . 44_666 ?
O15 K1 O3 80.7(4) 23_565 41_646 ?
O15 K1 O3 143.0(3) 23_565 44_666 ?
O15 K1 O3 143.0(3) . 41_646 ?
O15 K1 O3 80.7(4) . 44_666 ?
O15 K1 O15 106.8(5) 23_565 . ?
O15 K1 O16 56.9(4) 23_565 23_565 ?
O15 K1 O16 70.3(3) . 23_565 ?
O15 K1 O16 70.3(3) 23_565 . ?
O15 K1 O16 56.9(4) . . ?
O16 K1 C11 79.8(4) 23_565 23_565 ?
O16 K1 C11 79.8(4) . . ?
O16 K1 C11 78.0(4) . 23_565 ?
O16 K1 C11 78.0(4) 23_565 . ?
O16 K1 O2 153.4(4) . 44_666 ?
O16 K1 O2 70.5(3) . 41_646 ?
O16 K1 O2 70.5(3) 23_565 44_666 ?
O16 K1 O2 153.4(4) 23_565 41_646 ?
O16 K1 O3 94.6(4) . 41_646 ?
O16 K1 O3 135.4(4) 23_565 41_646 ?
O16 K1 O3 135.4(4) . 44_666 ?
O16 K1 O3 94.6(4) 23_565 44_666 ?
O16 K1 O16 84.4(5) 23_565 . ?
C2 O2 K1 109.8(10) . 42_566 ?
C2 O2 H2A 109.5 . . ?
K1 O2 H2A 57.4 42_566 . ?
C3 O3 K1 119.2(9) . 42_566 ?
C3 O3 H3A 109.5 . . ?
K1 O3 H3A 131.2 42_566 . ?
C4 O4 C11 119.8(15) . . ?
C1 O5 C5 112.3(16) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12A 109.5 . . ?
C13 O13 H13A 109.5 . . ?
C1 O14 C14 120.8(12) 5_565 . ?
C11 O15 K1 105.0(10) . . ?
C15 O15 C11 115.8(14) . . ?
C15 O15 K1 127.0(10) . . ?
C16 O16 K1 116.3(10) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 119.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -43(2) . . . . ?
C1 C2 C3 O3 173.8(14) . . . . ?
C1 C2 O2 K1 179.9(12) . . . 42_566 ?
C2 C1 O5 C5 -72(2) . . . . ?
C2 C3 C4 C5 37(2) . . . . ?
C2 C3 C4 O4 177.1(14) . . . . ?
C2 C3 O3 K1 -17.4(17) . . . 42_566 ?
C3 C2 O2 K1 -63.0(16) . . . 42_566 ?
C3 C4 C5 C6 -171.0(18) . . . . ?
C3 C4 C5 O5 -39(2) . . . . ?
C3 C4 O4 C11 106.5(18) . . . . ?
C4 C3 O3 K1 -158.1(12) . . . 42_566 ?
C4 C5 C6 O6 62(3) . . . . ?
C4 C5 O5 C1 53.6(18) . . . . ?
C5 C4 O4 C11 -112.7(18) . . . . ?
C6 C5 O5 C1 -170.7(16) . . . . ?
C11 C12 C13 C14 -53(2) . . . . ?
C11 C12 C13 O13 -172.5(15) . . . . ?
C12 C11 O4 C4 -134.4(16) . . . . ?
C12 C11 O15 C15 -58(2) . . . . ?
C12 C11 O15 K1 87.4(15) . . . . ?
C12 C13 C14 C15 59.3(18) . . . . ?
C12 C13 C14 O14 175.7(13) . . . . ?
C13 C14 C15 C16 -172.6(15) . . . . ?
C13 C14 C15 O15 -65.5(18) . . . . ?
C13 C14 O14 C1 129.5(13) . . . 5_565 ?
C14 C15 C16 O16 59(2) . . . . ?
C14 C15 O15 C11 67.0(18) . . . . ?
C14 C15 O15 K1 -69.4(16) . . . . ?
C15 C14 O14 C1 -115.0(16) . . . 5_565 ?
C15 C16 O16 K1 37(2) . . . . ?
C16 C15 O15 C11 176.2(14) . . . . ?
C16 C15 O15 K1 39.8(19) . . . . ?
K1 C11 C12 C13 101.3(16) . . . . ?
K1 C11 C12 O12 -129.6(12) . . . . ?
K1 C11 O4 C4 80(4) . . . . ?
K1 C11 O15 C15 -145.3(15) . . . . ?
O2 C2 C3 C4 -162.8(14) . . . . ?
O2 C2 C3 O3 54(2) . . . . ?
O3 C3 C4 C5 175.9(16) . . . . ?
O3 C3 C4 O4 -44(2) . . . . ?
O4 C4 C5 C6 49(3) . . . . ?
O4 C4 C5 O5 -179.5(14) . . . . ?
O4 C11 C12 C13 -66(2) . . . . ?
O4 C11 C12 O12 63.5(19) . . . . ?
O4 C11 O15 C15 51(2) . . . . ?
O4 C11 O15 K1 -163.5(12) . . . . ?
O5 C1 C2 C3 61(2) . . . . ?
O5 C1 C2 O2 -177.0(15) . . . . ?
O5 C5 C6 O6 -66.1(19) . . . . ?
O12 C12 C13 C14 176.2(13) . . . . ?
O12 C12 C13 O13 56.6(19) . . . . ?
O13 C13 C14 C15 177.9(15) . . . . ?
O13 C13 C14 O14 -65.7(17) . . . . ?
O14 C1 C2 C3 -75.5(19) 7_556 . . . ?
O14 C1 C2 O2 46(2) 7_556 . . . ?
O14 C1 O5 C5 66.1(19) 7_556 . . . ?
O14 C14 C15 C16 75.5(19) . . . . ?
O14 C14 C15 O15 -177.4(12) . . . . ?
O15 C11 C12 C13 50(2) . . . . ?
O15 C11 C12 O12 178.9(14) . . . . ?
O15 C11 O4 C4 112.9(17) . . . . ?
O15 C15 C16 O16 -48(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.246 -0.658 -0.551 14322.1 1811.8 ?


_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_0_25GPa
_database_code_depnum_ccdc_archive 'CCDC 1529145'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7

# start Validation Reply Form

_vrf_THETM01_CDMOF_a_0_25GPa     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_REFNR01_CDMOF_a_0_25GPa     
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT029_CDMOF_a_0_25GPa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.727 Note  
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT201_CDMOF_a_0_25GPa     
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT090_CDMOF_a_0_25GPa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.93 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT306_CDMOF_a_0_25GPa     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_0_25GPa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.038 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_CDMOF_a_0_25GPa     
;
PROBLEM: D-H Without Acceptor       O6     --  H6     ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
_vrf_PLAT911_CDMOF_a_0_25GPa     
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.333        136 Report
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample limiting the range of 
collected reflections'
;
# end Validation Reply Form
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0030 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2030 0.2500 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   31.3031(11)
_cell_length_b                   31.3031(11)
_cell_length_c                   31.3031(11)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30673(2)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    2435
_cell_measurement_temperature    295
_cell_measurement_theta_max      13.2400
_cell_measurement_theta_min      1.7750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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_absorpt_special_details   ?


# EXPERIMENTAL DATA 
_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.16GPa and then
compressed to 0.25GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.915
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_ambient_temperature      295
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         250000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 155.77  155
  2  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 -24.23  155
  3  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00-155.77  200
  4  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00  24.23  200
  5  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 -24.23  280
  6  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 155.77  280
  7  ω    -96.00 -30.00   0.20    0.70    --   15.00 -70.00  24.23  330
  8  ω    -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       'ω 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_source                   synchrotron
_diffrn_special_details          
'high-pressure measurement with diamond-anvil cell at 0.25 GPa'
_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_odcompleteness_completeness 77.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.25
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_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_coef       .
_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_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0955
_refine_ls_restrained_S_all      1.452
_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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2583
_refine_ls_wR_factor_ref         0.2807
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
 resulting in a low data:parameter ratio.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8513(8) 0.6844(7) 0.6450(11) 0.235(6) Uiso 1 1 d D . . . .
H1 H 0.8449 0.7151 0.6460 0.282 Uiso 1 1 calc R . . . .
C2 C 0.8930(7) 0.6740(7) 0.6656(10) 0.235(6) Uiso 1 1 d D . . . .
H2 H 0.8953 0.6839 0.6952 0.282 Uiso 1 1 calc R . . . .
C3 C 0.9017(7) 0.6261(7) 0.6600(11) 0.235(6) Uiso 1 1 d D . . . .
H3 H 0.9076 0.6211 0.6296 0.282 Uiso 1 1 calc R . . . .
C4 C 0.8627(9) 0.6005(7) 0.6715(13) 0.235(6) Uiso 1 1 d D . . . .
H4 H 0.8585 0.6082 0.7015 0.282 Uiso 1 1 calc R . . . .
C5 C 0.8211(8) 0.6139(9) 0.6521(12) 0.235(6) Uiso 1 1 d D . . . .
H5 H 0.8294 0.6086 0.6223 0.282 Uiso 1 1 calc R . . . .
C6 C 0.7812(10) 0.5877(10) 0.6513(11) 0.235(6) Uiso 1 1 d D . . . .
H6A H 0.7730 0.5846 0.6215 0.282 Uiso 1 1 calc R . . . .
H6B H 0.7887 0.5594 0.6614 0.282 Uiso 1 1 calc R . . . .
C11 C 0.8677(9) 0.5330(6) 0.7059(8) 0.235(6) Uiso 1 1 d D . . . .
H11 H 0.8658 0.5530 0.7299 0.282 Uiso 1 1 calc R . . . .
C12 C 0.9036(7) 0.5050(8) 0.7225(11) 0.235(6) Uiso 1 1 d D . . . .
H12 H 0.9034 0.4984 0.7531 0.282 Uiso 1 1 calc R . . . .
C13 C 0.9048(7) 0.4668(9) 0.6916(11) 0.235(6) Uiso 1 1 d D . . . .
H13 H 0.8980 0.4816 0.6649 0.282 Uiso 1 1 calc R . . . .
C14 C 0.8639(9) 0.4421(7) 0.6974(11) 0.235(6) Uiso 1 1 d D . . . .
H14 H 0.8611 0.4320 0.7269 0.282 Uiso 1 1 calc R . . . .
C15 C 0.8259(6) 0.4705(8) 0.6850(10) 0.235(6) Uiso 1 1 d D . . . .
H15 H 0.8252 0.4773 0.6544 0.282 Uiso 1 1 calc R . . . .
C16 C 0.7855(10) 0.4519(10) 0.7006(8) 0.235(6) Uiso 1 1 d D . . . .
H16A H 0.7630 0.4715 0.6924 0.282 Uiso 1 1 calc R . . . .
H16B H 0.7809 0.4259 0.6844 0.282 Uiso 1 1 calc R . . . .
K1 K 0.8144(4) 0.5000 0.8144(4) 0.307(9) Uani 1 2 d DS TU P . .
O2 O 0.9278(7) 0.6894(8) 0.6376(8) 0.253(4) Uiso 1 1 d D . . . .
H2A H 0.9502 0.6775 0.6442 0.380 Uiso 1 1 calc R . . . .
O3 O 0.9412(8) 0.6196(7) 0.6830(9) 0.253(4) Uiso 1 1 d D . . . .
H3A H 0.9496 0.5951 0.6793 0.380 Uiso 1 1 calc R . . . .
O4 O 0.8720(8) 0.5613(9) 0.6741(10) 0.253(4) Uiso 1 1 d D . . . .
O5 O 0.8142(6) 0.6592(8) 0.6473(8) 0.253(4) Uiso 1 1 d D . . . .
O6 O 0.7426(8) 0.6009(7) 0.6749(9) 0.253(4) Uiso 1 1 d D . . . .
H6 H 0.7392 0.5852 0.6956 0.380 Uiso 1 1 calc R . . . .
O12 O 0.9363(8) 0.5310(8) 0.7079(7) 0.253(4) Uiso 1 1 d D . . . .
H12A H 0.9583 0.5170 0.7058 0.380 Uiso 1 1 calc R . . . .
O13 O 0.9498(7) 0.4552(9) 0.6826(8) 0.253(4) Uiso 1 1 d D . . . .
H13A H 0.9506 0.4315 0.6715 0.380 Uiso 1 1 calc R . . . .
O14 O 0.8646(8) 0.4061(8) 0.6674(9) 0.253(4) Uiso 1 1 d D . . . .
O15 O 0.8259(6) 0.5091(6) 0.7128(7) 0.253(4) Uiso 1 1 d D . . . .
O16 O 0.7783(8) 0.4411(8) 0.7457(8) 0.253(4) Uiso 1 1 d D . . . .
H16 H 0.7701 0.4163 0.7476 0.380 Uiso 1 1 calc R . . . .
OA O 1.0000 0.5000 0.6763(12) 0.253(4) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.49(2) . ?
C1 O5 1.407(18) . ?
C1 O14 1.74(4) 7_556 ?
C2 H2 0.9800 . ?
C2 C3 1.53(2) . ?
C2 K1 3.43(2) 42_566 ?
C2 O2 1.48(2) . ?
C3 H3 0.9800 . ?
C3 C4 1.50(2) . ?
C3 O3 1.45(2) . ?
C4 H4 0.9800 . ?
C4 C5 1.49(2) . ?
C4 O4 1.27(3) . ?
C5 H5 0.9800 . ?
C5 C6 1.50(2) . ?
C5 O5 1.44(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.48(2) . ?
C11 H11 0.9800 . ?
C11 C12 1.52(2) . ?
C11 O4 1.34(3) . ?
C11 O15 1.522(19) . ?
C12 H12 0.9800 . ?
C12 C13 1.54(2) . ?
C12 O12 1.39(2) . ?
C13 H13 0.9800 . ?
C13 C14 1.51(2) . ?
C13 O13 1.48(2) . ?
C14 H14 0.9800 . ?
C14 C15 1.54(2) . ?
C14 O14 1.47(2) . ?
C15 H15 0.9800 . ?
C15 C16 1.47(2) . ?
C15 O15 1.49(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 O16 1.47(2) . ?
K1 C2 3.43(2) 44_666 ?
K1 C2 3.43(2) 41_646 ?
K1 O2 2.72(2) 44_666 ?
K1 O2 2.72(2) 41_646 ?
K1 O3 2.77(3) 44_666 ?
K1 O3 2.77(3) 41_646 ?
K1 O15 3.21(3) . ?
K1 O15 3.21(3) 23_565 ?
K1 O16 3.05(3) . ?
K1 O16 3.05(3) 23_565 ?
O2 K1 2.72(2) 42_566 ?
O2 H2A 0.8200 . ?
O3 K1 2.77(3) 42_566 ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O14 C1 1.74(4) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 112.3 . . ?
C2 C1 O14 97(2) . 7_556 ?
O5 C1 H1 112.3 . . ?
O5 C1 C2 125.3(16) . . ?
O5 C1 O14 94(2) . 7_556 ?
O14 C1 H1 112.3 7_556 . ?
C1 C2 H2 113.8 . . ?
C1 C2 C3 108.6(15) . . ?
C1 C2 K1 155.7(16) . 42_566 ?
C3 C2 H2 113.8 . . ?
C3 C2 K1 87.2(11) . 42_566 ?
K1 C2 H2 73.8 42_566 . ?
O2 C2 C1 109(2) . . ?
O2 C2 H2 113.8 . . ?
O2 C2 C3 96.9(18) . . ?
O2 C2 K1 49.8(12) . 42_566 ?
C2 C3 H3 107.5 . . ?
C4 C3 C2 110.4(17) . . ?
C4 C3 H3 107.5 . . ?
O3 C3 C2 103.3(18) . . ?
O3 C3 H3 107.5 . . ?
O3 C3 C4 120(2) . . ?
C3 C4 H4 101.9 . . ?
C5 C4 C3 117.4(17) . . ?
C5 C4 H4 101.9 . . ?
O4 C4 C3 110(3) . . ?
O4 C4 H4 101.9 . . ?
O4 C4 C5 120(3) . . ?
C4 C5 H5 96.3 . . ?
C4 C5 C6 125(2) . . ?
C6 C5 H5 96.3 . . ?
O5 C5 C4 116.6(14) . . ?
O5 C5 H5 96.3 . . ?
O5 C5 C6 114(2) . . ?
C5 C6 H6A 107.0 . . ?
C5 C6 H6B 107.0 . . ?
H6A C6 H6B 106.7 . . ?
O6 C6 C5 121(2) . . ?
O6 C6 H6A 107.0 . . ?
O6 C6 H6B 107.0 . . ?
C12 C11 H11 98.8 . . ?
C12 C11 O15 107.7(14) . . ?
O4 C11 H11 98.8 . . ?
O4 C11 C12 124(2) . . ?
O4 C11 O15 121(3) . . ?
O15 C11 H11 98.8 . . ?
C11 C12 H12 116.7 . . ?
C11 C12 C13 104.7(16) . . ?
C13 C12 H12 116.7 . . ?
O12 C12 C11 96(2) . . ?
O12 C12 H12 116.7 . . ?
O12 C12 C13 103(3) . . ?
C12 C13 H13 99.2 . . ?
C14 C13 C12 107.5(16) . . ?
C14 C13 H13 99.2 . . ?
O13 C13 C12 110(2) . . ?
O13 C13 H13 99.2 . . ?
O13 C13 C14 135(2) . . ?
C13 C14 H14 110.9 . . ?
C13 C14 C15 109.5(17) . . ?
C15 C14 H14 110.9 . . ?
O14 C14 C13 108(2) . . ?
O14 C14 H14 110.9 . . ?
O14 C14 C15 107.0(18) . . ?
C14 C15 H15 113.1 . . ?
C16 C15 C14 111(3) . . ?
C16 C15 H15 113.1 . . ?
C16 C15 O15 97.4(17) . . ?
O15 C15 C14 108.6(15) . . ?
O15 C15 H15 113.1 . . ?
C15 C16 H16A 106.6 . . ?
C15 C16 H16B 106.6 . . ?
H16A C16 H16B 106.6 . . ?
O16 C16 C15 123(3) . . ?
O16 C16 H16A 106.6 . . ?
O16 C16 H16B 106.6 . . ?
C2 K1 C2 156.4(11) 44_666 41_646 ?
O2 K1 C2 24.5(5) 41_646 41_646 ?
O2 K1 C2 139.6(9) 41_646 44_666 ?
O2 K1 C2 139.6(9) 44_666 41_646 ?
O2 K1 C2 24.5(5) 44_666 44_666 ?
O2 K1 O2 137.7(14) 44_666 41_646 ?
O2 K1 O3 57.5(6) 41_646 41_646 ?
O2 K1 O3 98.1(8) 41_646 44_666 ?
O2 K1 O3 57.5(6) 44_666 44_666 ?
O2 K1 O3 98.1(8) 44_666 41_646 ?
O2 K1 O15 88.2(6) 44_666 23_565 ?
O2 K1 O15 88.2(6) 41_646 . ?
O2 K1 O15 118.6(7) 41_646 23_565 ?
O2 K1 O15 118.6(7) 44_666 . ?
O2 K1 O16 70.8(8) 41_646 . ?
O2 K1 O16 151.3(10) 41_646 23_565 ?
O2 K1 O16 151.3(10) 44_666 . ?
O2 K1 O16 70.8(8) 44_666 23_565 ?
O3 K1 C2 42.7(5) 41_646 41_646 ?
O3 K1 C2 120.7(8) 44_666 41_646 ?
O3 K1 C2 120.7(8) 41_646 44_666 ?
O3 K1 C2 42.7(5) 44_666 44_666 ?
O3 K1 O3 113.5(12) 44_666 41_646 ?
O3 K1 O15 83.5(7) 41_646 23_565 ?
O3 K1 O15 142.6(5) 41_646 . ?
O3 K1 O15 142.6(5) 44_666 23_565 ?
O3 K1 O15 83.5(7) 44_666 . ?
O3 K1 O16 134.3(7) 41_646 23_565 ?
O3 K1 O16 97.8(7) 44_666 23_565 ?
O3 K1 O16 134.4(7) 44_666 . ?
O3 K1 O16 97.8(7) 41_646 . ?
O15 K1 C2 94.7(6) 23_565 41_646 ?
O15 K1 C2 94.7(6) . 44_666 ?
O15 K1 C2 99.9(5) 23_565 44_666 ?
O15 K1 C2 99.9(5) . 41_646 ?
O15 K1 O15 103.4(9) 23_565 . ?
O16 K1 C2 63.4(6) . 41_646 ?
O16 K1 C2 139.4(8) 23_565 41_646 ?
O16 K1 C2 139.4(8) . 44_666 ?
O16 K1 C2 63.4(6) 23_565 44_666 ?
O16 K1 O15 53.0(6) . . ?
O16 K1 O15 53.0(6) 23_565 23_565 ?
O16 K1 O15 70.1(7) . 23_565 ?
O16 K1 O15 70.1(7) 23_565 . ?
O16 K1 O16 81.0(11) 23_565 . ?
C2 O2 K1 105.7(15) . 42_566 ?
C2 O2 H2A 109.5 . . ?
K1 O2 H2A 29.5 42_566 . ?
C3 O3 K1 118.6(15) . 42_566 ?
C3 O3 H3A 109.5 . . ?
K1 O3 H3A 119.3 42_566 . ?
C4 O4 C11 132(4) . . ?
C1 O5 C5 115.7(14) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12A 109.5 . . ?
C13 O13 H13A 109.5 . . ?
C14 O14 C1 121(2) . 5_565 ?
C11 O15 K1 106.3(14) . . ?
C15 O15 C11 108.5(15) . . ?
C15 O15 K1 120.4(16) . . ?
C16 O16 K1 118.9(15) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 129.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -47(4) . . . . ?
C1 C2 C3 O3 -177(2) . . . . ?
C1 C2 O2 K1 167.2(16) . . . 42_566 ?
C2 C1 O5 C5 -29(5) . . . . ?
C2 C3 C4 C5 49(5) . . . . ?
C2 C3 C4 O4 -169(3) . . . . ?
C2 C3 O3 K1 -32(3) . . . 42_566 ?
C3 C2 O2 K1 -80.4(18) . . . 42_566 ?
C3 C4 C5 C6 165(3) . . . . ?
C3 C4 C5 O5 -37(5) . . . . ?
C3 C4 O4 C11 123(4) . . . . ?
C4 C3 O3 K1 -155(2) . . . 42_566 ?
C4 C5 C6 O6 114(4) . . . . ?
C4 C5 O5 C1 24(5) . . . . ?
C5 C4 O4 C11 -96(5) . . . . ?
C6 C5 O5 C1 -176(3) . . . . ?
C11 C12 C13 C14 -66(3) . . . . ?
C11 C12 C13 O13 140(2) . . . . ?
C12 C11 O4 C4 -128(3) . . . . ?
C12 C11 O15 C15 -66(2) . . . . ?
C12 C11 O15 K1 64.7(18) . . . . ?
C12 C13 C14 C15 63(3) . . . . ?
C12 C13 C14 O14 179(2) . . . . ?
C13 C14 C15 C16 -165(2) . . . . ?
C13 C14 C15 O15 -60(3) . . . . ?
C13 C14 O14 C1 133(2) . . . 5_565 ?
C14 C15 C16 O16 55(3) . . . . ?
C14 C15 O15 C11 60(3) . . . . ?
C14 C15 O15 K1 -63(2) . . . . ?
C15 C14 O14 C1 -110(2) . . . 5_565 ?
C15 C16 O16 K1 38(4) . . . . ?
C16 C15 O15 C11 175(2) . . . . ?
C16 C15 O15 K1 52(2) . . . . ?
K1 C2 C3 C4 152(2) 42_566 . . . ?
K1 C2 C3 O3 22(2) 42_566 . . . ?
O2 C2 C3 C4 -159(3) . . . . ?
O2 C2 C3 O3 71(3) . . . . ?
O3 C3 C4 C5 169(3) . . . . ?
O3 C3 C4 O4 -49(5) . . . . ?
O4 C4 C5 C6 27(7) . . . . ?
O4 C4 C5 O5 -176(4) . . . . ?
O4 C11 C12 C13 -83(3) . . . . ?
O4 C11 C12 O12 23(3) . . . . ?
O4 C11 O15 C15 86(3) . . . . ?
O4 C11 O15 K1 -144(2) . . . . ?
O5 C1 C2 C3 41(5) . . . . ?
O5 C1 C2 K1 170(3) . . . 42_566 ?
O5 C1 C2 O2 146(3) . . . . ?
O5 C5 C6 O6 -44(5) . . . . ?
O12 C12 C13 C14 -166(3) . . . . ?
O12 C12 C13 O13 40(3) . . . . ?
O13 C13 C14 C15 -153(4) . . . . ?
O13 C13 C14 O14 -37(5) . . . . ?
O14 C1 C2 C3 -59(2) 7_556 . . . ?
O14 C1 C2 K1 70(5) 7_556 . . 42_566 ?
O14 C1 C2 O2 45(2) 7_556 . . . ?
O14 C1 O5 C5 72(3) 7_556 . . . ?
O14 C14 C15 C16 78(3) . . . . ?
O14 C14 C15 O15 -176(2) . . . . ?
O15 C11 C12 C13 68(2) . . . . ?
O15 C11 C12 O12 173(2) . . . . ?
O15 C11 O4 C4 85(4) . . . . ?
O15 C15 C16 O16 -58(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.760 -0.022 -0.048 14195.0 5716.1 ?


_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_0_33GPa
_database_code_depnum_ccdc_archive 'CCDC 1529146'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7

# start Validation Reply Form
_vrf_THETM01_CDMOF_a_0_33GPa     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_REFNR01_CDMOF_a_0_33GPa     
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT029_CDMOF_a_0_33GPa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.737 Note  
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT201_CDMOF_a_0_33GPa     
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT306_CDMOF_a_0_33GPa     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_0_33GPa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
# end Validation Reply Form
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2030 0.2500 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   31.2695(18)
_cell_length_b                   31.2695(18)
_cell_length_c                   31.2695(18)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30575(3)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    1207
_cell_measurement_temperature    295
_cell_measurement_theta_max      10.3010
_cell_measurement_theta_min      1.9890
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55035
_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_absorpt_special_details   ?

# EXPERIMENTAL DATA 
_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.16GPa and then
compressed to 0.33GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.918
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_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          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.737
_diffrn_reflns_Laue_measured_fraction_max 0.737
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5461
_diffrn_reflns_point_group_measured_fraction_full 0.739
_diffrn_reflns_point_group_measured_fraction_max 0.739
_diffrn_reflns_theta_full        13.267
_diffrn_reflns_theta_max         13.267
_diffrn_reflns_theta_min         1.785
_diffrn_ambient_temperature      295
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         330000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.737
_diffrn_measured_fraction_theta_max 0.737
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 155.77  155
  2  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 -24.23  155
  3  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00-155.77  200
  4  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00  24.23  200
  5  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 -24.23  280
  6  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 155.77  280
  7  ω    -96.00 -30.00   0.20    0.70    --   15.00 -70.00  24.23  330
  8  ω    -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       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0002454000
_diffrn_orient_matrix_UB_12      0.0217413000
_diffrn_orient_matrix_UB_13      -0.0037440000
_diffrn_orient_matrix_UB_21      0.0188974000
_diffrn_orient_matrix_UB_22      -0.0017001000
_diffrn_orient_matrix_UB_23      -0.0112049000
_diffrn_orient_matrix_UB_31      -0.0113022000
_diffrn_orient_matrix_UB_32      -0.0033279000
_diffrn_orient_matrix_UB_33      -0.0185734000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   synchrotron
_diffrn_special_details          
'high-pressure measurement with diamond-anvil cell at 0.33 GPa'
_reflns_Friedel_coverage         0.603
_reflns_Friedel_fraction_full    0.743
_reflns_Friedel_fraction_max     0.743
_reflns_number_gt                384
_reflns_number_total             601
_reflns_odcompleteness_completeness 78.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.27
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.133
_refine_diff_density_min         -0.123
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details 
;
 Flack x determined using 91 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         601
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0814
_refine_ls_restrained_S_all      1.382
_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/[σ²(Fo²)+(0.1543P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2122
_refine_ls_wR_factor_ref         0.2317
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
 resulting in a low data:parameter ratio.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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-O4
 1.45 with sigma of 0.005
 C2-C3
 1.5 with sigma of 0.005
 C4-C3
 1.5 with sigma of 0.005
 C2-O3
 2.3 with sigma of 0.02
 O3-C3
 1.45 with sigma of 0.005
 C6-O6
 1.45 with sigma of 0.005
 C2-C5
 3 with sigma of 0.02
 C6-C5
 1.5 with sigma of 0.005
 C4-C5
 1.5 with sigma of 0.005
 O4-C12
 2.2 with sigma of 0.02
 O14-C14
 1.45 with sigma of 0.005
 C12-C13
 1.5 with sigma of 0.005
 C14-C13
 1.5 with sigma of 0.005
 O14-C13
 2.4 with sigma of 0.02
 C11-O4
 1.45 with sigma of 0.005
 C12-C11
 1.5 with sigma of 0.005
 C11-C14
 3 with sigma of 0.02
 C15-C14
 1.5 with sigma of 0.005
 C12-C15
 3 with sigma of 0.02
 C14-C15
 1.5 with sigma of 0.005
 O14-C15
 2.4 with sigma of 0.02
 C16-C15
 1.5 with sigma of 0.005
 C2-O2
 1.45 with sigma of 0.005
 O2-C3
 2.2 with sigma of 0.02
 O1AA-C14
 2.5 with sigma of 0.02
 O1AA-C13
 1.45 with sigma of 0.005
 C1-C4
 3 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.005
 C5-C1
 2.3 with sigma of 0.005
 O12-C12
 1.45 with sigma of 0.01
 C16-O16
 1.45 with sigma of 0.005
 O5-C6
 2.5 with sigma of 0.02
 O5-C3
 3 with sigma of 0.02
 O5-C5
 1.45 with sigma of 0.005
 O15-C13
 3 with sigma of 0.02
 O15-C11
 1.45 with sigma of 0.005
 O15-C15
 1.45 with sigma of 0.005
 O15-C16
 2.2 with sigma of 0.02
 O5-C1
 1.45 with sigma of 0.005
 C4-C2
 2.5 with sigma of 0.02
 C5-C3
 2.5 with sigma of 0.02
 O6-C5
 2.7 with sigma of 0.04
 C13-O14
 2.5 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.02
 O4-C12
 2.5 with sigma of 0.04
 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
 C13-C15
 2.4 with sigma of 0.02
 O14-C15
 2.5 with sigma of 0.04
 C15-C11
 2.4 with sigma of 0.02
 C3-C1
 2.5 with sigma of 0.02
 C1-C5
 2.5 with sigma of 0.02
 O2-C1
 2.5 with sigma of 0.04
 C1-O2
 2.5 with sigma of 0.04
 C15-O16
 2.5 with sigma of 0.04
 C2-O5
 2.5 with sigma of 0.02
 O5-C4
 2.5 with sigma of 0.02
 C14-O15
 2.4 with sigma of 0.02
 O15-C12
 2.4 with sigma of 0.02
3. 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(O1AA)=Uiso(O2)=Uiso(O3)=Uiso(O4)=Uiso(O5)=Uiso(O6)=Uiso(O12)=Uiso(O14)=
 Uiso(O15)=Uiso(O16)=FVAR(2)
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:
 O1AA(H1AA), O2(H2A), O3(H3A), O6(H6), O16(H16)
4.d Idealised tetrahedral OH refined as rotating group:
 O12(H12A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8449(7) 0.6874(6) 0.6339(8) 0.233(7) Uiso 1 1 d D . . . .
H1 H 0.8396 0.7182 0.6316 0.280 Uiso 1 1 calc R . . . .
C2 C 0.8837(6) 0.6799(6) 0.6611(8) 0.233(7) Uiso 1 1 d D . . . .
H2 H 0.8803 0.6943 0.6887 0.280 Uiso 1 1 calc R . . . .
C3 C 0.8915(6) 0.6330(6) 0.6680(9) 0.233(7) Uiso 1 1 d D . . . .
H3 H 0.9000 0.6253 0.6388 0.280 Uiso 1 1 calc R . . . .
C4 C 0.8521(7) 0.6058(6) 0.6717(9) 0.233(7) Uiso 1 1 d D . . . .
H4 H 0.8427 0.6092 0.7014 0.280 Uiso 1 1 calc R . . . .
C5 C 0.8149(7) 0.6207(6) 0.6450(8) 0.233(7) Uiso 1 1 d D . . . .
H5 H 0.8215 0.6139 0.6152 0.280 Uiso 1 1 calc R . . . .
C6 C 0.7753(8) 0.5962(9) 0.6569(7) 0.233(7) Uiso 1 1 d D . . . .
H6A H 0.7510 0.6074 0.6412 0.280 Uiso 1 1 calc R . . . .
H6B H 0.7788 0.5663 0.6492 0.280 Uiso 1 1 calc R . . . .
C11 C 0.8546(7) 0.5348(5) 0.7046(9) 0.233(7) Uiso 1 1 d D . . . .
H11 H 0.8552 0.5555 0.7281 0.280 Uiso 1 1 calc R . . . .
C12 C 0.8962(6) 0.5119(6) 0.7108(9) 0.233(7) Uiso 1 1 d D . . . .
H12 H 0.8953 0.5022 0.7406 0.280 Uiso 1 1 calc R . . . .
C13 C 0.8954(6) 0.4712(6) 0.6851(10) 0.233(7) Uiso 1 1 d D . . . .
H13 H 0.8921 0.4800 0.6552 0.280 Uiso 1 1 calc R . . . .
C14 C 0.8572(6) 0.4444(6) 0.6952(8) 0.233(7) Uiso 1 1 d D . . . .
H14 H 0.8599 0.4365 0.7254 0.280 Uiso 1 1 calc R . . . .
C15 C 0.8164(5) 0.4693(7) 0.6915(7) 0.233(7) Uiso 1 1 d D . . . .
H15 H 0.8094 0.4750 0.6615 0.280 Uiso 1 1 calc R . . . .
C16 C 0.7787(7) 0.4507(9) 0.7148(8) 0.233(7) Uiso 1 1 d D . . . .
H16A H 0.7543 0.4693 0.7099 0.280 Uiso 1 1 calc R . . . .
H16B H 0.7721 0.4233 0.7020 0.280 Uiso 1 1 calc R . . . .
K1 K 0.8097(3) 0.5000 0.8097(3) 0.294(8) Uani 1 2 d S T P . .
O1AA O 0.9385(6) 0.4546(8) 0.6889(7) 0.276(5) Uiso 1 1 d D . . . .
H1AA H 0.9399 0.4312 0.6773 0.414 Uiso 1 1 calc R . . . .
O2 O 0.9241(7) 0.6920(7) 0.6417(8) 0.276(5) Uiso 1 1 d D . . . .
H2A H 0.9436 0.6786 0.6530 0.414 Uiso 1 1 calc R . . . .
O3 O 0.9334(6) 0.6316(6) 0.6882(8) 0.276(5) Uiso 1 1 d D . . . .
H3A H 0.9384 0.6071 0.6961 0.414 Uiso 1 1 calc R . . . .
O4 O 0.8658(7) 0.5616(6) 0.6684(7) 0.276(5) Uiso 1 1 d D . . . .
O5 O 0.8061(6) 0.6661(7) 0.6473(7) 0.276(5) Uiso 1 1 d D . . . .
O6 O 0.7673(8) 0.5996(8) 0.7026(7) 0.276(5) Uiso 1 1 d D . . . .
H6 H 0.7788 0.5796 0.7150 0.414 Uiso 1 1 calc R . . . .
O12 O 0.9368(7) 0.5355(8) 0.7076(10) 0.276(5) Uiso 1 1 d D . . . .
H12A H 0.9569 0.5189 0.7104 0.414 Uiso 1 1 calc GR . . . .
O14 O 0.8544(7) 0.4046(6) 0.6717(8) 0.276(5) Uiso 1 1 d D . . . .
O15 O 0.8181(5) 0.5086(6) 0.7161(6) 0.276(5) Uiso 1 1 d D . . . .
O16 O 0.7833(7) 0.4446(8) 0.7604(8) 0.276(5) Uiso 1 1 d D . . . .
H16 H 0.7784 0.4195 0.7663 0.414 Uiso 1 1 calc R . . . .
OA O 1.0000 0.5000 0.6626(14) 0.320(16) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.501(7) . ?
C1 O5 1.445(7) . ?
C1 O14 1.33(3) 7_556 ?
C2 H2 0.9800 . ?
C2 C3 1.500(7) . ?
C2 O2 1.452(7) . ?
C3 H3 0.9800 . ?
C3 C4 1.504(7) . ?
C3 O3 1.454(7) . ?
C4 H4 0.9800 . ?
C4 C5 1.505(7) . ?
C4 O4 1.451(7) . ?
C5 H5 0.9800 . ?
C5 C6 1.502(7) . ?
C5 O5 1.450(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.456(7) . ?
C11 H11 0.9800 . ?
C11 C12 1.500(7) . ?
C11 O4 1.450(7) . ?
C11 O15 1.450(7) . ?
C12 H12 0.9800 . ?
C12 C13 1.504(7) . ?
C12 O12 1.472(13) . ?
C13 H13 0.9800 . ?
C13 C14 1.492(7) . ?
C13 O1AA 1.450(7) . ?
C14 H14 0.9800 . ?
C14 C15 1.498(5) . ?
C14 O14 1.448(7) . ?
C15 H15 0.9800 . ?
C15 C16 1.501(7) . ?
C15 O15 1.450(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 K1 3.48(3) . ?
C16 O16 1.445(7) . ?
K1 C16 3.48(3) 23_565 ?
K1 O2 2.82(2) 41_646 ?
K1 O2 2.82(2) 44_666 ?
K1 O3 2.78(2) 41_646 ?
K1 O3 2.78(2) 44_666 ?
K1 O15 2.95(2) . ?
K1 O15 2.95(2) 23_565 ?
K1 O16 2.46(2) . ?
K1 O16 2.46(2) 23_565 ?
O1AA H1AA 0.8200 . ?
O2 K1 2.82(2) 42_566 ?
O2 H2A 0.8200 . ?
O3 K1 2.78(2) 42_566 ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O14 C1 1.33(3) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 109.4 . . ?
O5 C1 H1 109.4 . . ?
O5 C1 C2 116.1(14) . . ?
O14 C1 H1 109.4 7_556 . ?
O14 C1 C2 106(2) 7_556 . ?
O14 C1 O5 106.2(19) 7_556 . ?
C1 C2 H2 109.9 . . ?
C3 C2 C1 111.5(12) . . ?
C3 C2 H2 109.9 . . ?
O2 C2 C1 115.1(18) . . ?
O2 C2 H2 109.9 . . ?
O2 C2 C3 100.0(14) . . ?
C2 C3 H3 98.9 . . ?
C2 C3 C4 115.5(12) . . ?
C4 C3 H3 98.9 . . ?
O3 C3 C2 103.9(14) . . ?
O3 C3 H3 98.9 . . ?
O3 C3 C4 133.3(18) . . ?
C3 C4 H4 105.1 . . ?
C3 C4 C5 114.6(11) . . ?
C5 C4 H4 105.1 . . ?
O4 C4 C3 106.9(18) . . ?
O4 C4 H4 105.1 . . ?
O4 C4 C5 119(2) . . ?
C4 C5 H5 107.4 . . ?
C6 C5 C4 110.1(19) . . ?
C6 C5 H5 107.4 . . ?
O5 C5 C4 114.9(13) . . ?
O5 C5 H5 107.4 . . ?
O5 C5 C6 109.4(15) . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
O6 C6 C5 110(2) . . ?
O6 C6 H6A 109.6 . . ?
O6 C6 H6B 109.6 . . ?
C12 C11 H11 101.6 . . ?
O4 C11 H11 101.6 . . ?
O4 C11 C12 99.6(13) . . ?
O15 C11 H11 101.6 . . ?
O15 C11 C12 112.4(13) . . ?
O15 C11 O4 135(2) . . ?
C11 C12 H12 104.3 . . ?
C11 C12 C13 108.6(12) . . ?
C13 C12 H12 104.3 . . ?
O12 C12 C11 120.0(18) . . ?
O12 C12 H12 104.3 . . ?
O12 C12 C13 114(2) . . ?
C12 C13 H13 106.0 . . ?
C14 C13 C12 112.1(12) . . ?
C14 C13 H13 106.0 . . ?
O1AA C13 C12 104(2) . . ?
O1AA C13 H13 106.0 . . ?
O1AA C13 C14 121.7(16) . . ?
C13 C14 H14 106.1 . . ?
C13 C14 C15 112.0(12) . . ?
C15 C14 H14 106.1 . . ?
O14 C14 C13 115.1(15) . . ?
O14 C14 H14 106.1 . . ?
O14 C14 C15 110.7(14) . . ?
C14 C15 H15 111.0 . . ?
C14 C15 C16 115.5(19) . . ?
C16 C15 H15 111.0 . . ?
O15 C15 C14 111.5(12) . . ?
O15 C15 H15 111.0 . . ?
O15 C15 C16 95.8(13) . . ?
C15 C16 H16A 108.1 . . ?
C15 C16 H16B 108.1 . . ?
C15 C16 K1 91.3(12) . . ?
H16A C16 H16B 107.3 . . ?
K1 C16 H16A 95.0 . . ?
K1 C16 H16B 143.4 . . ?
O16 C16 C15 116.8(19) . . ?
O16 C16 H16A 108.1 . . ?
O16 C16 H16B 108.1 . . ?
O16 C16 K1 36.0(12) . . ?
C16 K1 C16 73.8(9) . 23_565 ?
O2 K1 C16 76.2(7) 44_666 23_565 ?
O2 K1 C16 145.7(8) 41_646 23_565 ?
O2 K1 C16 145.7(8) 44_666 . ?
O2 K1 C16 76.2(7) 41_646 . ?
O2 K1 O2 136.9(12) 44_666 41_646 ?
O2 K1 O15 117.4(6) 44_666 . ?
O2 K1 O15 90.5(5) 44_666 23_565 ?
O2 K1 O15 117.4(6) 41_646 23_565 ?
O2 K1 O15 90.5(5) 41_646 . ?
O3 K1 C16 103.8(6) 44_666 23_565 ?
O3 K1 C16 122.4(6) 41_646 23_565 ?
O3 K1 C16 103.8(6) 41_646 . ?
O3 K1 C16 122.4(6) 44_666 . ?
O3 K1 O2 106.0(7) 44_666 41_646 ?
O3 K1 O2 106.0(7) 41_646 44_666 ?
O3 K1 O2 50.9(6) 44_666 44_666 ?
O3 K1 O2 50.9(6) 41_646 41_646 ?
O3 K1 O3 122.2(11) 44_666 41_646 ?
O3 K1 O15 136.2(5) 41_646 . ?
O3 K1 O15 136.2(5) 44_666 23_565 ?
O3 K1 O15 84.0(6) 44_666 . ?
O3 K1 O15 84.0(6) 41_646 23_565 ?
O15 K1 C16 76.1(6) . 23_565 ?
O15 K1 C16 38.7(4) 23_565 23_565 ?
O15 K1 C16 76.1(6) 23_565 . ?
O15 K1 C16 38.7(4) . . ?
O15 K1 O15 100.6(8) . 23_565 ?
O16 K1 C16 81.4(8) . 23_565 ?
O16 K1 C16 20.2(6) 23_565 23_565 ?
O16 K1 C16 20.1(6) . . ?
O16 K1 C16 81.4(8) 23_565 . ?
O16 K1 O2 64.9(8) . 41_646 ?
O16 K1 O2 157.4(9) . 44_666 ?
O16 K1 O2 157.4(9) 23_565 41_646 ?
O16 K1 O2 64.9(8) 23_565 44_666 ?
O16 K1 O3 83.9(7) 23_565 44_666 ?
O16 K1 O3 139.8(7) 23_565 41_646 ?
O16 K1 O3 83.9(7) . 41_646 ?
O16 K1 O3 139.8(7) . 44_666 ?
O16 K1 O15 70.0(7) 23_565 . ?
O16 K1 O15 70.0(7) . 23_565 ?
O16 K1 O15 58.1(7) 23_565 23_565 ?
O16 K1 O15 58.1(7) . . ?
O16 K1 O16 94.2(12) 23_565 . ?
C13 O1AA H1AA 109.5 . . ?
C2 O2 K1 120.1(15) . 42_566 ?
C2 O2 H2A 109.5 . . ?
K1 O2 H2A 29.7 42_566 . ?
C3 O3 K1 131.6(13) . 42_566 ?
C3 O3 H3A 109.5 . . ?
K1 O3 H3A 117.8 42_566 . ?
C11 O4 C4 115.0(14) . . ?
C1 O5 C5 106.2(7) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12A 109.5 . . ?
C1 O14 C14 127.1(19) 5_565 . ?
C11 O15 C15 112.2(13) . . ?
C11 O15 K1 111.5(15) . . ?
C15 O15 K1 116.4(14) . . ?
C16 O16 K1 123.9(18) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 126.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -35(3) . . . . ?
C1 C2 C3 O3 171(2) . . . . ?
C1 C2 O2 K1 172.5(15) . . . 42_566 ?
C2 C1 O5 C5 -62(2) . . . . ?
C2 C3 C4 C5 33(3) . . . . ?
C2 C3 C4 O4 167(2) . . . . ?
C2 C3 O3 K1 -21(3) . . . 42_566 ?
C3 C2 O2 K1 -67.9(19) . . . 42_566 ?
C3 C4 C5 C6 -170(2) . . . . ?
C3 C4 C5 O5 -46(3) . . . . ?
C3 C4 O4 C11 122(2) . . . . ?
C4 C3 O3 K1 -168(2) . . . 42_566 ?
C4 C5 C6 O6 55(3) . . . . ?
C4 C5 O5 C1 58(2) . . . . ?
C5 C4 O4 C11 -106(2) . . . . ?
C6 C5 O5 C1 -178(2) . . . . ?
C11 C12 C13 C14 -54(2) . . . . ?
C11 C12 C13 O1AA 172.9(19) . . . . ?
C12 C11 O4 C4 -135(2) . . . . ?
C12 C11 O15 C15 -58(3) . . . . ?
C12 C11 O15 K1 74.1(19) . . . . ?
C12 C13 C14 C15 53(2) . . . . ?
C12 C13 C14 O14 -180(2) . . . . ?
C13 C14 C15 C16 -160.0(19) . . . . ?
C13 C14 C15 O15 -52(2) . . . . ?
C13 C14 O14 C1 135(2) . . . 5_565 ?
C14 C15 C16 K1 84.7(14) . . . . ?
C14 C15 C16 O16 58(3) . . . . ?
C14 C15 O15 C11 55(3) . . . . ?
C14 C15 O15 K1 -75.3(17) . . . . ?
C15 C14 O14 C1 -97(3) . . . 5_565 ?
C15 C16 O16 K1 49(3) . . . . ?
C16 C15 O15 C11 175(2) . . . . ?
C16 C15 O15 K1 45.0(16) . . . . ?
O1AA C13 C14 C15 176(3) . . . . ?
O1AA C13 C14 O14 -56(3) . . . . ?
O2 C2 C3 C4 -157(2) . . . . ?
O2 C2 C3 O3 49(3) . . . . ?
O3 C3 C4 C5 178(3) . . . . ?
O3 C3 C4 O4 -48(4) . . . . ?
O4 C4 C5 C6 62(3) . . . . ?
O4 C4 C5 O5 -174.2(19) . . . . ?
O4 C11 C12 C13 -91(2) . . . . ?
O4 C11 C12 O12 42(3) . . . . ?
O4 C11 O15 C15 74(3) . . . . ?
O4 C11 O15 K1 -153.6(19) . . . . ?
O5 C1 C2 C3 52(3) . . . . ?
O5 C1 C2 O2 164.9(19) . . . . ?
O5 C5 C6 O6 -72(3) . . . . ?
O12 C12 C13 C14 170(2) . . . . ?
O12 C12 C13 O1AA 37(3) . . . . ?
O14 C1 C2 C3 -66(2) 7_556 . . . ?
O14 C1 C2 O2 47(2) 7_556 . . . ?
O14 C1 O5 C5 55(2) 7_556 . . . ?
O14 C14 C15 C16 70(2) . . . . ?
O14 C14 C15 O15 178.1(19) . . . . ?
O15 C11 C12 C13 57(2) . . . . ?
O15 C11 C12 O12 -170(3) . . . . ?
O15 C11 O4 C4 89(3) . . . . ?
O15 C15 C16 K1 -32.5(14) . . . . ?
O15 C15 C16 O16 -59(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.483 -0.058 -0.926 14421.2 4428.5 ?


_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_olex2_submission_original_sample_id CDMOF_alpha_3_033
_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 1.621
_oxdiff_exptl_absorpt_empirical_full_min 0.825
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# Please retain this information to preserve the provenance of 
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data_CDMOF_b_245K
_database_code_depnum_ccdc_archive 'CCDC 1529155'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_THETM01_CDMOF_b_245K        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly diffracting sample crystal'
;
_vrf_RINTA01_CDMOF_b_245K        
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: 'Possible structural changes caused by evacuation of guest molecules'
;
_vrf_PLAT201_CDMOF_b_245K        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         88 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT020_CDMOF_b_245K        
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.208 Report
RESPONSE: 'Possible structural changes caused by evacuation of guest molecules'
;
_vrf_PLAT090_CDMOF_b_245K        
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.91 Note  
RESPONSE: 'Data limited due to the poorly diffracting sample crystal; 
large number of parameters is the result of the complex molecular 
and crystal structures'
;
_vrf_PLAT241_CDMOF_b_245K        
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         K2 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT242_CDMOF_b_245K        
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         O6 Check 
RESPONSE: 'Poor data quality'
;
_vrf_PLAT306_CDMOF_b_245K        
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_b_245K        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04175 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_CDMOF_b_245K        
;
PROBLEM: D-H Without Acceptor       O26    --  H26    ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
_vrf_PLAT910_CDMOF_b_245K        
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          19 Note  
RESPONSE: 'Missing reflections may be due to the chosen strategy of 
the measurement; 
this was short measurement, aimed primarily at 
checking the unit-cell paremeters only'
;
# end Validation Reply Form
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


# CRYSTAL DATA
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_symmetry_space_group_name_H-M_alt 'R 3 2'
_cell_length_a                   43.260(16)
_cell_length_b                   43.260(16)
_cell_length_c                   28.104(16)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_volume                     45547(30)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    1157
_cell_measurement_temperature    244.98(10)
_cell_measurement_theta_max      10.7500
_cell_measurement_theta_min      2.9290
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.925
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             13392
_exptl_crystal_preparation       ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  54.00   1.00   15.00    --  -18.72   0.00-150.00  122
  2  ω    -73.00  20.00   1.00   15.00    --  -18.72 -19.00  60.00   93
  3  ω    -40.00   8.00   1.00   15.00    --  -18.72  57.00  60.00   48
  4  ω    -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       'ω 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_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_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_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.67
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_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_coef       .
_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_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0812
_refine_ls_restrained_S_all      1.108
_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/[σ²(Fo²)+(0.0963P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.2034
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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)
;

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7465(5) 0.6657(7) 0.4033(8) 0.148(12) Uiso 1 1 d D U . . .
H1 H 0.7555 0.6818 0.3759 0.177 Uiso 1 1 calc R . . . .
C2 C 0.7325(6) 0.6768(5) 0.4470(8) 0.117(11) Uiso 1 1 d D U . . .
H2 H 0.7162 0.6847 0.4356 0.141 Uiso 1 1 calc R . . . .
C3 C 0.7154(7) 0.6525(7) 0.4875(9) 0.193(15) Uiso 1 1 d D U . . .
H3 H 0.7325 0.6450 0.4969 0.232 Uiso 1 1 calc R . . . .
C4 C 0.6818(6) 0.6182(6) 0.4758(8) 0.181(15) Uiso 1 1 d D U . . .
H4 H 0.6631 0.6238 0.4677 0.217 Uiso 1 1 calc R . . . .
C5 C 0.6889(8) 0.6018(6) 0.4331(9) 0.180(14) Uiso 1 1 d D U . . .
H5 H 0.7029 0.5916 0.4458 0.216 Uiso 1 1 calc R . . . .
C6 C 0.6613(8) 0.5726(9) 0.4025(13) 0.240(18) Uiso 1 1 d D U . . .
H6B H 0.6723 0.5694 0.3742 0.288 Uiso 1 1 calc R . . . .
H6A H 0.6497 0.5502 0.4198 0.288 Uiso 1 1 calc R . . . .
C11 C 0.8625(6) 0.6626(8) 0.3681(11) 0.178(15) Uiso 1 1 d D U . . .
H11 H 0.8824 0.6668 0.3474 0.214 Uiso 1 1 calc R . . . .
C12 C 0.8635(7) 0.6982(6) 0.3800(12) 0.209(16) Uiso 1 1 d D U . . .
H12 H 0.8617 0.7087 0.3499 0.250 Uiso 1 1 calc R . . . .
C13 C 0.8311(6) 0.6897(6) 0.4088(12) 0.172(14) Uiso 1 1 d D U . . .
H13 H 0.8359 0.6817 0.4392 0.206 Uiso 1 1 calc R . . . .
C14 C 0.7983(5) 0.6579(6) 0.3921(8) 0.098(10) Uiso 1 1 d D U . . .
H14 H 0.7931 0.6665 0.3626 0.118 Uiso 1 1 calc R . . . .
C15 C 0.7967(5) 0.6244(6) 0.3764(9) 0.094(10) Uiso 1 1 d D U . . .
H15 H 0.7988 0.6111 0.4033 0.113 Uiso 1 1 calc R . . . .
C16 C 0.7674(8) 0.6006(8) 0.3434(10) 0.169(14) Uiso 1 1 d D U . . .
H16A H 0.7697 0.5800 0.3354 0.202 Uiso 1 1 calc R . . . .
H16B H 0.7445 0.5921 0.3589 0.202 Uiso 1 1 calc R . . . .
C21 C 0.9403(9) 0.6230(9) 0.4619(10) 0.168(14) Uiso 1 1 d D U . . .
H21 H 0.9614 0.6202 0.4625 0.202 Uiso 1 1 calc R . . . .
C22 C 0.9540(10) 0.6629(10) 0.4682(11) 0.219(17) Uiso 1 1 d D U . . .
H22 H 0.9708 0.6772 0.4431 0.262 Uiso 1 1 calc R . . . .
C23 C 0.9195(10) 0.6632(9) 0.4647(14) 0.255(19) Uiso 1 1 d D U . . .
H23 H 0.9065 0.6548 0.4948 0.305 Uiso 1 1 calc R . . . .
C24 C 0.8952(9) 0.6452(8) 0.4252(11) 0.177(14) Uiso 1 1 d D U . . .
H24 H 0.9115 0.6588 0.3993 0.212 Uiso 1 1 calc R . . . .
C25 C 0.8901(8) 0.6100(8) 0.4127(11) 0.198(15) Uiso 1 1 d D U . . .
H25 H 0.8754 0.5935 0.4379 0.238 Uiso 1 1 calc R . . . .
C26 C 0.8736(7) 0.5924(8) 0.3663(10) 0.191(15) Uiso 1 1 d D U . . .
H26B H 0.8618 0.5667 0.3702 0.230 Uiso 1 1 calc R . . . .
H26A H 0.8557 0.5985 0.3574 0.230 Uiso 1 1 calc R . . . .
C31 C 0.9369(6) 0.5514(9) 0.6175(8) 0.238(18) Uiso 1 1 d D U . . .
H31 H 0.9468 0.5388 0.6351 0.286 Uiso 1 1 calc R . . . .
C32 C 0.9625(11) 0.5915(9) 0.6182(12) 0.234(18) Uiso 1 1 d D U . . .
H32 H 0.9848 0.5946 0.6047 0.281 Uiso 1 1 calc R . . . .
C33 C 0.9494(10) 0.6096(6) 0.5822(13) 0.200(16) Uiso 1 1 d D U . . .
H33 H 0.9293 0.6112 0.5954 0.240 Uiso 1 1 calc R . . . .
C34 C 0.9376(8) 0.5850(8) 0.5393(10) 0.150(12) Uiso 1 1 d D U . . .
H34 H 0.9575 0.5849 0.5227 0.179 Uiso 1 1 calc R . . . .
C35 C 0.9050(8) 0.5487(7) 0.5423(8) 0.170(14) Uiso 1 1 d D U . . .
H35 H 0.8870 0.5511 0.5604 0.204 Uiso 1 1 calc R . . . .
C36 C 0.8869(6) 0.5270(9) 0.4988(9) 0.230(18) Uiso 1 1 d D U . . .
H36A H 0.8714 0.5024 0.5081 0.276 Uiso 1 1 calc R . . . .
H36B H 0.8722 0.5357 0.4849 0.276 Uiso 1 1 calc R . . . .
C41 C 0.8374(5) 0.4928(8) 0.7526(10) 0.147(13) Uiso 1 1 d D U . . .
H41 H 0.8306 0.4785 0.7818 0.176 Uiso 1 1 calc R . . . .
C42 C 0.8685(7) 0.5290(7) 0.7647(9) 0.112(11) Uiso 1 1 d D U . . .
H42 H 0.8857 0.5230 0.7784 0.135 Uiso 1 1 calc R . . . .
C43 C 0.8857(7) 0.5460(6) 0.7183(9) 0.112(11) Uiso 1 1 d D U . . .
H43 H 0.8714 0.5561 0.7062 0.134 Uiso 1 1 calc R . . . .
C44 C 0.8879(5) 0.5254(6) 0.6782(8) 0.062(8) Uiso 1 1 d D U . . .
H44 H 0.9054 0.5190 0.6893 0.074 Uiso 1 1 calc R . . . .
C45 C 0.8552(7) 0.4902(7) 0.6728(8) 0.110(10) Uiso 1 1 d D U . . .
H45 H 0.8376 0.4961 0.6600 0.132 Uiso 1 1 calc R . . . .
C46 C 0.8554(8) 0.4648(7) 0.6376(10) 0.116(11) Uiso 1 1 d D U . . .
H46A H 0.8611 0.4757 0.6063 0.139 Uiso 1 1 calc R . . . .
H46B H 0.8320 0.4435 0.6362 0.139 Uiso 1 1 calc R . . . .
C51 C 0.7065(7) 0.4694(8) 0.7797(10) 0.184(14) Uiso 1 1 d D U . . .
H51 H 0.6830 0.4561 0.7948 0.221 Uiso 1 1 calc R . . . .
C52 C 0.7334(6) 0.4899(5) 0.8195(8) 0.103(10) Uiso 1 1 d D U . . .
H52 H 0.7357 0.4747 0.8434 0.124 Uiso 1 1 calc R . . . .
C53 C 0.7645(7) 0.5077(7) 0.7858(10) 0.137(12) Uiso 1 1 d D U . . .
H53 H 0.7644 0.5244 0.7623 0.165 Uiso 1 1 calc R . . . .
C54 C 0.7761(5) 0.4814(6) 0.7697(9) 0.107(10) Uiso 1 1 d D U . . .
H54 H 0.7770 0.4663 0.7951 0.129 Uiso 1 1 calc R . . . .
C55 C 0.7483(6) 0.4611(7) 0.7315(9) 0.124(11) Uiso 1 1 d D U . . .
H55 H 0.7481 0.4789 0.7101 0.148 Uiso 1 1 calc R . . . .
C56 C 0.7517(9) 0.4349(8) 0.7015(9) 0.211(17) Uiso 1 1 d D U . . .
H56A H 0.7295 0.4183 0.6860 0.253 Uiso 1 1 calc R . . . .
H56B H 0.7706 0.4462 0.6781 0.253 Uiso 1 1 calc R . . . .
C61 C 0.6218(9) 0.5096(8) 0.7005(14) 0.243(18) Uiso 1 1 d D U . . .
H61 H 0.5996 0.5104 0.7002 0.292 Uiso 1 1 calc R . . . .
C62 C 0.6484(9) 0.5330(8) 0.7364(12) 0.179(15) Uiso 1 1 d D U . . .
H62 H 0.6371 0.5262 0.7678 0.215 Uiso 1 1 calc R . . . .
C63 C 0.6803(8) 0.5266(7) 0.7359(10) 0.156(13) Uiso 1 1 d D U . . .
H63 H 0.6983 0.5395 0.7114 0.188 Uiso 1 1 calc R . . . .
C64 C 0.6674(9) 0.4870(8) 0.7402(12) 0.175(14) Uiso 1 1 d D U . . .
H64 H 0.6534 0.4760 0.7690 0.210 Uiso 1 1 calc R . . . .
C65 C 0.6472(9) 0.4699(7) 0.6945(11) 0.152(13) Uiso 1 1 d D U . . .
H65 H 0.6636 0.4813 0.6678 0.182 Uiso 1 1 calc R . . . .
C66 C 0.6330(10) 0.4301(8) 0.6913(14) 0.220(17) Uiso 1 1 d D U . . .
H66A H 0.6180 0.4194 0.6636 0.263 Uiso 1 1 calc R . . . .
H66B H 0.6518 0.4241 0.6922 0.263 Uiso 1 1 calc R . . . .
C71 C 0.6344(7) 0.5752(6) 0.5302(10) 0.223(16) Uiso 1 1 d D U . . .
H71 H 0.6231 0.5805 0.5036 0.268 Uiso 1 1 calc R . . . .
C72 C 0.6247(9) 0.5896(9) 0.5710(10) 0.189(15) Uiso 1 1 d D U . . .
H72 H 0.5987 0.5783 0.5746 0.226 Uiso 1 1 calc R . . . .
C73 C 0.6412(9) 0.5784(7) 0.6106(10) 0.148(12) Uiso 1 1 d D U . . .
H73 H 0.6664 0.5913 0.6012 0.178 Uiso 1 1 calc R . . . .
C74 C 0.6342(8) 0.5407(6) 0.6125(10) 0.147(13) Uiso 1 1 d D U . . .
H74 H 0.6087 0.5292 0.6201 0.177 Uiso 1 1 calc R . . . .
C75 C 0.6303(7) 0.5230(6) 0.5659(9) 0.121(11) Uiso 1 1 d D U . . .
H75 H 0.6547 0.5283 0.5589 0.145 Uiso 1 1 calc R . . . .
C76 C 0.6099(7) 0.4837(6) 0.5656(10) 0.197(16) Uiso 1 1 d D U . . .
H76A H 0.6098 0.4762 0.5331 0.237 Uiso 1 1 calc R . . . .
H76B H 0.6233 0.4756 0.5843 0.237 Uiso 1 1 calc R . . . .
K1 K 0.89413(19) 0.7910(2) 0.4180(3) 0.157(3) Uani 1 1 d D U . . .
K2 K 0.6667 0.6374(3) 0.3333 0.306(11) Uani 1 2 d DS TU P . .
K3 K 0.9757(3) 0.6423(3) 0.3333 0.236(7) Uani 1 2 d S TU P . .
O2 O 0.7650(6) 0.7076(6) 0.4610(8) 0.191(2) Uiso 1 1 d D U . . .
H2A H 0.7659 0.7092 0.4901 0.287 Uiso 1 1 calc R . . . .
O3 O 0.7097(6) 0.6674(6) 0.5298(8) 0.191(2) Uiso 1 1 d D U . . .
H3A H 0.6882 0.6583 0.5347 0.287 Uiso 1 1 calc R . . . .
O4 O 0.6723(6) 0.5986(6) 0.5204(7) 0.191(2) Uiso 1 1 d D U . . .
O5 O 0.7118(6) 0.6264(6) 0.3964(7) 0.191(2) Uiso 1 1 d D U . . .
O6 O 0.6351(6) 0.5837(6) 0.3893(8) 0.191(2) Uiso 1 1 d D U . . .
H6 H 0.6155 0.5694 0.4004 0.287 Uiso 1 1 calc R . . . .
O12 O 0.8929(6) 0.7269(6) 0.4079(8) 0.191(2) Uiso 1 1 d D U . . .
H12A H 0.8946 0.7189 0.4336 0.287 Uiso 1 1 calc R . . . .
O13 O 0.8281(6) 0.7210(5) 0.4226(8) 0.191(2) Uiso 1 1 d D U . . .
H13A H 0.8070 0.7147 0.4273 0.287 Uiso 1 1 calc R . . . .
O14 O 0.7680(6) 0.6515(6) 0.4228(7) 0.191(2) Uiso 1 1 d D U . . .
O15 O 0.8282(6) 0.6389(5) 0.3454(7) 0.191(2) Uiso 1 1 d D U . . .
O16 O 0.7690(6) 0.6203(6) 0.2995(9) 0.191(2) Uiso 1 1 d D U . . .
H16 H 0.7889 0.6287 0.2876 0.287 Uiso 1 1 calc R . . . .
O22 O 0.9674(6) 0.6772(6) 0.5158(8) 0.191(2) Uiso 1 1 d D U . . .
H22A H 0.9676 0.6961 0.5192 0.287 Uiso 1 1 calc R . . . .
O23 O 0.9273(6) 0.6996(7) 0.4554(8) 0.191(2) Uiso 1 1 d D U . . .
H23A H 0.9322 0.7107 0.4804 0.287 Uiso 1 1 calc R . . . .
O24 O 0.8672(6) 0.6530(6) 0.4141(9) 0.191(2) Uiso 1 1 d D U . . .
O25 O 0.9249(6) 0.6120(6) 0.4148(9) 0.191(2) Uiso 1 1 d D U . . .
O26 O 0.8999(6) 0.6031(6) 0.3284(8) 0.191(2) Uiso 1 1 d D U . . .
H26 H 0.8942 0.6116 0.3064 0.287 Uiso 1 1 calc R . . . .
O32 O 0.9699(6) 0.5999(6) 0.6683(9) 0.191(2) Uiso 1 1 d D U . . .
H32A H 0.9850 0.6211 0.6713 0.287 Uiso 1 1 calc R . . . .
O33 O 0.9801(6) 0.6438(6) 0.5795(8) 0.191(2) Uiso 1 1 d D U . . .
H33A H 0.9750 0.6576 0.5667 0.287 Uiso 1 1 calc R . . . .
O34 O 0.9155(7) 0.5995(6) 0.5046(9) 0.191(2) Uiso 1 1 d . U . . .
O35 O 0.9199(6) 0.5328(5) 0.5738(9) 0.191(2) Uiso 1 1 d D U . . .
O36 O 0.9118(6) 0.5284(6) 0.4631(8) 0.191(2) Uiso 1 1 d D U . . .
H36 H 0.9191 0.5467 0.4473 0.287 Uiso 1 1 calc R . . . .
O42 O 0.8644(6) 0.5487(6) 0.8016(8) 0.191(2) Uiso 1 1 d . U . . .
H42A H 0.8795 0.5698 0.7987 0.287 Uiso 1 1 calc R . . . .
O43 O 0.9182(6) 0.5756(6) 0.7317(8) 0.191(2) Uiso 1 1 d D U . . .
H43A H 0.9317 0.5827 0.7089 0.287 Uiso 1 1 calc R . . . .
O44 O 0.9000(6) 0.5383(6) 0.6305(8) 0.191(2) Uiso 1 1 d D U . . .
O45 O 0.8397(6) 0.4728(5) 0.7182(10) 0.191(2) Uiso 1 1 d D U . . .
O46 O 0.8837(6) 0.4547(6) 0.6527(8) 0.191(2) Uiso 1 1 d . U . . .
H46 H 0.9021 0.4728 0.6607 0.287 Uiso 1 1 calc R . . . .
O52 O 0.7208(5) 0.5134(6) 0.8384(7) 0.191(2) Uiso 1 1 d D U . . .
H52A H 0.7375 0.5308 0.8512 0.287 Uiso 1 1 calc R . . . .
O53 O 0.7922(6) 0.5227(6) 0.8258(9) 0.191(2) Uiso 1 1 d . U . . .
H53A H 0.8117 0.5271 0.8153 0.287 Uiso 1 1 calc R . . . .
O54 O 0.8075(7) 0.4978(6) 0.7393(8) 0.191(2) Uiso 1 1 d D U . . .
O55 O 0.7133(6) 0.4433(5) 0.7570(7) 0.191(2) Uiso 1 1 d D U . . .
O56 O 0.7609(6) 0.4187(6) 0.7401(9) 0.191(2) Uiso 1 1 d D U . . .
H56 H 0.7824 0.4302 0.7451 0.287 Uiso 1 1 calc R . . . .
O62 O 0.6596(6) 0.5707(6) 0.7287(8) 0.191(2) Uiso 1 1 d D U . . .
H62A H 0.6757 0.5831 0.7473 0.287 Uiso 1 1 calc R . . . .
O63 O 0.6911(6) 0.5386(6) 0.7844(8) 0.191(2) Uiso 1 1 d D U . . .
H63A H 0.7098 0.5389 0.7902 0.287 Uiso 1 1 calc R . . . .
O64 O 0.7031(7) 0.4905(6) 0.7408(9) 0.191(2) Uiso 1 1 d D U . . .
O65 O 0.6179(6) 0.4753(7) 0.6884(8) 0.191(2) Uiso 1 1 d D U . . .
O66 O 0.6118(6) 0.4206(6) 0.7371(9) 0.191(2) Uiso 1 1 d . U . . .
H66 H 0.6157 0.4069 0.7526 0.287 Uiso 1 1 calc R . . . .
O72 O 0.6418(6) 0.6291(7) 0.5674(8) 0.191(2) Uiso 1 1 d D U . . .
H72A H 0.6438 0.6376 0.5940 0.287 Uiso 1 1 calc R . . . .
O73 O 0.6424(6) 0.5974(6) 0.6542(8) 0.191(2) Uiso 1 1 d D U . . .
H73A H 0.6537 0.5937 0.6746 0.229 Uiso 1 1 calc R . . . .
O74 O 0.6475(7) 0.5312(7) 0.6643(10) 0.191(2) Uiso 1 1 d D U . . .
O75 O 0.6216(6) 0.5385(6) 0.5245(8) 0.191(2) Uiso 1 1 d D U . . .
O76 O 0.5733(6) 0.4642(5) 0.5823(8) 0.191(2) Uiso 1 1 d D U . . .
H76 H 0.5727 0.4684 0.6107 0.287 Uiso 1 1 calc R . . . .
OA O 0.7526(9) 0.6988(10) 0.5829(14) 0.337(12) Uiso 1 1 d . U . . .
OB O 0.9488(10) 0.7127(10) 0.5661(14) 0.337(12) Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.55(2) . ?
C1 O5 1.62(2) . ?
C1 O14 1.45(2) . ?
C2 H2 0.9800 . ?
C2 C3 1.47(2) . ?
C2 O2 1.427(19) . ?
C3 H3 0.9800 . ?
C3 C4 1.506(7) . ?
C3 O3 1.43(2) . ?
C4 H4 0.9800 . ?
C4 C5 1.503(7) . ?
C4 O4 1.45(2) . ?
C5 H5 0.9800 . ?
C5 C6 1.500(8) . ?
C5 O5 1.458(14) . ?
C6 H6B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 K2 3.32(4) . ?
C6 O6 1.48(2) . ?
C11 H11 0.9800 . ?
C11 C12 1.56(3) . ?
C11 O15 1.46(2) . ?
C11 O24 1.40(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.49(2) . ?
C12 O12 1.481(17) . ?
C13 H13 0.9800 . ?
C13 C14 1.47(2) . ?
C13 O13 1.48(2) . ?
C14 H14 0.9800 . ?
C14 C15 1.481(19) . ?
C14 O14 1.478(13) . ?
C15 H15 0.9800 . ?
C15 C16 1.49(2) . ?
C15 O15 1.468(13) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 O16 1.48(2) . ?
C21 H21 0.9800 . ?
C21 C22 1.53(2) . ?
C21 O25 1.452(14) . ?
C21 O34 1.59(3) . ?
C22 H22 0.9800 . ?
C22 C23 1.50(3) . ?
C22 O22 1.467(19) . ?
C23 H23 0.9800 . ?
C23 C24 1.46(2) . ?
C23 O23 1.46(2) . ?
C24 H24 0.9800 . ?
C24 C25 1.47(2) . ?
C24 O24 1.45(3) . ?
C25 H25 0.9800 . ?
C25 C26 1.50(2) . ?
C25 O25 1.463(14) . ?
C26 H26B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 O26 1.453(7) . ?
C31 H31 0.9800 . ?
C31 C32 1.52(2) . ?
C31 O35 1.451(7) . ?
C31 O44 1.45(2) . ?
C32 H32 0.9800 . ?
C32 C33 1.55(2) . ?
C32 K3 3.30(3) 8_655 ?
C32 O32 1.45(2) . ?
C33 H33 0.9800 . ?
C33 C34 1.52(2) . ?
C33 O33 1.41(2) . ?
C34 H34 0.9800 . ?
C34 C35 1.499(3) . ?
C34 O34 1.69(3) . ?
C35 H35 0.9800 . ?
C35 C36 1.500(3) . ?
C35 O35 1.453(7) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 O36 1.450(3) . ?
C41 H41 0.9800 . ?
C41 C42 1.51(2) . ?
C41 O45 1.33(3) . ?
C41 O54 1.464(13) . ?
C42 H42 0.9800 . ?
C42 C43 1.50(2) . ?
C42 O42 1.41(3) . ?
C43 H43 0.9800 . ?
C43 C44 1.467(17) . ?
C43 O43 1.40(2) . ?
C44 H44 0.9800 . ?
C44 C45 1.48(2) . ?
C44 O44 1.445(13) . ?
C45 H45 0.9800 . ?
C45 C46 1.48(2) . ?
C45 O45 1.46(2) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 O46 1.55(3) . ?
C51 H51 0.9800 . ?
C51 C52 1.54(2) . ?
C51 O55 1.448(13) . ?
C51 O64 1.48(2) . ?
C52 H52 0.9800 . ?
C52 C53 1.504(17) . ?
C52 K1 3.36(2) 10_566 ?
C52 O52 1.471(18) . ?
C53 H53 0.9800 . ?
C53 C54 1.53(2) . ?
C53 O53 1.53(3) . ?
C54 H54 0.9800 . ?
C54 C55 1.52(2) . ?
C54 O54 1.45(2) . ?
C55 H55 0.9800 . ?
C55 C56 1.48(2) . ?
C55 O55 1.50(2) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 O56 1.453(8) . ?
C61 H61 0.9800 . ?
C61 C62 1.48(2) . ?
C61 K1 3.16(3) 9_565 ?
C61 O65 1.45(2) . ?
C61 O74 1.45(2) . ?
C62 H62 0.9800 . ?
C62 C63 1.54(2) . ?
C62 O62 1.46(2) . ?
C63 H63 0.9800 . ?
C63 C64 1.52(2) . ?
C63 O63 1.449(7) . ?
C64 H64 0.9800 . ?
C64 C65 1.518(18) . ?
C64 O64 1.48(3) . ?
C65 H65 0.9800 . ?
C65 C66 1.52(2) . ?
C65 O65 1.41(3) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C66 O66 1.51(4) . ?
C71 H71 0.9800 . ?
C71 C72 1.47(2) . ?
C71 O4 1.458(14) . ?
C71 O75 1.40(2) . ?
C72 H72 0.9800 . ?
C72 C73 1.52(2) . ?
C72 O72 1.49(2) . ?
C73 H73 0.9800 . ?
C73 C74 1.504(7) . ?
C73 O73 1.46(2) . ?
C74 H74 0.9800 . ?
C74 C75 1.48(2) . ?
C74 O74 1.69(3) . ?
C75 H75 0.9800 . ?
C75 C76 1.47(2) . ?
C75 O75 1.49(2) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C76 O76 1.449(7) . ?
K1 C52 3.36(2) 10_566 ?
K1 C61 3.16(3) 14_654 ?
K1 O12 2.76(2) . ?
K1 O13 2.95(2) . ?
K1 O45 2.86(3) 15_664 ?
K1 O46 2.86(2) 15_664 ?
K1 O52 2.84(2) 10_566 ?
K1 O53 2.97(2) 10_566 ?
K1 O65 2.73(2) 14_654 ?
K1 O66 2.62(2) 14_654 ?
K2 C6 3.32(4) 17_655 ?
K2 O5 2.85(2) . ?
K2 O5 2.85(2) 17_655 ?
K2 O6 2.56(2) 17_655 ?
K2 O6 2.56(2) . ?
K2 O72 3.28(2) 14_654 ?
K2 O72 3.28(2) 6_556 ?
K2 O73 3.13(2) 14_654 ?
K2 O73 3.13(2) 6_556 ?
K3 C32 3.30(3) 15_664 ?
K3 C32 3.30(3) 5_766 ?
K3 O25 2.99(2) . ?
K3 O25 2.99(2) 18_545 ?
K3 O26 2.85(3) 18_545 ?
K3 O26 2.84(3) . ?
K3 O32 2.66(2) 15_664 ?
K3 O32 2.66(2) 5_766 ?
K3 O33 2.96(2) 15_664 ?
K3 O33 2.96(2) 5_766 ?
O2 H2A 0.8200 . ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O16 H16 0.8200 . ?
O22 H22A 0.8200 . ?
O23 H23A 0.8200 . ?
O26 H26 0.8200 . ?
O32 K3 2.66(2) 8_655 ?
O32 H32A 0.8200 . ?
O33 K3 2.96(2) 8_655 ?
O33 H33A 0.8200 . ?
O36 H36 0.8200 . ?
O42 H42A 0.8200 . ?
O43 H43A 0.8200 . ?
O45 K1 2.86(3) 8_655 ?
O46 K1 2.86(2) 8_655 ?
O46 H46 0.8200 . ?
O52 K1 2.84(2) 10_566 ?
O52 H52A 0.8200 . ?
O53 K1 2.97(2) 10_566 ?
O53 H53A 0.8200 . ?
O56 H56 0.8200 . ?
O62 H62A 0.8200 . ?
O63 H63A 0.8200 . ?
O65 K1 2.73(2) 9_565 ?
O66 K1 2.62(2) 9_565 ?
O66 H66 0.8200 . ?
O72 K2 3.28(2) 9_565 ?
O72 H72A 0.8200 . ?
O73 K2 3.13(2) 9_565 ?
O73 H73A 0.8200 . ?
O76 H76 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 118.9 . . ?
C2 C1 O5 96.9(12) . . ?
O5 C1 H1 118.9 . . ?
O14 C1 H1 118.9 . . ?
O14 C1 C2 105.2(18) . . ?
O14 C1 O5 93.2(19) . . ?
C1 C2 H2 108.0 . . ?
C3 C2 C1 121.7(19) . . ?
C3 C2 H2 108.0 . . ?
O2 C2 C1 98.9(17) . . ?
O2 C2 H2 108.0 . . ?
O2 C2 C3 111(2) . . ?
C2 C3 H3 104.6 . . ?
C2 C3 C4 115.4(15) . . ?
C4 C3 H3 104.6 . . ?
O3 C3 C2 117(2) . . ?
O3 C3 H3 104.6 . . ?
O3 C3 C4 109(2) . . ?
C3 C4 H4 108.6 . . ?
C5 C4 C3 108.3(14) . . ?
C5 C4 H4 108.6 . . ?
O4 C4 C3 104(2) . . ?
O4 C4 H4 108.6 . . ?
O4 C4 C5 119(2) . . ?
C4 C5 H5 103.9 . . ?
C6 C5 C4 126(3) . . ?
C6 C5 H5 103.9 . . ?
O5 C5 C4 116.4(12) . . ?
O5 C5 H5 103.9 . . ?
O5 C5 C6 100(2) . . ?
C5 C6 H6B 110.4 . . ?
C5 C6 H6A 110.4 . . ?
C5 C6 K2 86(2) . . ?
H6B C6 H6A 108.6 . . ?
K2 C6 H6B 78.9 . . ?
K2 C6 H6A 156.7 . . ?
O6 C6 C5 107(3) . . ?
O6 C6 H6B 110.4 . . ?
O6 C6 H6A 110.4 . . ?
O6 C6 K2 47.4(16) . . ?
C12 C11 H11 111.0 . . ?
O15 C11 H11 111.0 . . ?
O15 C11 C12 107.8(19) . . ?
O24 C11 H11 111.0 . . ?
O24 C11 C12 99(3) . . ?
O24 C11 O15 116(2) . . ?
C11 C12 H12 107.7 . . ?
C13 C12 C11 108(2) . . ?
C13 C12 H12 107.7 . . ?
O12 C12 C11 122(3) . . ?
O12 C12 H12 107.7 . . ?
O12 C12 C13 103(2) . . ?
C12 C13 H13 102.9 . . ?
C14 C13 C12 114(2) . . ?
C14 C13 H13 102.9 . . ?
C14 C13 O13 117(2) . . ?
O13 C13 C12 114.6(19) . . ?
O13 C13 H13 102.9 . . ?
C13 C14 H14 102.3 . . ?
C13 C14 C15 124.0(17) . . ?
C13 C14 O14 109.8(17) . . ?
C15 C14 H14 102.3 . . ?
C15 C14 O14 112.9(18) . . ?
O14 C14 H14 102.3 . . ?
C14 C15 H15 111.7 . . ?
C14 C15 C16 118(2) . . ?
C16 C15 H15 111.7 . . ?
O15 C15 C14 100.3(16) . . ?
O15 C15 H15 111.7 . . ?
O15 C15 C16 102(2) . . ?
C15 C16 H16A 109.7 . . ?
C15 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
O16 C16 C15 110(2) . . ?
O16 C16 H16A 109.7 . . ?
O16 C16 H16B 109.7 . . ?
C22 C21 H21 106.2 . . ?
C22 C21 O34 113(3) . . ?
O25 C21 H21 106.2 . . ?
O25 C21 C22 109(2) . . ?
O25 C21 O34 115(3) . . ?
O34 C21 H21 106.2 . . ?
C21 C22 H22 112.1 . . ?
C23 C22 C21 100(3) . . ?
C23 C22 H22 112.1 . . ?
O22 C22 C21 115(3) . . ?
O22 C22 H22 112.1 . . ?
O22 C22 C23 104(3) . . ?
C22 C23 H23 109.4 . . ?
C24 C23 C22 120(3) . . ?
C24 C23 H23 109.4 . . ?
C24 C23 O23 99(2) . . ?
O23 C23 C22 109(3) . . ?
O23 C23 H23 109.4 . . ?
C23 C24 H24 97.8 . . ?
C23 C24 C25 115(2) . . ?
C25 C24 H24 97.8 . . ?
O24 C24 C23 120(2) . . ?
O24 C24 H24 97.8 . . ?
O24 C24 C25 119(2) . . ?
C24 C25 H25 106.7 . . ?
C24 C25 C26 121(2) . . ?
C26 C25 H25 106.7 . . ?
O25 C25 C24 108(2) . . ?
O25 C25 H25 106.7 . . ?
O25 C25 C26 106.2(19) . . ?
C25 C26 H26B 109.2 . . ?
C25 C26 H26A 109.2 . . ?
H26B C26 H26A 107.9 . . ?
O26 C26 C25 112(2) . . ?
O26 C26 H26B 109.2 . . ?
O26 C26 H26A 109.2 . . ?
C32 C31 H31 110.9 . . ?
O35 C31 H31 110.9 . . ?
O35 C31 C32 121(2) . . ?
O44 C31 H31 110.9 . . ?
O44 C31 C32 118(3) . . ?
O44 C31 O35 81.1(17) . . ?
C31 C32 H32 105.1 . . ?
C31 C32 C33 109(2) . . ?
C31 C32 K3 154(2) . 8_655 ?
C33 C32 H32 105.1 . . ?
C33 C32 K3 95.3(18) . 8_655 ?
K3 C32 H32 76.4 8_655 . ?
O32 C32 C31 104(3) . . ?
O32 C32 H32 105.1 . . ?
O32 C32 C33 127(3) . . ?
O32 C32 K3 51.8(15) . 8_655 ?
C32 C33 H33 110.4 . . ?
C34 C33 C32 104(2) . . ?
C34 C33 H33 110.4 . . ?
O33 C33 C32 100(3) . . ?
O33 C33 H33 110.4 . . ?
O33 C33 C34 120(3) . . ?
C33 C34 H34 112.9 . . ?
C33 C34 O34 105(3) . . ?
C35 C34 C33 120(2) . . ?
C35 C34 H34 112.9 . . ?
C35 C34 O34 91(2) . . ?
O34 C34 H34 112.9 . . ?
C34 C35 H35 107.3 . . ?
C34 C35 C36 122(2) . . ?
C36 C35 H35 107.3 . . ?
O35 C35 C34 97(2) . . ?
O35 C35 H35 107.3 . . ?
O35 C35 C36 115(2) . . ?
C35 C36 H36A 108.9 . . ?
C35 C36 H36B 108.9 . . ?
H36A C36 H36B 107.8 . . ?
O36 C36 C35 113.2(16) . . ?
O36 C36 H36A 108.9 . . ?
O36 C36 H36B 108.9 . . ?
C42 C41 H41 107.2 . . ?
O45 C41 H41 107.2 . . ?
O45 C41 C42 121.5(19) . . ?
O45 C41 O54 106(2) . . ?
O54 C41 H41 107.2 . . ?
O54 C41 C42 107(3) . . ?
C41 C42 H42 102.3 . . ?
C43 C42 C41 106(2) . . ?
C43 C42 H42 102.3 . . ?
O42 C42 C41 119(3) . . ?
O42 C42 H42 102.3 . . ?
O42 C42 C43 122(2) . . ?
C42 C43 H43 104.5 . . ?
C44 C43 C42 122(2) . . ?
C44 C43 H43 104.5 . . ?
O43 C43 C42 104(2) . . ?
O43 C43 H43 104.5 . . ?
O43 C43 C44 115(2) . . ?
C43 C44 H44 102.8 . . ?
C43 C44 C45 112.6(18) . . ?
C45 C44 H44 102.8 . . ?
O44 C44 C43 127(2) . . ?
O44 C44 H44 102.8 . . ?
O44 C44 C45 106(2) . . ?
C44 C45 H45 103.8 . . ?
C44 C45 C46 118(2) . . ?
C46 C45 H45 103.8 . . ?
O45 C45 C44 113.4(18) . . ?
O45 C45 H45 103.8 . . ?
O45 C45 C46 112(2) . . ?
C45 C46 H46A 109.9 . . ?
C45 C46 H46B 109.9 . . ?
C45 C46 O46 109(2) . . ?
H46A C46 H46B 108.3 . . ?
O46 C46 H46A 109.9 . . ?
O46 C46 H46B 109.9 . . ?
C52 C51 H51 106.7 . . ?
O55 C51 H51 106.7 . . ?
O55 C51 C52 112.4(16) . . ?
O55 C51 O64 106(2) . . ?
O64 C51 H51 106.7 . . ?
O64 C51 C52 118(2) . . ?
C51 C52 H52 114.4 . . ?
C51 C52 K1 159.5(13) . 10_566 ?
C53 C52 C51 93.5(19) . . ?
C53 C52 H52 114.4 . . ?
C53 C52 K1 99.3(14) . 10_566 ?
K1 C52 H52 74.6 10_566 . ?
O52 C52 C51 103.1(19) . . ?
O52 C52 H52 114.4 . . ?
O52 C52 C53 114.8(16) . . ?
O52 C52 K1 57.0(11) . 10_566 ?
C52 C53 H53 118.2 . . ?
C52 C53 C54 110.4(18) . . ?
C52 C53 O53 93.7(19) . . ?
C54 C53 H53 118.2 . . ?
O53 C53 H53 118.2 . . ?
O53 C53 C54 93.0(19) . . ?
C53 C54 H54 114.6 . . ?
C55 C54 C53 100.2(18) . . ?
C55 C54 H54 114.6 . . ?
O54 C54 C53 113(2) . . ?
O54 C54 H54 114.6 . . ?
O54 C54 C55 98(2) . . ?
C54 C55 H55 107.2 . . ?
C56 C55 C54 119(2) . . ?
C56 C55 H55 107.2 . . ?
C56 C55 O55 110(2) . . ?
O55 C55 C54 105.3(17) . . ?
O55 C55 H55 107.2 . . ?
C55 C56 H56A 112.6 . . ?
C55 C56 H56B 112.6 . . ?
H56A C56 H56B 110.1 . . ?
O56 C56 C55 96(2) . . ?
O56 C56 H56A 112.6 . . ?
O56 C56 H56B 112.6 . . ?
C62 C61 H61 114.8 . . ?
C62 C61 K1 109(2) . 9_565 ?
K1 C61 H61 73.3 9_565 . ?
O65 C61 H61 114.8 . . ?
O65 C61 C62 121(3) . . ?
O65 C61 K1 59.4(16) . 9_565 ?
O65 C61 O74 99(3) . . ?
O74 C61 H61 114.8 . . ?
O74 C61 C62 87(2) . . ?
O74 C61 K1 157(2) . 9_565 ?
C61 C62 H62 107.9 . . ?
C61 C62 C63 109(2) . . ?
C63 C62 H62 107.9 . . ?
O62 C62 C61 112(2) . . ?
O62 C62 H62 107.9 . . ?
O62 C62 C63 112(3) . . ?
C62 C63 H63 115.8 . . ?
C64 C63 C62 110(2) . . ?
C64 C63 H63 115.8 . . ?
O63 C63 C62 95(2) . . ?
O63 C63 H63 115.8 . . ?
O63 C63 C64 102(2) . . ?
C63 C64 H64 113.6 . . ?
C63 C64 C65 106(2) . . ?
C65 C64 H64 113.6 . . ?
O64 C64 C63 96(2) . . ?
O64 C64 H64 113.6 . . ?
O64 C64 C65 112(3) . . ?
C64 C65 H65 107.9 . . ?
C66 C65 C64 114(3) . . ?
C66 C65 H65 107.9 . . ?
O65 C65 C64 112(2) . . ?
O65 C65 H65 107.9 . . ?
O65 C65 C66 107(3) . . ?
C65 C66 H66A 112.5 . . ?
C65 C66 H66B 112.5 . . ?
H66A C66 H66B 110.1 . . ?
O66 C66 C65 96(2) . . ?
O66 C66 H66A 112.5 . . ?
O66 C66 H66B 112.5 . . ?
C72 C71 H71 102.4 . . ?
O4 C71 H71 102.4 . . ?
O4 C71 C72 108(2) . . ?
O75 C71 H71 102.4 . . ?
O75 C71 C72 122(2) . . ?
O75 C71 O4 116(2) . . ?
C71 C72 H72 111.7 . . ?
C71 C72 C73 99(2) . . ?
C71 C72 O72 110(2) . . ?
C73 C72 H72 111.7 . . ?
O72 C72 H72 111.7 . . ?
O72 C72 C73 112(2) . . ?
C72 C73 H73 100.9 . . ?
C74 C73 C72 120(3) . . ?
C74 C73 H73 100.9 . . ?
O73 C73 C72 109(2) . . ?
O73 C73 H73 100.9 . . ?
O73 C73 C74 121(2) . . ?
C73 C74 H74 97.0 . . ?
C73 C74 O74 113(2) . . ?
C75 C74 C73 116(2) . . ?
C75 C74 H74 97.0 . . ?
C75 C74 O74 127(2) . . ?
O74 C74 H74 97.0 . . ?
C74 C75 H75 103.0 . . ?
C74 C75 O75 116(2) . . ?
C76 C75 C74 116.7(17) . . ?
C76 C75 H75 103.1 . . ?
C76 C75 O75 112.1(19) . . ?
O75 C75 H75 103.1 . . ?
C75 C76 H76A 107.0 . . ?
C75 C76 H76B 107.0 . . ?
H76A C76 H76B 106.7 . . ?
O76 C76 C75 122(2) . . ?
O76 C76 H76A 107.0 . . ?
O76 C76 H76B 107.0 . . ?
C61 K1 C52 109.3(8) 14_654 10_566 ?
O12 K1 C52 130.9(7) . 10_566 ?
O12 K1 C61 104.7(8) . 14_654 ?
O12 K1 O13 56.7(6) . . ?
O12 K1 O45 88.9(6) . 15_664 ?
O12 K1 O46 72.8(7) . 15_664 ?
O12 K1 O52 131.6(7) . 10_566 ?
O12 K1 O53 94.4(7) . 10_566 ?
O13 K1 C52 115.2(6) . 10_566 ?
O13 K1 C61 59.4(7) . 14_654 ?
O13 K1 O53 113.5(7) . 10_566 ?
O45 K1 C52 95.3(7) 15_664 10_566 ?
O45 K1 C61 129.9(9) 15_664 14_654 ?
O45 K1 O13 143.8(6) 15_664 . ?
O45 K1 O53 77.0(7) 15_664 10_566 ?
O46 K1 C52 150.1(7) 15_664 10_566 ?
O46 K1 C61 74.7(8) 15_664 14_654 ?
O46 K1 O13 92.7(7) 15_664 . ?
O46 K1 O45 63.6(7) 15_664 15_664 ?
O46 K1 O53 138.4(7) 15_664 10_566 ?
O52 K1 C52 25.7(4) 10_566 10_566 ?
O52 K1 C61 86.3(8) 10_566 14_654 ?
O52 K1 O13 93.9(6) 10_566 . ?
O52 K1 O45 119.9(7) 10_566 15_664 ?
O52 K1 O46 153.0(6) 10_566 15_664 ?
O52 K1 O53 60.5(6) 10_566 10_566 ?
O53 K1 C52 40.4(6) 10_566 10_566 ?
O53 K1 C61 146.3(9) 10_566 14_654 ?
O65 K1 C52 106.2(7) 14_654 10_566 ?
O65 K1 C61 27.2(5) 14_654 14_654 ?
O65 K1 O12 119.9(8) 14_654 . ?
O65 K1 O13 85.7(8) 14_654 . ?
O65 K1 O45 105.0(8) 14_654 15_664 ?
O65 K1 O46 63.3(7) 14_654 15_664 ?
O65 K1 O52 91.1(6) 14_654 10_566 ?
O65 K1 O53 145.6(8) 14_654 10_566 ?
O66 K1 C52 62.0(7) 14_654 10_566 ?
O66 K1 C61 81.5(8) 14_654 14_654 ?
O66 K1 O12 159.2(8) 14_654 . ?
O66 K1 O13 138.2(7) 14_654 . ?
O66 K1 O45 72.5(6) 14_654 15_664 ?
O66 K1 O46 90.2(7) 14_654 15_664 ?
O66 K1 O52 67.8(7) 14_654 10_566 ?
O66 K1 O53 90.4(7) 14_654 10_566 ?
O66 K1 O65 58.9(8) 14_654 14_654 ?
C6 K2 C6 72.0(12) 17_655 . ?
O5 K2 C6 85.2(7) 17_655 . ?
O5 K2 C6 42.2(6) 17_655 17_655 ?
O5 K2 C6 42.2(7) . . ?
O5 K2 C6 85.1(7) . 17_655 ?
O5 K2 O5 118.7(9) . 17_655 ?
O5 K2 O72 83.2(6) . 6_556 ?
O5 K2 O72 115.5(6) . 14_654 ?
O5 K2 O72 115.5(6) 17_655 6_556 ?
O5 K2 O72 83.2(6) 17_655 14_654 ?
O5 K2 O73 81.7(6) . 14_654 ?
O5 K2 O73 134.6(6) 17_655 14_654 ?
O5 K2 O73 134.6(6) . 6_556 ?
O5 K2 O73 81.7(6) 17_655 6_556 ?
O6 K2 C6 82.4(9) . 17_655 ?
O6 K2 C6 25.2(6) . . ?
O6 K2 C6 82.4(9) 17_655 . ?
O6 K2 C6 25.2(7) 17_655 17_655 ?
O6 K2 O5 77.4(6) 17_655 . ?
O6 K2 O5 64.3(7) 17_655 17_655 ?
O6 K2 O5 77.4(6) . 17_655 ?
O6 K2 O5 64.3(7) . . ?
O6 K2 O6 100.3(11) 17_655 . ?
O6 K2 O72 156.2(7) . 14_654 ?
O6 K2 O72 58.4(6) . 6_556 ?
O6 K2 O72 156.3(7) 17_655 6_556 ?
O6 K2 O72 58.4(6) 17_655 14_654 ?
O6 K2 O73 84.2(7) 17_655 14_654 ?
O6 K2 O73 143.4(7) 17_655 6_556 ?
O6 K2 O73 143.4(7) . 14_654 ?
O6 K2 O73 84.2(7) . 6_556 ?
O72 K2 C6 74.0(8) 14_654 17_655 ?
O72 K2 C6 74.0(8) 6_556 . ?
O72 K2 C6 140.3(8) 14_654 . ?
O72 K2 C6 140.3(8) 6_556 17_655 ?
O72 K2 O72 144.4(9) 14_654 6_556 ?
O73 K2 C6 123.9(6) 6_556 17_655 ?
O73 K2 C6 109.1(8) 6_556 . ?
O73 K2 C6 123.9(6) 14_654 . ?
O73 K2 C6 109.1(8) 14_654 17_655 ?
O73 K2 O72 51.8(6) 14_654 14_654 ?
O73 K2 O72 106.5(7) 14_654 6_556 ?
O73 K2 O72 106.5(6) 6_556 14_654 ?
O73 K2 O72 51.8(6) 6_556 6_556 ?
O73 K2 O73 113.7(9) 14_654 6_556 ?
C32 K3 C32 142.9(16) 5_766 15_664 ?
O25 K3 C32 106.5(8) . 15_664 ?
O25 K3 C32 95.1(9) 18_545 15_664 ?
O25 K3 C32 95.1(9) . 5_766 ?
O25 K3 C32 106.5(8) 18_545 5_766 ?
O25 K3 O25 108.0(10) 18_545 . ?
O26 K3 C32 135.2(9) 18_545 15_664 ?
O26 K3 C32 81.2(9) 18_545 5_766 ?
O26 K3 C32 135.2(9) . 5_766 ?
O26 K3 C32 81.2(9) . 15_664 ?
O26 K3 O25 53.1(7) 18_545 18_545 ?
O26 K3 O25 64.7(7) 18_545 . ?
O26 K3 O25 64.7(7) . 18_545 ?
O26 K3 O25 53.1(7) . . ?
O26 K3 O26 57.9(9) 18_545 . ?
O26 K3 O33 103.8(7) 18_545 5_766 ?
O26 K3 O33 103.8(7) . 15_664 ?
O26 K3 O33 126.8(7) 18_545 15_664 ?
O26 K3 O33 126.8(7) . 5_766 ?
O32 K3 C32 133.3(9) 5_766 15_664 ?
O32 K3 C32 133.3(9) 15_664 5_766 ?
O32 K3 C32 25.4(6) 15_664 15_664 ?
O32 K3 C32 25.4(6) 5_766 5_766 ?
O32 K3 O25 117.1(7) 5_766 . ?
O32 K3 O25 117.1(7) 15_664 18_545 ?
O32 K3 O25 86.9(7) 5_766 18_545 ?
O32 K3 O25 86.9(7) 15_664 . ?
O32 K3 O26 138.7(8) 5_766 . ?
O32 K3 O26 81.3(7) 5_766 18_545 ?
O32 K3 O26 138.7(8) 15_664 18_545 ?
O32 K3 O26 81.3(7) 15_664 . ?
O32 K3 O32 140.0(11) 5_766 15_664 ?
O32 K3 O33 95.4(8) 15_664 5_766 ?
O32 K3 O33 65.0(7) 15_664 15_664 ?
O32 K3 O33 65.0(7) 5_766 5_766 ?
O32 K3 O33 95.4(8) 5_766 15_664 ?
O33 K3 C32 42.1(8) 15_664 15_664 ?
O33 K3 C32 42.1(8) 5_766 5_766 ?
O33 K3 C32 115.9(9) 15_664 5_766 ?
O33 K3 C32 115.9(9) 5_766 15_664 ?
O33 K3 O25 147.4(6) 5_766 18_545 ?
O33 K3 O25 73.8(6) 5_766 . ?
O33 K3 O25 73.8(6) 15_664 18_545 ?
O33 K3 O25 147.4(6) 15_664 . ?
O33 K3 O33 122.8(10) 15_664 5_766 ?
C2 O2 H2A 109.5 . . ?
C3 O3 H3A 109.5 . . ?
C4 O4 C71 117.4(17) . . ?
C1 O5 K2 104.6(13) . . ?
C5 O5 C1 128.1(16) . . ?
C5 O5 K2 106.9(18) . . ?
C6 O6 K2 107(2) . . ?
C6 O6 H6 109.5 . . ?
K2 O6 H6 142.8 . . ?
C12 O12 K1 118.2(16) . . ?
C12 O12 H12A 109.5 . . ?
K1 O12 H12A 112.0 . . ?
C13 O13 K1 116.4(13) . . ?
C13 O13 H13A 109.5 . . ?
K1 O13 H13A 133.8 . . ?
C1 O14 C14 113.5(15) . . ?
C11 O15 C15 116.0(16) . . ?
C16 O16 H16 109.5 . . ?
C22 O22 H22A 109.5 . . ?
C23 O23 H23A 109.5 . . ?
C11 O24 C24 122(2) . . ?
C21 O25 C25 110(2) . . ?
C21 O25 K3 116.1(19) . . ?
C25 O25 K3 120.3(19) . . ?
C26 O26 K3 129.7(17) . . ?
C26 O26 H26 109.5 . . ?
K3 O26 H26 106.5 . . ?
C32 O32 K3 102.8(19) . 8_655 ?
C32 O32 H32A 109.5 . . ?
K3 O32 H32A 9.1 8_655 . ?
C33 O33 K3 115(2) . 8_655 ?
C33 O33 H33A 109.5 . . ?
K3 O33 H33A 119.0 8_655 . ?
C21 O34 C34 110(2) . . ?
C31 O35 C35 118.4(12) . . ?
C36 O36 H36 109.5 . . ?
C42 O42 H42A 109.5 . . ?
C43 O43 H43A 109.5 . . ?
C44 O44 C31 120.1(16) . . ?
C41 O45 C45 117(2) . . ?
C41 O45 K1 110.8(18) . 8_655 ?
C45 O45 K1 109.5(18) . 8_655 ?
C46 O46 K1 109.9(15) . 8_655 ?
C46 O46 H46 109.5 . . ?
K1 O46 H46 85.6 8_655 . ?
C52 O52 K1 97.3(13) . 10_566 ?
C52 O52 H52A 109.5 . . ?
K1 O52 H52A 31.1 10_566 . ?
C53 O53 K1 116.3(13) . 10_566 ?
C53 O53 H53A 109.5 . . ?
K1 O53 H53A 133.0 10_566 . ?
C54 O54 C41 117.1(16) . . ?
C51 O55 C55 110.9(18) . . ?
C56 O56 H56 109.5 . . ?
C62 O62 H62A 109.5 . . ?
C63 O63 H63A 109.5 . . ?
C64 O64 C51 112(2) . . ?
C61 O65 K1 93.5(19) . 9_565 ?
C65 O65 C61 119(2) . . ?
C65 O65 K1 114.6(19) . 9_565 ?
C66 O66 K1 121.0(19) . 9_565 ?
C66 O66 H66 109.5 . . ?
K1 O66 H66 128.8 9_565 . ?
C72 O72 K2 113.0(16) . 9_565 ?
C72 O72 H72A 109.5 . . ?
K2 O72 H72A 11.3 9_565 . ?
C73 O73 K2 129.3(16) . 9_565 ?
C73 O73 H73A 109.5 . . ?
K2 O73 H73A 116.1 9_565 . ?
C61 O74 C74 121(3) . . ?
C71 O75 C75 112(2) . . ?
C76 O76 H76 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -61(3) . . . . ?
C1 C2 C3 O3 168(2) . . . . ?
C2 C1 O5 C5 -35(3) . . . . ?
C2 C1 O5 K2 90.3(14) . . . . ?
C2 C1 O14 C14 -147.8(17) . . . . ?
C2 C3 C4 C5 49(3) . . . . ?
C2 C3 C4 O4 176(2) . . . . ?
C3 C4 C5 C6 -165(3) . . . . ?
C3 C4 C5 O5 -38(4) . . . . ?
C3 C4 O4 C71 148(2) . . . . ?
C4 C5 C6 K2 94(3) . . . . ?
C4 C5 C6 O6 50(4) . . . . ?
C4 C5 O5 C1 37(4) . . . . ?
C4 C5 O5 K2 -88(3) . . . . ?
C5 C4 O4 C71 -92(3) . . . . ?
C5 C6 O6 K2 68(3) . . . . ?
C6 C5 O5 C1 176(2) . . . . ?
C6 C5 O5 K2 51(2) . . . . ?
C11 C12 C13 C14 -41(4) . . . . ?
C11 C12 C13 O13 -179(2) . . . . ?
C11 C12 O12 K1 174(2) . . . . ?
C12 C11 O15 C15 -71(3) . . . . ?
C12 C11 O24 C24 -126(2) . . . . ?
C12 C13 C14 C15 42(4) . . . . ?
C12 C13 C14 O14 180(2) . . . . ?
C12 C13 O13 K1 -19(3) . . . . ?
C13 C12 O12 K1 -65(3) . . . . ?
C13 C14 C15 C16 -156(3) . . . . ?
C13 C14 C15 O15 -46(3) . . . . ?
C13 C14 O14 C1 97(3) . . . . ?
C14 C13 O13 K1 -155.9(19) . . . . ?
C14 C15 C16 O16 58(3) . . . . ?
C14 C15 O15 C11 61(3) . . . . ?
C15 C14 O14 C1 -120(2) . . . . ?
C16 C15 O15 C11 -177(2) . . . . ?
C21 C22 C23 C24 -50(4) . . . . ?
C21 C22 C23 O23 -163(3) . . . . ?
C22 C21 O25 C25 -75(3) . . . . ?
C22 C21 O25 K3 67(3) . . . . ?
C22 C21 O34 C34 -106(3) . . . . ?
C22 C23 C24 C25 43(5) . . . . ?
C22 C23 C24 O24 -163(3) . . . . ?
C23 C24 C25 C26 -165(3) . . . . ?
C23 C24 C25 O25 -42(4) . . . . ?
C23 C24 O24 C11 128(3) . . . . ?
C24 C25 C26 O26 87(3) . . . . ?
C24 C25 O25 C21 58(3) . . . . ?
C24 C25 O25 K3 -81(2) . . . . ?
C25 C24 O24 C11 -79(4) . . . . ?
C25 C26 O26 K3 10(4) . . . . ?
C26 C25 O25 C21 -170(3) . . . . ?
C26 C25 O25 K3 51(3) . . . . ?
C31 C32 C33 C34 -41(4) . . . . ?
C31 C32 C33 O33 -166(3) . . . . ?
C31 C32 O32 K3 169(2) . . . 8_655 ?
C32 C31 O35 C35 -45(4) . . . . ?
C32 C31 O44 C44 -98(3) . . . . ?
C32 C33 C34 C35 69(4) . . . . ?
C32 C33 C34 O34 169(3) . . . . ?
C32 C33 O33 K3 -29(3) . . . 8_655 ?
C33 C32 O32 K3 -64(4) . . . 8_655 ?
C33 C34 C35 C36 165(3) . . . . ?
C33 C34 C35 O35 -70(3) . . . . ?
C33 C34 O34 C21 101(3) . . . . ?
C34 C33 O33 K3 -142(3) . . . 8_655 ?
C34 C35 C36 O36 42(4) . . . . ?
C34 C35 O35 C31 52(3) . . . . ?
C35 C34 O34 C21 -137(2) . . . . ?
C36 C35 O35 C31 -178.0(19) . . . . ?
C41 C42 C43 C44 -35(4) . . . . ?
C41 C42 C43 O43 -168(2) . . . . ?
C42 C41 O45 C45 -47(4) . . . . ?
C42 C41 O45 K1 80(3) . . . 8_655 ?
C42 C41 O54 C54 -116(2) . . . . ?
C42 C43 C44 C45 39(4) . . . . ?
C42 C43 C44 O44 172(2) . . . . ?
C43 C44 C45 C46 -172(2) . . . . ?
C43 C44 C45 O45 -39(3) . . . . ?
C43 C44 O44 C31 94(3) . . . . ?
C44 C45 C46 O46 63(3) . . . . ?
C44 C45 O45 C41 44(3) . . . . ?
C44 C45 O45 K1 -83(2) . . . 8_655 ?
C45 C44 O44 C31 -130(3) . . . . ?
C45 C46 O46 K1 48(2) . . . 8_655 ?
C46 C45 O45 C41 -179(2) . . . . ?
C46 C45 O45 K1 54(3) . . . 8_655 ?
C51 C52 C53 C54 -76(2) . . . . ?
C51 C52 C53 O53 -170.3(18) . . . . ?
C51 C52 O52 K1 174.8(17) . . . 10_566 ?
C52 C51 O55 C55 -65(3) . . . . ?
C52 C51 O64 C64 -115(2) . . . . ?
C52 C53 C54 C55 80(2) . . . . ?
C52 C53 C54 O54 -176(2) . . . . ?
C52 C53 O53 K1 -32.8(19) . . . 10_566 ?
C53 C52 O52 K1 -85(2) . . . 10_566 ?
C53 C54 C55 C56 173(2) . . . . ?
C53 C54 C55 O55 -63(2) . . . . ?
C53 C54 O54 C41 128(2) . . . . ?
C54 C53 O53 K1 -143.4(14) . . . 10_566 ?
C54 C55 C56 O56 44(3) . . . . ?
C54 C55 O55 C51 60(3) . . . . ?
C55 C54 O54 C41 -127(2) . . . . ?
C56 C55 O55 C51 -170(2) . . . . ?
C61 C62 C63 C64 -51(3) . . . . ?
C61 C62 C63 O63 -156(3) . . . . ?
C62 C61 O65 C65 -26(5) . . . . ?
C62 C61 O65 K1 95(3) . . . 9_565 ?
C62 C61 O74 C74 -143(2) . . . . ?
C62 C63 C64 C65 67(3) . . . . ?
C62 C63 C64 O64 -178(2) . . . . ?
C63 C64 C65 C66 178(3) . . . . ?
C63 C64 C65 O65 -60(4) . . . . ?
C63 C64 O64 C51 132(2) . . . . ?
C64 C65 C66 O66 56(3) . . . . ?
C64 C65 O65 C61 40(4) . . . . ?
C64 C65 O65 K1 -69(3) . . . 9_565 ?
C65 C64 O64 C51 -117(3) . . . . ?
C65 C66 O66 K1 56(3) . . . 9_565 ?
C66 C65 O65 C61 166(3) . . . . ?
C66 C65 O65 K1 57(3) . . . 9_565 ?
C71 C72 C73 C74 -49(4) . . . . ?
C71 C72 C73 O73 166(2) . . . . ?
C71 C72 O72 K2 -167.0(19) . . . 9_565 ?
C72 C71 O4 C4 -114(3) . . . . ?
C72 C71 O75 C75 -57(4) . . . . ?
C72 C73 C74 C75 34(4) . . . . ?
C72 C73 C74 O74 -168(2) . . . . ?
C72 C73 O73 K2 -19(4) . . . 9_565 ?
C73 C72 O72 K2 -58(3) . . . 9_565 ?
C73 C74 C75 C76 -156(3) . . . . ?
C73 C74 C75 O75 -20(4) . . . . ?
C73 C74 O74 C61 104(3) . . . . ?
C74 C73 O73 K2 -164(2) . . . 9_565 ?
C74 C75 C76 O76 57(4) . . . . ?
C74 C75 O75 C71 28(3) . . . . ?
C75 C74 O74 C61 -100(4) . . . . ?
C76 C75 O75 C71 166(2) . . . . ?
K1 C52 C53 C54 120.3(18) 10_566 . . . ?
K1 C52 C53 O53 25.7(15) 10_566 . . . ?
K1 C61 C62 C63 95(3) 9_565 . . . ?
K1 C61 C62 O62 -141(2) 9_565 . . . ?
K1 C61 O65 C65 -121(3) 9_565 . . . ?
K1 C61 O74 C74 80(6) 9_565 . . . ?
K3 C32 C33 C34 148(2) 8_655 . . . ?
K3 C32 C33 O33 23(3) 8_655 . . . ?
O2 C2 C3 C4 -177(2) . . . . ?
O2 C2 C3 O3 52(3) . . . . ?
O3 C3 C4 C5 -177(2) . . . . ?
O3 C3 C4 O4 -50(3) . . . . ?
O4 C4 C5 C6 77(4) . . . . ?
O4 C4 C5 O5 -155(2) . . . . ?
O4 C71 C72 C73 -76(3) . . . . ?
O4 C71 C72 O72 42(3) . . . . ?
O4 C71 O75 C75 79(3) . . . . ?
O5 C1 C2 C3 46(3) . . . . ?
O5 C1 C2 O2 167.5(18) . . . . ?
O5 C1 O14 C14 114.1(18) . . . . ?
O5 C5 C6 K2 -39.9(19) . . . . ?
O5 C5 C6 O6 -83(3) . . . . ?
O12 C12 C13 C14 -171(2) . . . . ?
O12 C12 C13 O13 50(4) . . . . ?
O13 C13 C14 C15 179(2) . . . . ?
O13 C13 C14 O14 -43(3) . . . . ?
O14 C1 C2 C3 -50(3) . . . . ?
O14 C1 C2 O2 72(2) . . . . ?
O14 C1 O5 C5 70(3) . . . . ?
O14 C1 O5 K2 -163.9(11) . . . . ?
O14 C14 C15 C16 67(3) . . . . ?
O14 C14 C15 O15 177.0(18) . . . . ?
O15 C11 C12 C13 54(3) . . . . ?
O15 C11 C12 O12 173(3) . . . . ?
O15 C11 O24 C24 119(3) . . . . ?
O15 C15 C16 O16 -51(3) . . . . ?
O22 C22 C23 C24 -170(3) . . . . ?
O22 C22 C23 O23 77(4) . . . . ?
O23 C23 C24 C25 161(3) . . . . ?
O23 C23 C24 O24 -45(5) . . . . ?
O24 C11 C12 C13 -67(3) . . . . ?
O24 C11 C12 O12 52(3) . . . . ?
O24 C11 O15 C15 39(4) . . . . ?
O24 C24 C25 C26 41(4) . . . . ?
O24 C24 C25 O25 164(3) . . . . ?
O25 C21 C22 C23 64(3) . . . . ?
O25 C21 C22 O22 175(2) . . . . ?
O25 C21 O34 C34 127(3) . . . . ?
O25 C25 C26 O26 -37(4) . . . . ?
O32 C32 C33 C34 -167(3) . . . . ?
O32 C32 C33 O33 68(5) . . . . ?
O33 C33 C34 C35 180(3) . . . . ?
O33 C33 C34 O34 -80(4) . . . . ?
O34 C21 C22 C23 -66(3) . . . . ?
O34 C21 C22 O22 45(4) . . . . ?
O34 C21 O25 C25 54(3) . . . . ?
O34 C21 O25 K3 -164.8(18) . . . . ?
O34 C34 C35 C36 57(3) . . . . ?
O34 C34 C35 O35 -177.8(19) . . . . ?
O35 C31 C32 C33 36(4) . . . . ?
O35 C31 C32 K3 -166(4) . . . 8_655 ?
O35 C31 C32 O32 174(2) . . . . ?
O35 C31 O44 C44 141(2) . . . . ?
O35 C35 C36 O36 -75(3) . . . . ?
O42 C42 C43 C44 -176(2) . . . . ?
O42 C42 C43 O43 52(4) . . . . ?
O43 C43 C44 C45 167(2) . . . . ?
O43 C43 C44 O44 -60(4) . . . . ?
O44 C31 C32 C33 -61(3) . . . . ?
O44 C31 C32 K3 97(6) . . . 8_655 ?
O44 C31 C32 O32 76(3) . . . . ?
O44 C31 O35 C35 73(3) . . . . ?
O44 C44 C45 C46 45(3) . . . . ?
O44 C44 C45 O45 179(2) . . . . ?
O45 C41 C42 C43 39(4) . . . . ?
O45 C41 C42 O42 -180(3) . . . . ?
O45 C41 O54 C54 113(2) . . . . ?
O45 C45 C46 O46 -71(3) . . . . ?
O52 C52 C53 C54 178(2) . . . . ?
O52 C52 C53 O53 84(2) . . . . ?
O53 C53 C54 C55 175(2) . . . . ?
O53 C53 C54 O54 -81(2) . . . . ?
O54 C41 C42 C43 -83(3) . . . . ?
O54 C41 C42 O42 59(3) . . . . ?
O54 C41 O45 C45 76(3) . . . . ?
O54 C41 O45 K1 -157.6(15) . . . 8_655 ?
O54 C54 C55 C56 58(3) . . . . ?
O54 C54 C55 O55 -177.9(18) . . . . ?
O55 C51 C52 C53 66(3) . . . . ?
O55 C51 C52 K1 -165(4) . . . 10_566 ?
O55 C51 C52 O52 -178(2) . . . . ?
O55 C51 O64 C64 118(2) . . . . ?
O55 C55 C56 O56 -78(3) . . . . ?
O62 C62 C63 C64 -176(2) . . . . ?
O62 C62 C63 O63 80(3) . . . . ?
O63 C63 C64 C65 167(3) . . . . ?
O63 C63 C64 O64 -78(3) . . . . ?
O64 C51 C52 C53 -58(2) . . . . ?
O64 C51 C52 K1 71(6) . . . 10_566 ?
O64 C51 C52 O52 59(3) . . . . ?
O64 C51 O55 C55 65(3) . . . . ?
O64 C64 C65 C66 74(4) . . . . ?
O64 C64 C65 O65 -164(2) . . . . ?
O65 C61 C62 C63 30(4) . . . . ?
O65 C61 C62 O62 155(3) . . . . ?
O65 C61 O74 C74 96(3) . . . . ?
O65 C65 C66 O66 -68(3) . . . . ?
O72 C72 C73 C74 -165(3) . . . . ?
O72 C72 C73 O73 50(3) . . . . ?
O73 C73 C74 C75 175(3) . . . . ?
O73 C73 C74 O74 -28(4) . . . . ?
O74 C61 C62 C63 -69(3) . . . . ?
O74 C61 C62 O62 56(3) . . . . ?
O74 C61 O65 C65 66(3) . . . . ?
O74 C61 O65 K1 -172.8(19) . . . 9_565 ?
O74 C74 C75 C76 50(4) . . . . ?
O74 C74 C75 O75 -174(2) . . . . ?
O75 C71 C72 C73 63(4) . . . . ?
O75 C71 C72 O72 -179(3) . . . . ?
O75 C71 O4 C4 104(3) . . . . ?
O75 C75 C76 O76 -80(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.410 -0.380 -0.217 21262.9 1470.3 ?


_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_0_41GPa
_database_code_depnum_ccdc_archive 'CCDC 1529147'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7

# start Validation Reply Form
_vrf_THETM01_CDMOF_a_0_41GPa     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_REFNR01_CDMOF_a_0_41GPa     
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT029_CDMOF_a_0_41GPa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.717 Note  
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT201_CDMOF_a_0_41GPa     
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT241_CDMOF_a_0_41GPa     
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O4 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT242_CDMOF_a_0_41GPa     
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C11 Check 
RESPONSE: 'Poor data quality'
;
_vrf_PLAT306_CDMOF_a_0_41GPa     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_0_41GPa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.033 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_CDMOF_a_0_41GPa     
;
PROBLEM: D-H Without Acceptor       O16    --  H16    ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
# end Validation Reply Form

# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0030 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2030 0.2500 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   31.238(2)
_cell_length_b                   31.238(2)
_cell_length_c                   31.238(2)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30481(4)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    1027
_cell_measurement_temperature    295
_cell_measurement_theta_max      8.5420
_cell_measurement_theta_min      1.9920
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88316
_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_absorpt_special_details   ?
# EXPERIMENTAL DATA 
_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.16GPa and then
compressed to 0.41GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.921
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8928
_exptl_crystal_preparation       ?
_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          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.717
_diffrn_reflns_Laue_measured_fraction_max 0.716
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2510
_diffrn_reflns_point_group_measured_fraction_full 0.697
_diffrn_reflns_point_group_measured_fraction_max 0.697
_diffrn_reflns_theta_full        13.249
_diffrn_reflns_theta_max         13.249
_diffrn_reflns_theta_min         1.787
_diffrn_ambient_temperature      295
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         410000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.717
_diffrn_measured_fraction_theta_max 0.716
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 155.77  155
  2  ω   -105.00 -74.00   0.20    0.70    --   15.00  70.00 -24.23  155
  3  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00-155.77  200
  4  ω   -106.00 -66.00   0.20    0.70    --  -15.00 -70.00  24.23  200
  5  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 -24.23  280
  6  ω   -150.00 -94.00   0.20    0.70    --  -15.00  70.00 155.77  280
  7  ω    -96.00 -30.00   0.20    0.70    --   15.00 -70.00  24.23  330
  8  ω    -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       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0000867000
_diffrn_orient_matrix_UB_12      0.0217333000
_diffrn_orient_matrix_UB_13      -0.0038172000
_diffrn_orient_matrix_UB_21      0.0189471000
_diffrn_orient_matrix_UB_22      -0.0018735000
_diffrn_orient_matrix_UB_23      -0.0111495000
_diffrn_orient_matrix_UB_31      -0.0112953000
_diffrn_orient_matrix_UB_32      -0.0033232000
_diffrn_orient_matrix_UB_33      -0.0186197000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_source                   synchrotron
_diffrn_special_details          
'high-pressure measurement with diamond-anvil cell at 0.41 GPa'
_reflns_Friedel_coverage         0.550
_reflns_Friedel_fraction_full    0.664
_reflns_Friedel_fraction_max     0.664
_reflns_number_gt                288
_reflns_number_total             558
_reflns_odcompleteness_completeness 75.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.25
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.126
_refine_diff_density_min         -0.109
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details 
;
 Flack x determined using 64 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.39(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         558
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0922
_refine_ls_restrained_S_all      1.298
_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/[σ²(Fo²)+(0.1624P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2328
_refine_ls_wR_factor_ref         0.2494
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
 resulting in a low data:parameter ratio.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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
 C6-C5
 1.5 with sigma of 0.005
 C5-C1
 2.3 with sigma of 0.005
 C2-C5
 3 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.005
 C4-O4
 1.45 with sigma of 0.005
 C4-C5
 1.5 with sigma of 0.005
 C1-C4
 3 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.005
 C4-C3
 1.5 with sigma of 0.005
 C2-O3
 2.3 with sigma of 0.02
 C2-O2
 1.45 with sigma of 0.005
 O3-C3
 1.45 with sigma of 0.005
 O2-C3
 2.2 with sigma of 0.02
 C14-C13
 1.5 with sigma of 0.005
 O14-C14
 1.5 with sigma of 0.01
 O14-C13
 2.4 with sigma of 0.02
 O4-C12
 2.2 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.005
 O13-C13
 1.45 with sigma of 0.005
 O13-C14
 2.5 with sigma of 0.02
 O14-C15
 2.4 with sigma of 0.02
 C15-C14
 1.5 with sigma of 0.005
 C14-C15
 1.5 with sigma of 0.005
 C12-C15
 3 with sigma of 0.02
 C16-C15
 1.5 with sigma of 0.005
 C16-O16
 1.45 with sigma of 0.005
 C11-O4
 1.45 with sigma of 0.005
 C11-C14
 3 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.005
 C12-O12
 1.45 with sigma of 0.005
 C6-O6
 1.45 with sigma of 0.005
 O5-C5
 1.45 with sigma of 0.005
 O5-C6
 2.5 with sigma of 0.02
 O5-C1
 1.45 with sigma of 0.005
 O5-C3
 3.1 with sigma of 0.02
 O15-C13
 3 with sigma of 0.02
 O15-C15
 1.45 with sigma of 0.005
 O15-C16
 2.2 with sigma of 0.02
 O15-C11
 1.45 with sigma of 0.005
 C1-C5
 2.5 with sigma of 0.02
 C4-C2
 2.5 with sigma of 0.02
 C5-C3
 2.5 with sigma of 0.02
 C3-C1
 2.5 with sigma of 0.02
 O2-C1
 2.5 with sigma of 0.04
 C1-O2
 2.5 with sigma of 0.04
 C13-O14
 2.5 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.02
 O4-C12
 2.5 with sigma of 0.04
 O14-C15
 2.5 with sigma of 0.04
 C13-C15
 2.4 with sigma of 0.02
 C15-O16
 2.5 with sigma of 0.04
 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
 O6-C5
 2.7 with sigma of 0.04
 C5-O6
 2.5 with sigma of 0.04
 C2-O5
 2.5 with sigma of 0.02
 O5-C4
 2.5 with sigma of 0.02
 C14-O15
 2.4 with sigma of 0.02
 O15-C12
 2.4 with sigma of 0.02
3. 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)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3A), C4(H4), C5(H5), C11(H11), C12(H12A), C13(H13A),
 C14(H14), C15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C16(H16B,H16A)
4.c Tetrahedral OH refined with riding coordinates:
 O2(H2), O3(H3), O6(H6), O12(H12), O13(H13), O16(H16)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8508(8) 0.6884(7) 0.6393(10) 0.243(8) Uiso 1 1 d D . . . .
H1 H 0.8460 0.7194 0.6380 0.291 Uiso 1 1 calc R . . . .
C2 C 0.8879(8) 0.6785(6) 0.6681(9) 0.243(8) Uiso 1 1 d D . . . .
H2A H 0.8834 0.6915 0.6963 0.291 Uiso 1 1 calc R . . . .
C3 C 0.8961(7) 0.6314(7) 0.6728(11) 0.243(8) Uiso 1 1 d D . . . .
H3A H 0.9010 0.6285 0.6420 0.291 Uiso 1 1 calc R . . . .
C4 C 0.8572(8) 0.6033(6) 0.6704(11) 0.243(8) Uiso 1 1 d D . . . .
H4 H 0.8460 0.6068 0.6995 0.291 Uiso 1 1 calc R . . . .
C5 C 0.8203(7) 0.6210(7) 0.6450(9) 0.243(8) Uiso 1 1 d D . . . .
H5 H 0.8236 0.6123 0.6151 0.291 Uiso 1 1 calc R . . . .
C6 C 0.7840(10) 0.5961(9) 0.6644(10) 0.243(8) Uiso 1 1 d D . . . .
H6A H 0.7577 0.6071 0.6521 0.291 Uiso 1 1 calc R . . . .
H6B H 0.7868 0.5667 0.6547 0.291 Uiso 1 1 calc R . . . .
C11 C 0.8602(8) 0.5355(6) 0.7107(10) 0.243(8) Uiso 1 1 d D . . . .
H11 H 0.8599 0.5575 0.7330 0.291 Uiso 1 1 calc R . . . .
C12 C 0.9009(8) 0.5117(7) 0.7198(8) 0.243(8) Uiso 1 1 d D . . . .
H12A H 0.9033 0.5069 0.7507 0.291 Uiso 1 1 calc R . . . .
C13 C 0.9016(7) 0.4693(8) 0.6972(10) 0.243(8) Uiso 1 1 d D . . . .
H13A H 0.8909 0.4823 0.6707 0.291 Uiso 1 1 calc R . . . .
C14 C 0.8615(8) 0.4440(6) 0.7024(8) 0.243(8) Uiso 1 1 d D . . . .
H14 H 0.8618 0.4303 0.7306 0.291 Uiso 1 1 calc R . . . .
C15 C 0.8212(6) 0.4697(8) 0.6981(9) 0.243(8) Uiso 1 1 d D . . . .
H15 H 0.8200 0.4776 0.6677 0.291 Uiso 1 1 calc R . . . .
C16 C 0.7759(7) 0.4575(10) 0.7092(10) 0.243(8) Uiso 1 1 d D . . . .
H16B H 0.7582 0.4829 0.7070 0.291 Uiso 1 1 calc R . . . .
H16A H 0.7658 0.4373 0.6878 0.291 Uiso 1 1 calc R . . . .
K1 K 0.8069(3) 0.5000 0.8069(3) 0.311(10) Uani 1 2 d S T P . .
O2 O 0.9285(9) 0.6926(9) 0.6503(10) 0.333(7) Uiso 1 1 d D . . . .
H2 H 0.9250 0.6999 0.6253 0.499 Uiso 1 1 calc R . . . .
O3 O 0.9418(7) 0.6290(9) 0.6812(11) 0.333(7) Uiso 1 1 d D . . . .
H3 H 0.9486 0.6040 0.6855 0.499 Uiso 1 1 calc R . . . .
O4 O 0.8724(10) 0.5594(8) 0.6728(8) 0.333(7) Uiso 1 1 d D . . . .
O5 O 0.8107(7) 0.6663(8) 0.6462(8) 0.333(7) Uiso 1 1 d D . . . .
O6 O 0.7778(9) 0.5947(10) 0.7106(10) 0.333(7) Uiso 1 1 d D . . . .
H6 H 0.7784 0.5698 0.7187 0.499 Uiso 1 1 calc R . . . .
O12 O 0.9366(8) 0.5377(9) 0.7054(9) 0.333(7) Uiso 1 1 d D . . . .
H12 H 0.9591 0.5253 0.7106 0.499 Uiso 1 1 calc R . . . .
O13 O 0.9387(8) 0.4522(10) 0.6752(8) 0.333(7) Uiso 1 1 d D . . . .
H13 H 0.9326 0.4292 0.6643 0.499 Uiso 1 1 calc R . . . .
O14 O 0.8585(9) 0.4098(8) 0.6686(10) 0.333(7) Uiso 1 1 d D . . . .
O15 O 0.8224(7) 0.5102(7) 0.7206(8) 0.333(7) Uiso 1 1 d D . . . .
O16 O 0.7692(10) 0.4386(10) 0.7510(9) 0.333(7) Uiso 1 1 d D . . . .
H16 H 0.7755 0.4131 0.7502 0.499 Uiso 1 1 calc R . . . .
OA O 1.0000 0.5000 0.6785(13) 0.30(2) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.500(7) . ?
C1 O5 1.444(7) . ?
C1 O14 1.67(4) 7_556 ?
C2 H2A 0.9800 . ?
C2 C3 1.500(7) . ?
C2 O2 1.454(7) . ?
C3 H3A 0.9800 . ?
C3 C4 1.503(7) . ?
C3 O3 1.452(7) . ?
C4 H4 0.9800 . ?
C4 C5 1.504(7) . ?
C4 O4 1.454(7) . ?
C5 H5 0.9800 . ?
C5 C6 1.504(7) . ?
C5 O5 1.447(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.454(7) . ?
C11 H11 0.9800 . ?
C11 C12 1.499(7) . ?
C11 O4 1.450(7) . ?
C11 O15 1.453(7) . ?
C12 H12A 0.9800 . ?
C12 C13 1.501(7) . ?
C12 O12 1.453(7) . ?
C13 H13A 0.9800 . ?
C13 C14 1.492(7) . ?
C13 O13 1.449(7) . ?
C14 H14 0.9800 . ?
C14 C15 1.500(5) . ?
C14 O14 1.505(13) . ?
C15 H15 0.9800 . ?
C15 C16 1.504(7) . ?
C15 O15 1.448(7) . ?
C16 H16B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 K1 3.47(3) . ?
C16 O16 1.449(7) . ?
K1 C16 3.47(3) 23_565 ?
K1 O2 2.60(3) 44_666 ?
K1 O2 2.60(3) 41_646 ?
K1 O3 2.73(3) 41_646 ?
K1 O3 2.73(3) 44_666 ?
K1 O15 2.76(3) 23_565 ?
K1 O15 2.76(3) . ?
K1 O16 2.85(3) 23_565 ?
K1 O16 2.85(3) . ?
O2 K1 2.60(3) 42_566 ?
O2 H2 0.8200 . ?
O3 K1 2.73(3) 42_566 ?
O3 H3 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12 0.8200 . ?
O13 H13 0.8200 . ?
O14 C1 1.67(4) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 110.4 . . ?
C2 C1 O14 111(2) . 7_556 ?
O5 C1 H1 110.4 . . ?
O5 C1 C2 118.7(15) . . ?
O5 C1 O14 95(2) . 7_556 ?
O14 C1 H1 110.4 7_556 . ?
C1 C2 H2A 110.1 . . ?
C1 C2 C3 113.3(13) . . ?
C3 C2 H2A 110.1 . . ?
O2 C2 C1 112(2) . . ?
O2 C2 H2A 110.1 . . ?
O2 C2 C3 100.6(14) . . ?
C2 C3 H3A 91.2 . . ?
C2 C3 C4 115.4(12) . . ?
C4 C3 H3A 91.2 . . ?
O3 C3 C2 103.8(15) . . ?
O3 C3 H3A 91.2 . . ?
O3 C3 C4 140.7(17) . . ?
C3 C4 H4 100.0 . . ?
C3 C4 C5 115.6(12) . . ?
C5 C4 H4 100.0 . . ?
O4 C4 C3 107(2) . . ?
O4 C4 H4 100.0 . . ?
O4 C4 C5 129(3) . . ?
C4 C5 H5 108.6 . . ?
C4 C5 C6 100(2) . . ?
C6 C5 H5 108.6 . . ?
O5 C5 C4 120.4(14) . . ?
O5 C5 H5 108.6 . . ?
O5 C5 C6 109.9(16) . . ?
C5 C6 H6A 107.1 . . ?
C5 C6 H6B 107.1 . . ?
H6A C6 H6B 106.8 . . ?
O6 C6 C5 121(2) . . ?
O6 C6 H6A 107.1 . . ?
O6 C6 H6B 107.1 . . ?
C12 C11 H11 102.8 . . ?
O4 C11 H11 102.8 . . ?
O4 C11 C12 100.8(13) . . ?
O4 C11 O15 132(3) . . ?
O15 C11 H11 102.8 . . ?
O15 C11 C12 112.2(13) . . ?
C11 C12 H12A 109.2 . . ?
C11 C12 C13 111.2(13) . . ?
C13 C12 H12A 109.2 . . ?
O12 C12 C11 108.4(18) . . ?
O12 C12 H12A 109.2 . . ?
O12 C12 C13 110(2) . . ?
C12 C13 H13A 91.5 . . ?
C14 C13 C12 113.8(12) . . ?
C14 C13 H13A 91.5 . . ?
O13 C13 C12 124.1(19) . . ?
O13 C13 H13A 91.5 . . ?
O13 C13 C14 121.9(16) . . ?
C13 C14 H14 108.8 . . ?
C13 C14 C15 114.3(13) . . ?
C13 C14 O14 110.7(15) . . ?
C15 C14 H14 108.8 . . ?
C15 C14 O14 105.4(15) . . ?
O14 C14 H14 108.8 . . ?
C14 C15 H15 104.6 . . ?
C14 C15 C16 129(2) . . ?
C16 C15 H15 104.6 . . ?
O15 C15 C14 113.7(13) . . ?
O15 C15 H15 104.6 . . ?
O15 C15 C16 97.8(14) . . ?
C15 C16 H16B 108.2 . . ?
C15 C16 H16A 108.2 . . ?
C15 C16 K1 81.0(13) . . ?
H16B C16 H16A 107.3 . . ?
K1 C16 H16B 84.6 . . ?
K1 C16 H16A 161.0 . . ?
O16 C16 C15 117(2) . . ?
O16 C16 H16B 108.2 . . ?
O16 C16 H16A 108.2 . . ?
O16 C16 K1 53.2(16) . . ?
C16 K1 C16 69.8(9) . 23_565 ?
O2 K1 C16 79.6(9) 44_666 23_565 ?
O2 K1 C16 79.6(9) 41_646 . ?
O2 K1 C16 141.5(9) 44_666 . ?
O2 K1 C16 141.5(9) 41_646 23_565 ?
O2 K1 O2 136.9(15) 44_666 41_646 ?
O2 K1 O3 101.2(10) 44_666 41_646 ?
O2 K1 O3 49.8(8) 41_646 41_646 ?
O2 K1 O3 49.8(8) 44_666 44_666 ?
O2 K1 O3 101.2(10) 41_646 44_666 ?
O2 K1 O15 113.7(7) 44_666 . ?
O2 K1 O15 90.9(7) 44_666 23_565 ?
O2 K1 O15 90.9(7) 41_646 . ?
O2 K1 O15 113.7(7) 41_646 23_565 ?
O2 K1 O16 68.8(9) 41_646 . ?
O2 K1 O16 153.5(11) 44_666 . ?
O2 K1 O16 68.8(9) 44_666 23_565 ?
O2 K1 O16 153.5(11) 41_646 23_565 ?
O3 K1 C16 115.4(7) 44_666 23_565 ?
O3 K1 C16 115.4(7) 41_646 . ?
O3 K1 C16 125.4(8) 41_646 23_565 ?
O3 K1 C16 125.4(8) 44_666 . ?
O3 K1 O3 104.1(14) 44_666 41_646 ?
O3 K1 O15 85.8(8) 41_646 23_565 ?
O3 K1 O15 140.4(7) 41_646 . ?
O3 K1 O15 140.4(7) 44_666 23_565 ?
O3 K1 O15 85.8(8) 44_666 . ?
O3 K1 O16 146.6(9) 44_666 . ?
O3 K1 O16 146.6(9) 41_646 23_565 ?
O3 K1 O16 93.3(8) 41_646 . ?
O3 K1 O16 93.3(8) 44_666 23_565 ?
O15 K1 C16 39.9(5) 23_565 23_565 ?
O15 K1 C16 39.9(5) . . ?
O15 K1 C16 80.6(7) . 23_565 ?
O15 K1 C16 80.6(7) 23_565 . ?
O15 K1 O15 110.9(10) . 23_565 ?
O15 K1 O16 68.0(8) 23_565 . ?
O15 K1 O16 63.3(8) 23_565 23_565 ?
O15 K1 O16 63.3(8) . . ?
O15 K1 O16 68.0(8) . 23_565 ?
O16 K1 C16 73.9(8) 23_565 . ?
O16 K1 C16 24.1(4) . . ?
O16 K1 C16 73.9(8) . 23_565 ?
O16 K1 C16 24.1(4) 23_565 23_565 ?
O16 K1 O16 86.9(13) 23_565 . ?
C2 O2 K1 123.7(18) . 42_566 ?
C2 O2 H2 109.5 . . ?
K1 O2 H2 126.8 42_566 . ?
C3 O3 K1 129.8(17) . 42_566 ?
C3 O3 H3 109.5 . . ?
K1 O3 H3 120.2 42_566 . ?
C11 O4 C4 116.2(18) . . ?
C1 O5 C5 106.6(7) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12 109.5 . . ?
C13 O13 H13 109.5 . . ?
C14 O14 C1 114(2) . 5_565 ?
C11 O15 K1 114.4(17) . . ?
C15 O15 C11 113.2(14) . . ?
C15 O15 K1 111.6(17) . . ?
C16 O16 K1 102.7(19) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 125.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -32(4) . . . . ?
C1 C2 C3 O3 151(3) . . . . ?
C1 C2 O2 K1 170.2(19) . . . 42_566 ?
C2 C1 O5 C5 -55(3) . . . . ?
C2 C3 C4 C5 26(4) . . . . ?
C2 C3 C4 O4 176(3) . . . . ?
C2 C3 O3 K1 5(4) . . . 42_566 ?
C3 C2 O2 K1 -69(3) . . . 42_566 ?
C3 C4 C5 C6 -157(3) . . . . ?
C3 C4 C5 O5 -37(4) . . . . ?
C3 C4 O4 C11 114(3) . . . . ?
C4 C3 O3 K1 -170(4) . . . 42_566 ?
C4 C5 C6 O6 52(3) . . . . ?
C4 C5 O5 C1 48(3) . . . . ?
C5 C4 O4 C11 -102(3) . . . . ?
C6 C5 O5 C1 163(2) . . . . ?
C11 C12 C13 C14 -48(3) . . . . ?
C11 C12 C13 O13 137(3) . . . . ?
C12 C11 O4 C4 -140(2) . . . . ?
C12 C11 O15 C15 -57(3) . . . . ?
C12 C11 O15 K1 73(2) . . . . ?
C12 C13 C14 C15 43(3) . . . . ?
C12 C13 C14 O14 162(2) . . . . ?
C13 C14 C15 C16 -167(2) . . . . ?
C13 C14 C15 O15 -44(3) . . . . ?
C13 C14 O14 C1 126(2) . . . 5_565 ?
C14 C15 C16 K1 89(2) . . . . ?
C14 C15 C16 O16 49(4) . . . . ?
C14 C15 O15 C11 51(3) . . . . ?
C14 C15 O15 K1 -80(2) . . . . ?
C15 C14 O14 C1 -110(2) . . . 5_565 ?
C15 C16 O16 K1 54(3) . . . . ?
C16 C15 O15 C11 -170(2) . . . . ?
C16 C15 O15 K1 59(2) . . . . ?
O2 C2 C3 C4 -152(3) . . . . ?
O2 C2 C3 O3 31(3) . . . . ?
O3 C3 C4 C5 -159(4) . . . . ?
O3 C3 C4 O4 -9(6) . . . . ?
O4 C4 C5 C6 61(3) . . . . ?
O4 C4 C5 O5 -179(3) . . . . ?
O4 C11 C12 C13 -90(2) . . . . ?
O4 C11 C12 O12 31(3) . . . . ?
O4 C11 O15 C15 73(3) . . . . ?
O4 C11 O15 K1 -157.7(18) . . . . ?
O5 C1 C2 C3 49(3) . . . . ?
O5 C1 C2 O2 163(2) . . . . ?
O5 C5 C6 O6 -76(4) . . . . ?
O12 C12 C13 C14 -168(2) . . . . ?
O12 C12 C13 O13 18(4) . . . . ?
O13 C13 C14 C15 -142(3) . . . . ?
O13 C13 C14 O14 -23(4) . . . . ?
O14 C1 C2 C3 -59(3) 7_556 . . . ?
O14 C1 C2 O2 54(2) 7_556 . . . ?
O14 C1 O5 C5 63(2) 7_556 . . . ?
O14 C14 C15 C16 71(3) . . . . ?
O14 C14 C15 O15 -166(2) . . . . ?
O15 C11 C12 C13 54(3) . . . . ?
O15 C11 C12 O12 175(3) . . . . ?
O15 C11 O4 C4 87(4) . . . . ?
O15 C15 C16 K1 -40.1(17) . . . . ?
O15 C15 C16 O16 -81(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.318 -0.891 -0.931 14624.9 4139.1 ?


_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_olex2_submission_original_sample_id CDMOF_alpha_4_041
_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 1.552
_oxdiff_exptl_absorpt_empirical_full_min 0.689
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_b_195K
_database_code_depnum_ccdc_archive 'CCDC 1529153'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7

# start Validation Reply Form
_vrf_THETM01_CDMOF_b_195K        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly diffracting sample crystal'
;
_vrf_PLAT201_CDMOF_b_195K        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         88 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT090_CDMOF_b_195K        
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.91 Note  
RESPONSE: 'Data limited due to the poorly diffracting sample crystal; 
large number of parameters is the result of the complex molecular 
and crystal structures'
;
_vrf_PLAT213_CDMOF_b_195K        
;
PROBLEM: Atom K2              has ADP max/min Ratio .....        4.3 prolat
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT241_CDMOF_b_195K        
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         K2 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT242_CDMOF_b_195K        
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         O6 Check 
RESPONSE: 'Poor data quality'
;
_vrf_PLAT306_CDMOF_b_195K        
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_b_195K        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.04425 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_CDMOF_b_195K        
;
PROBLEM: D-H Without Acceptor       O2     --  H2A    ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
_vrf_PLAT910_CDMOF_b_195K        
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          19 Note  
RESPONSE: 'Missing reflections may be due to the chosen strategy of the 
measurement; this was short measurement, aimed primarily at 
checking the unit-cell paremeters only'
;
# end Validation Reply Form

# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_symmetry_space_group_name_H-M_alt 'R 3 2'
_cell_length_a                   43.367(6)
_cell_length_b                   43.367(6)
_cell_length_c                   28.090(5)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_volume                     45752(12)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    2207
_cell_measurement_temperature    194.98(10)
_cell_measurement_theta_max      12.3070
_cell_measurement_theta_min      2.9330
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23992
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.920
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1558
_diffrn_reflns_av_unetI/netI     0.0972
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_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            21398
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        13.734
_diffrn_reflns_theta_max         13.734
_diffrn_reflns_theta_min         2.773
_diffrn_ambient_environment      'ispropanol:water mother liquor'
_diffrn_ambient_temperature      194.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  54.00   1.00   15.00    --  -18.72   0.00-150.00  122
  2  ω    -73.00  20.00   1.00   15.00    --  -18.72 -19.00  60.00   93
  3  ω    -40.00   8.00   1.00   15.00    --  -18.72  57.00  60.00   48
  4  ω    -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       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0072561000
_diffrn_orient_matrix_UB_12      0.0127133000
_diffrn_orient_matrix_UB_13      -0.0185151000
_diffrn_orient_matrix_UB_21      -0.0159376000
_diffrn_orient_matrix_UB_22      0.0008026000
_diffrn_orient_matrix_UB_23      -0.0008858000
_diffrn_orient_matrix_UB_31      0.0070017000
_diffrn_orient_matrix_UB_32      0.0138052000
_diffrn_orient_matrix_UB_33      0.0171433000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                2537
_reflns_number_total             3106
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.68
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.345
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 
;
 Flack x determined using 791 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.42(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         3106
_refine_ls_number_restraints     358
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.1122
_refine_ls_restrained_S_all      1.476
_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/[σ²(Fo²)+(0.1621P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2798
_refine_ls_wR_factor_ref         0.2938
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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, H3A of O3, H2A of O2, H43A of O43, H42A of O42, H36 of O36,
  H33A of O33, H32A of O32, H26 of O26, H23A of O23, H22A of O22, H16 of O16,
  H13A of O13, H12A of O12, H6 of O6, H46 of O46, H52A of O52, H53A of O53, H56
  of O56, H62A of O62, H63A of O63, H66 of O66, H72A of O72
2. Restrained distances
 C64-C65
 1.5 with sigma of 0.02
 C65-C66
 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
 C35-C36
 1.5 with sigma of 0.002
 C64-C63
 1.5 with sigma of 0.02
 C4-C1
 3.5 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.005
 C13-C14
 1.5 with sigma of 0.02
 C13-C12
 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
 C31-O35
 1.45 with sigma of 0.005
 C33-O35
 3 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
 C35-O36
 2.45 with sigma of 0.02
 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
 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
 C65-C64
 1.5 with sigma of 0.02
 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
 O54-C41
 1.45 with sigma of 0.01
 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
 O14-C14
 1.45 with sigma of 0.01
 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
 C62-C61
 1.5 with sigma of 0.02
 C62-O62
 1.45 with sigma of 0.02
 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
 C62-C63
 1.5 with sigma of 0.02
 C32-C33
 1.5 with sigma of 0.02
 C36-C35
 1.5 with sigma of 0.02
 C61-O74
 1.45 with sigma of 0.02
 C61-C62
 1.5 with sigma of 0.02
 C61-O65
 1.45 with sigma of 0.02
 O36-C36
 1.45 with sigma of 0.01
 O75-C75
 1.45 with sigma of 0.02
 C41-O45
 1.45 with sigma of 0.02
 C71-O75
 1.45 with sigma of 0.01
 C71-C72
 1.5 with sigma of 0.02
 O73-C73
 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
 O34-C21
 1.45 with sigma of 0.02
 C21-O34
 1.45 with sigma of 0.01
 C43-C44
 1.5 with sigma of 0.02
 C44-C43
 1.5 with sigma of 0.01
 C72-C71
 1.5 with sigma of 0.01
 C71-O4
 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
 C34-C35
 1.5 with sigma of 0.02
 C34-O34
 1.45 with sigma of 0.01
 C33-O33
 1.45 with sigma of 0.01
 O72-C72
 1.45 with sigma of 0.02
 C41-C42
 1.5 with sigma of 0.01
 C34-C33
 1.5 with sigma of 0.01
 C44-C45
 1.5 with sigma of 0.01
 C35-O35
 1.45 with sigma of 0.01
 C52-C53
 1.5 with sigma of 0.02
 C54-C55
 1.5 with sigma of 0.02
 C54-C53
 1.5 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-O64
 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
 C56-C55
 1.5 with sigma of 0.02
 C51-C52
 1.5 with sigma of 0.02
 C55-O55
 1.45 with sigma of 0.02
 O55-C51
 1.45 with sigma of 0.01
 O55-C55
 1.45 with sigma of 0.01
 O64-C51
 1.45 with sigma of 0.02
 C51-O55
 1.45 with sigma of 0.02
 C1-K2
 3.8 with sigma of 0.02
 C12-K1
 3.8 with sigma of 0.02
 O2-C2
 1.45 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C4-C3
 1.5 with sigma of 0.005
 C5-C3
 2.5 with sigma of 0.02
 C3-O3
 1.45 with sigma of 0.01
 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
 C4-C71
 2.5 with sigma of 0.01
 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
 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
 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
 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
 O62-C61
 2.5 with sigma of 0.04
 O62-C63
 2.5 with sigma of 0.04
 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
 C35-C33
 2.5 with sigma of 0.04
 C33-C31
 2.5 with sigma of 0.04
 C32-O35
 2.5 with sigma of 0.04
 C31-C35
 2.5 with sigma of 0.04
 C63-C61
 2.5 with sigma of 0.04
 C72-O75
 2.5 with sigma of 0.04
 C31-O32
 2.5 with sigma of 0.04
 C24-O23
 2.5 with sigma of 0.04
 C72-O4
 2.5 with sigma of 0.04
 C74-C76
 2.5 with sigma of 0.01
 C61-C74
 2.5 with sigma of 0.04
 O73-C74
 2.5 with sigma of 0.02
 C72-O73
 2.5 with sigma of 0.02
 C24-C11
 2.5 with sigma of 0.01
 O23-C24
 2.5 with sigma of 0.02
 O23-C22
 2.5 with sigma of 0.02
 C41-C43
 2.5 with sigma of 0.01
 O43-C42
 2.5 with sigma of 0.01
 O42-C43
 2.5 with sigma of 0.01
 O42-C41
 2.5 with sigma of 0.01
 O75-C72
 2.5 with sigma of 0.01
 C32-C34
 2.5 with sigma of 0.04
 C34-C32
 2.5 with sigma of 0.04
 O35-C34
 2.5 with sigma of 0.04
 O33-C34
 2.5 with sigma of 0.04
 C34-C21
 2.5 with sigma of 0.01
 C34-O33
 2.45 with sigma of 0.01
 O33-C32
 2.45 with sigma of 0.01
 C34-C36
 2.5 with sigma of 0.01
 O36-C35
 2.4 with sigma of 0.02
 C53-C55
 2.5 with sigma of 0.04
 C54-C41
 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
 O52-C53
 2.5 with sigma of 0.04
 C53-O52
 2.5 with sigma of 0.01
 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
 C55-C51 = C54-O55
 2.5 with sigma of 0.04
 C55-C51
 2.5 with sigma of 0.01
 C41-C45
 2.5 with sigma of 0.04
 C42-C44
 2.5 with sigma of 0.04
 C43-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
 C11-C13
 2.5 with sigma of 0.04
 C12-C14
 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
 C74-O73
 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
 O75-C76
 2.5 with sigma of 0.04
 O76-C75
 2.5 with sigma of 0.04
 O26-C25
 2.5 with sigma of 0.04
 C26-O25
 2.5 with sigma of 0.04
 O75-C74
 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
 C21-C25
 2.5 with sigma of 0.04
 C23-O24
 2.5 with sigma of 0.04
 C36-C34
 2.5 with sigma of 0.04
 C36-O35
 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-C5
 2.5 with sigma of 0.04
 O4-C72
 2.5 with sigma of 0.04
 O4-O75
 2.5 with sigma of 0.04
 C64-C62
 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
 C62-C64
 2.5 with sigma of 0.04
 C1-C14
 2.5 with sigma of 0.04
 C51-C55
 2.5 with sigma of 0.04
 O2-C1
 2.5 with sigma of 0.04
 C6-O5
 2.5 with sigma of 0.04
 C6-C4
 2.5 with sigma of 0.04
 O25-C22
 2.5 with sigma of 0.01
 C21-C23
 2.5 with sigma of 0.01
 C22-C24
 2.5 with sigma of 0.01
 C23-C25
 2.5 with sigma of 0.01
 C24-O25
 2.5 with sigma of 0.01
 C14-C1
 2.5 with sigma of 0.01
 C51-C64
 2.5 with sigma of 0.01
 C1-C3
 2.5 with sigma of 0.04
 C3-O2
 2.5 with sigma of 0.04
 O4-C3
 2.5 with sigma of 0.04
 C3-C1
 2.5 with sigma of 0.01
 O3-C2
 2.5 with sigma of 0.04
 O3-C4
 2.5 with sigma of 0.04
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(H6A,H6B), C16(H16A,H16B), C26(H26A,H26B), 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)
;

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7440(5) 0.6619(8) 0.4083(8) 0.148(16) Uiso 1 1 d D U . . .
H1 H 0.7530 0.6789 0.3817 0.177 Uiso 1 1 calc R . . . .
C2 C 0.7326(8) 0.6746(6) 0.4518(10) 0.148(17) Uiso 1 1 d D U . . .
H2 H 0.7168 0.6825 0.4386 0.177 Uiso 1 1 calc R . . . .
C3 C 0.7122(8) 0.6511(7) 0.4881(9) 0.176(19) Uiso 1 1 d D U . . .
H3 H 0.7284 0.6434 0.5002 0.212 Uiso 1 1 calc R . . . .
C4 C 0.6796(7) 0.6160(6) 0.4766(9) 0.128(16) Uiso 1 1 d D U . . .
H4 H 0.6599 0.6201 0.4683 0.154 Uiso 1 1 calc R . . . .
C5 C 0.6884(9) 0.6004(6) 0.4344(10) 0.158(17) Uiso 1 1 d D U . . .
H5 H 0.7039 0.5921 0.4473 0.190 Uiso 1 1 calc R . . . .
C6 C 0.6598(10) 0.5688(9) 0.4084(17) 0.25(2) Uiso 1 1 d D U . . .
H6A H 0.6692 0.5614 0.3822 0.294 Uiso 1 1 calc R . . . .
H6B H 0.6460 0.5488 0.4294 0.294 Uiso 1 1 calc R . . . .
C11 C 0.8624(6) 0.6661(8) 0.3673(10) 0.090(12) Uiso 1 1 d D U . . .
H11 H 0.8827 0.6726 0.3462 0.108 Uiso 1 1 calc R . . . .
C12 C 0.8615(7) 0.6980(6) 0.3838(13) 0.131(16) Uiso 1 1 d D U . . .
H12 H 0.8591 0.7089 0.3546 0.158 Uiso 1 1 calc R . . . .
C13 C 0.8294(7) 0.6906(7) 0.4134(14) 0.148(17) Uiso 1 1 d D U . . .
H13 H 0.8330 0.6817 0.4438 0.178 Uiso 1 1 calc R . . . .
C14 C 0.7983(6) 0.6594(7) 0.3917(11) 0.089(13) Uiso 1 1 d D U . . .
H14 H 0.7933 0.6685 0.3625 0.107 Uiso 1 1 calc R . . . .
C15 C 0.7978(6) 0.6265(7) 0.3773(11) 0.089(13) Uiso 1 1 d D U . . .
H15 H 0.8016 0.6143 0.4042 0.106 Uiso 1 1 calc R . . . .
C16 C 0.7671(9) 0.6015(9) 0.3462(11) 0.110(14) Uiso 1 1 d D U . . .
H16A H 0.7679 0.5797 0.3415 0.132 Uiso 1 1 calc R . . . .
H16B H 0.7448 0.5954 0.3620 0.132 Uiso 1 1 calc R . . . .
C21 C 0.9379(7) 0.6208(6) 0.4599(8) 0.066(11) Uiso 1 1 d D U . . .
H21 H 0.9603 0.6205 0.4618 0.079 Uiso 1 1 calc R . . . .
C22 C 0.9472(9) 0.6595(8) 0.4700(12) 0.174(19) Uiso 1 1 d D U . . .
H22 H 0.9657 0.6731 0.4463 0.209 Uiso 1 1 calc R . . . .
C23 C 0.9193(10) 0.6666(8) 0.4570(15) 0.21(2) Uiso 1 1 d D U . . .
H23 H 0.9049 0.6584 0.4860 0.247 Uiso 1 1 calc R . . . .
C24 C 0.8921(9) 0.6435(8) 0.4216(14) 0.22(2) Uiso 1 1 d D U . . .
H24 H 0.9064 0.6567 0.3939 0.264 Uiso 1 1 calc R . . . .
C25 C 0.8909(8) 0.6105(7) 0.4086(12) 0.172(18) Uiso 1 1 d D U . . .
H25 H 0.8775 0.5947 0.4352 0.207 Uiso 1 1 calc R . . . .
C26 C 0.8737(8) 0.5868(9) 0.3660(10) 0.134(16) Uiso 1 1 d D U . . .
H26A H 0.8677 0.5626 0.3737 0.161 Uiso 1 1 calc R . . . .
H26B H 0.8518 0.5866 0.3583 0.161 Uiso 1 1 calc R . . . .
C31 C 0.9337(7) 0.5443(8) 0.6147(9) 0.21(2) Uiso 1 1 d D U . . .
H31 H 0.9418 0.5294 0.6303 0.247 Uiso 1 1 calc R . . . .
C32 C 0.9600(11) 0.5830(7) 0.6143(12) 0.21(2) Uiso 1 1 d D U . . .
H32 H 0.9820 0.5854 0.6008 0.256 Uiso 1 1 calc R . . . .
C33 C 0.9515(8) 0.6072(6) 0.5853(8) 0.154(17) Uiso 1 1 d D U . . .
H33 H 0.9329 0.6091 0.6026 0.185 Uiso 1 1 calc R . . . .
C34 C 0.9362(9) 0.5914(6) 0.5373(8) 0.166(18) Uiso 1 1 d D U . . .
H34 H 0.9550 0.5904 0.5193 0.199 Uiso 1 1 calc R . . . .
C35 C 0.9061(8) 0.5539(6) 0.5429(8) 0.20(2) Uiso 1 1 d D U . . .
H35 H 0.8881 0.5555 0.5619 0.242 Uiso 1 1 calc R . . . .
C36 C 0.8885(7) 0.5376(9) 0.4964(11) 0.24(3) Uiso 1 1 d D U . . .
H36A H 0.8672 0.5148 0.5021 0.289 Uiso 1 1 calc R . . . .
H36B H 0.8815 0.5530 0.4805 0.289 Uiso 1 1 calc R . . . .
C41 C 0.8373(5) 0.4902(5) 0.7522(9) 0.096(13) Uiso 1 1 d D U . . .
H41 H 0.8302 0.4764 0.7818 0.116 Uiso 1 1 calc R . . . .
C42 C 0.8673(7) 0.5270(6) 0.7624(9) 0.111(14) Uiso 1 1 d D U . . .
H42 H 0.8846 0.5212 0.7759 0.133 Uiso 1 1 calc R . . . .
C43 C 0.8868(8) 0.5454(6) 0.7164(8) 0.105(14) Uiso 1 1 d D U . . .
H43 H 0.8706 0.5527 0.7026 0.126 Uiso 1 1 calc R . . . .
C44 C 0.8876(7) 0.5219(7) 0.6785(9) 0.076(12) Uiso 1 1 d D U . . .
H44 H 0.9060 0.5163 0.6881 0.091 Uiso 1 1 calc R . . . .
C45 C 0.8546(8) 0.4870(7) 0.6717(9) 0.084(12) Uiso 1 1 d D U . . .
H45 H 0.8372 0.4932 0.6595 0.101 Uiso 1 1 calc R . . . .
C46 C 0.8580(9) 0.4655(8) 0.6331(11) 0.082(12) Uiso 1 1 d D U . . .
H46A H 0.8689 0.4801 0.6051 0.098 Uiso 1 1 calc R . . . .
H46B H 0.8348 0.4458 0.6244 0.098 Uiso 1 1 calc R . . . .
C51 C 0.7062(7) 0.4666(8) 0.7808(10) 0.129(15) Uiso 1 1 d D U . . .
H51 H 0.6830 0.4531 0.7964 0.155 Uiso 1 1 calc R . . . .
C52 C 0.7348(7) 0.4894(7) 0.8172(10) 0.097(13) Uiso 1 1 d D U . . .
H52 H 0.7366 0.4739 0.8410 0.116 Uiso 1 1 calc R . . . .
C53 C 0.7704(8) 0.5103(8) 0.7909(13) 0.115(14) Uiso 1 1 d D U . . .
H53 H 0.7709 0.5284 0.7695 0.138 Uiso 1 1 calc R . . . .
C54 C 0.7785(5) 0.4853(7) 0.7660(9) 0.047(10) Uiso 1 1 d D U . . .
H54 H 0.7801 0.4702 0.7907 0.056 Uiso 1 1 calc R . . . .
C55 C 0.7497(7) 0.4604(8) 0.7317(10) 0.087(13) Uiso 1 1 d D U . . .
H55 H 0.7473 0.4772 0.7108 0.105 Uiso 1 1 calc R . . . .
C56 C 0.7554(10) 0.4383(9) 0.6973(10) 0.142(17) Uiso 1 1 d D U . . .
H56A H 0.7350 0.4238 0.6773 0.170 Uiso 1 1 calc R . . . .
H56B H 0.7769 0.4512 0.6785 0.170 Uiso 1 1 calc R . . . .
C61 C 0.6261(10) 0.5114(9) 0.6923(13) 0.20(2) Uiso 1 1 d D U . . .
H61 H 0.6032 0.5108 0.6940 0.237 Uiso 1 1 calc R . . . .
C62 C 0.6485(10) 0.5324(9) 0.7339(14) 0.146(17) Uiso 1 1 d D U . . .
H62 H 0.6343 0.5234 0.7630 0.175 Uiso 1 1 calc R . . . .
C63 C 0.6809(10) 0.5275(9) 0.7383(13) 0.176(19) Uiso 1 1 d D U . . .
H63 H 0.6972 0.5391 0.7116 0.211 Uiso 1 1 calc R . . . .
C64 C 0.6701(11) 0.4891(9) 0.7407(14) 0.165(18) Uiso 1 1 d D U . . .
H64 H 0.6552 0.4770 0.7684 0.198 Uiso 1 1 calc R . . . .
C65 C 0.6523(11) 0.4720(9) 0.6939(12) 0.119(15) Uiso 1 1 d D U . . .
H65 H 0.6682 0.4850 0.6674 0.143 Uiso 1 1 calc R . . . .
C66 C 0.6396(12) 0.4325(9) 0.6890(17) 0.176(19) Uiso 1 1 d D U . . .
H66A H 0.6588 0.4274 0.6936 0.212 Uiso 1 1 calc R . . . .
H66B H 0.6281 0.4230 0.6587 0.212 Uiso 1 1 calc R . . . .
C71 C 0.6320(7) 0.5729(6) 0.5292(9) 0.184(19) Uiso 1 1 d D U . . .
H71 H 0.6203 0.5786 0.5036 0.221 Uiso 1 1 calc R . . . .
C72 C 0.6242(10) 0.5863(8) 0.5738(9) 0.19(2) Uiso 1 1 d D U . . .
H72 H 0.5984 0.5733 0.5791 0.233 Uiso 1 1 calc R . . . .
C73 C 0.6417(11) 0.5803(8) 0.6153(11) 0.134(16) Uiso 1 1 d D U . . .
H73 H 0.6671 0.5935 0.6077 0.161 Uiso 1 1 calc R . . . .
C74 C 0.6319(12) 0.5419(8) 0.6126(11) 0.148(17) Uiso 1 1 d D U . . .
H74 H 0.6061 0.5286 0.6179 0.177 Uiso 1 1 calc R . . . .
C75 C 0.6373(9) 0.5284(7) 0.5653(10) 0.120(15) Uiso 1 1 d D U . . .
H75 H 0.6626 0.5379 0.5583 0.144 Uiso 1 1 calc R . . . .
C76 C 0.6165(8) 0.4878(7) 0.5636(13) 0.167(19) Uiso 1 1 d D U . . .
H76A H 0.6175 0.4807 0.5312 0.200 Uiso 1 1 calc R . . . .
H76B H 0.6289 0.4792 0.5834 0.200 Uiso 1 1 calc R . . . .
K1 K 0.8933(2) 0.7918(3) 0.4184(4) 0.130(4) Uani 1 1 d D U . . .
K2 K 0.6667 0.6395(4) 0.3333 0.306(16) Uani 1 2 d DS TU P . .
K3 K 0.9736(5) 0.6402(5) 0.3333 0.258(12) Uani 1 2 d S TU P . .
O2 O 0.7650(7) 0.7072(6) 0.4612(10) 0.160(3) Uiso 1 1 d D U . . .
H2A H 0.7674 0.7106 0.4901 0.240 Uiso 1 1 calc R . . . .
O3 O 0.7027(7) 0.6630(7) 0.5319(8) 0.160(3) Uiso 1 1 d D U . . .
H3A H 0.7187 0.6831 0.5387 0.240 Uiso 1 1 calc R . . . .
O4 O 0.6703(6) 0.5942(7) 0.5193(9) 0.160(3) Uiso 1 1 d D U . . .
O5 O 0.7096(7) 0.6255(7) 0.3969(7) 0.160(3) Uiso 1 1 d D U . . .
O6 O 0.6391(8) 0.5854(8) 0.3916(11) 0.160(3) Uiso 1 1 d D U . . .
H6 H 0.6184 0.5734 0.4006 0.240 Uiso 1 1 calc R . . . .
O12 O 0.8909(7) 0.7271(7) 0.4092(10) 0.160(3) Uiso 1 1 d D U . . .
H12A H 0.8974 0.7191 0.4308 0.240 Uiso 1 1 calc R . . . .
O13 O 0.8267(7) 0.7210(7) 0.4260(10) 0.160(3) Uiso 1 1 d D U . . .
H13A H 0.8057 0.7149 0.4307 0.240 Uiso 1 1 calc R . . . .
O14 O 0.7666(6) 0.6480(7) 0.4219(9) 0.160(3) Uiso 1 1 d D U . . .
O15 O 0.8280(7) 0.6415(7) 0.3430(8) 0.160(3) Uiso 1 1 d D U . . .
O16 O 0.7683(8) 0.6174(8) 0.3002(11) 0.160(3) Uiso 1 1 d D U . . .
H16 H 0.7884 0.6259 0.2890 0.240 Uiso 1 1 calc R . . . .
O22 O 0.9653(7) 0.6741(8) 0.5143(9) 0.160(3) Uiso 1 1 d D U . . .
H22A H 0.9660 0.6930 0.5195 0.240 Uiso 1 1 calc R . . . .
O23 O 0.9264(7) 0.7026(6) 0.4557(9) 0.160(3) Uiso 1 1 d D U . . .
H23A H 0.9451 0.7150 0.4413 0.240 Uiso 1 1 calc R . . . .
O24 O 0.8674(7) 0.6529(7) 0.4152(11) 0.160(3) Uiso 1 1 d D U . . .
O25 O 0.9253(7) 0.6111(6) 0.4114(9) 0.160(3) Uiso 1 1 d D U . . .
O26 O 0.8973(8) 0.5991(7) 0.3252(10) 0.160(3) Uiso 1 1 d D U . . .
H26 H 0.8866 0.6006 0.3020 0.240 Uiso 1 1 calc R . . . .
O32 O 0.9693(8) 0.5996(7) 0.6600(10) 0.160(3) Uiso 1 1 d D U . . .
H32A H 0.9525 0.5889 0.6783 0.240 Uiso 1 1 calc R . . . .
O33 O 0.9815(7) 0.6426(5) 0.5821(9) 0.160(3) Uiso 1 1 d D U . . .
H33A H 0.9756 0.6555 0.5681 0.240 Uiso 1 1 calc R . . . .
O34 O 0.9188(7) 0.6050(8) 0.5045(10) 0.160(3) Uiso 1 1 d D U . . .
O35 O 0.9154(8) 0.5306(5) 0.5698(10) 0.160(3) Uiso 1 1 d D U . . .
O36 O 0.9130(8) 0.5326(8) 0.4665(9) 0.160(3) Uiso 1 1 d D U . . .
H36 H 0.9036 0.5117 0.4581 0.240 Uiso 1 1 calc R . . . .
O42 O 0.8656(7) 0.5469(6) 0.7985(7) 0.160(3) Uiso 1 1 d D U . . .
H42A H 0.8735 0.5675 0.7894 0.240 Uiso 1 1 calc R . . . .
O43 O 0.9184(6) 0.5793(6) 0.7243(10) 0.160(3) Uiso 1 1 d D U . . .
H43A H 0.9192 0.5851 0.7522 0.240 Uiso 1 1 calc R . . . .
O44 O 0.8989(7) 0.5395(8) 0.6327(9) 0.160(3) Uiso 1 1 d D U . . .
O45 O 0.8395(7) 0.4689(6) 0.7150(10) 0.160(3) Uiso 1 1 d D U . . .
O46 O 0.8813(8) 0.4523(8) 0.6535(10) 0.160(3) Uiso 1 1 d . U . . .
H46 H 0.8881 0.4609 0.6801 0.240 Uiso 1 1 calc R . . . .
O52 O 0.7227(7) 0.5115(7) 0.8399(9) 0.160(3) Uiso 1 1 d D U . . .
H52A H 0.7385 0.5261 0.8572 0.240 Uiso 1 1 calc R . . . .
O53 O 0.7958(8) 0.5246(8) 0.8257(11) 0.160(3) Uiso 1 1 d . U . . .
H53A H 0.8060 0.5464 0.8243 0.240 Uiso 1 1 calc R . . . .
O54 O 0.8106(7) 0.4993(8) 0.7390(10) 0.160(3) Uiso 1 1 d D U . . .
O55 O 0.7150(6) 0.4425(5) 0.7559(8) 0.160(3) Uiso 1 1 d D U . . .
O56 O 0.7590(8) 0.4194(8) 0.7377(11) 0.160(3) Uiso 1 1 d D U . . .
H56 H 0.7801 0.4257 0.7416 0.240 Uiso 1 1 calc R . . . .
O62 O 0.6598(8) 0.5699(8) 0.7289(10) 0.160(3) Uiso 1 1 d D U . . .
H62A H 0.6487 0.5752 0.7476 0.240 Uiso 1 1 calc R . . . .
O63 O 0.6979(8) 0.5438(8) 0.7829(10) 0.160(3) Uiso 1 1 d D U . . .
H63A H 0.7074 0.5331 0.7940 0.240 Uiso 1 1 calc R . . . .
O64 O 0.7042(9) 0.4881(8) 0.7405(10) 0.160(3) Uiso 1 1 d D U . . .
O65 O 0.6195(8) 0.4753(8) 0.6915(10) 0.160(3) Uiso 1 1 d D U . . .
O66 O 0.6112(8) 0.4181(8) 0.7335(10) 0.160(3) Uiso 1 1 d . U . . .
H66 H 0.6195 0.4123 0.7556 0.240 Uiso 1 1 calc R . . . .
O72 O 0.6354(8) 0.6236(7) 0.5650(10) 0.160(3) Uiso 1 1 d D U . . .
H72A H 0.6429 0.6349 0.5898 0.240 Uiso 1 1 calc R . . . .
O73 O 0.6390(8) 0.5943(7) 0.6602(9) 0.160(3) Uiso 1 1 d D U . . .
H73A H 0.6571 0.6000 0.6758 0.192 Uiso 1 1 calc R . . . .
O74 O 0.6480(8) 0.5376(8) 0.6587(12) 0.160(3) Uiso 1 1 d D U . . .
O75 O 0.6185(7) 0.5352(6) 0.5254(9) 0.160(3) Uiso 1 1 d D U . . .
O76 O 0.5794(8) 0.4695(7) 0.5782(10) 0.160(3) Uiso 1 1 d D U . . .
H76 H 0.5700 0.4808 0.5693 0.240 Uiso 1 1 calc R . . . .
OA O 0.7557(10) 0.7013(11) 0.5861(14) 0.228(12) Uiso 1 1 d . U . . .
OB O 0.9576(11) 0.7070(10) 0.5701(14) 0.228(12) Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.52(2) . ?
C1 O5 1.57(2) . ?
C1 O14 1.44(2) . ?
C2 H2 0.9800 . ?
C2 C3 1.40(2) . ?
C2 O2 1.44(2) . ?
C3 H3 0.9800 . ?
C3 C4 1.506(7) . ?
C3 O3 1.470(14) . ?
C4 H4 0.9800 . ?
C4 C5 1.507(7) . ?
C4 O4 1.46(2) . ?
C5 H5 0.9800 . ?
C5 C6 1.501(8) . ?
C5 O5 1.463(14) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.48(3) . ?
C11 H11 0.9800 . ?
C11 C12 1.48(3) . ?
C11 O15 1.49(2) . ?
C11 O24 1.52(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.51(2) . ?
C12 O12 1.454(18) . ?
C13 H13 0.9800 . ?
C13 C14 1.48(2) . ?
C13 O13 1.42(2) . ?
C14 H14 0.9800 . ?
C14 C15 1.47(2) . ?
C14 O14 1.473(14) . ?
C15 H15 0.9800 . ?
C15 C16 1.51(2) . ?
C15 O15 1.491(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 O16 1.45(2) . ?
C21 H21 0.9800 . ?
C21 C22 1.54(2) . ?
C21 O25 1.449(13) . ?
C21 O34 1.470(13) . ?
C22 H22 0.9800 . ?
C22 C23 1.44(2) . ?
C22 O22 1.437(18) . ?
C23 H23 0.9800 . ?
C23 C24 1.48(2) . ?
C23 O23 1.43(2) . ?
C24 H24 0.9800 . ?
C24 C25 1.45(2) . ?
C24 O24 1.34(2) . ?
C25 H25 0.9800 . ?
C25 C26 1.51(2) . ?
C25 O25 1.482(14) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 O26 1.451(8) . ?
C31 H31 0.9800 . ?
C31 C32 1.49(2) . ?
C31 O35 1.451(7) . ?
C31 O44 1.50(2) . ?
C32 H32 0.9800 . ?
C32 C33 1.512(19) . ?
C32 O32 1.43(2) . ?
C33 H33 0.9800 . ?
C33 C34 1.506(13) . ?
C33 O33 1.436(14) . ?
C34 H34 0.9800 . ?
C34 C35 1.500(3) . ?
C34 O34 1.487(14) . ?
C35 H35 0.9800 . ?
C35 C36 1.500(3) . ?
C35 O35 1.468(14) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 O36 1.453(15) . ?
C41 H41 0.9800 . ?
C41 C42 1.497(14) . ?
C41 K1 3.51(2) 8_655 ?
C41 O45 1.43(2) . ?
C41 O54 1.446(14) . ?
C42 H42 0.9800 . ?
C42 C43 1.53(2) . ?
C42 O42 1.36(3) . ?
C43 H43 0.9800 . ?
C43 C44 1.490(13) . ?
C43 O43 1.44(2) . ?
C44 H44 0.9800 . ?
C44 C45 1.487(14) . ?
C44 O44 1.450(14) . ?
C45 H45 0.9800 . ?
C45 C46 1.49(2) . ?
C45 O45 1.42(2) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 O46 1.50(3) . ?
C51 H51 0.9800 . ?
C51 C52 1.53(2) . ?
C51 O55 1.457(12) . ?
C51 O64 1.497(19) . ?
C52 H52 0.9800 . ?
C52 C53 1.533(19) . ?
C52 K1 3.39(2) 10_566 ?
C52 O52 1.45(2) . ?
C53 H53 0.9800 . ?
C53 C54 1.47(2) . ?
C53 O53 1.37(4) . ?
C54 H54 0.9800 . ?
C54 C55 1.52(2) . ?
C54 O54 1.43(2) . ?
C55 H55 0.9800 . ?
C55 C56 1.465(18) . ?
C55 O55 1.470(12) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 O56 1.453(8) . ?
C61 H61 0.9800 . ?
C61 C62 1.50(2) . ?
C61 K1 3.34(4) 9_565 ?
C61 O65 1.44(2) . ?
C61 O74 1.42(3) . ?
C62 H62 0.9800 . ?
C62 C63 1.53(3) . ?
C62 O62 1.45(2) . ?
C63 H63 0.9800 . ?
C63 C64 1.49(3) . ?
C63 O63 1.448(8) . ?
C64 H64 0.9800 . ?
C64 C65 1.518(19) . ?
C64 O64 1.50(4) . ?
C65 H65 0.9800 . ?
C65 C66 1.52(2) . ?
C65 O65 1.50(4) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C66 O66 1.64(5) . ?
C71 H71 0.9800 . ?
C71 C72 1.492(13) . ?
C71 O4 1.469(14) . ?
C71 O75 1.439(12) . ?
C72 H72 0.9800 . ?
C72 C73 1.48(2) . ?
C72 O72 1.458(19) . ?
C73 H73 0.9800 . ?
C73 C74 1.499(8) . ?
C73 O73 1.43(2) . ?
C74 H74 0.9800 . ?
C74 C75 1.52(2) . ?
C74 O74 1.53(4) . ?
C75 H75 0.9800 . ?
C75 C76 1.52(2) . ?
C75 O75 1.498(19) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C76 O76 1.451(8) . ?
K1 C41 3.51(2) 15_664 ?
K1 C52 3.39(2) 10_566 ?
K1 C61 3.34(4) 14_654 ?
K1 O12 2.77(3) . ?
K1 O13 2.99(3) . ?
K1 O45 2.80(3) 15_664 ?
K1 O46 2.84(3) 15_664 ?
K1 O52 2.73(3) 10_566 ?
K1 O53 3.02(3) 10_566 ?
K1 O65 2.68(3) 14_654 ?
K1 O66 2.66(3) 14_654 ?
K2 O5 2.86(3) . ?
K2 O5 2.86(3) 17_655 ?
K2 O6 2.61(3) . ?
K2 O6 2.61(3) 17_655 ?
K2 O72 3.37(3) 6_556 ?
K2 O72 3.37(3) 14_654 ?
K2 O73 3.13(3) 6_556 ?
K2 O73 3.13(3) 14_654 ?
K3 O25 2.85(3) . ?
K3 O25 2.85(3) 18_545 ?
K3 O26 2.87(4) . ?
K3 O26 2.87(4) 18_545 ?
K3 O32 2.72(3) 5_766 ?
K3 O32 2.72(3) 15_664 ?
K3 O33 2.91(3) 5_766 ?
K3 O33 2.91(3) 15_664 ?
O2 H2A 0.8200 . ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O16 H16 0.8200 . ?
O22 H22A 0.8200 . ?
O23 H23A 0.8200 . ?
O26 H26 0.8200 . ?
O32 K3 2.72(3) 8_655 ?
O32 H32A 0.8200 . ?
O33 K3 2.91(3) 8_655 ?
O33 H33A 0.8200 . ?
O36 H36 0.8200 . ?
O42 H42A 0.8200 . ?
O43 H43A 0.8200 . ?
O45 K1 2.80(3) 8_655 ?
O46 K1 2.84(3) 8_655 ?
O46 H46 0.8200 . ?
O52 K1 2.73(3) 10_566 ?
O52 H52A 0.8200 . ?
O53 K1 3.02(3) 10_566 ?
O53 H53A 0.8200 . ?
O56 H56 0.8200 . ?
O62 H62A 0.8200 . ?
O63 H63A 0.8200 . ?
O65 K1 2.68(3) 9_565 ?
O66 K1 2.66(3) 9_565 ?
O66 H66 0.8200 . ?
O72 K2 3.37(3) 9_565 ?
O72 H72A 0.8200 . ?
O73 K2 3.13(3) 9_565 ?
O73 H73A 0.8200 . ?
O76 H76 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 114.8 . . ?
C2 C1 O5 102.1(13) . . ?
O5 C1 H1 114.8 . . ?
O14 C1 H1 114.8 . . ?
O14 C1 C2 111(2) . . ?
O14 C1 O5 98(2) . . ?
C1 C2 H2 103.5 . . ?
C3 C2 C1 121.7(19) . . ?
C3 C2 H2 103.5 . . ?
C3 C2 O2 122(3) . . ?
O2 C2 C1 99.7(19) . . ?
O2 C2 H2 103.5 . . ?
C2 C3 H3 101.6 . . ?
C2 C3 C4 120.8(17) . . ?
C2 C3 O3 123(2) . . ?
C4 C3 H3 101.6 . . ?
O3 C3 H3 101.6 . . ?
O3 C3 C4 104.4(19) . . ?
C3 C4 H4 109.4 . . ?
C3 C4 C5 107.5(14) . . ?
C5 C4 H4 109.4 . . ?
O4 C4 C3 107(2) . . ?
O4 C4 H4 109.4 . . ?
O4 C4 C5 114(2) . . ?
C4 C5 H5 104.4 . . ?
C6 C5 C4 121(3) . . ?
C6 C5 H5 104.4 . . ?
O5 C5 C4 116.1(13) . . ?
O5 C5 H5 104.4 . . ?
O5 C5 C6 105(2) . . ?
C5 C6 H6A 112.2 . . ?
C5 C6 H6B 112.2 . . ?
H6A C6 H6B 109.8 . . ?
O6 C6 C5 98(3) . . ?
O6 C6 H6A 112.2 . . ?
O6 C6 H6B 112.2 . . ?
C12 C11 H11 111.3 . . ?
C12 C11 O15 109(2) . . ?
C12 C11 O24 99(3) . . ?
O15 C11 H11 111.3 . . ?
O15 C11 O24 115(2) . . ?
O24 C11 H11 111.3 . . ?
C11 C12 H12 104.5 . . ?
C11 C12 C13 115(2) . . ?
C13 C12 H12 104.5 . . ?
O12 C12 C11 123(3) . . ?
O12 C12 H12 104.5 . . ?
O12 C12 C13 103(2) . . ?
C12 C13 H13 104.5 . . ?
C14 C13 C12 107(2) . . ?
C14 C13 H13 104.5 . . ?
O13 C13 C12 116(2) . . ?
O13 C13 H13 104.5 . . ?
O13 C13 C14 119(2) . . ?
C13 C14 H14 105.1 . . ?
C15 C14 C13 124(2) . . ?
C15 C14 H14 105.1 . . ?
C15 C14 O14 106(2) . . ?
O14 C14 C13 110(2) . . ?
O14 C14 H14 105.1 . . ?
C14 C15 H15 112.7 . . ?
C14 C15 C16 116(3) . . ?
C14 C15 O15 99.8(19) . . ?
C16 C15 H15 112.7 . . ?
O15 C15 H15 112.7 . . ?
O15 C15 C16 102(3) . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
O16 C16 C15 111(3) . . ?
O16 C16 H16A 109.3 . . ?
O16 C16 H16B 109.3 . . ?
C22 C21 H21 106.3 . . ?
O25 C21 H21 106.3 . . ?
O25 C21 C22 110.2(14) . . ?
O25 C21 O34 129(3) . . ?
O34 C21 H21 106.3 . . ?
O34 C21 C22 97(2) . . ?
C21 C22 H22 102.7 . . ?
C23 C22 C21 113.3(16) . . ?
C23 C22 H22 102.7 . . ?
C23 C22 O22 117(3) . . ?
O22 C22 C21 115(2) . . ?
O22 C22 H22 102.7 . . ?
C22 C23 H23 99.5 . . ?
C22 C23 C24 119.8(16) . . ?
C24 C23 H23 99.5 . . ?
O23 C23 C22 120(2) . . ?
O23 C23 H23 99.5 . . ?
O23 C23 C24 112(2) . . ?
C23 C24 H24 94.6 . . ?
C25 C24 C23 117.3(13) . . ?
C25 C24 H24 94.6 . . ?
O24 C24 C23 111.8(19) . . ?
O24 C24 H24 94.6 . . ?
O24 C24 C25 128.9(19) . . ?
C24 C25 H25 102.2 . . ?
C24 C25 C26 129(3) . . ?
C24 C25 O25 115.4(16) . . ?
C26 C25 H25 102.2 . . ?
O25 C25 H25 102.2 . . ?
O25 C25 C26 101.8(18) . . ?
C25 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
O26 C26 C25 111(2) . . ?
O26 C26 H26A 109.4 . . ?
O26 C26 H26B 109.4 . . ?
C32 C31 H31 115.0 . . ?
C32 C31 O44 108(3) . . ?
O35 C31 H31 115.0 . . ?
O35 C31 C32 114.2(19) . . ?
O35 C31 O44 86(2) . . ?
O44 C31 H31 115.0 . . ?
C31 C32 H32 106.2 . . ?
C31 C32 C33 118(2) . . ?
C33 C32 H32 106.2 . . ?
O32 C32 C31 115(3) . . ?
O32 C32 H32 106.2 . . ?
O32 C32 C33 104(3) . . ?
C32 C33 H33 106.7 . . ?
C34 C33 C32 112(2) . . ?
C34 C33 H33 106.7 . . ?
O33 C33 C32 111.8(16) . . ?
O33 C33 H33 106.7 . . ?
O33 C33 C34 112.9(14) . . ?
C33 C34 H34 107.2 . . ?
C35 C34 C33 110.3(16) . . ?
C35 C34 H34 107.2 . . ?
O34 C34 C33 125(3) . . ?
O34 C34 H34 107.2 . . ?
O34 C34 C35 99(2) . . ?
C34 C35 H35 105.7 . . ?
C36 C35 C34 112.5(10) . . ?
C36 C35 H35 105.7 . . ?
O35 C35 C34 114(2) . . ?
O35 C35 H35 105.7 . . ?
O35 C35 C36 112(2) . . ?
C35 C36 H36A 109.8 . . ?
C35 C36 H36B 109.8 . . ?
H36A C36 H36B 108.2 . . ?
O36 C36 C35 109.5(15) . . ?
O36 C36 H36A 109.8 . . ?
O36 C36 H36B 109.8 . . ?
C42 C41 H41 109.3 . . ?
C42 C41 K1 106.1(18) . 8_655 ?
K1 C41 H41 72.6 8_655 . ?
O45 C41 H41 109.3 . . ?
O45 C41 C42 121.8(19) . . ?
O45 C41 K1 49.7(15) . 8_655 ?
O45 C41 O54 108(2) . . ?
O54 C41 H41 109.3 . . ?
O54 C41 C42 98(2) . . ?
O54 C41 K1 153.3(17) . 8_655 ?
C41 C42 H42 99.6 . . ?
C41 C42 C43 110.7(15) . . ?
C43 C42 H42 99.6 . . ?
O42 C42 C41 121.7(18) . . ?
O42 C42 H42 99.6 . . ?
O42 C42 C43 119.3(18) . . ?
C42 C43 H43 101.8 . . ?
C44 C43 C42 116.2(19) . . ?
C44 C43 H43 101.8 . . ?
O43 C43 C42 113.5(17) . . ?
O43 C43 H43 101.8 . . ?
O43 C43 C44 118(2) . . ?
C43 C44 H44 105.9 . . ?
C45 C44 C43 117(2) . . ?
C45 C44 H44 105.9 . . ?
O44 C44 C43 113(2) . . ?
O44 C44 H44 105.9 . . ?
O44 C44 C45 109(2) . . ?
C44 C45 H45 104.3 . . ?
C46 C45 C44 113(2) . . ?
C46 C45 H45 104.3 . . ?
O45 C45 C44 113.4(19) . . ?
O45 C45 H45 104.3 . . ?
O45 C45 C46 116(3) . . ?
C45 C46 H46A 110.8 . . ?
C45 C46 H46B 110.8 . . ?
C45 C46 O46 105(3) . . ?
H46A C46 H46B 108.9 . . ?
O46 C46 H46A 110.8 . . ?
O46 C46 H46B 110.8 . . ?
C52 C51 H51 110.3 . . ?
O55 C51 H51 110.3 . . ?
O55 C51 C52 111.5(15) . . ?
O55 C51 O64 102(2) . . ?
O64 C51 H51 110.3 . . ?
O64 C51 C52 113(3) . . ?
C51 C52 H52 109.4 . . ?
C51 C52 C53 108(2) . . ?
C51 C52 K1 155.8(14) . 10_566 ?
C53 C52 H52 109.4 . . ?
C53 C52 K1 91.6(16) . 10_566 ?
K1 C52 H52 75.5 10_566 . ?
O52 C52 C51 106(2) . . ?
O52 C52 H52 109.4 . . ?
O52 C52 C53 114.2(17) . . ?
O52 C52 K1 51.5(14) . 10_566 ?
C52 C53 H53 112.5 . . ?
C54 C53 C52 110(2) . . ?
C54 C53 H53 112.5 . . ?
O53 C53 C52 106(3) . . ?
O53 C53 H53 112.5 . . ?
O53 C53 C54 104(3) . . ?
C53 C54 H54 106.3 . . ?
C53 C54 C55 114(2) . . ?
C55 C54 H54 106.3 . . ?
O54 C54 C53 119(2) . . ?
O54 C54 H54 106.3 . . ?
O54 C54 C55 104(2) . . ?
C54 C55 H55 101.9 . . ?
C56 C55 C54 122(2) . . ?
C56 C55 H55 101.9 . . ?
C56 C55 O55 115(2) . . ?
O55 C55 C54 110.0(17) . . ?
O55 C55 H55 101.9 . . ?
C55 C56 H56A 114.1 . . ?
C55 C56 H56B 114.1 . . ?
H56A C56 H56B 111.3 . . ?
O56 C56 C55 87(2) . . ?
O56 C56 H56A 114.1 . . ?
O56 C56 H56B 114.1 . . ?
C62 C61 H61 108.7 . . ?
C62 C61 K1 98(2) . 9_565 ?
K1 C61 H61 68.2 9_565 . ?
O65 C61 H61 108.7 . . ?
O65 C61 C62 113(3) . . ?
O65 C61 K1 50.8(18) . 9_565 ?
O74 C61 H61 108.7 . . ?
O74 C61 C62 94(3) . . ?
O74 C61 K1 168(2) . 9_565 ?
O74 C61 O65 123(3) . . ?
C61 C62 H62 108.6 . . ?
C61 C62 C63 110(2) . . ?
C63 C62 H62 108.6 . . ?
O62 C62 C61 111(3) . . ?
O62 C62 H62 108.6 . . ?
O62 C62 C63 110(3) . . ?
C62 C63 H63 110.4 . . ?
C64 C63 C62 111(3) . . ?
C64 C63 H63 110.4 . . ?
O63 C63 C62 106(3) . . ?
O63 C63 H63 110.4 . . ?
O63 C63 C64 108(3) . . ?
C63 C64 H64 112.7 . . ?
C63 C64 C65 108(2) . . ?
C63 C64 O64 106(3) . . ?
C65 C64 H64 112.7 . . ?
O64 C64 H64 112.7 . . ?
O64 C64 C65 105(3) . . ?
C64 C65 H65 109.6 . . ?
C64 C65 C66 116(3) . . ?
C66 C65 H65 109.6 . . ?
O65 C65 C64 106(2) . . ?
O65 C65 H65 109.6 . . ?
O65 C65 C66 106(3) . . ?
C65 C66 H66A 112.1 . . ?
C65 C66 H66B 112.1 . . ?
C65 C66 O66 98(3) . . ?
H66A C66 H66B 109.8 . . ?
O66 C66 H66A 112.1 . . ?
O66 C66 H66B 112.1 . . ?
C72 C71 H71 105.6 . . ?
O4 C71 H71 105.6 . . ?
O4 C71 C72 109(2) . . ?
O75 C71 H71 105.6 . . ?
O75 C71 C72 117.6(13) . . ?
O75 C71 O4 113(2) . . ?
C71 C72 H72 108.5 . . ?
C73 C72 C71 111(2) . . ?
C73 C72 H72 108.5 . . ?
O72 C72 C71 106(2) . . ?
O72 C72 H72 108.5 . . ?
O72 C72 C73 114(3) . . ?
C72 C73 H73 104.5 . . ?
C72 C73 C74 106(3) . . ?
C74 C73 H73 104.5 . . ?
O73 C73 C72 118(2) . . ?
O73 C73 H73 104.5 . . ?
O73 C73 C74 119(2) . . ?
C73 C74 H74 104.8 . . ?
C73 C74 C75 118(2) . . ?
C73 C74 O74 101(2) . . ?
C75 C74 H74 104.8 . . ?
C75 C74 O74 122(3) . . ?
O74 C74 H74 104.8 . . ?
C74 C75 H75 111.8 . . ?
C74 C75 C76 111.0(19) . . ?
C76 C75 H75 111.8 . . ?
O75 C75 C74 112(3) . . ?
O75 C75 H75 111.8 . . ?
O75 C75 C76 98(2) . . ?
C75 C76 H76A 107.7 . . ?
C75 C76 H76B 107.7 . . ?
H76A C76 H76B 107.1 . . ?
O76 C76 C75 119(2) . . ?
O76 C76 H76A 107.7 . . ?
O76 C76 H76B 107.7 . . ?
C52 K1 C41 81.4(7) 10_566 15_664 ?
C61 K1 C41 146.7(8) 14_654 15_664 ?
C61 K1 C52 113.1(8) 14_654 10_566 ?
O12 K1 C41 85.6(7) . 15_664 ?
O12 K1 C52 128.9(8) . 10_566 ?
O12 K1 C61 104.6(8) . 14_654 ?
O12 K1 O13 55.8(7) . . ?
O12 K1 O45 90.4(8) . 15_664 ?
O12 K1 O46 74.5(8) . 15_664 ?
O12 K1 O53 91.1(9) . 10_566 ?
O13 K1 C41 140.5(6) . 15_664 ?
O13 K1 C52 114.4(8) . 10_566 ?
O13 K1 C61 62.7(9) . 14_654 ?
O13 K1 O53 111.2(8) . 10_566 ?
O45 K1 C41 22.9(5) 15_664 15_664 ?
O45 K1 C52 95.7(8) 15_664 10_566 ?
O45 K1 C61 124.0(9) 15_664 14_654 ?
O45 K1 O13 144.1(7) 15_664 . ?
O45 K1 O46 60.6(8) 15_664 15_664 ?
O45 K1 O53 78.0(8) 15_664 10_566 ?
O46 K1 C41 80.8(8) 15_664 15_664 ?
O46 K1 C52 149.1(9) 15_664 10_566 ?
O46 K1 C61 72.0(9) 15_664 14_654 ?
O46 K1 O13 95.3(8) 15_664 . ?
O46 K1 O53 135.4(9) 15_664 10_566 ?
O52 K1 C41 105.9(7) 10_566 15_664 ?
O52 K1 C52 24.5(5) 10_566 10_566 ?
O52 K1 C61 91.1(8) 10_566 14_654 ?
O52 K1 O12 131.4(9) 10_566 . ?
O52 K1 O13 95.3(8) 10_566 . ?
O52 K1 O45 118.4(8) 10_566 15_664 ?
O52 K1 O46 152.9(9) 10_566 15_664 ?
O52 K1 O53 61.6(8) 10_566 10_566 ?
O53 K1 C41 55.8(7) 10_566 15_664 ?
O53 K1 C52 41.8(7) 10_566 10_566 ?
O53 K1 C61 152.0(9) 10_566 14_654 ?
O65 K1 C41 124.1(8) 14_654 15_664 ?
O65 K1 C52 106.8(8) 14_654 10_566 ?
O65 K1 C61 24.7(6) 14_654 14_654 ?
O65 K1 O12 121.1(9) 14_654 . ?
O65 K1 O13 87.3(9) 14_654 . ?
O65 K1 O45 102.9(9) 14_654 15_664 ?
O65 K1 O46 64.3(9) 14_654 15_664 ?
O65 K1 O52 91.5(8) 14_654 10_566 ?
O65 K1 O53 147.6(9) 14_654 10_566 ?
O66 K1 C41 78.2(7) 14_654 15_664 ?
O66 K1 C52 65.3(8) 14_654 10_566 ?
O66 K1 C61 81.2(9) 14_654 14_654 ?
O66 K1 O12 156.7(10) 14_654 . ?
O66 K1 O13 141.1(9) 14_654 . ?
O66 K1 O45 68.4(8) 14_654 15_664 ?
O66 K1 O46 86.4(9) 14_654 15_664 ?
O66 K1 O52 69.9(9) 14_654 10_566 ?
O66 K1 O53 93.4(9) 14_654 10_566 ?
O66 K1 O65 58.5(9) 14_654 14_654 ?
O5 K2 O5 114.8(11) . 17_655 ?
O5 K2 O72 112.3(7) 17_655 6_556 ?
O5 K2 O72 82.1(6) . 6_556 ?
O5 K2 O72 82.1(6) 17_655 14_654 ?
O5 K2 O72 112.3(7) . 14_654 ?
O5 K2 O73 136.1(6) . 6_556 ?
O5 K2 O73 136.1(6) 17_655 14_654 ?
O5 K2 O73 79.2(7) 17_655 6_556 ?
O5 K2 O73 79.2(7) . 14_654 ?
O6 K2 O5 58.1(9) . . ?
O6 K2 O5 78.8(8) . 17_655 ?
O6 K2 O5 58.1(9) 17_655 17_655 ?
O6 K2 O5 78.8(8) 17_655 . ?
O6 K2 O6 95.8(15) . 17_655 ?
O6 K2 O72 150.8(10) . 14_654 ?
O6 K2 O72 150.8(10) 17_655 6_556 ?
O6 K2 O72 55.1(8) 17_655 14_654 ?
O6 K2 O72 55.1(8) . 6_556 ?
O6 K2 O73 135.4(9) 17_655 6_556 ?
O6 K2 O73 87.2(9) 17_655 14_654 ?
O6 K2 O73 87.2(9) . 6_556 ?
O6 K2 O73 135.4(9) . 14_654 ?
O72 K2 O72 154.1(11) 14_654 6_556 ?
O73 K2 O72 54.8(7) 6_556 6_556 ?
O73 K2 O72 110.8(7) 6_556 14_654 ?
O73 K2 O72 54.8(7) 14_654 14_654 ?
O73 K2 O72 110.8(7) 14_654 6_556 ?
O73 K2 O73 120.8(12) 14_654 6_556 ?
O25 K3 O25 107.9(11) . 18_545 ?
O25 K3 O26 55.0(8) . . ?
O25 K3 O26 54.9(8) 18_545 18_545 ?
O25 K3 O26 62.2(8) 18_545 . ?
O25 K3 O26 62.2(8) . 18_545 ?
O25 K3 O33 146.8(7) . 15_664 ?
O25 K3 O33 74.9(7) . 5_766 ?
O25 K3 O33 146.8(7) 18_545 5_766 ?
O25 K3 O33 74.9(7) 18_545 15_664 ?
O26 K3 O26 55.5(12) . 18_545 ?
O26 K3 O33 103.0(8) 18_545 5_766 ?
O26 K3 O33 129.8(9) . 5_766 ?
O26 K3 O33 129.8(9) 18_545 15_664 ?
O26 K3 O33 103.0(8) . 15_664 ?
O32 K3 O25 113.6(8) 15_664 18_545 ?
O32 K3 O25 92.4(8) 15_664 . ?
O32 K3 O25 113.6(8) 5_766 . ?
O32 K3 O25 92.4(8) 5_766 18_545 ?
O32 K3 O26 139.7(11) 15_664 18_545 ?
O32 K3 O26 139.7(11) 5_766 . ?
O32 K3 O26 84.4(9) 15_664 . ?
O32 K3 O26 84.4(9) 5_766 18_545 ?
O32 K3 O32 135.8(15) 15_664 5_766 ?
O32 K3 O33 99.1(9) 5_766 15_664 ?
O32 K3 O33 99.1(9) 15_664 5_766 ?
O32 K3 O33 58.2(8) 15_664 15_664 ?
O32 K3 O33 58.2(8) 5_766 5_766 ?
O33 K3 O33 121.4(14) 15_664 5_766 ?
C2 O2 H2A 109.5 . . ?
C3 O3 H3A 109.5 . . ?
C4 O4 C71 114.9(17) . . ?
C1 O5 K2 107.8(16) . . ?
C5 O5 C1 122.0(19) . . ?
C5 O5 K2 112(2) . . ?
C6 O6 K2 121(3) . . ?
C6 O6 H6 109.5 . . ?
K2 O6 H6 128.7 . . ?
C12 O12 K1 120(2) . . ?
C12 O12 H12A 109.5 . . ?
K1 O12 H12A 121.1 . . ?
C13 O13 K1 116.5(16) . . ?
C13 O13 H13A 109.5 . . ?
K1 O13 H13A 133.5 . . ?
C1 O14 C14 115.0(17) . . ?
C15 O15 C11 111.2(15) . . ?
C16 O16 H16 109.5 . . ?
C22 O22 H22A 109.5 . . ?
C23 O23 H23A 109.5 . . ?
C24 O24 C11 122(3) . . ?
C21 O25 C25 107(2) . . ?
C21 O25 K3 120.5(18) . . ?
C25 O25 K3 118(2) . . ?
C26 O26 K3 123.1(19) . . ?
C26 O26 H26 109.5 . . ?
K3 O26 H26 122.4 . . ?
C32 O32 K3 118(2) . 8_655 ?
C32 O32 H32A 109.5 . . ?
K3 O32 H32A 129.6 8_655 . ?
C33 O33 K3 114.7(13) . 8_655 ?
C33 O33 H33A 109.5 . . ?
K3 O33 H33A 121.7 8_655 . ?
C21 O34 C34 115.7(15) . . ?
C31 O35 C35 116.7(13) . . ?
C36 O36 H36 109.5 . . ?
C42 O42 H42A 109.5 . . ?
C43 O43 H43A 109.5 . . ?
C44 O44 C31 114.9(17) . . ?
C41 O45 K1 107.4(18) . 8_655 ?
C45 O45 C41 116(2) . . ?
C45 O45 K1 113(2) . 8_655 ?
C46 O46 K1 118.5(19) . 8_655 ?
C46 O46 H46 109.5 . . ?
K1 O46 H46 37.0 8_655 . ?
C52 O52 K1 104.0(17) . 10_566 ?
C52 O52 H52A 109.5 . . ?
K1 O52 H52A 18.1 10_566 . ?
C53 O53 K1 112.0(18) . 10_566 ?
C53 O53 H53A 109.5 . . ?
K1 O53 H53A 79.1 10_566 . ?
C54 O54 C41 119.5(18) . . ?
C51 O55 C55 114.2(13) . . ?
C56 O56 H56 109.5 . . ?
C62 O62 H62A 109.5 . . ?
C63 O63 H63A 109.5 . . ?
C51 O64 C64 112(2) . . ?
C61 O65 C65 115(3) . . ?
C61 O65 K1 104(2) . 9_565 ?
C65 O65 K1 121(2) . 9_565 ?
C66 O66 K1 124(2) . 9_565 ?
C66 O66 H66 109.5 . . ?
K1 O66 H66 119.2 9_565 . ?
C72 O72 K2 111.5(16) . 9_565 ?
C72 O72 H72A 109.5 . . ?
K2 O72 H72A 18.5 9_565 . ?
C73 O73 K2 121.0(15) . 9_565 ?
C73 O73 H73A 109.5 . . ?
K2 O73 H73A 98.0 9_565 . ?
C61 O74 C74 120(3) . . ?
C71 O75 C75 103(2) . . ?
C76 O76 H76 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -47(5) . . . . ?
C1 C2 C3 O3 176(3) . . . . ?
C2 C1 O5 C5 -42(3) . . . . ?
C2 C1 O5 K2 89.8(18) . . . . ?
C2 C1 O14 C14 -136(2) . . . . ?
C2 C3 C4 C5 42(4) . . . . ?
C2 C3 C4 O4 165(3) . . . . ?
C3 C4 C5 C6 -169(3) . . . . ?
C3 C4 C5 O5 -40(4) . . . . ?
C3 C4 O4 C71 140(2) . . . . ?
C4 C5 C6 O6 63(4) . . . . ?
C4 C5 O5 C1 47(4) . . . . ?
C4 C5 O5 K2 -83(3) . . . . ?
C5 C4 O4 C71 -101(3) . . . . ?
C5 C6 O6 K2 63(3) . . . . ?
C6 C5 O5 C1 -177(3) . . . . ?
C6 C5 O5 K2 53(3) . . . . ?
C11 C12 C13 C14 -39(4) . . . . ?
C11 C12 C13 O13 -175(3) . . . . ?
C11 C12 O12 K1 165(2) . . . . ?
C12 C11 O15 C15 -67(3) . . . . ?
C12 C11 O24 C24 -132(2) . . . . ?
C12 C13 C14 C15 47(4) . . . . ?
C12 C13 C14 O14 173(3) . . . . ?
C12 C13 O13 K1 -18(4) . . . . ?
C13 C12 O12 K1 -63(3) . . . . ?
C13 C14 C15 C16 -167(3) . . . . ?
C13 C14 C15 O15 -58(4) . . . . ?
C13 C14 O14 C1 95(3) . . . . ?
C14 C13 O13 K1 -148(2) . . . . ?
C14 C15 C16 O16 65(4) . . . . ?
C14 C15 O15 C11 64(3) . . . . ?
C15 C14 O14 C1 -128(3) . . . . ?
C16 C15 O15 C11 -177(2) . . . . ?
C21 C22 C23 C24 -22(6) . . . . ?
C21 C22 C23 O23 -168(3) . . . . ?
C22 C21 O25 C25 -67(3) . . . . ?
C22 C21 O25 K3 72(3) . . . . ?
C22 C21 O34 C34 -113(2) . . . . ?
C22 C23 C24 C25 12(7) . . . . ?
C22 C23 C24 O24 177(4) . . . . ?
C23 C24 C25 C26 -162(4) . . . . ?
C23 C24 C25 O25 -30(6) . . . . ?
C23 C24 O24 C11 117(4) . . . . ?
C24 C25 C26 O26 85(4) . . . . ?
C24 C25 O25 C21 57(4) . . . . ?
C24 C25 O25 K3 -82(3) . . . . ?
C25 C24 O24 C11 -80(6) . . . . ?
C25 C26 O26 K3 26(4) . . . . ?
C26 C25 O25 C21 -158(2) . . . . ?
C26 C25 O25 K3 62(3) . . . . ?
C31 C32 C33 C34 -43(4) . . . . ?
C31 C32 C33 O33 -171(3) . . . . ?
C31 C32 O32 K3 168(2) . . . 8_655 ?
C32 C31 O35 C35 -38(4) . . . . ?
C32 C31 O44 C44 -113(3) . . . . ?
C32 C33 C34 C35 50(4) . . . . ?
C32 C33 C34 O34 168(3) . . . . ?
C32 C33 O33 K3 -34(3) . . . 8_655 ?
C33 C32 O32 K3 -61(3) . . . 8_655 ?
C33 C34 C35 C36 177(3) . . . . ?
C33 C34 C35 O35 -54(4) . . . . ?
C33 C34 O34 C21 113(3) . . . . ?
C34 C33 O33 K3 -161(2) . . . 8_655 ?
C34 C35 C36 O36 68(4) . . . . ?
C34 C35 O35 C31 49(3) . . . . ?
C35 C34 O34 C21 -125(3) . . . . ?
C36 C35 O35 C31 178(2) . . . . ?
C41 C42 C43 C44 -31(4) . . . . ?
C41 C42 C43 O43 -173(3) . . . . ?
C42 C41 O45 C45 -42(4) . . . . ?
C42 C41 O45 K1 84(3) . . . 8_655 ?
C42 C41 O54 C54 -119(3) . . . . ?
C42 C43 C44 C45 39(4) . . . . ?
C42 C43 C44 O44 166(3) . . . . ?
C43 C44 C45 C46 180(3) . . . . ?
C43 C44 C45 O45 -46(4) . . . . ?
C43 C44 O44 C31 115(3) . . . . ?
C44 C45 C46 O46 74(3) . . . . ?
C44 C45 O45 C41 45(4) . . . . ?
C44 C45 O45 K1 -79(3) . . . 8_655 ?
C45 C44 O44 C31 -114(3) . . . . ?
C45 C46 O46 K1 35(3) . . . 8_655 ?
C46 C45 O45 C41 178(3) . . . . ?
C46 C45 O45 K1 54(3) . . . 8_655 ?
C51 C52 C53 C54 -57(3) . . . . ?
C51 C52 C53 O53 -169(3) . . . . ?
C51 C52 O52 K1 169.6(19) . . . 10_566 ?
C52 C51 O55 C55 -57(3) . . . . ?
C52 C51 O64 C64 -112(3) . . . . ?
C52 C53 C54 C55 56(4) . . . . ?
C52 C53 C54 O54 180(3) . . . . ?
C52 C53 O53 K1 -32(3) . . . 10_566 ?
C53 C52 O52 K1 -71(3) . . . 10_566 ?
C53 C54 C55 C56 168(3) . . . . ?
C53 C54 C55 O55 -52(3) . . . . ?
C53 C54 O54 C41 118(3) . . . . ?
C54 C53 O53 K1 -146.7(16) . . . 10_566 ?
C54 C55 C56 O56 65(3) . . . . ?
C54 C55 O55 C51 51(3) . . . . ?
C55 C54 O54 C41 -113(3) . . . . ?
C56 C55 O55 C51 -166(3) . . . . ?
C61 C62 C63 C64 -54(4) . . . . ?
C61 C62 C63 O63 -171(3) . . . . ?
C62 C61 O65 C65 -54(4) . . . . ?
C62 C61 O65 K1 82(3) . . . 9_565 ?
C62 C61 O74 C74 -151(3) . . . . ?
C62 C63 C64 C65 64(4) . . . . ?
C62 C63 C64 O64 175(3) . . . . ?
C63 C64 C65 C66 179(3) . . . . ?
C63 C64 C65 O65 -63(4) . . . . ?
C63 C64 O64 C51 128(3) . . . . ?
C64 C65 C66 O66 61(4) . . . . ?
C64 C65 O65 C61 60(4) . . . . ?
C64 C65 O65 K1 -67(3) . . . 9_565 ?
C65 C64 O64 C51 -119(3) . . . . ?
C65 C66 O66 K1 44(3) . . . 9_565 ?
C66 C65 O65 C61 -176(3) . . . . ?
C66 C65 O65 K1 56(3) . . . 9_565 ?
C71 C72 C73 C74 -50(4) . . . . ?
C71 C72 C73 O73 175(3) . . . . ?
C71 C72 O72 K2 -166.4(19) . . . 9_565 ?
C72 C71 O4 C4 -114(2) . . . . ?
C72 C71 O75 C75 -62(3) . . . . ?
C72 C73 C74 C75 50(5) . . . . ?
C72 C73 C74 O74 -175(3) . . . . ?
C72 C73 O73 K2 -35(4) . . . 9_565 ?
C73 C72 O72 K2 -44(3) . . . 9_565 ?
C73 C74 C75 C76 -163(3) . . . . ?
C73 C74 C75 O75 -55(4) . . . . ?
C73 C74 O74 C61 123(4) . . . . ?
C74 C73 O73 K2 -164(3) . . . 9_565 ?
C74 C75 C76 O76 48(4) . . . . ?
C74 C75 O75 C71 54(3) . . . . ?
C75 C74 O74 C61 -104(4) . . . . ?
C76 C75 O75 C71 170(2) . . . . ?
K1 C41 C42 C43 86(3) 8_655 . . . ?
K1 C41 C42 O42 -126(3) 8_655 . . . ?
K1 C41 O45 C45 -127(3) 8_655 . . . ?
K1 C41 O54 C54 84(4) 8_655 . . . ?
K1 C52 C53 C54 137(3) 10_566 . . . ?
K1 C52 C53 O53 26(2) 10_566 . . . ?
K1 C61 C62 C63 99(3) 9_565 . . . ?
K1 C61 C62 O62 -139(3) 9_565 . . . ?
K1 C61 O65 C65 -136(3) 9_565 . . . ?
K1 C61 O74 C74 33(14) 9_565 . . . ?
O2 C2 C3 C4 -176(3) . . . . ?
O2 C2 C3 O3 47(6) . . . . ?
O3 C3 C4 C5 -175(3) . . . . ?
O3 C3 C4 O4 -52(3) . . . . ?
O4 C4 C5 C6 73(4) . . . . ?
O4 C4 C5 O5 -159(3) . . . . ?
O4 C71 C72 C73 -65(3) . . . . ?
O4 C71 C72 O72 59(3) . . . . ?
O4 C71 O75 C75 65(3) . . . . ?
O5 C1 C2 C3 41(4) . . . . ?
O5 C1 C2 O2 179(3) . . . . ?
O5 C1 O14 C14 118(2) . . . . ?
O5 C5 C6 O6 -71(4) . . . . ?
O12 C12 C13 C14 -176(3) . . . . ?
O12 C12 C13 O13 48(4) . . . . ?
O13 C13 C14 C15 -180(3) . . . . ?
O13 C13 C14 O14 -53(4) . . . . ?
O14 C1 C2 C3 -62(4) . . . . ?
O14 C1 C2 O2 76(3) . . . . ?
O14 C1 O5 C5 71(3) . . . . ?
O14 C1 O5 K2 -157.1(13) . . . . ?
O14 C14 C15 C16 65(3) . . . . ?
O14 C14 C15 O15 173(2) . . . . ?
O15 C11 C12 C13 52(4) . . . . ?
O15 C11 C12 O12 180(3) . . . . ?
O15 C11 O24 C24 112(3) . . . . ?
O15 C15 C16 O16 -42(4) . . . . ?
O22 C22 C23 C24 -160(4) . . . . ?
O22 C22 C23 O23 54(6) . . . . ?
O23 C23 C24 C25 161(4) . . . . ?
O23 C23 C24 O24 -34(6) . . . . ?
O24 C11 C12 C13 -68(3) . . . . ?
O24 C11 C12 O12 60(4) . . . . ?
O24 C11 O15 C15 42(3) . . . . ?
O24 C24 C25 C26 35(7) . . . . ?
O24 C24 C25 O25 168(4) . . . . ?
O25 C21 C22 C23 50(4) . . . . ?
O25 C21 C22 O22 -170(3) . . . . ?
O25 C21 O34 C34 124(3) . . . . ?
O25 C25 C26 O26 -52(4) . . . . ?
O32 C32 C33 C34 -172(3) . . . . ?
O32 C32 C33 O33 60(4) . . . . ?
O33 C33 C34 C35 177(3) . . . . ?
O33 C33 C34 O34 -65(4) . . . . ?
O34 C21 C22 C23 -85(4) . . . . ?
O34 C21 C22 O22 54(4) . . . . ?
O34 C21 O25 C25 51(3) . . . . ?
O34 C21 O25 K3 -170.1(19) . . . . ?
O34 C34 C35 C36 44(3) . . . . ?
O34 C34 C35 O35 173(2) . . . . ?
O35 C31 C32 C33 36(5) . . . . ?
O35 C31 C32 O32 159(3) . . . . ?
O35 C31 O44 C44 133(2) . . . . ?
O35 C35 C36 O36 -63(3) . . . . ?
O42 C42 C43 C44 180(3) . . . . ?
O42 C42 C43 O43 38(5) . . . . ?
O43 C43 C44 C45 179(3) . . . . ?
O43 C43 C44 O44 -53(4) . . . . ?
O44 C31 C32 C33 -58(4) . . . . ?
O44 C31 C32 O32 66(4) . . . . ?
O44 C31 O35 C35 70(3) . . . . ?
O44 C44 C45 C46 51(3) . . . . ?
O44 C44 C45 O45 -175(3) . . . . ?
O45 C41 C42 C43 33(4) . . . . ?
O45 C41 C42 O42 -179(3) . . . . ?
O45 C41 O54 C54 113(3) . . . . ?
O45 C45 C46 O46 -59(3) . . . . ?
O52 C52 C53 C54 -175(3) . . . . ?
O52 C52 C53 O53 74(4) . . . . ?
O53 C53 C54 C55 169(3) . . . . ?
O53 C53 C54 O54 -68(3) . . . . ?
O54 C41 C42 C43 -84(3) . . . . ?
O54 C41 C42 O42 64(4) . . . . ?
O54 C41 O45 C45 70(3) . . . . ?
O54 C41 O45 K1 -163.2(16) . . . 8_655 ?
O54 C54 C55 C56 37(4) . . . . ?
O54 C54 C55 O55 177(2) . . . . ?
O55 C51 C52 C53 58(3) . . . . ?
O55 C51 C52 K1 -159(4) . . . 10_566 ?
O55 C51 C52 O52 -179(2) . . . . ?
O55 C51 O64 C64 128(2) . . . . ?
O55 C55 C56 O56 -73(3) . . . . ?
O62 C62 C63 C64 -177(3) . . . . ?
O62 C62 C63 O63 66(4) . . . . ?
O63 C63 C64 C65 -180(3) . . . . ?
O63 C63 C64 O64 -69(4) . . . . ?
O64 C51 C52 C53 -55(3) . . . . ?
O64 C51 C52 K1 88(6) . . . 10_566 ?
O64 C51 C52 O52 68(3) . . . . ?
O64 C51 O55 C55 64(3) . . . . ?
O64 C64 C65 C66 67(4) . . . . ?
O64 C64 C65 O65 -176(3) . . . . ?
O65 C61 C62 C63 48(4) . . . . ?
O65 C61 C62 O62 170(3) . . . . ?
O65 C61 O74 C74 89(4) . . . . ?
O65 C65 C66 O66 -56(3) . . . . ?
O72 C72 C73 C74 -170(3) . . . . ?
O72 C72 C73 O73 55(4) . . . . ?
O73 C73 C74 C75 -176(3) . . . . ?
O73 C73 C74 O74 -41(5) . . . . ?
O74 C61 C62 C63 -81(3) . . . . ?
O74 C61 C62 O62 41(4) . . . . ?
O74 C61 O65 C65 57(4) . . . . ?
O74 C61 O65 K1 -167(3) . . . 9_565 ?
O74 C74 C75 C76 71(4) . . . . ?
O74 C74 C75 O75 179(3) . . . . ?
O75 C71 C72 C73 65(4) . . . . ?
O75 C71 C72 O72 -171(3) . . . . ?
O75 C71 O4 C4 114(3) . . . . ?
O75 C75 C76 O76 -69(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.076 -0.374 -0.108 21275.4 1582.4 ?


_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 2.496
_oxdiff_exptl_absorpt_empirical_full_min 0.599
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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#######################################################################

data_CDMOF_a_0_57GPa
_database_code_depnum_ccdc_archive 'CCDC 1529149'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7

# start Validation Reply Form
_vrf_REFNR01_CDMOF_a_0_57GPa     
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_RINTA01_CDMOF_a_0_57GPa     
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: 'Crystals of this compound dissolve when compressed;
pressure-induced dissolution influence the crystal quality 
and therefore quality of collected data'
;
_vrf_THETM01_CDMOF_a_0_57GPa     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT029_CDMOF_a_0_57GPa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.790 Note  
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT090_CDMOF_a_0_57GPa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.38 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT201_CDMOF_a_0_57GPa     
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT241_CDMOF_a_0_57GPa     
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O4 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT242_CDMOF_a_0_57GPa     
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C11 Check 
RESPONSE: 'Poor data quality'
;
_vrf_PLAT306_CDMOF_a_0_57GPa     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_0_57GPa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.039 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT910_CDMOF_a_0_57GPa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          31 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample limiting the range of 
collected reflections'
;
_vrf_PLAT911_CDMOF_a_0_57GPa     
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.249         16 Report
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample limiting the range of 
collected reflections'
;
# end Validation Reply Form
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   31.179(11)
_cell_length_b                   31.179(11)
_cell_length_c                   31.179(11)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30309(18)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    149
_cell_measurement_temperature    295
_cell_measurement_theta_max      8.7690
_cell_measurement_theta_min      4.6480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?

# EXPERIMENTAL DATA 
_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.1GPa and then
compressed to 0.57GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.926
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8928
_exptl_crystal_recrystallization_method 
'Compressed crystal that was grown in situ from methano:water solution in the diamond-anvil cell at 0.1 GPa.'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3847
_diffrn_reflns_av_unetI/netI     0.1671
_diffrn_reflns_Laue_measured_fraction_full 0.790
_diffrn_reflns_Laue_measured_fraction_max 0.790
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3862
_diffrn_reflns_point_group_measured_fraction_full 0.823
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        10.213
_diffrn_reflns_theta_max         10.213
_diffrn_reflns_theta_min         4.714
_diffrn_ambient_temperature      295
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         570000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.790
_diffrn_measured_fraction_theta_max 0.790
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   10.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   10.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   10.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   10.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   10.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   10.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   10.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   10.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   10.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   10.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   10.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   10.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   10.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   10.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   10.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   10.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0026630000
_diffrn_orient_matrix_UB_12      0.0015808000
_diffrn_orient_matrix_UB_13      0.0225279000
_diffrn_orient_matrix_UB_21      0.0187021000
_diffrn_orient_matrix_UB_22      0.0125278000
_diffrn_orient_matrix_UB_23      -0.0033899000
_diffrn_orient_matrix_UB_31      -0.0125930000
_diffrn_orient_matrix_UB_32      0.0189554000
_diffrn_orient_matrix_UB_33      0.0002699000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          
'high-pressure measurement in diamond-anvil cell at 0.59 GPa'
_reflns_Friedel_coverage         0.564
_reflns_Friedel_fraction_full    0.887
_reflns_Friedel_fraction_max     0.887
_reflns_number_gt                254
_reflns_number_total             283
_reflns_odcompleteness_completeness 83.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     10.19
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.056
_refine_diff_density_min         -0.048
_refine_diff_density_rms         0.012
_refine_ls_abs_structure_details 
;
 Flack x determined using 55 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         283
_refine_ls_number_restraints     71
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0640
_refine_ls_restrained_S_all      1.501
_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/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1406
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
 resulting in a low data:parameter ratio.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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
 C16-O16
 1.45 with sigma of 0.002
 C6-C5
 1.5 with sigma of 0.002
 C6-O6
 1.45 with sigma of 0.002
 C16-C15
 1.5 with sigma of 0.002
 C14-C15
 1.5 with sigma of 0.002
 O14-C15
 2.4 with sigma of 0.02
 C14-O14
 1.45 with sigma of 0.002
 C11-O4
 1.45 with sigma of 0.002
 C11-C14
 3 with sigma of 0.02
 C4-O4
 1.45 with sigma of 0.002
 C4-C5
 1.5 with sigma of 0.002
 C12-O4
 2 with sigma of 0.02
 C12-C15
 3 with sigma of 0.02
 C15-C12
 3 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.002
 C5-C1
 2.3 with sigma of 0.002
 C1-C4
 2.8 with sigma of 0.02
 O5-C6
 2.5 with sigma of 0.02
 O15-C16
 2.2 with sigma of 0.02
 O5-C5
 1.45 with sigma of 0.002
 O15-C15
 1.45 with sigma of 0.002
 O15-C11
 1.45 with sigma of 0.002
 O5-C1
 1.45 with sigma of 0.002
 C14-C13
 1.5 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.02
 C2-C5
 3 with sigma of 0.02
 C5-C2
 3 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.002
 O15-C13
 3 with sigma of 0.02
 O13-C13
 1.45 with sigma of 0.002
 O3-C3
 1.45 with sigma of 0.002
 C4-C3
 1.5 with sigma of 0.002
 O5-C3
 3 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.002
 C2-O3
 2.3 with sigma of 0.02
 C2-O2
 1.45 with sigma of 0.002
 O2-C3
 2.2 with sigma of 0.02
 C12-O12
 1.45 with sigma of 0.02
 O12-C12
 1.45 with sigma of 0.02
 O14-C15
 2.5 with sigma of 0.04
 C15-C11
 2.4 with sigma of 0.02
 C11-C4
 2.5 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.02
 C4-C11
 2.5 with sigma of 0.04
 O4-C5
 2.5 with sigma of 0.04
 O4-C12
 2.5 with sigma of 0.04
 C1-C5
 2.5 with sigma of 0.02
 C14-O15
 2.4 with sigma of 0.02
 O5-C4
 2.5 with sigma of 0.02
 O15-C12
 2.4 with sigma of 0.02
 O4-O15
 2.5 with sigma of 0.04
 O13-C14
 2.5 with sigma of 0.04
 O13-C12
 2.5 with sigma of 0.04
 C13-C15
 2.4 with sigma of 0.02
 C13-O14
 2.5 with sigma of 0.04
 C11-C13
 2.4 with sigma of 0.02
 C4-C2
 2.5 with sigma of 0.02
 C2-O5
 2.5 with sigma of 0.02
 C5-C3
 2.5 with sigma of 0.02
 O4-C3
 2.5 with sigma of 0.04
 C3-C1
 2.5 with sigma of 0.02
 O2-C1
 2.5 with sigma of 0.04
 O2-C3
 2.5 with sigma of 0.04
 O12-C13
 2.4 with sigma of 0.04
 O12-C11
 2.6 with sigma of 0.04
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)=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(H16B,H16A)
5.c Tetrahedral OH refined with riding coordinates:
 O2(H2A), O3(H3A), O6(H6), O12(H12A), O13(H13A), O16(H16)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8572(9) 0.6770(8) 0.6301(10) 0.222(10) Uiso 1 1 d D . . . .
H1 H 0.8501 0.7076 0.6288 0.266 Uiso 1 1 calc R . . . .
C2 C 0.8957(8) 0.6758(7) 0.6590(10) 0.222(10) Uiso 1 1 d D . . . .
H2 H 0.8908 0.6935 0.6845 0.266 Uiso 1 1 calc R . . . .
C3 C 0.9047(7) 0.6303(8) 0.6716(11) 0.222(10) Uiso 1 1 d D . . . .
H3 H 0.9138 0.6210 0.6430 0.266 Uiso 1 1 calc R . . . .
C4 C 0.8664(8) 0.6012(7) 0.6738(11) 0.222(10) Uiso 1 1 d D . . . .
H4 H 0.8561 0.6078 0.7027 0.266 Uiso 1 1 calc R . . . .
C5 C 0.8272(7) 0.6121(8) 0.6481(11) 0.222(10) Uiso 1 1 d D . . . .
H5 H 0.8353 0.6043 0.6188 0.266 Uiso 1 1 calc R . . . .
C6 C 0.7886(9) 0.5845(10) 0.6566(13) 0.222(10) Uiso 1 1 d D . . . .
H6A H 0.7653 0.5899 0.6367 0.266 Uiso 1 1 calc R . . . .
H6B H 0.7954 0.5541 0.6572 0.266 Uiso 1 1 calc R . . . .
C11 C 0.8665(9) 0.5373(7) 0.7201(9) 0.222(10) Uiso 1 1 d D . . . .
H11 H 0.8688 0.5588 0.7429 0.266 Uiso 1 1 calc R . . . .
C12 C 0.9064(8) 0.5106(9) 0.7169(11) 0.222(10) Uiso 1 1 d D . . . .
H12 H 0.9138 0.5004 0.7457 0.266 Uiso 1 1 calc R . . . .
C13 C 0.9004(8) 0.4723(10) 0.6882(13) 0.222(10) Uiso 1 1 d D . . . .
H13 H 0.9038 0.4808 0.6582 0.266 Uiso 1 1 calc R . . . .
C14 C 0.8580(9) 0.4498(8) 0.6942(11) 0.222(10) Uiso 1 1 d D . . . .
H14 H 0.8574 0.4373 0.7231 0.266 Uiso 1 1 calc R . . . .
C15 C 0.8216(7) 0.4809(10) 0.6903(9) 0.222(10) Uiso 1 1 d D . . . .
H15 H 0.8157 0.4910 0.6611 0.266 Uiso 1 1 calc R . . . .
C16 C 0.7852(11) 0.4577(11) 0.7115(12) 0.222(10) Uiso 1 1 d D . . . .
H16B H 0.7609 0.4766 0.7069 0.266 Uiso 1 1 calc R . . . .
H16A H 0.7802 0.4333 0.6928 0.266 Uiso 1 1 calc R . . . .
K1 K 0.8046(3) 0.5000 0.8046(3) 0.268(11) Uani 1 2 d S TU P . .
O2 O 0.9349(10) 0.6888(9) 0.6376(11) 0.309(8) Uiso 1 1 d D . . . .
H2A H 0.9533 0.6703 0.6410 0.463 Uiso 1 1 calc R . . . .
O3 O 0.9475(8) 0.6314(11) 0.6897(10) 0.309(8) Uiso 1 1 d D . . . .
H3A H 0.9584 0.6075 0.6879 0.463 Uiso 1 1 calc R . . . .
O4 O 0.8752(10) 0.5558(7) 0.6783(10) 0.309(8) Uiso 1 1 d D . . . .
O5 O 0.8177(7) 0.6575(8) 0.6449(9) 0.309(8) Uiso 1 1 d D . . . .
O6 O 0.7807(10) 0.6021(11) 0.6989(12) 0.309(8) Uiso 1 1 d D . . . .
H6 H 0.7779 0.6282 0.6971 0.463 Uiso 1 1 calc R . . . .
O12 O 0.9420(10) 0.5370(10) 0.7008(11) 0.309(8) Uiso 1 1 d D . . . .
H12A H 0.9644 0.5232 0.7018 0.463 Uiso 1 1 calc R . . . .
O13 O 0.9278(10) 0.4358(10) 0.6974(12) 0.309(8) Uiso 1 1 d D . . . .
H13A H 0.9162 0.4138 0.6887 0.463 Uiso 1 1 calc R . . . .
O14 O 0.8538(10) 0.4154(10) 0.6632(10) 0.309(8) Uiso 1 1 d D . . . .
O15 O 0.8261(8) 0.5143(9) 0.7223(9) 0.309(8) Uiso 1 1 d D . . . .
O16 O 0.7774(10) 0.4404(10) 0.7540(11) 0.309(8) Uiso 1 1 d D . . . .
H16 H 0.7650 0.4173 0.7519 0.463 Uiso 1 1 calc R . . . .
OA O 0.9592(15) 0.4592(15) 0.7500 0.35(2) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.501(3) . ?
C1 O5 1.450(3) . ?
C1 O14 1.49(4) 7_556 ?
C2 H2 0.9800 . ?
C2 C3 1.500(3) . ?
C2 K1 3.50(2) 42_566 ?
C2 O2 1.450(3) . ?
C3 H3 0.9800 . ?
C3 C4 1.500(3) . ?
C3 O3 1.450(3) . ?
C4 H4 0.9800 . ?
C4 C5 1.500(3) . ?
C4 O4 1.450(3) . ?
C5 H5 0.9800 . ?
C5 C6 1.500(3) . ?
C5 O5 1.450(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.450(3) . ?
C11 H11 0.9800 . ?
C11 C12 1.500(3) . ?
C11 K1 3.47(3) . ?
C11 O4 1.450(3) . ?
C11 O15 1.450(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.50(2) . ?
C12 O12 1.47(2) . ?
C13 H13 0.9800 . ?
C13 C14 1.51(2) . ?
C13 O13 1.450(3) . ?
C14 H14 0.9800 . ?
C14 C15 1.500(3) . ?
C14 O14 1.450(3) . ?
C15 H15 0.9800 . ?
C15 C16 1.500(3) . ?
C15 O15 1.451(3) . ?
C16 H16B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 K1 3.25(4) . ?
C16 O16 1.450(3) . ?
K1 C11 3.47(3) 23_565 ?
K1 C16 3.25(4) 23_565 ?
K1 O2 2.72(4) 44_666 ?
K1 O2 2.72(4) 41_646 ?
K1 O3 2.59(3) 44_666 ?
K1 O3 2.59(3) 41_646 ?
K1 O15 2.69(3) . ?
K1 O15 2.69(3) 23_565 ?
K1 O16 2.58(3) 23_565 ?
K1 O16 2.58(3) . ?
O2 K1 2.72(4) 42_566 ?
O2 H2A 0.8200 . ?
O3 K1 2.59(3) 42_566 ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O14 C1 1.49(4) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 103.3 . . ?
O5 C1 H1 103.3 . . ?
O5 C1 C2 118.5(16) . . ?
O5 C1 O14 97(2) . 7_556 ?
O14 C1 H1 103.3 7_556 . ?
O14 C1 C2 129(3) 7_556 . ?
C1 C2 H2 110.4 . . ?
C1 C2 K1 159.0(15) . 42_566 ?
C3 C2 C1 109.3(13) . . ?
C3 C2 H2 110.4 . . ?
C3 C2 K1 84.6(10) . 42_566 ?
K1 C2 H2 77.5 42_566 . ?
O2 C2 C1 113(2) . . ?
O2 C2 H2 110.4 . . ?
O2 C2 C3 103.1(15) . . ?
O2 C2 K1 46.9(16) . 42_566 ?
C2 C3 H3 95.4 . . ?
C4 C3 C2 115.8(13) . . ?
C4 C3 H3 95.4 . . ?
O3 C3 C2 104.6(16) . . ?
O3 C3 H3 95.4 . . ?
O3 C3 C4 137(2) . . ?
C3 C4 H4 100.2 . . ?
C3 C4 C5 119.2(13) . . ?
C5 C4 H4 100.2 . . ?
O4 C4 C3 116(2) . . ?
O4 C4 H4 100.2 . . ?
O4 C4 C5 115(2) . . ?
C4 C5 H5 103.3 . . ?
C4 C5 C6 116(2) . . ?
C6 C5 H5 103.3 . . ?
O5 C5 C4 115.0(15) . . ?
O5 C5 H5 103.3 . . ?
O5 C5 C6 114.1(18) . . ?
C5 C6 H6A 112.8 . . ?
C5 C6 H6B 112.8 . . ?
H6A C6 H6B 110.3 . . ?
O6 C6 C5 95(2) . . ?
O6 C6 H6A 112.8 . . ?
O6 C6 H6B 112.8 . . ?
C12 C11 H11 111.5 . . ?
C12 C11 K1 109.0(16) . . ?
K1 C11 H11 73.6 . . ?
O4 C11 H11 111.5 . . ?
O4 C11 C12 90.3(13) . . ?
O4 C11 K1 157.1(19) . . ?
O15 C11 H11 111.5 . . ?
O15 C11 C12 116.7(14) . . ?
O15 C11 K1 46.8(14) . . ?
O15 C11 O4 114(2) . . ?
C11 C12 H12 108.4 . . ?
C11 C12 C13 112.2(14) . . ?
C13 C12 H12 108.4 . . ?
O12 C12 C11 110(2) . . ?
O12 C12 H12 108.4 . . ?
O12 C12 C13 110(3) . . ?
C12 C13 H13 109.8 . . ?
C12 C13 C14 113.9(18) . . ?
C14 C13 H13 109.8 . . ?
O13 C13 C12 116(3) . . ?
O13 C13 H13 109.8 . . ?
O13 C13 C14 97(2) . . ?
C13 C14 H14 108.5 . . ?
C15 C14 C13 110.7(17) . . ?
C15 C14 H14 108.5 . . ?
O14 C14 C13 110(3) . . ?
O14 C14 H14 108.5 . . ?
O14 C14 C15 110.7(17) . . ?
C14 C15 H15 115.2 . . ?
C14 C15 C16 103(3) . . ?
C16 C15 H15 115.2 . . ?
O15 C15 C14 109.6(15) . . ?
O15 C15 H15 115.2 . . ?
O15 C15 C16 96.7(15) . . ?
C15 C16 H16B 103.4 . . ?
C15 C16 H16A 103.4 . . ?
C15 C16 K1 93.3(16) . . ?
H16B C16 H16A 105.2 . . ?
K1 C16 H16B 91.9 . . ?
K1 C16 H16A 152.3 . . ?
O16 C16 C15 135(3) . . ?
O16 C16 H16B 103.4 . . ?
O16 C16 H16A 103.4 . . ?
O16 C16 K1 50.6(18) . . ?
C11 K1 C11 163.4(10) . 23_565 ?
C16 K1 C11 63.9(5) 23_565 23_565 ?
C16 K1 C11 102.6(8) 23_565 . ?
C16 K1 C11 102.6(8) . 23_565 ?
C16 K1 C11 63.9(5) . . ?
C16 K1 C16 80.2(15) . 23_565 ?
O2 K1 C11 102.2(7) 41_646 23_565 ?
O2 K1 C11 102.2(7) 44_666 . ?
O2 K1 C11 86.5(7) 44_666 23_565 ?
O2 K1 C11 86.5(7) 41_646 . ?
O2 K1 C16 83.6(10) 44_666 23_565 ?
O2 K1 C16 83.6(10) 41_646 . ?
O2 K1 C16 155.4(10) 44_666 . ?
O2 K1 C16 155.4(10) 41_646 23_565 ?
O2 K1 O2 117.2(14) 44_666 41_646 ?
O3 K1 C11 139.5(8) 41_646 . ?
O3 K1 C11 139.5(8) 44_666 23_565 ?
O3 K1 C11 53.9(9) 41_646 23_565 ?
O3 K1 C11 53.9(9) 44_666 . ?
O3 K1 C16 117.5(9) 41_646 23_565 ?
O3 K1 C16 116.4(9) 41_646 . ?
O3 K1 C16 117.5(9) 44_666 . ?
O3 K1 C16 116.4(9) 44_666 23_565 ?
O3 K1 O2 87.5(10) 44_666 41_646 ?
O3 K1 O2 87.5(10) 41_646 44_666 ?
O3 K1 O2 54.9(8) 41_646 41_646 ?
O3 K1 O2 54.9(8) 44_666 44_666 ?
O3 K1 O3 107.2(15) 44_666 41_646 ?
O3 K1 O15 145.5(8) 41_646 . ?
O3 K1 O15 76.6(10) 41_646 23_565 ?
O3 K1 O15 76.6(10) 44_666 . ?
O3 K1 O15 145.5(8) 44_666 23_565 ?
O15 K1 C11 140.9(11) . 23_565 ?
O15 K1 C11 23.1(4) 23_565 23_565 ?
O15 K1 C11 23.1(4) . . ?
O15 K1 C11 140.9(10) 23_565 . ?
O15 K1 C16 42.3(6) . . ?
O15 K1 C16 88.6(9) . 23_565 ?
O15 K1 C16 88.6(9) 23_565 . ?
O15 K1 C16 42.3(6) 23_565 23_565 ?
O15 K1 O2 91.8(8) . 41_646 ?
O15 K1 O2 119.3(8) 23_565 41_646 ?
O15 K1 O2 91.8(8) 23_565 44_666 ?
O15 K1 O2 119.3(8) . 44_666 ?
O15 K1 O15 120.1(12) 23_565 . ?
O16 K1 C11 81.3(9) 23_565 . ?
O16 K1 C11 81.3(9) . 23_565 ?
O16 K1 C11 87.7(9) 23_565 23_565 ?
O16 K1 C11 87.7(9) . . ?
O16 K1 C16 83.3(10) 23_565 . ?
O16 K1 C16 25.7(6) . . ?
O16 K1 C16 25.7(6) 23_565 23_565 ?
O16 K1 C16 83.3(10) . 23_565 ?
O16 K1 O2 165.0(10) 23_565 41_646 ?
O16 K1 O2 74.2(10) 23_565 44_666 ?
O16 K1 O2 165.0(10) . 44_666 ?
O16 K1 O2 74.2(10) . 41_646 ?
O16 K1 O3 138.7(10) . 44_666 ?
O16 K1 O3 92.2(10) 23_565 44_666 ?
O16 K1 O3 138.7(10) 23_565 41_646 ?
O16 K1 O3 92.2(10) . 41_646 ?
O16 K1 O15 67.6(10) . . ?
O16 K1 O15 73.6(9) 23_565 . ?
O16 K1 O15 73.6(9) . 23_565 ?
O16 K1 O15 67.6(10) 23_565 23_565 ?
O16 K1 O16 96.6(14) . 23_565 ?
C2 O2 K1 110(2) . 42_566 ?
C2 O2 H2A 109.5 . . ?
K1 O2 H2A 56.3 42_566 . ?
C3 O3 K1 128.8(17) . 42_566 ?
C3 O3 H3A 109.5 . . ?
K1 O3 H3A 116.2 42_566 . ?
C11 O4 C4 116(2) . . ?
C1 O5 C5 105.1(3) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12A 109.5 . . ?
C13 O13 H13A 109.5 . . ?
C14 O14 C1 120(3) . 5_565 ?
C11 O15 C15 114.1(14) . . ?
C11 O15 K1 110.0(18) . . ?
C15 O15 K1 120.8(17) . . ?
C16 O16 K1 104(2) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 146.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -30(4) . . . . ?
C1 C2 C3 O3 166(3) . . . . ?
C1 C2 O2 K1 172.6(17) . . . 42_566 ?
C2 C1 O5 C5 -65(2) . . . . ?
C2 C3 C4 C5 24(5) . . . . ?
C2 C3 C4 O4 169(3) . . . . ?
C2 C3 O3 K1 -4(4) . . . 42_566 ?
C3 C2 O2 K1 -70(2) . . . 42_566 ?
C3 C4 C5 C6 -172(3) . . . . ?
C3 C4 C5 O5 -36(4) . . . . ?
C3 C4 O4 C11 107(4) . . . . ?
C4 C3 O3 K1 -163(4) . . . 42_566 ?
C4 C5 C6 O6 71(3) . . . . ?
C4 C5 O5 C1 52(3) . . . . ?
C5 C4 O4 C11 -106(3) . . . . ?
C6 C5 O5 C1 -171(3) . . . . ?
C11 C12 C13 C14 -42(3) . . . . ?
C11 C12 C13 O13 -153(3) . . . . ?
C12 C11 O4 C4 -140(2) . . . . ?
C12 C11 O15 C15 -48(3) . . . . ?
C12 C11 O15 K1 92(2) . . . . ?
C12 C13 C14 C15 53(4) . . . . ?
C12 C13 C14 O14 176(3) . . . . ?
C13 C14 C15 C16 -161(3) . . . . ?
C13 C14 C15 O15 -59(3) . . . . ?
C13 C14 O14 C1 108(3) . . . 5_565 ?
C14 C15 C16 K1 92.0(15) . . . . ?
C14 C15 C16 O16 59(4) . . . . ?
C14 C15 O15 C11 57(3) . . . . ?
C14 C15 O15 K1 -78(2) . . . . ?
C15 C14 O14 C1 -130(3) . . . 5_565 ?
C15 C16 O16 K1 44(5) . . . . ?
C16 C15 O15 C11 163(3) . . . . ?
C16 C15 O15 K1 28(3) . . . . ?
K1 C2 C3 C4 166(3) 42_566 . . . ?
K1 C2 C3 O3 2(2) 42_566 . . . ?
K1 C11 C12 C13 90(2) . . . . ?
K1 C11 C12 O12 -148(2) . . . . ?
K1 C11 O4 C4 72(5) . . . . ?
K1 C11 O15 C15 -139(3) . . . . ?
O2 C2 C3 C4 -150(3) . . . . ?
O2 C2 C3 O3 46(3) . . . . ?
O3 C3 C4 C5 -179(4) . . . . ?
O3 C3 C4 O4 -33(7) . . . . ?
O4 C4 C5 C6 42(4) . . . . ?
O4 C4 C5 O5 178(3) . . . . ?
O4 C11 C12 C13 -78(2) . . . . ?
O4 C11 C12 O12 44(3) . . . . ?
O4 C11 O15 C15 55(3) . . . . ?
O4 C11 O15 K1 -165.3(16) . . . . ?
O5 C1 C2 C3 55(3) . . . . ?
O5 C1 C2 K1 -176(4) . . . 42_566 ?
O5 C1 C2 O2 169(2) . . . . ?
O5 C5 C6 O6 -66(4) . . . . ?
O12 C12 C13 C14 -164(3) . . . . ?
O12 C12 C13 O13 84(3) . . . . ?
O13 C13 C14 C15 175(3) . . . . ?
O13 C13 C14 O14 -62(3) . . . . ?
O14 C1 C2 C3 -73(3) 7_556 . . . ?
O14 C1 C2 K1 57(5) 7_556 . . 42_566 ?
O14 C1 C2 O2 41(3) 7_556 . . . ?
O14 C1 O5 C5 76(3) 7_556 . . . ?
O14 C14 C15 C16 77(3) . . . . ?
O14 C14 C15 O15 179(3) . . . . ?
O15 C11 C12 C13 39(3) . . . . ?
O15 C11 C12 O12 161(3) . . . . ?
O15 C11 O4 C4 100(3) . . . . ?
O15 C15 C16 K1 -19.9(19) . . . . ?
O15 C15 C16 O16 -52(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.196 -0.912 -0.042 15420.4 496.7 ?


_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_olex2_submission_original_sample_id CDMOF_alpha_9_059
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
;
_oxdiff_exptl_absorpt_empirical_full_max 1.000
_oxdiff_exptl_absorpt_empirical_full_min 1.000
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_b_220K
_database_code_depnum_ccdc_archive 'CCDC 1529154'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_THETM01_CDMOF_b_220K        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly diffracting sample crystal'
;
_vrf_PLAT201_CDMOF_b_220K        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         88 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT241_CDMOF_b_220K        
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         K2 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT090_CDMOF_b_220K        
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.07 Note  
RESPONSE: 'Data limited due to the poorly diffracting sample crystal; 
large number of parameters is the result of the complex molecular 
and crystal structures'
;
_vrf_PLAT242_CDMOF_b_220K        
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         O6 Check 
RESPONSE: 'Poor data quality'
;
_vrf_PLAT306_CDMOF_b_220K        
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_b_220K        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.032 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT410_CDMOF_b_220K        
;
PROBLEM: Short Intra H...H Contact  H21    ..  H34     ..       1.83 Ang.  
RESPONSE: 'Result of the strained conformation'...
;
_vrf_PLAT420_CDMOF_b_220K        
;
PROBLEM: D-H Without Acceptor       O26    --  H26    ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
_vrf_PLAT910_CDMOF_b_220K        
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          19 Note  
RESPONSE: 'Missing reflections may be due to the chosen strategy of the 
measurement; this was short measurement, aimed primarily at 
checking the unit-cell paremeters only'
;
# end Validation Reply Form

# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
# CRYSTAL DATA
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_H-M_alt        'R 3 2'
_space_group_name_Hall           'R 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_symmetry_space_group_name_H-M_alt 'R 3 2'
_cell_length_a                   43.643(13)
_cell_length_b                   43.643(13)
_cell_length_c                   28.059(13)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_volume                     46284(20)
_cell_formula_units_Z            18
_cell_measurement_reflns_used    1785
_cell_measurement_temperature    219.98(10)
_cell_measurement_theta_max      11.8570
_cell_measurement_theta_min      2.9400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30559
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.910
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1632
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_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            21248
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        13.698
_diffrn_reflns_theta_max         13.698
_diffrn_reflns_theta_min         2.762
_diffrn_ambient_environment      'ispropanol:water mother liquor'
_diffrn_ambient_temperature      219.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  54.00   1.00   15.00    --  -18.72   0.00-150.00  122
  2  ω    -73.00  20.00   1.00   15.00    --  -18.72 -19.00  60.00   93
  3  ω    -40.00   8.00   1.00   15.00    --  -18.72  57.00  60.00   48
  4  ω    -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       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0054142000
_diffrn_orient_matrix_UB_12      -0.0127217000
_diffrn_orient_matrix_UB_13      0.0184868000
_diffrn_orient_matrix_UB_21      -0.0167542000
_diffrn_orient_matrix_UB_22      -0.0008704000
_diffrn_orient_matrix_UB_23      0.0008553000
_diffrn_orient_matrix_UB_31      -0.0066131000
_diffrn_orient_matrix_UB_32      -0.0136594000
_diffrn_orient_matrix_UB_33      -0.0171618000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                2440
_reflns_number_total             3100
_reflns_odcompleteness_completeness 98.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     13.67
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.176
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 
;
 Flack x determined using 770 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     328
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0740
_refine_ls_restrained_S_all      1.337
_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/[σ²(Fo²)+(0.0558P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1618
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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:
  H2A of O2, H3A of O3, H6 of O6, H12A of O12, H13A of O13, H16 of O16, H22A
  of O22, H23A of O23, H76 of O76, H72A of O72, H66 of O66, H63A of O63, H62A
  of O62, H56 of O56, H53A of O53, H52A of O52, H46 of O46, H43A of O43, H42A
  of O42, H36 of O36, H33A of O33, H32A of O32, H26 of O26
2. Restrained distances
 C64-C65
 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
 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
 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
 C31-O35
 1.45 with sigma of 0.005
 C33-O35
 3 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
 C35-O36
 2.45 with sigma of 0.02
 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
 C65-C64
 1.5 with sigma of 0.02
 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
 O54-C41
 1.45 with sigma of 0.01
 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
 O14-C14
 1.45 with sigma of 0.01
 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
 C62-C61
 1.5 with sigma of 0.02
 C62-O62
 1.45 with sigma of 0.02
 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
 C62-C63
 1.5 with sigma of 0.02
 C32-C33
 1.5 with sigma of 0.02
 C36-C35
 1.5 with sigma of 0.02
 C61-O74
 1.45 with sigma of 0.02
 C61-C62
 1.5 with sigma of 0.02
 C61-O65
 1.45 with sigma of 0.02
 O36-C36
 1.45 with sigma of 0.01
 O75-C75
 1.45 with sigma of 0.02
 C41-O45
 1.45 with sigma of 0.02
 C71-O75
 1.45 with sigma of 0.01
 C71-C72
 1.5 with sigma of 0.02
 O73-C73
 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
 O34-C21
 1.45 with sigma of 0.02
 C21-O34
 1.45 with sigma of 0.01
 C6-K2
 3.8 with sigma of 0.02
 C1-K2
 3.8 with sigma of 0.02
 C43-C44
 1.5 with sigma of 0.02
 C44-C43
 1.5 with sigma of 0.01
 C72-C71
 1.5 with sigma of 0.01
 C71-O4
 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
 C34-C35
 1.5 with sigma of 0.02
 C34-O34
 1.45 with sigma of 0.01
 C33-O33
 1.45 with sigma of 0.01
 O72-C72
 1.45 with sigma of 0.02
 C41-C42
 1.5 with sigma of 0.01
 C34-C33
 1.5 with sigma of 0.01
 C44-C45
 1.5 with sigma of 0.01
 C35-O35
 1.45 with sigma of 0.01
 C52-C53
 1.5 with sigma of 0.02
 C54-C55
 1.5 with sigma of 0.02
 C54-C53
 1.5 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-O64
 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
 C56-C55
 1.5 with sigma of 0.02
 O64-C51
 1.45 with sigma of 0.02
 C51-O55
 1.45 with sigma of 0.02
 C51-C52
 1.5 with sigma of 0.02
 C55-O55
 1.45 with sigma of 0.02
 O55-C51
 1.45 with sigma of 0.01
 O55-C55
 1.45 with sigma of 0.01
 C43-C45
 2.5 with sigma of 0.04
 C11-C13
 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
 O25-C24
 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
 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
 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
 C4-C71
 2.5 with sigma of 0.01
 C1-C14
 2.5 with sigma of 0.01
 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
 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
 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
 O75-C76
 2.5 with sigma of 0.02
 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
 O45-C44
 2.5 with sigma of 0.04
 C35-C33
 2.5 with sigma of 0.04
 C33-C31
 2.5 with sigma of 0.04
 C32-O35
 2.5 with sigma of 0.04
 C31-C35
 2.5 with sigma of 0.04
 O65-C64
 2.5 with sigma of 0.04
 C61-C65
 2.5 with sigma of 0.04
 C63-C61
 2.5 with sigma of 0.04
 C72-O75
 2.5 with sigma of 0.04
 C31-O32
 2.5 with sigma of 0.04
 C24-O23
 2.5 with sigma of 0.04
 C72-O4
 2.5 with sigma of 0.04
 O75-C74
 2.5 with sigma of 0.04
 C74-C76
 2.5 with sigma of 0.01
 C61-C74
 2.5 with sigma of 0.04
 O73-C74
 2.5 with sigma of 0.02
 C72-O73
 2.5 with sigma of 0.02
 C24-C11
 2.5 with sigma of 0.01
 C71-C75
 2.5 with sigma of 0.02
 O23-C24
 2.5 with sigma of 0.02
 O23-C22
 2.5 with sigma of 0.02
 O45-C42
 2.5 with sigma of 0.01
 C41-C43
 2.5 with sigma of 0.01
 C42-C44
 2.5 with sigma of 0.01
 O43-C42
 2.5 with sigma of 0.01
 O42-C43
 2.5 with sigma of 0.01
 O42-C41
 2.5 with sigma of 0.01
 O4-O75
 2.5 with sigma of 0.01
 O4-C72
 2.5 with sigma of 0.01
 O75-C72
 2.5 with sigma of 0.01
 O26-C25
 2.5 with sigma of 0.01
 C32-C34
 2.5 with sigma of 0.04
 C34-C32
 2.5 with sigma of 0.04
 O35-C34
 2.5 with sigma of 0.04
 O33-C34
 2.5 with sigma of 0.04
 C34-C21
 2.5 with sigma of 0.01
 C34-O33
 2.45 with sigma of 0.01
 O33-C32
 2.45 with sigma of 0.01
 C36-C34
 2.5 with sigma of 0.01
 C36-O35
 2.5 with sigma of 0.01
 C34-C36
 2.5 with sigma of 0.01
 O36-C35
 2.4 with sigma of 0.02
 C53-C55
 2.5 with sigma of 0.04
 C54-C41
 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
 O52-C53
 2.5 with sigma of 0.04
 C53-O52
 2.5 with sigma of 0.01
 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
 C55-C51 = C54-O55
 2.5 with sigma of 0.04
 C55-C51
 2.5 with sigma of 0.01
3. 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
4. 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
5. 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(C31)=Uiso(C32)=Uiso(C33)=Uiso(C34)=Uiso(C35)=Uiso(C36)=FVAR(2)
 Uiso(OA)=Uiso(OB)=FVAR(3)
 Uiso(C51)=Uiso(C52)=Uiso(C53)=Uiso(C54)=Uiso(C55)=Uiso(C56)=FVAR(4)
6.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)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C16(H16A,H16B), C26(H26A,H26B), C36(H36A,H36B), C46(H46A,H46B),
 C56(H56A,H56B), C66(H66A,H66B), C76(H76A,H76B)
6.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)
;

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7445(5) 0.6625(6) 0.4046(7) 0.133(12) Uiso 1 1 d D U . . .
H1 H 0.7534 0.6775 0.3763 0.159 Uiso 1 1 calc R . . . .
C2 C 0.7283(6) 0.6746(4) 0.4453(8) 0.116(10) Uiso 1 1 d D U . . .
H2 H 0.7135 0.6837 0.4324 0.139 Uiso 1 1 calc R . . . .
C3 C 0.7115(6) 0.6515(5) 0.4870(8) 0.129(11) Uiso 1 1 d D U . . .
H3 H 0.7292 0.6449 0.4952 0.155 Uiso 1 1 calc R . . . .
C4 C 0.6799(5) 0.6158(5) 0.4767(7) 0.134(11) Uiso 1 1 d D U . . .
H4 H 0.6598 0.6188 0.4675 0.161 Uiso 1 1 calc R . . . .
C5 C 0.6891(7) 0.5994(5) 0.4359(8) 0.159(13) Uiso 1 1 d D U . . .
H5 H 0.7042 0.5910 0.4499 0.191 Uiso 1 1 calc R . . . .
C6 C 0.6590(8) 0.5673(6) 0.4128(11) 0.252(18) Uiso 1 1 d D U . . .
H6A H 0.6462 0.5487 0.4359 0.303 Uiso 1 1 calc R . . . .
H6B H 0.6674 0.5584 0.3873 0.303 Uiso 1 1 calc R . . . .
C11 C 0.8612(5) 0.6679(6) 0.3702(9) 0.103(10) Uiso 1 1 d D U . . .
H11 H 0.8802 0.6744 0.3468 0.123 Uiso 1 1 calc R . . . .
C12 C 0.8606(5) 0.7019(5) 0.3826(8) 0.099(10) Uiso 1 1 d D U . . .
H12 H 0.8589 0.7137 0.3538 0.119 Uiso 1 1 calc R . . . .
C13 C 0.8299(6) 0.6921(6) 0.4156(9) 0.126(11) Uiso 1 1 d D U . . .
H13 H 0.8365 0.6858 0.4459 0.151 Uiso 1 1 calc R . . . .
C14 C 0.7992(5) 0.6595(6) 0.3984(10) 0.168(13) Uiso 1 1 d D U . . .
H14 H 0.7944 0.6684 0.3689 0.202 Uiso 1 1 calc R . . . .
C15 C 0.7972(5) 0.6270(6) 0.3798(9) 0.120(11) Uiso 1 1 d D U . . .
H15 H 0.8030 0.6160 0.4061 0.144 Uiso 1 1 calc R . . . .
C16 C 0.7695(8) 0.5978(8) 0.3503(10) 0.201(16) Uiso 1 1 d D U . . .
H16A H 0.7764 0.5803 0.3437 0.242 Uiso 1 1 calc R . . . .
H16B H 0.7472 0.5864 0.3673 0.242 Uiso 1 1 calc R . . . .
C21 C 0.9337(7) 0.6228(6) 0.4653(7) 0.147(12) Uiso 1 1 d D U . . .
H21 H 0.9548 0.6203 0.4672 0.176 Uiso 1 1 calc R . . . .
C22 C 0.9518(7) 0.6620(6) 0.4684(9) 0.120(11) Uiso 1 1 d D U . . .
H22 H 0.9704 0.6726 0.4442 0.144 Uiso 1 1 calc R . . . .
C23 C 0.9220(6) 0.6672(6) 0.4551(9) 0.109(10) Uiso 1 1 d D U . . .
H23 H 0.9068 0.6572 0.4831 0.131 Uiso 1 1 calc R . . . .
C24 C 0.8962(5) 0.6466(5) 0.4158(7) 0.073(9) Uiso 1 1 d D U . . .
H24 H 0.9109 0.6587 0.3879 0.088 Uiso 1 1 calc R . . . .
C25 C 0.8909(7) 0.6112(7) 0.4082(7) 0.191(14) Uiso 1 1 d D U . . .
H25 H 0.8729 0.5951 0.4307 0.229 Uiso 1 1 calc R . . . .
C26 C 0.8796(5) 0.5960(6) 0.3588(8) 0.166(13) Uiso 1 1 d D U . . .
H26A H 0.8696 0.5706 0.3605 0.199 Uiso 1 1 calc R . . . .
H26B H 0.8611 0.6005 0.3480 0.199 Uiso 1 1 calc R . . . .
C31 C 0.9345(5) 0.5484(6) 0.6208(6) 0.194(7) Uiso 1 1 d D U . . .
H31 H 0.9435 0.5356 0.6394 0.233 Uiso 1 1 calc R . . . .
C32 C 0.9585(8) 0.5876(5) 0.6181(9) 0.194(7) Uiso 1 1 d D U . . .
H32 H 0.9796 0.5890 0.6038 0.233 Uiso 1 1 calc R . . . .
C33 C 0.9516(7) 0.6094(5) 0.5848(7) 0.194(7) Uiso 1 1 d D U . . .
H33 H 0.9323 0.6110 0.6002 0.233 Uiso 1 1 calc R . . . .
C34 C 0.9359(7) 0.5921(4) 0.5382(7) 0.194(7) Uiso 1 1 d D U . . .
H34 H 0.9560 0.5953 0.5189 0.233 Uiso 1 1 calc R . . . .
C35 C 0.9121(7) 0.5528(4) 0.5417(6) 0.194(7) Uiso 1 1 d D U . . .
H35 H 0.8929 0.5540 0.5581 0.233 Uiso 1 1 calc R . . . .
C36 C 0.8914(5) 0.5357(6) 0.4975(7) 0.194(7) Uiso 1 1 d D U . . .
H36A H 0.8820 0.5501 0.4849 0.233 Uiso 1 1 calc R . . . .
H36B H 0.8715 0.5128 0.5056 0.233 Uiso 1 1 calc R . . . .
C41 C 0.8354(4) 0.4902(4) 0.7521(7) 0.123(11) Uiso 1 1 d D U . . .
H41 H 0.8276 0.4759 0.7812 0.148 Uiso 1 1 calc R . . . .
C42 C 0.8637(5) 0.5263(4) 0.7631(6) 0.089(9) Uiso 1 1 d D U . . .
H42 H 0.8816 0.5207 0.7738 0.107 Uiso 1 1 calc R . . . .
C43 C 0.8827(6) 0.5478(5) 0.7199(6) 0.116(11) Uiso 1 1 d D U . . .
H43 H 0.8700 0.5594 0.7080 0.139 Uiso 1 1 calc R . . . .
C44 C 0.8861(6) 0.5269(6) 0.6805(6) 0.118(11) Uiso 1 1 d D U . . .
H44 H 0.9048 0.5226 0.6921 0.142 Uiso 1 1 calc R . . . .
C45 C 0.8558(6) 0.4903(6) 0.6730(8) 0.102(10) Uiso 1 1 d D U . . .
H45 H 0.8372 0.4948 0.6614 0.122 Uiso 1 1 calc R . . . .
C46 C 0.8533(5) 0.4627(5) 0.6383(7) 0.055(8) Uiso 1 1 d D U . . .
H46A H 0.8569 0.4716 0.6059 0.066 Uiso 1 1 calc R . . . .
H46B H 0.8303 0.4414 0.6403 0.066 Uiso 1 1 calc R . . . .
C51 C 0.7076(5) 0.4705(5) 0.7790(7) 0.065(4) Uiso 1 1 d D U . . .
H51 H 0.6840 0.4569 0.7933 0.078 Uiso 1 1 calc R . . . .
C52 C 0.7333(5) 0.4879(5) 0.8202(6) 0.065(4) Uiso 1 1 d D U . . .
H52 H 0.7327 0.4710 0.8436 0.078 Uiso 1 1 calc R . . . .
C53 C 0.7670(5) 0.5056(5) 0.7906(7) 0.065(4) Uiso 1 1 d D U . . .
H53 H 0.7662 0.5222 0.7678 0.078 Uiso 1 1 calc R . . . .
C54 C 0.7754(4) 0.4812(5) 0.7665(7) 0.065(4) Uiso 1 1 d D U . . .
H54 H 0.7760 0.4644 0.7892 0.078 Uiso 1 1 calc R . . . .
C55 C 0.7477(5) 0.4614(5) 0.7269(7) 0.065(4) Uiso 1 1 d D U . . .
H55 H 0.7484 0.4788 0.7043 0.078 Uiso 1 1 calc R . . . .
C56 C 0.7537(5) 0.4354(5) 0.7004(6) 0.065(4) Uiso 1 1 d D U . . .
H56A H 0.7342 0.4211 0.6790 0.078 Uiso 1 1 calc R . . . .
H56B H 0.7757 0.4469 0.6826 0.078 Uiso 1 1 calc R . . . .
C61 C 0.6258(7) 0.5125(7) 0.6890(9) 0.138(12) Uiso 1 1 d D U . . .
H61 H 0.6046 0.5149 0.6878 0.166 Uiso 1 1 calc R . . . .
C62 C 0.6516(8) 0.5353(7) 0.7256(11) 0.167(14) Uiso 1 1 d D U . . .
H62 H 0.6355 0.5240 0.7524 0.201 Uiso 1 1 calc R . . . .
C63 C 0.6786(6) 0.5261(6) 0.7428(8) 0.103(10) Uiso 1 1 d D U . . .
H63 H 0.6993 0.5405 0.7227 0.124 Uiso 1 1 calc R . . . .
C64 C 0.6713(8) 0.4897(7) 0.7350(11) 0.158(13) Uiso 1 1 d D U . . .
H64 H 0.6567 0.4757 0.7618 0.190 Uiso 1 1 calc R . . . .
C65 C 0.6499(7) 0.4732(7) 0.6905(9) 0.115(11) Uiso 1 1 d D U . . .
H65 H 0.6638 0.4869 0.6629 0.138 Uiso 1 1 calc R . . . .
C66 C 0.6406(8) 0.4358(7) 0.6835(11) 0.186(14) Uiso 1 1 d D U . . .
H66A H 0.6609 0.4325 0.6863 0.223 Uiso 1 1 calc R . . . .
H66B H 0.6284 0.4260 0.6537 0.223 Uiso 1 1 calc R . . . .
C71 C 0.6322(5) 0.5709(4) 0.5280(7) 0.151(12) Uiso 1 1 d D U . . .
H71 H 0.6212 0.5753 0.5003 0.182 Uiso 1 1 calc R . . . .
C72 C 0.6198(6) 0.5840(5) 0.5689(7) 0.153(12) Uiso 1 1 d D U . . .
H72 H 0.5941 0.5731 0.5723 0.183 Uiso 1 1 calc R . . . .
C73 C 0.6386(6) 0.5771(6) 0.6094(8) 0.077(9) Uiso 1 1 d D U . . .
H73 H 0.6632 0.5922 0.5996 0.093 Uiso 1 1 calc R . . . .
C74 C 0.6361(7) 0.5416(5) 0.6081(8) 0.107(10) Uiso 1 1 d D U . . .
H74 H 0.6108 0.5279 0.6159 0.129 Uiso 1 1 calc R . . . .
C75 C 0.6340(7) 0.5213(6) 0.5636(9) 0.181(14) Uiso 1 1 d D U . . .
H75 H 0.6581 0.5278 0.5540 0.217 Uiso 1 1 calc R . . . .
C76 C 0.6131(6) 0.4823(5) 0.5695(11) 0.27(2) Uiso 1 1 d D U . . .
H76A H 0.6117 0.4713 0.5388 0.327 Uiso 1 1 calc R . . . .
H76B H 0.6258 0.4751 0.5910 0.327 Uiso 1 1 calc R . . . .
K1 K 0.89440(19) 0.78995(17) 0.4184(3) 0.151(3) Uani 1 1 d . U . . .
K2 K 0.6667 0.6394(3) 0.3333 0.325(11) Uani 1 2 d DS TU P . .
K3 K 0.9738(2) 0.6404(2) 0.3333 0.229(7) Uani 1 2 d S TU P . .
O2 O 0.7620(5) 0.7030(5) 0.4623(7) 0.1657(17) Uiso 1 1 d D U . . .
H2A H 0.7613 0.7043 0.4914 0.249 Uiso 1 1 calc R . . . .
O3 O 0.7084(5) 0.6667(5) 0.5320(7) 0.1657(17) Uiso 1 1 d D U . . .
H3A H 0.6933 0.6510 0.5488 0.249 Uiso 1 1 calc R . . . .
O4 O 0.6705(4) 0.5932(4) 0.5182(6) 0.1657(17) Uiso 1 1 d D U . . .
O5 O 0.7105(5) 0.6238(5) 0.3982(6) 0.1657(17) Uiso 1 1 d D U . . .
O6 O 0.6366(5) 0.5818(5) 0.3939(7) 0.1657(17) Uiso 1 1 d D U . . .
H6 H 0.6163 0.5699 0.4039 0.249 Uiso 1 1 calc R . . . .
O12 O 0.8931(5) 0.7261(5) 0.4111(7) 0.1657(17) Uiso 1 1 d D U . . .
H12A H 0.8966 0.7145 0.4312 0.249 Uiso 1 1 calc R . . . .
O13 O 0.8249(5) 0.7223(5) 0.4265(7) 0.1657(17) Uiso 1 1 d D U . . .
H13A H 0.8038 0.7152 0.4312 0.249 Uiso 1 1 calc R . . . .
O14 O 0.7663(5) 0.6500(5) 0.4247(7) 0.1657(17) Uiso 1 1 d D U . . .
O15 O 0.8274(6) 0.6418(5) 0.3465(6) 0.1657(17) Uiso 1 1 d D U . . .
O16 O 0.7658(5) 0.6133(5) 0.3053(7) 0.1657(17) Uiso 1 1 d D U . . .
H16 H 0.7847 0.6226 0.2909 0.249 Uiso 1 1 calc R . . . .
O22 O 0.9663(5) 0.6773(5) 0.5154(7) 0.1657(17) Uiso 1 1 d D U . . .
H22A H 0.9559 0.6872 0.5258 0.249 Uiso 1 1 calc R . . . .
O23 O 0.9289(5) 0.7039(5) 0.4567(6) 0.1657(17) Uiso 1 1 d D U . . .
H23A H 0.9483 0.7167 0.4689 0.249 Uiso 1 1 calc R . . . .
O24 O 0.8699(5) 0.6551(5) 0.4100(8) 0.1657(17) Uiso 1 1 d D U . . .
O25 O 0.9234(5) 0.6103(5) 0.4172(7) 0.1657(17) Uiso 1 1 d D U . . .
O26 O 0.9079(5) 0.6101(5) 0.3238(6) 0.1657(17) Uiso 1 1 d D U . . .
H26 H 0.8997 0.6092 0.2973 0.249 Uiso 1 1 calc R . . . .
O32 O 0.9723(5) 0.6044(5) 0.6641(7) 0.1657(17) Uiso 1 1 d D U . . .
H32A H 0.9569 0.5947 0.6845 0.249 Uiso 1 1 calc R . . . .
O33 O 0.9792(4) 0.6457(4) 0.5817(6) 0.1657(17) Uiso 1 1 d D U . . .
H33A H 0.9736 0.6561 0.5624 0.249 Uiso 1 1 calc R . . . .
O34 O 0.9149(5) 0.6009(5) 0.5064(8) 0.1657(17) Uiso 1 1 d D U . . .
O35 O 0.9160(5) 0.5312(4) 0.5772(7) 0.1657(17) Uiso 1 1 d D U . . .
O36 O 0.9123(5) 0.5312(5) 0.4608(6) 0.1657(17) Uiso 1 1 d D U . . .
H36 H 0.9040 0.5101 0.4553 0.249 Uiso 1 1 calc R . . . .
O42 O 0.8626(5) 0.5442(4) 0.8042(5) 0.1657(17) Uiso 1 1 d D U . . .
H42A H 0.8699 0.5651 0.7978 0.249 Uiso 1 1 calc R . . . .
O43 O 0.9190(4) 0.5741(5) 0.7262(7) 0.1657(17) Uiso 1 1 d D U . . .
H43A H 0.9225 0.5805 0.7542 0.249 Uiso 1 1 calc R . . . .
O44 O 0.8976(5) 0.5394(5) 0.6320(7) 0.1657(17) Uiso 1 1 d D U . . .
O45 O 0.8406(5) 0.4709(4) 0.7149(7) 0.1657(17) Uiso 1 1 d D U . . .
O46 O 0.8831(5) 0.4550(5) 0.6532(7) 0.1657(17) Uiso 1 1 d . U . . .
H46 H 0.8780 0.4445 0.6787 0.249 Uiso 1 1 calc R . . . .
O52 O 0.7222(5) 0.5118(5) 0.8393(6) 0.1657(17) Uiso 1 1 d D U . . .
H52A H 0.7380 0.5266 0.8563 0.249 Uiso 1 1 calc R . . . .
O53 O 0.7953(5) 0.5244(5) 0.8252(7) 0.1657(17) Uiso 1 1 d . U . . .
H53A H 0.8137 0.5261 0.8148 0.249 Uiso 1 1 calc R . . . .
O54 O 0.8075(5) 0.4967(5) 0.7348(7) 0.1657(17) Uiso 1 1 d D U . . .
O55 O 0.7137(4) 0.4453(4) 0.7525(6) 0.1657(17) Uiso 1 1 d D U . . .
O56 O 0.7552(5) 0.4148(5) 0.7400(7) 0.1657(17) Uiso 1 1 d D U . . .
H56 H 0.7757 0.4192 0.7436 0.249 Uiso 1 1 calc R . . . .
O62 O 0.6604(5) 0.5711(5) 0.7390(7) 0.1657(17) Uiso 1 1 d D U . . .
H62A H 0.6706 0.5761 0.7649 0.249 Uiso 1 1 calc R . . . .
O63 O 0.6899(5) 0.5412(5) 0.7899(7) 0.1657(17) Uiso 1 1 d D U . . .
H63A H 0.6998 0.5318 0.8032 0.249 Uiso 1 1 calc R . . . .
O64 O 0.7047(6) 0.4932(5) 0.7419(7) 0.1657(17) Uiso 1 1 d D U . . .
O65 O 0.6179(5) 0.4770(6) 0.6939(7) 0.1657(17) Uiso 1 1 d D U . . .
O66 O 0.6144(5) 0.4207(5) 0.7294(7) 0.1657(17) Uiso 1 1 d . U . . .
H66 H 0.6259 0.4219 0.7532 0.249 Uiso 1 1 calc R . . . .
O72 O 0.6399(5) 0.6232(5) 0.5681(7) 0.1657(17) Uiso 1 1 d D U . . .
H72A H 0.6433 0.6308 0.5955 0.249 Uiso 1 1 calc R . . . .
O73 O 0.6385(5) 0.5945(5) 0.6540(7) 0.1657(17) Uiso 1 1 d D U . . .
H73A H 0.6567 0.5999 0.6689 0.199 Uiso 1 1 calc R . . . .
O74 O 0.6494(6) 0.5308(6) 0.6542(9) 0.1657(17) Uiso 1 1 d D U . . .
O75 O 0.6184(4) 0.5330(4) 0.5259(6) 0.1657(17) Uiso 1 1 d D U . . .
O76 O 0.5775(5) 0.4687(5) 0.5876(7) 0.1657(17) Uiso 1 1 d D U . . .
H76 H 0.5690 0.4800 0.5761 0.249 Uiso 1 1 calc R . . . .
OA O 0.7536(6) 0.7006(7) 0.5925(10) 0.245(8) Uiso 1 1 d . U . . .
OB O 0.9496(7) 0.7114(7) 0.5716(9) 0.245(8) Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.568(19) . ?
C1 O5 1.607(19) . ?
C1 O14 1.427(18) . ?
C2 H2 0.9800 . ?
C2 C3 1.478(19) . ?
C2 O2 1.450(18) . ?
C3 H3 0.9800 . ?
C3 C4 1.502(7) . ?
C3 O3 1.465(18) . ?
C4 H4 0.9800 . ?
C4 C5 1.508(7) . ?
C4 O4 1.448(18) . ?
C5 H5 0.9800 . ?
C5 C6 1.504(7) . ?
C5 O5 1.460(13) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.50(2) . ?
C11 H11 0.9800 . ?
C11 C12 1.54(2) . ?
C11 O15 1.495(18) . ?
C11 O24 1.38(2) . ?
C12 H12 0.9800 . ?
C12 C13 1.506(19) . ?
C12 K1 3.50(2) . ?
C12 O12 1.507(16) . ?
C13 H13 0.9800 . ?
C13 C14 1.467(19) . ?
C13 O13 1.470(18) . ?
C14 H14 0.9800 . ?
C14 C15 1.473(19) . ?
C14 O14 1.475(13) . ?
C15 H15 0.9800 . ?
C15 C16 1.49(2) . ?
C15 O15 1.477(13) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 O16 1.48(2) . ?
C21 H21 0.9800 . ?
C21 C22 1.49(2) . ?
C21 O25 1.441(13) . ?
C21 O34 1.461(12) . ?
C22 H22 0.9800 . ?
C22 C23 1.47(2) . ?
C22 O22 1.471(17) . ?
C23 H23 0.9800 . ?
C23 C24 1.511(18) . ?
C23 O23 1.475(19) . ?
C24 H24 0.9800 . ?
C24 C25 1.458(19) . ?
C24 O24 1.384(19) . ?
C25 H25 0.9800 . ?
C25 C26 1.509(19) . ?
C25 O25 1.462(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 O26 1.451(7) . ?
C31 H31 0.9800 . ?
C31 C32 1.50(2) . ?
C31 O35 1.452(7) . ?
C31 O44 1.49(2) . ?
C32 H32 0.9800 . ?
C32 C33 1.469(17) . ?
C32 K3 3.51(2) 8_655 ?
C32 O32 1.46(2) . ?
C33 H33 0.9800 . ?
C33 C34 1.493(12) . ?
C33 O33 1.433(13) . ?
C34 H34 0.9800 . ?
C34 C35 1.498(3) . ?
C34 O34 1.463(13) . ?
C35 H35 0.9800 . ?
C35 C36 1.497(3) . ?
C35 O35 1.442(12) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C36 O36 1.452(13) . ?
C41 H41 0.9800 . ?
C41 C42 1.472(12) . ?
C41 O45 1.428(17) . ?
C41 O54 1.464(13) . ?
C42 H42 0.9800 . ?
C42 C43 1.503(16) . ?
C42 O42 1.407(16) . ?
C43 H43 0.9800 . ?
C43 C44 1.487(12) . ?
C43 O43 1.427(18) . ?
C44 H44 0.9800 . ?
C44 C45 1.495(13) . ?
C44 O44 1.457(13) . ?
C45 H45 0.9800 . ?
C45 C46 1.510(18) . ?
C45 O45 1.405(18) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C46 O46 1.56(2) . ?
C51 H51 0.9800 . ?
C51 C52 1.521(18) . ?
C51 O55 1.461(11) . ?
C51 O64 1.482(16) . ?
C52 H52 0.9800 . ?
C52 C53 1.520(15) . ?
C52 K1 3.416(16) 10_566 ?
C52 O52 1.456(16) . ?
C53 H53 0.9800 . ?
C53 C54 1.457(17) . ?
C53 O53 1.46(2) . ?
C54 H54 0.9800 . ?
C54 C55 1.548(18) . ?
C54 O54 1.504(17) . ?
C55 H55 0.9800 . ?
C55 C56 1.485(15) . ?
C55 O55 1.470(11) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 O56 1.451(7) . ?
C61 H61 0.9800 . ?
C61 C62 1.482(18) . ?
C61 K1 3.49(3) 9_565 ?
C61 O65 1.42(2) . ?
C61 O74 1.35(2) . ?
C62 H62 0.9800 . ?
C62 C63 1.50(2) . ?
C62 O62 1.46(2) . ?
C63 H63 0.9800 . ?
C63 C64 1.47(2) . ?
C63 O63 1.449(7) . ?
C64 H64 0.9800 . ?
C64 C65 1.511(17) . ?
C64 O64 1.40(3) . ?
C65 H65 0.9800 . ?
C65 C66 1.48(2) . ?
C65 O65 1.49(2) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C66 O66 1.63(3) . ?
C71 H71 0.9800 . ?
C71 C72 1.501(11) . ?
C71 O4 1.478(12) . ?
C71 O75 1.448(11) . ?
C72 H72 0.9800 . ?
C72 C73 1.52(2) . ?
C72 O72 1.485(16) . ?
C73 H73 0.9800 . ?
C73 C74 1.496(7) . ?
C73 O73 1.465(17) . ?
C74 H74 0.9800 . ?
C74 C75 1.51(2) . ?
C74 O74 1.58(3) . ?
C75 H75 0.9800 . ?
C75 C76 1.49(2) . ?
C75 O75 1.481(17) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
C76 O76 1.452(7) . ?
K1 C52 3.416(16) 10_566 ?
K1 C61 3.49(3) 14_654 ?
K1 O12 2.77(2) . ?
K1 O13 3.00(2) . ?
K1 O45 2.82(2) 15_664 ?
K1 O46 2.84(2) 15_664 ?
K1 O52 2.83(2) 10_566 ?
K1 O53 3.00(2) 10_566 ?
K1 O65 2.69(2) 14_654 ?
K1 O66 2.83(2) 14_654 ?
K2 O5 2.95(2) 17_655 ?
K2 O5 2.95(2) . ?
K2 O6 2.76(2) . ?
K2 O6 2.76(2) 17_655 ?
K2 O72 3.360(19) 6_556 ?
K2 O72 3.36(2) 14_654 ?
K2 O73 3.150(19) 6_556 ?
K2 O73 3.150(19) 14_654 ?
K3 C32 3.51(2) 15_664 ?
K3 C32 3.51(2) 5_766 ?
K3 O25 3.03(2) . ?
K3 O25 3.03(2) 18_545 ?
K3 O26 2.51(2) 18_545 ?
K3 O26 2.51(2) . ?
K3 O32 2.557(19) 5_766 ?
K3 O32 2.557(19) 15_664 ?
K3 O33 2.976(17) 5_766 ?
K3 O33 2.976(17) 15_664 ?
O2 H2A 0.8200 . ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O16 H16 0.8200 . ?
O22 H22A 0.8200 . ?
O23 H23A 0.8200 . ?
O26 H26 0.8200 . ?
O32 K3 2.557(19) 8_655 ?
O32 H32A 0.8200 . ?
O33 K3 2.976(17) 8_655 ?
O33 H33A 0.8200 . ?
O36 H36 0.8200 . ?
O42 H42A 0.8200 . ?
O43 H43A 0.8200 . ?
O45 K1 2.82(2) 8_655 ?
O46 K1 2.84(2) 8_655 ?
O46 H46 0.8200 . ?
O52 K1 2.83(2) 10_566 ?
O52 H52A 0.8200 . ?
O53 K1 3.00(2) 10_566 ?
O53 H53A 0.8200 . ?
O56 H56 0.8200 . ?
O62 H62A 0.8200 . ?
O63 H63A 0.8200 . ?
O65 K1 2.69(2) 9_565 ?
O66 K1 2.83(2) 9_565 ?
O66 H66 0.8200 . ?
O72 K2 3.360(19) 9_565 ?
O72 H72A 0.8200 . ?
O73 K2 3.151(19) 9_565 ?
O73 H73A 0.8200 . ?
O76 H76 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 117.3 . . ?
C2 C1 O5 95.8(11) . . ?
O5 C1 H1 117.3 . . ?
O14 C1 H1 117.3 . . ?
O14 C1 C2 110.0(18) . . ?
O14 C1 O5 95.0(18) . . ?
C1 C2 H2 111.5 . . ?
C3 C2 C1 119.8(18) . . ?
C3 C2 H2 111.5 . . ?
O2 C2 C1 95.3(16) . . ?
O2 C2 H2 111.5 . . ?
O2 C2 C3 105.6(19) . . ?
C2 C3 H3 101.1 . . ?
C2 C3 C4 116.2(14) . . ?
C4 C3 H3 101.1 . . ?
O3 C3 C2 119.9(18) . . ?
O3 C3 H3 101.1 . . ?
O3 C3 C4 113.0(19) . . ?
C3 C4 H4 109.4 . . ?
C3 C4 C5 108.3(13) . . ?
C5 C4 H4 109.4 . . ?
O4 C4 C3 110.6(18) . . ?
O4 C4 H4 109.4 . . ?
O4 C4 C5 109.8(18) . . ?
C4 C5 H5 105.2 . . ?
C6 C5 C4 117(3) . . ?
C6 C5 H5 105.2 . . ?
O5 C5 C4 115.3(12) . . ?
O5 C5 H5 105.2 . . ?
O5 C5 C6 108(2) . . ?
C5 C6 H6A 111.3 . . ?
C5 C6 H6B 111.3 . . ?
C5 C6 O6 102(2) . . ?
H6A C6 H6B 109.2 . . ?
O6 C6 H6A 111.3 . . ?
O6 C6 H6B 111.3 . . ?
C12 C11 H11 107.0 . . ?
O15 C11 H11 107.0 . . ?
O15 C11 C12 110.5(15) . . ?
O24 C11 H11 107.0 . . ?
O24 C11 C12 110(2) . . ?
O24 C11 O15 114.5(19) . . ?
C11 C12 H12 111.3 . . ?
C11 C12 K1 157.3(13) . . ?
C13 C12 C11 108.0(17) . . ?
C13 C12 H12 111.3 . . ?
C13 C12 K1 87.8(11) . . ?
K1 C12 H12 76.2 . . ?
O12 C12 C11 109.3(19) . . ?
O12 C12 H12 111.3 . . ?
O12 C12 C13 105.4(18) . . ?
O12 C12 K1 49.3(10) . . ?
C12 C13 H13 105.5 . . ?
C14 C13 C12 108.9(18) . . ?
C14 C13 H13 105.5 . . ?
O13 C13 C12 112.6(17) . . ?
O13 C13 H13 105.5 . . ?
O13 C13 C14 117.8(18) . . ?
C13 C14 H14 99.4 . . ?
C13 C14 O14 113.2(18) . . ?
C15 C14 C13 129.7(17) . . ?
C15 C14 H14 99.4 . . ?
C15 C14 O14 109.1(18) . . ?
O14 C14 H14 99.4 . . ?
C14 C15 H15 107.3 . . ?
C14 C15 C16 131(2) . . ?
C14 C15 O15 101.1(16) . . ?
C16 C15 H15 107.3 . . ?
O15 C15 H15 107.3 . . ?
O15 C15 C16 101(2) . . ?
C15 C16 H16A 110.1 . . ?
C15 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
O16 C16 C15 108(2) . . ?
O16 C16 H16A 110.1 . . ?
O16 C16 H16B 110.1 . . ?
C22 C21 H21 97.9 . . ?
O25 C21 H21 97.9 . . ?
O25 C21 C22 112.1(17) . . ?
O25 C21 O34 122(2) . . ?
O34 C21 H21 97.9 . . ?
O34 C21 C22 121(2) . . ?
C21 C22 H22 109.9 . . ?
C23 C22 C21 99(2) . . ?
C23 C22 H22 109.9 . . ?
O22 C22 C21 116(2) . . ?
O22 C22 H22 109.9 . . ?
O22 C22 C23 111.8(18) . . ?
C22 C23 H23 100.5 . . ?
C22 C23 C24 123(2) . . ?
C22 C23 O23 116.4(17) . . ?
C24 C23 H23 100.5 . . ?
O23 C23 H23 100.5 . . ?
O23 C23 C24 110.8(16) . . ?
C23 C24 H24 99.7 . . ?
C25 C24 C23 114.4(17) . . ?
C25 C24 H24 99.7 . . ?
O24 C24 C23 113.4(17) . . ?
O24 C24 H24 99.7 . . ?
O24 C24 C25 123.8(17) . . ?
C24 C25 H25 108.0 . . ?
C24 C25 C26 116.4(18) . . ?
C24 C25 O25 111(2) . . ?
C26 C25 H25 108.0 . . ?
O25 C25 H25 108.0 . . ?
O25 C25 C26 104.9(14) . . ?
C25 C26 H26A 108.7 . . ?
C25 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
O26 C26 C25 114.3(14) . . ?
O26 C26 H26A 108.7 . . ?
O26 C26 H26B 108.7 . . ?
C32 C31 H31 115.4 . . ?
O35 C31 H31 115.4 . . ?
O35 C31 C32 116.1(15) . . ?
O35 C31 O44 78.1(14) . . ?
O44 C31 H31 115.4 . . ?
O44 C31 C32 111(2) . . ?
C31 C32 H32 101.0 . . ?
C31 C32 K3 150.3(13) . 8_655 ?
C33 C32 C31 121.4(19) . . ?
C33 C32 H32 101.0 . . ?
C33 C32 K3 87.4(10) . 8_655 ?
K3 C32 H32 78.1 8_655 . ?
O32 C32 C31 114.0(17) . . ?
O32 C32 H32 101.0 . . ?
O32 C32 C33 113.9(19) . . ?
O32 C32 K3 39.5(11) . 8_655 ?
C32 C33 H33 103.1 . . ?
C32 C33 C34 114.7(18) . . ?
C34 C33 H33 103.1 . . ?
O33 C33 C32 115.0(15) . . ?
O33 C33 H33 103.1 . . ?
O33 C33 C34 115.2(14) . . ?
C33 C34 H34 105.1 . . ?
C35 C34 C33 113.7(13) . . ?
C35 C34 H34 105.1 . . ?
C35 C34 O34 99.8(15) . . ?
O34 C34 C33 126(2) . . ?
O34 C34 H34 105.1 . . ?
C34 C35 H35 95.4 . . ?
C34 C35 C36 114.7(7) . . ?
C34 C35 O35 123.6(14) . . ?
C36 C35 H35 95.4 . . ?
C36 C35 O35 119.1(11) . . ?
O35 C35 H35 95.4 . . ?
C35 C36 H36A 109.0 . . ?
C35 C36 H36B 109.0 . . ?
C35 C36 O36 113.1(14) . . ?
H36A C36 H36B 107.8 . . ?
O36 C36 H36A 109.0 . . ?
O36 C36 H36B 109.0 . . ?
C42 C41 H41 110.1 . . ?
O45 C41 H41 110.1 . . ?
O45 C41 C42 119.3(12) . . ?
O45 C41 O54 105.4(17) . . ?
O54 C41 H41 110.1 . . ?
O54 C41 C42 101.3(16) . . ?
C41 C42 H42 98.2 . . ?
C41 C42 C43 114.0(11) . . ?
C43 C42 H42 98.2 . . ?
O42 C42 C41 121.6(12) . . ?
O42 C42 H42 98.2 . . ?
O42 C42 C43 118.4(12) . . ?
C42 C43 H43 108.5 . . ?
C44 C43 C42 114.2(12) . . ?
C44 C43 H43 108.5 . . ?
O43 C43 C42 116.6(16) . . ?
O43 C43 H43 108.5 . . ?
O43 C43 C44 100.1(18) . . ?
C43 C44 H44 102.5 . . ?
C43 C44 C45 117.1(15) . . ?
C45 C44 H44 102.5 . . ?
O44 C44 C43 125.9(19) . . ?
O44 C44 H44 102.5 . . ?
O44 C44 C45 102.9(18) . . ?
C44 C45 H45 102.1 . . ?
C44 C45 C46 128(2) . . ?
C46 C45 H45 102.1 . . ?
O45 C45 C44 115.1(16) . . ?
O45 C45 H45 102.1 . . ?
O45 C45 C46 103.7(19) . . ?
C45 C46 H46A 110.7 . . ?
C45 C46 H46B 110.7 . . ?
C45 C46 O46 105.3(18) . . ?
H46A C46 H46B 108.8 . . ?
O46 C46 H46A 110.7 . . ?
O46 C46 H46B 110.7 . . ?
C52 C51 H51 106.3 . . ?
O55 C51 H51 106.3 . . ?
O55 C51 C52 113.2(13) . . ?
O55 C51 O64 104.7(16) . . ?
O64 C51 H51 106.3 . . ?
O64 C51 C52 119.3(19) . . ?
C51 C52 H52 113.7 . . ?
C51 C52 C53 97.1(15) . . ?
C51 C52 K1 156.7(11) . 10_566 ?
C53 C52 H52 113.7 . . ?
C53 C52 K1 93.5(10) . 10_566 ?
K1 C52 H52 80.4 10_566 . ?
O52 C52 C51 102.2(16) . . ?
O52 C52 H52 113.7 . . ?
O52 C52 C53 114.8(14) . . ?
O52 C52 K1 54.5(10) . 10_566 ?
C52 C53 H53 110.6 . . ?
C54 C53 C52 114.5(16) . . ?
C54 C53 H53 110.6 . . ?
C54 C53 O53 105.4(16) . . ?
O53 C53 C52 104.9(16) . . ?
O53 C53 H53 110.6 . . ?
C53 C54 H54 110.8 . . ?
C53 C54 C55 109.2(15) . . ?
C53 C54 O54 117.7(18) . . ?
C55 C54 H54 110.8 . . ?
O54 C54 H54 110.8 . . ?
O54 C54 C55 96.8(15) . . ?
C54 C55 H55 108.6 . . ?
C56 C55 C54 113.5(16) . . ?
C56 C55 H55 108.6 . . ?
O55 C55 C54 103.6(13) . . ?
O55 C55 H55 108.6 . . ?
O55 C55 C56 113.6(16) . . ?
C55 C56 H56A 111.8 . . ?
C55 C56 H56B 111.8 . . ?
H56A C56 H56B 109.6 . . ?
O56 C56 C55 99.7(16) . . ?
O56 C56 H56A 111.8 . . ?
O56 C56 H56B 111.8 . . ?
C62 C61 H61 113.2 . . ?
C62 C61 K1 104.9(18) . 9_565 ?
K1 C61 H61 76.0 9_565 . ?
O65 C61 H61 113.2 . . ?
O65 C61 C62 111(2) . . ?
O65 C61 K1 45.4(13) . 9_565 ?
O74 C61 H61 113.2 . . ?
O74 C61 C62 90(2) . . ?
O74 C61 K1 157.9(18) . 9_565 ?
O74 C61 O65 114(2) . . ?
C61 C62 H62 94.6 . . ?
C61 C62 C63 119(2) . . ?
C63 C62 H62 94.6 . . ?
O62 C62 C61 127(2) . . ?
O62 C62 H62 94.6 . . ?
O62 C62 C63 112(2) . . ?
C62 C63 H63 103.8 . . ?
C64 C63 C62 117.9(19) . . ?
C64 C63 H63 103.8 . . ?
O63 C63 C62 108(2) . . ?
O63 C63 H63 103.8 . . ?
O63 C63 C64 118(2) . . ?
C63 C64 H64 106.3 . . ?
C63 C64 C65 113(2) . . ?
C65 C64 H64 106.3 . . ?
O64 C64 C63 102(2) . . ?
O64 C64 H64 106.3 . . ?
O64 C64 C65 122(3) . . ?
C64 C65 H65 108.2 . . ?
C66 C65 C64 113(2) . . ?
C66 C65 H65 108.2 . . ?
C66 C65 O65 112(2) . . ?
O65 C65 C64 106.6(19) . . ?
O65 C65 H65 108.2 . . ?
C65 C66 H66A 112.7 . . ?
C65 C66 H66B 112.7 . . ?
C65 C66 O66 95(2) . . ?
H66A C66 H66B 110.2 . . ?
O66 C66 H66A 112.7 . . ?
O66 C66 H66B 112.7 . . ?
C72 C71 H71 103.1 . . ?
O4 C71 H71 103.1 . . ?
O4 C71 C72 113.2(12) . . ?
O75 C71 H71 103.1 . . ?
O75 C71 C72 116.1(11) . . ?
O75 C71 O4 115.8(12) . . ?
C71 C72 H72 115.7 . . ?
C71 C72 C73 99.5(16) . . ?
C73 C72 H72 115.7 . . ?
O72 C72 C71 108.0(14) . . ?
O72 C72 H72 115.7 . . ?
O72 C72 C73 100.0(17) . . ?
C72 C73 H73 100.2 . . ?
C74 C73 C72 114.8(19) . . ?
C74 C73 H73 100.2 . . ?
O73 C73 C72 113.4(15) . . ?
O73 C73 H73 100.2 . . ?
O73 C73 C74 122.6(17) . . ?
C73 C74 H74 96.0 . . ?
C73 C74 C75 125.5(19) . . ?
C73 C74 O74 116.2(17) . . ?
C75 C74 H74 96.0 . . ?
C75 C74 O74 115.0(18) . . ?
O74 C74 H74 96.0 . . ?
C74 C75 H75 108.4 . . ?
C76 C75 C74 113.9(17) . . ?
C76 C75 H75 108.4 . . ?
O75 C75 C74 106.9(18) . . ?
O75 C75 H75 108.4 . . ?
O75 C75 C76 110.6(19) . . ?
C75 C76 H76A 108.5 . . ?
C75 C76 H76B 108.5 . . ?
H76A C76 H76B 107.5 . . ?
O76 C76 C75 115.1(18) . . ?
O76 C76 H76A 108.5 . . ?
O76 C76 H76B 108.5 . . ?
C52 K1 C12 145.4(6) 10_566 . ?
C52 K1 C61 110.4(5) 10_566 14_654 ?
C61 K1 C12 82.0(6) 14_654 . ?
O12 K1 C12 24.4(4) . . ?
O12 K1 C52 131.0(6) . 10_566 ?
O12 K1 C61 106.4(6) . 14_654 ?
O12 K1 O13 60.9(5) . . ?
O12 K1 O45 90.7(6) . 15_664 ?
O12 K1 O46 75.5(6) . 15_664 ?
O12 K1 O52 132.1(6) . 10_566 ?
O12 K1 O53 91.9(6) . 10_566 ?
O12 K1 O66 158.4(6) . 14_654 ?
O13 K1 C12 43.9(4) . . ?
O13 K1 C52 113.4(5) . 10_566 ?
O13 K1 C61 60.1(6) . 14_654 ?
O45 K1 C12 104.7(5) 15_664 . ?
O45 K1 C52 95.2(6) 15_664 10_566 ?
O45 K1 C61 123.2(6) 15_664 14_654 ?
O45 K1 O13 148.5(6) 15_664 . ?
O45 K1 O46 60.8(6) 15_664 15_664 ?
O45 K1 O52 118.4(6) 15_664 10_566 ?
O45 K1 O53 78.6(6) 15_664 10_566 ?
O45 K1 O66 70.8(5) 15_664 14_654 ?
O46 K1 C12 67.2(6) 15_664 . ?
O46 K1 C52 146.9(6) 15_664 10_566 ?
O46 K1 C61 71.6(6) 15_664 14_654 ?
O46 K1 O13 96.5(6) 15_664 . ?
O46 K1 O53 136.9(6) 15_664 10_566 ?
O52 K1 C12 132.9(6) 10_566 . ?
O52 K1 C52 24.8(4) 10_566 10_566 ?
O52 K1 C61 89.2(5) 10_566 14_654 ?
O52 K1 O13 92.1(6) 10_566 . ?
O52 K1 O46 151.0(5) 10_566 15_664 ?
O52 K1 O53 61.4(5) 10_566 10_566 ?
O52 K1 O66 68.7(6) 10_566 14_654 ?
O53 K1 C12 113.9(6) 10_566 . ?
O53 K1 C52 42.6(5) 10_566 10_566 ?
O53 K1 C61 150.3(6) 10_566 14_654 ?
O53 K1 O13 113.2(6) 10_566 . ?
O65 K1 C12 99.1(6) 14_654 . ?
O65 K1 C52 102.7(6) 14_654 10_566 ?
O65 K1 C61 22.0(5) 14_654 14_654 ?
O65 K1 O12 122.6(7) 14_654 . ?
O65 K1 O13 82.1(7) 14_654 . ?
O65 K1 O45 105.1(6) 14_654 15_664 ?
O65 K1 O46 66.3(6) 14_654 15_664 ?
O65 K1 O52 87.7(6) 14_654 10_566 ?
O65 K1 O53 144.8(6) 14_654 10_566 ?
O65 K1 O66 55.6(6) 14_654 14_654 ?
O66 K1 C12 149.5(6) 14_654 . ?
O66 K1 C52 64.0(5) 14_654 10_566 ?
O66 K1 C61 76.5(6) 14_654 14_654 ?
O66 K1 O13 132.9(6) 14_654 . ?
O66 K1 O46 85.5(6) 14_654 15_664 ?
O66 K1 O53 95.1(6) 14_654 10_566 ?
O5 K2 O5 112.7(8) . 17_655 ?
O5 K2 O72 113.2(5) 17_655 6_556 ?
O5 K2 O72 85.8(4) . 6_556 ?
O5 K2 O72 85.8(4) 17_655 14_654 ?
O5 K2 O72 113.2(5) . 14_654 ?
O5 K2 O73 133.3(5) 17_655 14_654 ?
O5 K2 O73 81.6(5) . 14_654 ?
O5 K2 O73 133.3(5) . 6_556 ?
O5 K2 O73 81.6(5) 17_655 6_556 ?
O6 K2 O5 58.6(6) . . ?
O6 K2 O5 77.0(6) 17_655 . ?
O6 K2 O5 58.6(6) 17_655 17_655 ?
O6 K2 O5 77.0(6) . 17_655 ?
O6 K2 O6 95.5(9) 17_655 . ?
O6 K2 O72 59.1(5) . 6_556 ?
O6 K2 O72 154.4(7) 17_655 6_556 ?
O6 K2 O72 59.1(5) 17_655 14_654 ?
O6 K2 O72 154.4(7) . 14_654 ?
O6 K2 O73 138.9(6) . 14_654 ?
O6 K2 O73 84.4(5) 17_655 14_654 ?
O6 K2 O73 138.9(6) 17_655 6_556 ?
O6 K2 O73 84.4(5) . 6_556 ?
O72 K2 O72 146.4(8) 14_654 6_556 ?
O73 K2 O72 112.0(5) 14_654 6_556 ?
O73 K2 O72 49.0(5) 14_654 14_654 ?
O73 K2 O72 49.0(5) 6_556 6_556 ?
O73 K2 O72 112.0(5) 6_556 14_654 ?
O73 K2 O73 121.7(8) 14_654 6_556 ?
C32 K3 C32 138.9(11) 5_766 15_664 ?
O25 K3 C32 96.6(6) 18_545 15_664 ?
O25 K3 C32 106.9(5) . 15_664 ?
O25 K3 C32 106.9(5) 18_545 5_766 ?
O25 K3 C32 96.6(6) . 5_766 ?
O25 K3 O25 109.3(8) 18_545 . ?
O26 K3 C32 78.2(7) 18_545 5_766 ?
O26 K3 C32 78.2(7) . 15_664 ?
O26 K3 C32 142.4(8) 18_545 15_664 ?
O26 K3 C32 142.4(8) . 5_766 ?
O26 K3 O25 57.5(6) 18_545 18_545 ?
O26 K3 O25 64.4(6) 18_545 . ?
O26 K3 O25 57.5(6) . . ?
O26 K3 O25 64.4(6) . 18_545 ?
O26 K3 O26 66.3(9) 18_545 . ?
O26 K3 O32 80.2(6) . 15_664 ?
O26 K3 O32 145.4(7) 18_545 15_664 ?
O26 K3 O32 145.3(7) . 5_766 ?
O26 K3 O32 80.2(6) 18_545 5_766 ?
O26 K3 O33 102.8(6) 18_545 5_766 ?
O26 K3 O33 102.8(6) . 15_664 ?
O26 K3 O33 132.6(6) . 5_766 ?
O26 K3 O33 132.6(6) 18_545 15_664 ?
O32 K3 C32 21.3(5) 5_766 5_766 ?
O32 K3 C32 21.3(5) 15_664 15_664 ?
O32 K3 C32 131.2(7) 5_766 15_664 ?
O32 K3 C32 131.2(7) 15_664 5_766 ?
O32 K3 O25 90.9(6) 15_664 . ?
O32 K3 O25 115.8(6) 5_766 . ?
O32 K3 O25 115.8(6) 15_664 18_545 ?
O32 K3 O25 90.9(6) 5_766 18_545 ?
O32 K3 O32 134.2(10) 5_766 15_664 ?
O32 K3 O33 61.5(6) 15_664 15_664 ?
O32 K3 O33 61.5(6) 5_766 5_766 ?
O32 K3 O33 93.4(6) 15_664 5_766 ?
O32 K3 O33 93.4(6) 5_766 15_664 ?
O33 K3 C32 110.5(7) 5_766 15_664 ?
O33 K3 C32 110.5(7) 15_664 5_766 ?
O33 K3 C32 43.4(3) 5_766 5_766 ?
O33 K3 C32 43.4(3) 15_664 15_664 ?
O33 K3 O25 149.8(5) 5_766 18_545 ?
O33 K3 O25 75.9(5) 15_664 18_545 ?
O33 K3 O25 149.9(5) 15_664 . ?
O33 K3 O25 75.9(5) 5_766 . ?
O33 K3 O33 115.2(8) 5_766 15_664 ?
C2 O2 H2A 109.5 . . ?
C3 O3 H3A 109.5 . . ?
C4 O4 C71 116.2(15) . . ?
C1 O5 K2 101.1(12) . . ?
C5 O5 C1 127.0(16) . . ?
C5 O5 K2 111.4(16) . . ?
C6 O6 K2 119.2(16) . . ?
C6 O6 H6 109.5 . . ?
K2 O6 H6 131.3 . . ?
C12 O12 K1 106.3(13) . . ?
C12 O12 H12A 109.5 . . ?
K1 O12 H12A 130.6 . . ?
C13 O13 K1 109.6(12) . . ?
C13 O13 H13A 109.5 . . ?
K1 O13 H13A 140.8 . . ?
C1 O14 C14 115.9(15) . . ?
C15 O15 C11 112.3(14) . . ?
C16 O16 H16 109.5 . . ?
C22 O22 H22A 109.5 . . ?
C23 O23 H23A 109.5 . . ?
C24 O24 C11 129(2) . . ?
C21 O25 C25 105.9(18) . . ?
C21 O25 K3 122.8(15) . . ?
C25 O25 K3 110.7(14) . . ?
C26 O26 K3 131.3(14) . . ?
C26 O26 H26 109.5 . . ?
K3 O26 H26 118.9 . . ?
C32 O32 K3 119.3(15) . 8_655 ?
C32 O32 H32A 109.5 . . ?
K3 O32 H32A 127.5 8_655 . ?
C33 O33 K3 111.2(10) . 8_655 ?
C33 O33 H33A 109.5 . . ?
K3 O33 H33A 135.3 8_655 . ?
C21 O34 C34 115.5(13) . . ?
C31 O35 C35 117.3(12) . . ?
C36 O36 H36 109.5 . . ?
C42 O42 H42A 109.5 . . ?
C43 O43 H43A 109.5 . . ?
C44 O44 C31 114.9(15) . . ?
C41 O45 K1 109.2(14) . 8_655 ?
C45 O45 C41 115.1(16) . . ?
C45 O45 K1 113.5(16) . 8_655 ?
C46 O46 K1 109.7(12) . 8_655 ?
C46 O46 H46 109.5 . . ?
K1 O46 H46 15.9 8_655 . ?
C52 O52 K1 100.8(12) . 10_566 ?
C52 O52 H52A 109.5 . . ?
K1 O52 H52A 18.3 10_566 . ?
C53 O53 K1 113.2(12) . 10_566 ?
C53 O53 H53A 109.5 . . ?
K1 O53 H53A 137.2 10_566 . ?
C41 O54 C54 113.3(13) . . ?
C51 O55 C55 114.1(12) . . ?
C56 O56 H56 109.5 . . ?
C62 O62 H62A 109.5 . . ?
C63 O63 H63A 109.5 . . ?
C64 O64 C51 117(2) . . ?
C61 O65 C65 113(2) . . ?
C61 O65 K1 112.5(17) . 9_565 ?
C65 O65 K1 125.3(16) . 9_565 ?
C66 O66 K1 124.3(14) . 9_565 ?
C66 O66 H66 109.5 . . ?
K1 O66 H66 110.9 9_565 . ?
C72 O72 K2 118.1(12) . 9_565 ?
C72 O72 H72A 109.5 . . ?
K2 O72 H72A 18.5 9_565 . ?
C73 O73 K2 127.7(12) . 9_565 ?
C73 O73 H73A 109.5 . . ?
K2 O73 H73A 97.4 9_565 . ?
C61 O74 C74 119(2) . . ?
C71 O75 C75 111.3(15) . . ?
C76 O76 H76 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -61(3) . . . . ?
C1 C2 C3 O3 157(2) . . . . ?
C2 C1 O5 C5 -44(3) . . . . ?
C2 C1 O5 K2 84.0(13) . . . . ?
C2 C1 O14 C14 -141.3(17) . . . . ?
C2 C3 C4 C5 48(3) . . . . ?
C2 C3 C4 O4 168(2) . . . . ?
C3 C4 C5 C6 -167(2) . . . . ?
C3 C4 C5 O5 -39(3) . . . . ?
C3 C4 O4 C71 139.7(17) . . . . ?
C4 C5 C6 O6 62(3) . . . . ?
C4 C5 O5 C1 44(4) . . . . ?
C4 C5 O5 K2 -79(2) . . . . ?
C5 C4 O4 C71 -101(2) . . . . ?
C5 C6 O6 K2 56(3) . . . . ?
C6 C5 O5 C1 177(2) . . . . ?
C6 C5 O5 K2 53(2) . . . . ?
C11 C12 C13 C14 -42(3) . . . . ?
C11 C12 C13 O13 -175.0(19) . . . . ?
C11 C12 O12 K1 171.0(14) . . . . ?
C12 C11 O15 C15 -70(2) . . . . ?
C12 C11 O24 C24 -127(2) . . . . ?
C12 C13 C14 C15 42(4) . . . . ?
C12 C13 C14 O14 -172.6(19) . . . . ?
C12 C13 O13 K1 -27(2) . . . . ?
C13 C12 O12 K1 -73.1(19) . . . . ?
C13 C14 C15 C16 -161(3) . . . . ?
C13 C14 C15 O15 -46(4) . . . . ?
C13 C14 O14 C1 93(3) . . . . ?
C14 C13 O13 K1 -155.4(19) . . . . ?
C14 C15 C16 O16 59(4) . . . . ?
C14 C15 O15 C11 55(3) . . . . ?
C15 C14 O14 C1 -115(2) . . . . ?
C16 C15 O15 C11 -170(2) . . . . ?
C21 C22 C23 C24 -41(3) . . . . ?
C21 C22 C23 O23 176(2) . . . . ?
C22 C21 O25 C25 -79(3) . . . . ?
C22 C21 O25 K3 49(3) . . . . ?
C22 C21 O34 C34 -90(3) . . . . ?
C22 C23 C24 C25 29(4) . . . . ?
C22 C23 C24 O24 179(2) . . . . ?
C23 C24 C25 C26 -154(2) . . . . ?
C23 C24 C25 O25 -34(3) . . . . ?
C23 C24 O24 C11 121(3) . . . . ?
C24 C25 C26 O26 77(3) . . . . ?
C24 C25 O25 C21 57(2) . . . . ?
C24 C25 O25 K3 -78.7(18) . . . . ?
C25 C24 O24 C11 -92(3) . . . . ?
C25 C26 O26 K3 21(3) . . . . ?
C26 C25 O25 C21 -176.8(18) . . . . ?
C26 C25 O25 K3 48(2) . . . . ?
C31 C32 C33 C34 -35(4) . . . . ?
C31 C32 C33 O33 -172(2) . . . . ?
C31 C32 O32 K3 162.9(18) . . . 8_655 ?
C32 C31 O35 C35 -21(3) . . . . ?
C32 C31 O44 C44 -106(2) . . . . ?
C32 C33 C34 C35 32(4) . . . . ?
C32 C33 C34 O34 156(2) . . . . ?
C32 C33 O33 K3 -20(3) . . . 8_655 ?
C33 C32 O32 K3 -52(3) . . . 8_655 ?
C33 C34 C35 C36 170(2) . . . . ?
C33 C34 C35 O35 -29(4) . . . . ?
C33 C34 O34 C21 101(3) . . . . ?
C34 C33 O33 K3 -157(2) . . . 8_655 ?
C34 C35 C36 O36 78(3) . . . . ?
C34 C35 O35 C31 23(4) . . . . ?
C35 C34 O34 C21 -130(2) . . . . ?
C36 C35 O35 C31 -176.4(18) . . . . ?
C41 C42 C43 C44 -34(3) . . . . ?
C41 C42 C43 O43 -149.7(18) . . . . ?
C42 C41 O45 C45 -44(3) . . . . ?
C42 C41 O45 K1 85(2) . . . 8_655 ?
C42 C41 O54 C54 -114.6(17) . . . . ?
C42 C43 C44 C45 36(3) . . . . ?
C42 C43 C44 O44 169(2) . . . . ?
C43 C44 C45 C46 -175(2) . . . . ?
C43 C44 C45 O45 -41(3) . . . . ?
C43 C44 O44 C31 104(3) . . . . ?
C44 C45 C46 O46 62(3) . . . . ?
C44 C45 O45 C41 43(3) . . . . ?
C44 C45 O45 K1 -84(2) . . . 8_655 ?
C45 C44 O44 C31 -118(2) . . . . ?
C45 C46 O46 K1 53.0(18) . . . 8_655 ?
C46 C45 O45 C41 -172.1(17) . . . . ?
C46 C45 O45 K1 61.1(19) . . . 8_655 ?
C51 C52 C53 C54 -65(2) . . . . ?
C51 C52 C53 O53 179.5(16) . . . . ?
C51 C52 O52 K1 -179.6(12) . . . 10_566 ?
C52 C51 O55 C55 -66(2) . . . . ?
C52 C51 O64 C64 -121(2) . . . . ?
C52 C53 C54 C55 68(2) . . . . ?
C52 C53 C54 O54 177.3(17) . . . . ?
C52 C53 O53 K1 -25.3(18) . . . 10_566 ?
C53 C52 O52 K1 -75.8(17) . . . 10_566 ?
C53 C54 C55 C56 -179.4(17) . . . . ?
C53 C54 C55 O55 -56(2) . . . . ?
C53 C54 O54 C41 115(2) . . . . ?
C54 C53 O53 K1 -146.6(13) . . . 10_566 ?
C54 C55 C56 O56 54(2) . . . . ?
C54 C55 O55 C51 56(2) . . . . ?
C55 C54 O54 C41 -129.2(16) . . . . ?
C56 C55 O55 C51 179.7(16) . . . . ?
C61 C62 C63 C64 -19(4) . . . . ?
C61 C62 C63 O63 -156(2) . . . . ?
C62 C61 O65 C65 -58(3) . . . . ?
C62 C61 O65 K1 91(2) . . . 9_565 ?
C62 C61 O74 C74 -136.1(19) . . . . ?
C62 C63 C64 C65 31(4) . . . . ?
C62 C63 C64 O64 164(2) . . . . ?
C63 C64 C65 C66 -177(2) . . . . ?
C63 C64 C65 O65 -53(3) . . . . ?
C63 C64 O64 C51 123(2) . . . . ?
C64 C65 C66 O66 67(3) . . . . ?
C64 C65 O65 C61 70(3) . . . . ?
C64 C65 O65 K1 -74(2) . . . 9_565 ?
C65 C64 O64 C51 -110(3) . . . . ?
C65 C66 O66 K1 46(2) . . . 9_565 ?
C66 C65 O65 C61 -166(2) . . . . ?
C66 C65 O65 K1 51(3) . . . 9_565 ?
C71 C72 C73 C74 -45(2) . . . . ?
C71 C72 C73 O73 166.7(17) . . . . ?
C71 C72 O72 K2 -163.8(13) . . . 9_565 ?
C72 C71 O4 C4 -105(2) . . . . ?
C72 C71 O75 C75 -72(2) . . . . ?
C72 C73 C74 C75 32(4) . . . . ?
C72 C73 C74 O74 -169.6(19) . . . . ?
C72 C73 O73 K2 -32(3) . . . 9_565 ?
C73 C72 O72 K2 -60.3(16) . . . 9_565 ?
C73 C74 C75 C76 -148(2) . . . . ?
C73 C74 C75 O75 -26(3) . . . . ?
C73 C74 O74 C61 91(3) . . . . ?
C74 C73 O73 K2 -176.5(17) . . . 9_565 ?
C74 C75 C76 O76 54(3) . . . . ?
C74 C75 O75 C71 41(2) . . . . ?
C75 C74 O74 C61 -108(3) . . . . ?
C76 C75 O75 C71 165.0(16) . . . . ?
K1 C12 C13 C14 154.4(19) . . . . ?
K1 C12 C13 O13 21.7(19) . . . . ?
K1 C52 C53 C54 135.3(16) 10_566 . . . ?
K1 C52 C53 O53 20.3(14) 10_566 . . . ?
K1 C61 C62 C63 79(3) 9_565 . . . ?
K1 C61 C62 O62 -118(3) 9_565 . . . ?
K1 C61 O65 C65 -148(2) 9_565 . . . ?
K1 C61 O74 C74 90(5) 9_565 . . . ?
K3 C32 C33 C34 153(2) 8_655 . . . ?
K3 C32 C33 O33 15(2) 8_655 . . . ?
O2 C2 C3 C4 -167(2) . . . . ?
O2 C2 C3 O3 51(3) . . . . ?
O3 C3 C4 C5 -168(2) . . . . ?
O3 C3 C4 O4 -47(3) . . . . ?
O4 C4 C5 C6 72(3) . . . . ?
O4 C4 C5 O5 -160(2) . . . . ?
O4 C71 C72 C73 -68.0(19) . . . . ?
O4 C71 C72 O72 36(2) . . . . ?
O4 C71 O75 C75 64(2) . . . . ?
O5 C1 C2 C3 49(2) . . . . ?
O5 C1 C2 O2 160.8(17) . . . . ?
O5 C1 O14 C14 120.7(18) . . . . ?
O5 C5 C6 O6 -70(3) . . . . ?
O12 C12 C13 C14 -159(2) . . . . ?
O12 C12 C13 O13 68(3) . . . . ?
O13 C13 C14 C15 172(3) . . . . ?
O13 C13 C14 O14 -43(3) . . . . ?
O14 C1 C2 C3 -48(2) . . . . ?
O14 C1 C2 O2 63(2) . . . . ?
O14 C1 O5 C5 67(2) . . . . ?
O14 C1 O5 K2 -165.3(11) . . . . ?
O14 C14 C15 C16 53(4) . . . . ?
O14 C14 C15 O15 167.8(19) . . . . ?
O15 C11 C12 C13 60(2) . . . . ?
O15 C11 C12 K1 -168(3) . . . . ?
O15 C11 C12 O12 173.8(17) . . . . ?
O15 C11 O24 C24 108(2) . . . . ?
O15 C15 C16 O16 -56(3) . . . . ?
O22 C22 C23 C24 -163(2) . . . . ?
O22 C22 C23 O23 54(3) . . . . ?
O23 C23 C24 C25 173.5(19) . . . . ?
O23 C23 C24 O24 -37(3) . . . . ?
O24 C11 C12 C13 -68(2) . . . . ?
O24 C11 C12 K1 64(5) . . . . ?
O24 C11 C12 O12 46(2) . . . . ?
O24 C11 O15 C15 55(3) . . . . ?
O24 C24 C25 C26 60(3) . . . . ?
O24 C24 C25 O25 -180(2) . . . . ?
O25 C21 C22 C23 66(3) . . . . ?
O25 C21 C22 O22 -174.2(19) . . . . ?
O25 C21 O34 C34 118(3) . . . . ?
O25 C25 C26 O26 -46(3) . . . . ?
O32 C32 C33 C34 -177(2) . . . . ?
O32 C32 C33 O33 46(4) . . . . ?
O33 C33 C34 C35 169(2) . . . . ?
O33 C33 C34 O34 -67(4) . . . . ?
O34 C21 C22 C23 -88(2) . . . . ?
O34 C21 C22 O22 32(3) . . . . ?
O34 C21 O25 C25 74(3) . . . . ?
O34 C21 O25 K3 -157.4(16) . . . . ?
O34 C34 C35 C36 33(3) . . . . ?
O34 C34 C35 O35 -166(2) . . . . ?
O35 C31 C32 C33 29(4) . . . . ?
O35 C31 C32 K3 -166(3) . . . 8_655 ?
O35 C31 C32 O32 171(2) . . . . ?
O35 C31 O44 C44 140.1(18) . . . . ?
O35 C35 C36 O36 -84(3) . . . . ?
O42 C42 C43 C44 173(2) . . . . ?
O42 C42 C43 O43 57(3) . . . . ?
O43 C43 C44 C45 161(2) . . . . ?
O43 C43 C44 O44 -66(3) . . . . ?
O44 C31 C32 C33 -58(3) . . . . ?
O44 C31 C32 K3 107(4) . . . 8_655 ?
O44 C31 C32 O32 85(3) . . . . ?
O44 C31 O35 C35 86(2) . . . . ?
O44 C44 C45 C46 42(3) . . . . ?
O44 C44 C45 O45 177(2) . . . . ?
O45 C41 C42 C43 39(3) . . . . ?
O45 C41 C42 O42 -169(2) . . . . ?
O45 C41 O54 C54 120.5(17) . . . . ?
O45 C45 C46 O46 -76(2) . . . . ?
O52 C52 C53 C54 -172.4(18) . . . . ?
O52 C52 C53 O53 73(2) . . . . ?
O53 C53 C54 C55 -176.8(16) . . . . ?
O53 C53 C54 O54 -68(2) . . . . ?
O54 C41 C42 C43 -76(2) . . . . ?
O54 C41 C42 O42 76(2) . . . . ?
O54 C41 O45 C45 69(2) . . . . ?
O54 C41 O45 K1 -162.3(11) . . . 8_655 ?
O54 C54 C55 C56 58(2) . . . . ?
O54 C54 C55 O55 -178.2(14) . . . . ?
O55 C51 C52 C53 61.3(19) . . . . ?
O55 C51 C52 K1 178(2) . . . 10_566 ?
O55 C51 C52 O52 178.6(15) . . . . ?
O55 C51 O64 C64 111(2) . . . . ?
O55 C55 C56 O56 -64(2) . . . . ?
O62 C62 C63 C64 175(2) . . . . ?
O62 C62 C63 O63 39(3) . . . . ?
O63 C63 C64 C65 163(2) . . . . ?
O63 C63 C64 O64 -64(3) . . . . ?
O64 C51 C52 C53 -62.5(19) . . . . ?
O64 C51 C52 K1 54(4) . . . 10_566 ?
O64 C51 C52 O52 55(2) . . . . ?
O64 C51 O55 C55 66(2) . . . . ?
O64 C64 C65 C66 61(4) . . . . ?
O64 C64 C65 O65 -175(2) . . . . ?
O65 C61 C62 C63 31(4) . . . . ?
O65 C61 C62 O62 -165(3) . . . . ?
O65 C61 O74 C74 111(2) . . . . ?
O65 C65 C66 O66 -54(2) . . . . ?
O72 C72 C73 C74 -155.8(19) . . . . ?
O72 C72 C73 O73 56(2) . . . . ?
O73 C73 C74 C75 176(2) . . . . ?
O73 C73 C74 O74 -25(4) . . . . ?
O74 C61 C62 C63 -85(3) . . . . ?
O74 C61 C62 O62 78(3) . . . . ?
O74 C61 O65 C65 42(3) . . . . ?
O74 C61 O65 K1 -169.2(17) . . . 9_565 ?
O74 C74 C75 C76 53(3) . . . . ?
O74 C74 C75 O75 175.4(19) . . . . ?
O75 C71 C72 C73 70(2) . . . . ?
O75 C71 C72 O72 173.4(18) . . . . ?
O75 C71 O4 C4 117.1(19) . . . . ?
O75 C75 C76 O76 -66(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.637 -0.310 -0.510 21814.9 1518.6 ?


_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 1.989
_oxdiff_exptl_absorpt_empirical_full_min 0.608
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_0_99GPa
_database_code_depnum_ccdc_archive 'CCDC 1529151'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_REFNR01_CDMOF_a_0_99GPa     
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_RINTA01_CDMOF_a_0_99GPa     
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: 'Crystals of this compound dissolve when compressed;
pressure-induced dissolution influence the crystal quality 
and therefore quality of collected data'
;
_vrf_THETM01_CDMOF_a_0_99GPa     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT020_CDMOF_a_0_99GPa     
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.297 Report
RESPONSE: 'Crystals of this compound dissolve when compressed;
pressure-induced dissolution influence the crystal quality 
and therefore quality of collected data'
;
_vrf_PLAT029_CDMOF_a_0_99GPa     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.732 Note  
RESPONSE: 'Theta angle was limited due to the poorly 
diffracting sample crystal and DAC construction'
;
_vrf_PLAT090_CDMOF_a_0_99GPa     
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       2.19 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample; this along with 
poorly diffracting sample crystal lowers the number of 
collected reflections'
;
_vrf_PLAT201_CDMOF_a_0_99GPa     
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT430_CDMOF_a_0_99GPa     
;
PROBLEM: Short Inter D...A Contact  Oa     ..  Oa      ..       2.18 Ang.  
RESPONSE: 'Short distance is due to the crystal structure compression'
;
_vrf_PLAT241_CDMOF_a_0_99GPa     
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         K1 Check 
RESPONSE: 'Poor data quality or unresolved disorder'
;
_vrf_PLAT306_CDMOF_a_0_99GPa     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_0_99GPa     
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.045 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_CDMOF_a_0_99GPa     
;
PROBLEM: D-H Without Acceptor       O6     --  H6     ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
_vrf_PLAT910_CDMOF_a_0_99GPa     
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          32 Note  
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample limiting the range of 
collected reflections'
;
_vrf_PLAT911_CDMOF_a_0_99GPa     
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.249         29 Report
RESPONSE: 'diamond-anvil cell construction limits 
access of the X-ray beam to the sample limiting the range of 
collected reflections'
;
# end Validation Reply Form
# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   30.968(6)
_cell_length_b                   30.968(6)
_cell_length_c                   30.968(6)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     29699(11)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    361
_cell_measurement_temperature    295
_cell_measurement_theta_max      8.8520
_cell_measurement_theta_min      4.6780
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67886
_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_absorpt_special_details   ?

# EXPERIMENTAL DATA 
_exptl_special_details           
; 
Data collected for the crystal grown in
diamond-anvil cell at 0.1GPa and then
compressed to 0.99GPa
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.945
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8928
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'Compressed crystal that was grown in situ from methano:water solution in the diamond-anvil cell at 0.1 GPa.'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2967
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 0.732
_diffrn_reflns_Laue_measured_fraction_max 0.729
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7547
_diffrn_reflns_point_group_measured_fraction_full 0.783
_diffrn_reflns_point_group_measured_fraction_max 0.781
_diffrn_reflns_theta_full        10.197
_diffrn_reflns_theta_max         10.197
_diffrn_reflns_theta_min         4.837
_diffrn_ambient_temperature      295
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         990000
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.732
_diffrn_measured_fraction_theta_max 0.729
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -35.00  19.75   0.75   20.00   0.00 -30.00   0.00    --    73
  2  φ    140.00 200.00   0.75   20.00   0.00 -30.00   0.00    --    80
  3  φ    160.00 217.00   0.75   20.00   0.00  30.00   0.00    --    76
  4  φ    -20.00  34.75   0.75   20.00   0.00  30.00   0.00    --    73
  5  ω    -24.00  24.00   0.75   20.00    --   30.00  39.46 -12.90   64
  6  ω    -24.00  24.00   0.75   20.00    --   30.00  39.46 167.10   64
  7  ω    -50.00  10.00   0.75   20.00    --  -30.00  39.46 167.10   80
  8  ω    -50.00  10.00   0.75   20.00    --  -30.00  39.46 -12.90   80
  9  ω    -64.00  -8.50   0.75   20.00    --  -30.00  81.40 -28.90   74
 10  ω    -64.00  -8.50   0.75   20.00    --  -30.00  81.40 151.10   74
 11  ω    -19.00   8.00   0.75   20.00    --   30.00  81.40 151.10   36
 12  ω    -19.00   8.00   0.75   20.00    --   30.00  81.40 -28.90   36
 13  ω    -43.00 -21.25   0.75   20.00    --   30.00 134.60 -56.90   29
 14  ω    -43.00 -21.25   0.75   20.00    --   30.00 134.60 123.10   29
 15  ω    -90.00 -36.00   0.75   20.00    --  -30.00 134.60 123.10   72
 16  ω    -90.00 -36.00   0.75   20.00    --  -30.00 134.60 -56.90   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0027204000
_diffrn_orient_matrix_UB_12      0.0015446000
_diffrn_orient_matrix_UB_13      0.0226885000
_diffrn_orient_matrix_UB_21      0.0189117000
_diffrn_orient_matrix_UB_22      0.0125009000
_diffrn_orient_matrix_UB_23      -0.0033111000
_diffrn_orient_matrix_UB_31      -0.0126269000
_diffrn_orient_matrix_UB_32      0.0191002000
_diffrn_orient_matrix_UB_33      0.0002382000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          
'high-pressure measurement in diamond-anvil cell at 0.99 GPa'
_reflns_Friedel_coverage         0.610
_reflns_Friedel_fraction_full    0.884
_reflns_Friedel_fraction_max     0.885
_reflns_number_gt                260
_reflns_number_total             264
_reflns_odcompleteness_completeness 82.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     10.18
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.107
_refine_diff_density_min         -0.092
_refine_diff_density_rms         0.024
_refine_ls_abs_structure_details 
;
 Flack x determined using 89 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.8(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         264
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0865
_refine_ls_restrained_S_all      1.786
_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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2315
_refine_ls_wR_factor_ref         0.2326
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The DAC imposes severe restrictions on which reflections can be collected,
 resulting in a low data:parameter ratio.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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
 C14-O14
 1.45 with sigma of 0.002
 C14-C13
 1.5 with sigma of 0.02
 O2-C3
 2.2 with sigma of 0.02
 C11-O4
 1.45 with sigma of 0.002
 C11-C14
 3 with sigma of 0.02
 C4-O4
 1.45 with sigma of 0.002
 C4-C3
 1.5 with sigma of 0.002
 C12-O4
 2 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.002
 C2-C3
 1.5 with sigma of 0.002
 C2-O2
 1.45 with sigma of 0.002
 C1-C4
 2.8 with sigma of 0.02
 C2-C1
 1.5 with sigma of 0.002
 O3-C3
 1.45 with sigma of 0.002
 C2-O3
 2.3 with sigma of 0.02
 C16-C15
 1.5 with sigma of 0.002
 C14-C15
 1.5 with sigma of 0.002
 O14-C15
 2.4 with sigma of 0.02
 C12-C15
 3 with sigma of 0.02
 C15-C12
 3 with sigma of 0.02
 C6-C5
 1.5 with sigma of 0.002
 C4-C5
 1.5 with sigma of 0.002
 C2-C5
 3 with sigma of 0.02
 C5-C2
 3 with sigma of 0.02
 C5-C1
 2.3 with sigma of 0.002
 C5-C4
 1.5 with sigma of 0.02
 C3-C4
 1.5 with sigma of 0.02
 O4-C4
 1.45 with sigma of 0.02
 C16-O16
 1.45 with sigma of 0.002
 C6-O6
 1.45 with sigma of 0.002
 O13-C13
 1.45 with sigma of 0.002
 C12-O12
 1.45 with sigma of 0.02
 O5-C6
 2.5 with sigma of 0.02
 O15-C16
 2.2 with sigma of 0.02
 O5-C3
 3 with sigma of 0.02
 O15-C13
 3 with sigma of 0.02
 O15-C11
 1.45 with sigma of 0.002
 O5-C1
 1.45 with sigma of 0.002
 O15-C15
 1.45 with sigma of 0.002
 O5-C5
 1.45 with sigma of 0.002
 C13-O14
 2.5 with sigma of 0.04
 C11-C13
 2.4 with sigma of 0.02
 C11-C4
 2.5 with sigma of 0.04
 C12-C14
 2.4 with sigma of 0.02
 O2-C3
 2.5 with sigma of 0.04
 C4-C2
 2.5 with sigma of 0.02
 O4-C3
 2.5 with sigma of 0.04
 O4-C12
 2.5 with sigma of 0.04
 C3-C1
 2.5 with sigma of 0.02
 O2-C1
 2.5 with sigma of 0.04
 C13-C15
 2.4 with sigma of 0.02
 O14-C15
 2.5 with sigma of 0.04
 C15-C11
 2.4 with sigma of 0.02
 C5-C3
 2.5 with sigma of 0.02
 O4-C5
 2.5 with sigma of 0.04
 C1-C5
 2.5 with sigma of 0.02
 C4-C11
 2.5 with sigma of 0.04
 C2-C4
 2.5 with sigma of 0.04
 C5-O6
 2.5 with sigma of 0.04
 O13-C14
 2.5 with sigma of 0.04
 O13-C12
 2.5 with sigma of 0.04
 O12-C11
 2.5 with sigma of 0.04
 C14-O15
 2.4 with sigma of 0.02
 O5-C4
 2.5 with sigma of 0.02
 O15-C12
 2.4 with sigma of 0.02
 C2-O5
 2.5 with sigma of 0.02
 O4-O15
 2.5 with sigma of 0.04
 C4-O5
 2.5 with sigma of 0.04
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(H2A), C3(H3A), C4(H4), C5(H5), C11(H11), C12(H12A), C13(H13A),
 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(H2), O3(H3), O6(H6), O12(H12), O13(H13), O16(H16)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8511(10) 0.6819(9) 0.6348(13) 0.202(14) Uiso 1 1 d D . . . .
H1 H 0.8457 0.7129 0.6313 0.243 Uiso 1 1 calc R . . . .
C2 C 0.8926(9) 0.6755(8) 0.6590(13) 0.202(14) Uiso 1 1 d D . . . .
H2A H 0.8906 0.6887 0.6876 0.243 Uiso 1 1 calc R . . . .
C3 C 0.9004(8) 0.6278(8) 0.6631(15) 0.202(14) Uiso 1 1 d D . . . .
H3A H 0.9066 0.6205 0.6329 0.243 Uiso 1 1 calc R . . . .
C4 C 0.8608(9) 0.6009(9) 0.6706(13) 0.202(14) Uiso 1 1 d D . . . .
H4 H 0.8533 0.6093 0.7002 0.243 Uiso 1 1 calc R . . . .
C5 C 0.8212(8) 0.6149(9) 0.6466(13) 0.202(14) Uiso 1 1 d D . . . .
H5 H 0.8256 0.6074 0.6161 0.243 Uiso 1 1 calc R . . . .
C6 C 0.7852(14) 0.5868(12) 0.6630(16) 0.202(14) Uiso 1 1 d D . . . .
H6A H 0.7628 0.5850 0.6412 0.243 Uiso 1 1 calc R . . . .
H6B H 0.7962 0.5579 0.6679 0.243 Uiso 1 1 calc R . . . .
C11 C 0.8654(10) 0.5344(8) 0.7174(11) 0.202(14) Uiso 1 1 d D . . . .
H11 H 0.8672 0.5550 0.7413 0.243 Uiso 1 1 calc R . . . .
C12 C 0.9067(9) 0.5093(10) 0.7141(16) 0.202(14) Uiso 1 1 d D . . . .
H12A H 0.9088 0.4953 0.7424 0.243 Uiso 1 1 calc R . . . .
C13 C 0.9025(9) 0.4717(13) 0.6835(16) 0.202(14) Uiso 1 1 d D . . . .
H13A H 0.8993 0.4841 0.6546 0.243 Uiso 1 1 calc R . . . .
C14 C 0.8622(10) 0.4453(10) 0.6914(14) 0.202(14) Uiso 1 1 d D . . . .
H14 H 0.8647 0.4327 0.7203 0.243 Uiso 1 1 calc R . . . .
C15 C 0.8226(8) 0.4732(11) 0.6911(13) 0.202(14) Uiso 1 1 d D . . . .
H15 H 0.8221 0.4869 0.6626 0.243 Uiso 1 1 calc R . . . .
C16 C 0.7765(10) 0.4619(17) 0.7007(15) 0.202(14) Uiso 1 1 d D . . . .
H16A H 0.7592 0.4880 0.7002 0.243 Uiso 1 1 calc R . . . .
H16B H 0.7657 0.4428 0.6784 0.243 Uiso 1 1 calc R . . . .
K1 K 0.8090(5) 0.5000 0.8090(5) 0.310(19) Uani 1 2 d S TU P . .
O2 O 0.9320(10) 0.6890(11) 0.6376(14) 0.238(11) Uiso 1 1 d D . . . .
H2 H 0.9511 0.6713 0.6424 0.357 Uiso 1 1 calc R . . . .
O3 O 0.9431(9) 0.6240(10) 0.6817(12) 0.238(11) Uiso 1 1 d D . . . .
H3 H 0.9424 0.6070 0.7020 0.357 Uiso 1 1 calc R . . . .
O4 O 0.8737(12) 0.5563(9) 0.6769(12) 0.238(11) Uiso 1 1 d D . . . .
O5 O 0.8116(8) 0.6607(9) 0.6482(11) 0.238(11) Uiso 1 1 d D . . . .
O6 O 0.7668(13) 0.6033(13) 0.7028(14) 0.238(11) Uiso 1 1 d D . . . .
H6 H 0.7861 0.6072 0.7205 0.357 Uiso 1 1 calc R . . . .
O12 O 0.9468(11) 0.5331(13) 0.7111(14) 0.238(11) Uiso 1 1 d D . . . .
H12 H 0.9657 0.5173 0.7014 0.357 Uiso 1 1 calc R . . . .
O13 O 0.9403(10) 0.4441(12) 0.6816(12) 0.238(11) Uiso 1 1 d D . . . .
H13 H 0.9386 0.4282 0.6605 0.357 Uiso 1 1 calc R . . . .
O14 O 0.8569(13) 0.4101(11) 0.6610(11) 0.238(11) Uiso 1 1 d D . . . .
O15 O 0.8268(9) 0.5083(9) 0.7218(10) 0.238(11) Uiso 1 1 d D . . . .
O16 O 0.7715(13) 0.4411(13) 0.7424(15) 0.238(11) Uiso 1 1 d D . . . .
H16 H 0.7698 0.4595 0.7613 0.357 Uiso 1 1 calc R . . . .
OA O 0.9751(12) 0.4751(12) 0.7500 0.238(11) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.501(3) . ?
C1 O5 1.450(3) . ?
C1 O14 1.54(5) 7_556 ?
C2 H2A 0.9800 . ?
C2 C3 1.500(3) . ?
C2 K1 3.50(3) 42_566 ?
C2 O2 1.450(3) . ?
C3 H3A 0.9800 . ?
C3 C4 1.500(3) . ?
C3 O3 1.449(3) . ?
C4 H4 0.9800 . ?
C4 C5 1.500(3) . ?
C4 O4 1.450(3) . ?
C5 H5 0.9800 . ?
C5 C6 1.500(3) . ?
C5 O5 1.450(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.450(3) . ?
C11 H11 0.9800 . ?
C11 C12 1.500(3) . ?
C11 K1 3.50(3) . ?
C11 O4 1.450(3) . ?
C11 O15 1.450(3) . ?
C12 H12A 0.9800 . ?
C12 C13 1.51(3) . ?
C12 O12 1.45(3) . ?
C13 H13A 0.9800 . ?
C13 C14 1.51(3) . ?
C13 O13 1.450(3) . ?
C14 H14 0.9800 . ?
C14 C15 1.500(3) . ?
C14 O14 1.450(3) . ?
C15 H15 0.9800 . ?
C15 C16 1.500(3) . ?
C15 O15 1.450(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 O16 1.450(3) . ?
K1 C2 3.50(3) 44_666 ?
K1 C2 3.50(3) 41_646 ?
K1 C11 3.50(3) 23_565 ?
K1 O2 2.68(4) 44_666 ?
K1 O2 2.68(4) 41_646 ?
K1 O3 2.74(3) 41_646 ?
K1 O3 2.74(3) 44_666 ?
K1 O15 2.77(4) 23_565 ?
K1 O15 2.77(4) . ?
K1 O16 2.99(5) 23_565 ?
K1 O16 2.99(5) . ?
O2 K1 2.68(4) 42_566 ?
O2 H2 0.8200 . ?
O3 K1 2.74(3) 42_566 ?
O3 H3 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12 0.8200 . ?
O13 H13 0.8200 . ?
O14 C1 1.54(5) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 109.4 . . ?
C2 C1 O14 107(3) . 7_556 ?
O5 C1 H1 109.4 . . ?
O5 C1 C2 121.2(18) . . ?
O5 C1 O14 100(3) . 7_556 ?
O14 C1 H1 109.4 7_556 . ?
C1 C2 H2A 110.2 . . ?
C1 C2 K1 159.3(16) . 42_566 ?
C3 C2 C1 108.1(14) . . ?
C3 C2 H2A 110.2 . . ?
C3 C2 K1 87.6(11) . 42_566 ?
K1 C2 H2A 75.2 42_566 . ?
O2 C2 C1 117(3) . . ?
O2 C2 H2A 110.2 . . ?
O2 C2 C3 100.7(16) . . ?
O2 C2 K1 44.8(18) . 42_566 ?
C2 C3 H3A 100.4 . . ?
C4 C3 C2 115.3(14) . . ?
C4 C3 H3A 100.4 . . ?
O3 C3 C2 105.2(17) . . ?
O3 C3 H3A 100.4 . . ?
O3 C3 C4 130(3) . . ?
C3 C4 H4 101.1 . . ?
C3 C4 C5 115.5(15) . . ?
C5 C4 H4 101.1 . . ?
O4 C4 C3 109(2) . . ?
O4 C4 H4 101.1 . . ?
O4 C4 C5 125(3) . . ?
C4 C5 H5 107.1 . . ?
C6 C5 C4 106(3) . . ?
C6 C5 H5 107.1 . . ?
O5 C5 C4 115.5(16) . . ?
O5 C5 H5 107.1 . . ?
O5 C5 C6 114(2) . . ?
C5 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
O6 C6 C5 112(3) . . ?
O6 C6 H6A 109.2 . . ?
O6 C6 H6B 109.2 . . ?
C12 C11 H11 109.8 . . ?
C12 C11 K1 109(2) . . ?
K1 C11 H11 67.3 . . ?
O4 C11 H11 109.8 . . ?
O4 C11 C12 91.9(15) . . ?
O4 C11 K1 159(2) . . ?
O4 C11 O15 119(3) . . ?
O15 C11 H11 109.8 . . ?
O15 C11 C12 115.0(15) . . ?
O15 C11 K1 48.8(16) . . ?
C11 C12 H12A 103.1 . . ?
C11 C12 C13 111.6(16) . . ?
C13 C12 H12A 103.1 . . ?
O12 C12 C11 118(3) . . ?
O12 C12 H12A 103.1 . . ?
O12 C12 C13 115(4) . . ?
C12 C13 H13A 106.2 . . ?
C12 C13 C14 113(2) . . ?
C14 C13 H13A 106.2 . . ?
O13 C13 C12 114(3) . . ?
O13 C13 H13A 106.2 . . ?
O13 C13 C14 111(3) . . ?
C13 C14 H14 107.5 . . ?
C15 C14 C13 111.3(19) . . ?
C15 C14 H14 107.5 . . ?
O14 C14 C13 113(3) . . ?
O14 C14 H14 107.5 . . ?
O14 C14 C15 109.6(18) . . ?
C14 C15 H15 105.5 . . ?
C14 C15 C16 130(4) . . ?
C16 C15 H15 105.5 . . ?
O15 C15 C14 110.7(16) . . ?
O15 C15 H15 105.5 . . ?
O15 C15 C16 97.4(17) . . ?
C15 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
O16 C16 C15 112(4) . . ?
O16 C16 H16A 109.1 . . ?
O16 C16 H16B 109.1 . . ?
C2 K1 C2 145.4(13) 44_666 41_646 ?
C11 K1 C2 105.0(7) 23_565 44_666 ?
C11 K1 C2 105.0(7) . 41_646 ?
C11 K1 C2 82.7(8) . 44_666 ?
C11 K1 C2 82.7(8) 23_565 41_646 ?
C11 K1 C11 154.5(14) . 23_565 ?
O2 K1 C2 130.9(13) 41_646 44_666 ?
O2 K1 C2 130.9(13) 44_666 41_646 ?
O2 K1 C2 22.4(5) 44_666 44_666 ?
O2 K1 C2 22.4(5) 41_646 41_646 ?
O2 K1 C11 87.1(8) 44_666 23_565 ?
O2 K1 C11 104.5(9) 44_666 . ?
O2 K1 C11 104.5(9) 41_646 23_565 ?
O2 K1 C11 87.1(8) 41_646 . ?
O2 K1 O2 126.1(19) 44_666 41_646 ?
O2 K1 O3 92.0(12) 44_666 41_646 ?
O2 K1 O3 92.0(12) 41_646 44_666 ?
O2 K1 O3 53.9(9) 41_646 41_646 ?
O2 K1 O3 53.9(9) 44_666 44_666 ?
O2 K1 O15 121.6(10) 44_666 . ?
O2 K1 O15 88.5(9) 44_666 23_565 ?
O2 K1 O15 88.5(9) 41_646 . ?
O2 K1 O15 121.6(10) 41_646 23_565 ?
O2 K1 O16 156.2(14) 44_666 . ?
O2 K1 O16 77.1(11) 44_666 23_565 ?
O2 K1 O16 77.1(11) 41_646 . ?
O2 K1 O16 156.2(14) 41_646 23_565 ?
O3 K1 C2 112.4(10) 44_666 41_646 ?
O3 K1 C2 41.9(6) 41_646 41_646 ?
O3 K1 C2 112.4(10) 41_646 44_666 ?
O3 K1 C2 41.9(6) 44_666 44_666 ?
O3 K1 C11 139.3(9) 44_666 23_565 ?
O3 K1 C11 139.3(9) 41_646 . ?
O3 K1 C11 60.7(10) 41_646 23_565 ?
O3 K1 C11 60.7(10) 44_666 . ?
O3 K1 O3 104.7(18) 44_666 41_646 ?
O3 K1 O15 141.1(8) 44_666 23_565 ?
O3 K1 O15 83.8(11) 41_646 23_565 ?
O3 K1 O15 83.8(11) 44_666 . ?
O3 K1 O15 141.1(8) 41_646 . ?
O3 K1 O16 139.5(12) 44_666 . ?
O3 K1 O16 99.9(11) 44_666 23_565 ?
O3 K1 O16 99.9(11) 41_646 . ?
O3 K1 O16 139.5(12) 41_646 23_565 ?
O15 K1 C2 99.5(7) 23_565 44_666 ?
O15 K1 C2 99.2(9) 23_565 41_646 ?
O15 K1 C2 99.5(7) . 41_646 ?
O15 K1 C2 99.2(9) . 44_666 ?
O15 K1 C11 132.6(13) 23_565 . ?
O15 K1 C11 132.6(13) . 23_565 ?
O15 K1 C11 23.2(4) . . ?
O15 K1 C11 23.2(4) 23_565 23_565 ?
O15 K1 O15 113.3(15) . 23_565 ?
O15 K1 O16 72.6(12) . 23_565 ?
O15 K1 O16 57.4(12) 23_565 23_565 ?
O15 K1 O16 57.4(12) . . ?
O15 K1 O16 72.6(12) 23_565 . ?
O16 K1 C2 145.9(12) . 44_666 ?
O16 K1 C2 68.0(9) . 41_646 ?
O16 K1 C2 145.9(12) 23_565 41_646 ?
O16 K1 C2 68.0(9) 23_565 44_666 ?
O16 K1 C11 81.0(11) . 23_565 ?
O16 K1 C11 79.6(11) 23_565 23_565 ?
O16 K1 C11 81.0(11) 23_565 . ?
O16 K1 C11 79.6(11) . . ?
O16 K1 O16 80.6(16) 23_565 . ?
C2 O2 K1 113(2) . 42_566 ?
C2 O2 H2 109.5 . . ?
K1 O2 H2 48.2 42_566 . ?
C3 O3 K1 124.6(17) . 42_566 ?
C3 O3 H3 109.5 . . ?
K1 O3 H3 114.9 42_566 . ?
C11 O4 C4 121(3) . . ?
C1 O5 C5 105.1(3) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12 109.5 . . ?
C13 O13 H13 109.5 . . ?
C14 O14 C1 115(3) . 5_565 ?
C11 O15 K1 108(2) . . ?
C15 O15 C11 115.4(17) . . ?
C15 O15 K1 124(2) . . ?
C16 O16 K1 108(3) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 26.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -38(4) . . . . ?
C1 C2 C3 O3 173(3) . . . . ?
C1 C2 O2 K1 168(2) . . . 42_566 ?
C2 C1 O5 C5 -59(3) . . . . ?
C2 C3 C4 C5 38(5) . . . . ?
C2 C3 C4 O4 -176(3) . . . . ?
C2 C3 O3 K1 -10(4) . . . 42_566 ?
C3 C2 O2 K1 -75(2) . . . 42_566 ?
C3 C4 C5 C6 -174(3) . . . . ?
C3 C4 C5 O5 -47(4) . . . . ?
C3 C4 O4 C11 117(4) . . . . ?
C4 C3 O3 K1 -154(3) . . . 42_566 ?
C4 C5 C6 O6 84(4) . . . . ?
C4 C5 O5 C1 53(3) . . . . ?
C5 C4 O4 C11 -100(4) . . . . ?
C6 C5 O5 C1 175(3) . . . . ?
C11 C12 C13 C14 -48(4) . . . . ?
C11 C12 C13 O13 -175(3) . . . . ?
C12 C11 O4 C4 -145(3) . . . . ?
C12 C11 O15 C15 -49(4) . . . . ?
C12 C11 O15 K1 94(3) . . . . ?
C12 C13 C14 C15 54(4) . . . . ?
C12 C13 C14 O14 178(3) . . . . ?
C13 C14 C15 C16 -175(3) . . . . ?
C13 C14 C15 O15 -55(4) . . . . ?
C13 C14 O14 C1 126(4) . . . 5_565 ?
C14 C15 C16 O16 54(4) . . . . ?
C14 C15 O15 C11 53(4) . . . . ?
C14 C15 O15 K1 -83(3) . . . . ?
C15 C14 O14 C1 -110(4) . . . 5_565 ?
C15 C16 O16 K1 56(4) . . . . ?
C16 C15 O15 C11 -169(3) . . . . ?
C16 C15 O15 K1 55(4) . . . . ?
K1 C2 C3 C4 156(3) 42_566 . . . ?
K1 C2 C3 O3 7(3) 42_566 . . . ?
K1 C11 C12 C13 97(3) . . . . ?
K1 C11 C12 O12 -125(4) . . . . ?
K1 C11 O4 C4 45(8) . . . . ?
K1 C11 O15 C15 -143(3) . . . . ?
O2 C2 C3 C4 -161(3) . . . . ?
O2 C2 C3 O3 50(4) . . . . ?
O3 C3 C4 C5 178(4) . . . . ?
O3 C3 C4 O4 -36(6) . . . . ?
O4 C4 C5 C6 47(4) . . . . ?
O4 C4 C5 O5 173(3) . . . . ?
O4 C11 C12 C13 -79(3) . . . . ?
O4 C11 C12 O12 58(5) . . . . ?
O4 C11 O15 C15 59(3) . . . . ?
O4 C11 O15 K1 -159(2) . . . . ?
O5 C1 C2 C3 52(4) . . . . ?
O5 C1 C2 K1 -170(5) . . . 42_566 ?
O5 C1 C2 O2 165(3) . . . . ?
O5 C5 C6 O6 -44(5) . . . . ?
O12 C12 C13 C14 174(4) . . . . ?
O12 C12 C13 O13 46(5) . . . . ?
O13 C13 C14 C15 -177(3) . . . . ?
O13 C13 C14 O14 -53(4) . . . . ?
O14 C1 C2 C3 -61(3) 7_556 . . . ?
O14 C1 C2 K1 77(6) 7_556 . . 42_566 ?
O14 C1 C2 O2 52(3) 7_556 . . . ?
O14 C1 O5 C5 58(3) 7_556 . . . ?
O14 C14 C15 C16 59(5) . . . . ?
O14 C14 C15 O15 179(3) . . . . ?
O15 C11 C12 C13 45(4) . . . . ?
O15 C11 C12 O12 -178(4) . . . . ?
O15 C11 O4 C4 95(4) . . . . ?
O15 C15 C16 O16 -72(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.065 -0.190 -0.048 14122.9 808.2 ?


_olex2_exptl_crystal_mounting_method 'Diamond-anvil cell'
_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 1.000
_oxdiff_exptl_absorpt_empirical_full_min 1.000
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CDMOF_a_295K
_database_code_depnum_ccdc_archive 'CCDC 1529157'
_audit_update_record             
;
2017-01-23 deposited with the CCDC.
2017-03-17 downloaded from the CCDC.
;
_audit_creation_date             2017-01-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
# start Validation Reply Form
_vrf_THETM01_CDMOF_a_295K        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: 'Theta angle was limited due to the poorly diffracting sample crystal'
;
_vrf_REFNR01_CDMOF_a_295K        
;
PROBLEM: Ratio of reflections to parameters is < 8 for a
RESPONSE: 'Complexity of the molecular and crystal structures; 
poorly diffracting sample'
;
_vrf_PLAT029_CDMOF_a_295K        
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.881 Note  
RESPONSE: 'Theta angle was limited due to the poorly diffracting sample crystal'
;
_vrf_PLAT201_CDMOF_a_295K        
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......         22 Report
RESPONSE: 'Low number of collected data hindered anisotropic refinement'
;
_vrf_PLAT090_CDMOF_a_295K        
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       4.76 Note  
RESPONSE: 'Data limited due to the poorly diffracting sample crystal'
;
_vrf_PLAT306_CDMOF_a_295K        
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         Oa Check 
RESPONSE: 'Isolated oxygent atoms are part of hydroxide ions present 
in the structure, assigment of hydrogen atoms was higly imprecise and 
therefore those hydrogen atoms were omitted'
;
_vrf_PLAT340_CDMOF_a_295K        
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.02 Ang.  
RESPONSE: 'Low data number enforced fixing bonds lengths 
which in turn resulted in lowering bond precision'
;
_vrf_PLAT420_CDMOF_a_295K        
;
PROBLEM: D-H Without Acceptor       O16    --  H16    ...     Please Check 
RESPONSE: 'Posible H-acceptor solvent (water or methanol) 
molecules masked for the refinement'
;
_vrf_PLAT911_CDMOF_a_295K        
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.333         52 Report
RESPONSE: 'Missing reflections may be due to the chosen strategy of 
the measurement; this was short measurement, aimed primarily at 
checking the unit-cell paremeters only'
;
# end Validation Reply Form

# CHEMICAL DATA 

_chemical_name_common            'γ-cyclodextrin-metal-organic framework'
_chemical_name_systematic        
'catena-((μ8-γ-Cyclodextrin)-di-potassium dihydroxide)'
_chemical_formula_moiety         'C48 H80 O40, 2(KOH)'
_chemical_formula_sum            'C48 H82 K2 O42'
_chemical_formula_weight         1409.34
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H82 K2 O40'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# CRYSTAL DATA

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_symmetry_space_group_name_H-M_alt 'I 4 3 2'
_cell_length_a                   31.2093(7)
_cell_length_b                   31.2093(7)
_cell_length_c                   31.2093(7)
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_volume                     30399(1)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    3924
_cell_measurement_temperature    295.01(10)
_cell_measurement_theta_max      13.0770
_cell_measurement_theta_min      3.1630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65227
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.881
_diffrn_reflns_Laue_measured_fraction_max 0.881
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19855
_diffrn_reflns_point_group_measured_fraction_full 0.905
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        13.690
_diffrn_reflns_theta_max         13.690
_diffrn_reflns_theta_min         2.769
_diffrn_ambient_environment      'ispropanol:water mother liquor'
_diffrn_ambient_temperature      295.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.881
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00  54.00   1.00   15.00    --  -18.72   0.00-150.00  122
  2  ω    -73.00  20.00   1.00   15.00    --  -18.72 -19.00  60.00   93
  3  ω    -40.00   8.00   1.00   15.00    --  -18.72  57.00  60.00   48
  4  ω    -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       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0147819000
_diffrn_orient_matrix_UB_12      -0.0169933000
_diffrn_orient_matrix_UB_13      -0.0030520000
_diffrn_orient_matrix_UB_21      -0.0171295000
_diffrn_orient_matrix_UB_22      0.0149371000
_diffrn_orient_matrix_UB_23      -0.0001549000
_diffrn_orient_matrix_UB_31      0.0021342000
_diffrn_orient_matrix_UB_32      0.0022125000
_diffrn_orient_matrix_UB_33      -0.0225166000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.637
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.946
_reflns_number_gt                663
_reflns_number_total             725
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'

# REFINEMENT DATA

_refine_diff_density_max         0.141
_refine_diff_density_min         -0.118
_refine_diff_density_rms         0.027
_refine_ls_abs_structure_details 
;
 Flack x determined using 243 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         725
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0485
_refine_ls_restrained_S_all      1.131
_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/[σ²(Fo²)+(0.0863P)²+47.2516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1326
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

The SQUEEZE/Olex2 program has been used to model some unspecified disorder.

Two hydrogen atoms from two hydroxide ions were omitted in the refinement, 
due to inability to precisely assigning their possitions. However those two 
hydrogen atoms were included in the chemical formula moiety and sum and 
therefore influenced chemical formula weight, crystal density and crystal F(000).              
;
_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
 C11-O4
 1.45 with sigma of 0.02
 O4-C4
 1.45 with sigma of 0.02
 C1-O5
 1.45 with sigma of 0.02
 C1-C2
 1.5 with sigma of 0.02
 C11-C12
 1.5 with sigma of 0.02
 O13-C13
 1.45 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.01
 C11-C4
 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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8488(5) 0.6802(6) 0.6274(5) 0.082(6) Uiso 1 1 d D . . . .
H1 H 0.8425 0.7109 0.6259 0.098 Uiso 1 1 calc R . . . .
C2 C 0.8861(5) 0.6770(5) 0.6548(5) 0.096(6) Uiso 1 1 d D . . . .
H2 H 0.8805 0.6914 0.6822 0.115 Uiso 1 1 calc R . . . .
C3 C 0.8963(6) 0.6296(5) 0.6627(5) 0.102(7) Uiso 1 1 d D . . . .
H3 H 0.9032 0.6190 0.6340 0.123 Uiso 1 1 calc R . . . .
C4 C 0.8580(5) 0.6037(5) 0.6751(5) 0.072(5) Uiso 1 1 d D . . . .
H4 H 0.8522 0.6128 0.7046 0.086 Uiso 1 1 calc R . . . .
C5 C 0.8185(6) 0.6162(6) 0.6515(6) 0.121(7) Uiso 1 1 d D . . . .
H5 H 0.8240 0.6050 0.6227 0.146 Uiso 1 1 calc R . . . .
C6 C 0.7735(5) 0.5977(6) 0.6618(6) 0.119(7) Uiso 1 1 d D . . . .
H6A H 0.7522 0.6091 0.6423 0.143 Uiso 1 1 calc R . . . .
H6B H 0.7735 0.5667 0.6599 0.143 Uiso 1 1 calc R . . . .
C11 C 0.8577(5) 0.5365(6) 0.7189(5) 0.103(6) Uiso 1 1 d D . . . .
H11 H 0.8571 0.5583 0.7415 0.124 Uiso 1 1 calc R . . . .
C12 C 0.8990(5) 0.5145(5) 0.7221(5) 0.087(6) Uiso 1 1 d D . . . .
H12 H 0.9001 0.5022 0.7510 0.104 Uiso 1 1 calc R . . . .
C13 C 0.8989(5) 0.4751(4) 0.6901(5) 0.074(5) Uiso 1 1 d D . . . .
H13 H 0.8989 0.4847 0.6602 0.089 Uiso 1 1 calc R . . . .
C14 C 0.8593(5) 0.4522(5) 0.7007(5) 0.083(5) Uiso 1 1 d . . . . .
H14 H 0.8607 0.4407 0.7298 0.100 Uiso 1 1 calc R . . . .
C15 C 0.8201(5) 0.4774(5) 0.6948(5) 0.082(6) Uiso 1 1 d . . . . .
H15 H 0.8187 0.4875 0.6651 0.098 Uiso 1 1 calc R . . . .
C16 C 0.7789(5) 0.4538(5) 0.7055(5) 0.104(6) Uiso 1 1 d . . . . .
H16A H 0.7548 0.4727 0.7006 0.125 Uiso 1 1 calc R . . . .
H16B H 0.7759 0.4294 0.6866 0.125 Uiso 1 1 calc R . . . .
K1 K 0.81023(12) 0.5000 0.81023(12) 0.111(2) Uani 1 2 d S T P . .
O2 O 0.9264(4) 0.6942(4) 0.6354(4) 0.145(3) Uiso 1 1 d . . . . .
H2A H 0.9439 0.6747 0.6328 0.217 Uiso 1 1 calc R . . . .
O3 O 0.9350(4) 0.6212(4) 0.6867(4) 0.145(3) Uiso 1 1 d . . . . .
H3A H 0.9347 0.5964 0.6954 0.217 Uiso 1 1 calc R . . . .
O4 O 0.8601(3) 0.5592(4) 0.6779(3) 0.090(4) Uiso 1 1 d D . . . .
O5 O 0.8130(4) 0.6622(4) 0.6438(4) 0.145(3) Uiso 1 1 d D . . . .
O6 O 0.7656(4) 0.6112(4) 0.7038(4) 0.145(3) Uiso 1 1 d . . . . .
H6 H 0.7746 0.5931 0.7206 0.217 Uiso 1 1 calc R . . . .
O12 O 0.9393(4) 0.5373(4) 0.7161(4) 0.138(5) Uiso 1 1 d . . . . .
H12A H 0.9585 0.5200 0.7115 0.207 Uiso 1 1 calc R . . . .
O13 O 0.9382(3) 0.4499(3) 0.7004(3) 0.107(4) Uiso 1 1 d D . . . .
H13A H 0.9313 0.4260 0.7089 0.160 Uiso 1 1 calc R . . . .
O14 O 0.8563(3) 0.4158(4) 0.6678(3) 0.094(4) Uiso 1 1 d . . . . .
O15 O 0.8219(3) 0.5135(3) 0.7228(3) 0.086(4) Uiso 1 1 d . . . . .
O16 O 0.7782(3) 0.4402(4) 0.7462(4) 0.130(5) Uiso 1 1 d . . . . .
H16 H 0.7820 0.4143 0.7468 0.195 Uiso 1 1 calc R . . . .
OA O 1.0000 0.5000 0.6643(6) 0.178(7) Uiso 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9800 . ?
C1 C2 1.448(14) . ?
C1 O5 1.353(13) . ?
C1 O14 1.420(15) 7_556 ?
C2 H2 0.9800 . ?
C2 C3 1.532(18) . ?
C2 O2 1.496(16) . ?
C3 H3 0.9800 . ?
C3 C4 1.494(15) . ?
C3 O3 1.447(16) . ?
C4 H4 0.9800 . ?
C4 C5 1.486(18) . ?
C4 O4 1.396(13) . ?
C5 H5 0.9800 . ?
C5 C6 1.551(17) . ?
C5 O5 1.468(18) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 O6 1.398(16) . ?
C11 H11 0.9800 . ?
C11 C12 1.463(11) . ?
C11 K1 3.407(16) . ?
C11 O4 1.466(14) . ?
C11 O15 1.332(15) . ?
C12 H12 0.9800 . ?
C12 C13 1.584(15) . ?
C12 O12 1.458(15) . ?
C13 H13 0.9800 . ?
C13 C14 1.464(17) . ?
C13 O13 1.494(13) . ?
C14 H14 0.9800 . ?
C14 C15 1.464(17) . ?
C14 O14 1.534(16) . ?
C15 H15 0.9800 . ?
C15 C16 1.518(17) . ?
C15 O15 1.426(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 O16 1.338(15) . ?
K1 C11 3.407(17) 23_565 ?
K1 O2 2.859(12) 44_666 ?
K1 O2 2.859(12) 41_646 ?
K1 O3 2.951(12) 41_646 ?
K1 O3 2.951(12) 44_666 ?
K1 O15 2.785(10) . ?
K1 O15 2.785(11) 23_565 ?
K1 O16 2.911(11) . ?
K1 O16 2.911(11) 23_565 ?
O2 K1 2.858(12) 42_566 ?
O2 H2A 0.8200 . ?
O3 K1 2.951(12) 42_566 ?
O3 H3A 0.8200 . ?
O6 H6 0.8200 . ?
O12 H12A 0.8200 . ?
O13 H13A 0.8200 . ?
O14 C1 1.420(15) 5_565 ?
O16 H16 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1 104.9 . . ?
O5 C1 H1 104.9 . . ?
O5 C1 C2 114.3(15) . . ?
O5 C1 O14 112.5(14) . 7_556 ?
O14 C1 H1 104.9 7_556 . ?
O14 C1 C2 114.2(14) 7_556 . ?
C1 C2 H2 109.9 . . ?
C1 C2 C3 109.1(15) . . ?
C1 C2 O2 114.3(14) . . ?
C3 C2 H2 109.9 . . ?
O2 C2 H2 109.9 . . ?
O2 C2 C3 103.7(13) . . ?
C2 C3 H3 103.2 . . ?
C4 C3 C2 113.5(15) . . ?
C4 C3 H3 103.2 . . ?
O3 C3 C2 115.6(14) . . ?
O3 C3 H3 103.2 . . ?
O3 C3 C4 115.8(13) . . ?
C3 C4 H4 103.7 . . ?
C5 C4 C3 113.2(14) . . ?
C5 C4 H4 103.7 . . ?
O4 C4 C3 121.2(14) . . ?
O4 C4 H4 103.7 . . ?
O4 C4 C5 109.3(14) . . ?
C4 C5 H5 102.5 . . ?
C4 C5 C6 123.5(15) . . ?
C6 C5 H5 102.5 . . ?
O5 C5 C4 115.7(15) . . ?
O5 C5 H5 102.5 . . ?
O5 C5 C6 106.9(16) . . ?
C5 C6 H6A 111.0 . . ?
C5 C6 H6B 111.0 . . ?
H6A C6 H6B 109.0 . . ?
O6 C6 C5 103.9(14) . . ?
O6 C6 H6A 111.0 . . ?
O6 C6 H6B 111.0 . . ?
C12 C11 H11 107.1 . . ?
C12 C11 K1 99.8(10) . . ?
C12 C11 O4 103.8(13) . . ?
K1 C11 H11 67.8 . . ?
O4 C11 H11 107.1 . . ?
O4 C11 K1 156.2(9) . . ?
O15 C11 H11 107.1 . . ?
O15 C11 C12 118.7(15) . . ?
O15 C11 K1 51.7(8) . . ?
O15 C11 O4 112.6(13) . . ?
C11 C12 H12 106.1 . . ?
C11 C12 C13 108.6(14) . . ?
C11 C12 O12 121.5(14) . . ?
C13 C12 H12 106.1 . . ?
O12 C12 H12 106.1 . . ?
O12 C12 C13 107.5(12) . . ?
C12 C13 H13 111.4 . . ?
C14 C13 C12 103.8(13) . . ?
C14 C13 H13 111.4 . . ?
C14 C13 O13 112.8(12) . . ?
O13 C13 C12 105.6(11) . . ?
O13 C13 H13 111.4 . . ?
C13 C14 H14 110.5 . . ?
C13 C14 O14 105.1(12) . . ?
C15 C14 C13 114.5(14) . . ?
C15 C14 H14 110.5 . . ?
C15 C14 O14 105.3(13) . . ?
O14 C14 H14 110.5 . . ?
C14 C15 H15 109.1 . . ?
C14 C15 C16 114.8(14) . . ?
C16 C15 H15 109.1 . . ?
O15 C15 C14 108.3(14) . . ?
O15 C15 H15 109.1 . . ?
O15 C15 C16 106.4(14) . . ?
C15 C16 H16A 109.2 . . ?
C15 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
O16 C16 C15 112.2(14) . . ?
O16 C16 H16A 109.2 . . ?
O16 C16 H16B 109.2 . . ?
C11 K1 C11 147.0(6) . 23_565 ?
O2 K1 C11 104.5(4) 41_646 23_565 ?
O2 K1 C11 88.3(4) 44_666 23_565 ?
O2 K1 C11 88.3(4) 41_646 . ?
O2 K1 C11 104.5(4) 44_666 . ?
O2 K1 O2 134.6(6) 44_666 41_646 ?
O2 K1 O3 57.6(3) 41_646 41_646 ?
O2 K1 O3 57.6(3) 44_666 44_666 ?
O2 K1 O3 97.0(4) 44_666 41_646 ?
O2 K1 O3 97.0(4) 41_646 44_666 ?
O2 K1 O16 154.9(4) 41_646 23_565 ?
O2 K1 O16 69.9(3) 44_666 23_565 ?
O2 K1 O16 154.9(4) 44_666 . ?
O2 K1 O16 69.9(3) 41_646 . ?
O3 K1 C11 145.3(4) 41_646 . ?
O3 K1 C11 58.8(4) 41_646 23_565 ?
O3 K1 C11 145.3(4) 44_666 23_565 ?
O3 K1 C11 58.8(4) 44_666 . ?
O3 K1 O3 115.1(5) 44_666 41_646 ?
O15 K1 C11 22.0(3) . . ?
O15 K1 C11 125.9(4) . 23_565 ?
O15 K1 C11 125.9(4) 23_565 . ?
O15 K1 C11 22.0(3) 23_565 23_565 ?
O15 K1 O2 117.8(3) . 44_666 ?
O15 K1 O2 117.8(3) 23_565 41_646 ?
O15 K1 O2 89.8(3) . 41_646 ?
O15 K1 O2 89.8(3) 23_565 44_666 ?
O15 K1 O3 144.1(4) . 41_646 ?
O15 K1 O3 80.4(3) 23_565 41_646 ?
O15 K1 O3 80.4(3) . 44_666 ?
O15 K1 O3 144.1(4) 23_565 44_666 ?
O15 K1 O15 106.3(5) . 23_565 ?
O15 K1 O16 69.9(3) 23_565 . ?
O15 K1 O16 57.9(3) 23_565 23_565 ?
O15 K1 O16 69.9(3) . 23_565 ?
O15 K1 O16 57.9(3) . . ?
O16 K1 C11 78.3(3) . 23_565 ?
O16 K1 C11 77.8(4) 23_565 23_565 ?
O16 K1 C11 77.8(4) . . ?
O16 K1 C11 78.3(3) 23_565 . ?
O16 K1 O3 135.4(3) . 44_666 ?
O16 K1 O3 94.0(3) 23_565 44_666 ?
O16 K1 O3 135.4(3) 23_565 41_646 ?
O16 K1 O3 94.0(3) . 41_646 ?
O16 K1 O16 86.5(5) 23_565 . ?
C2 O2 K1 114.7(8) . 42_566 ?
C2 O2 H2A 109.5 . . ?
K1 O2 H2A 59.3 42_566 . ?
C3 O3 K1 117.3(9) . 42_566 ?
C3 O3 H3A 109.5 . . ?
K1 O3 H3A 133.1 42_566 . ?
C4 O4 C11 122.3(12) . . ?
C1 O5 C5 111.8(14) . . ?
C6 O6 H6 109.5 . . ?
C12 O12 H12A 109.5 . . ?
C13 O13 H13A 109.5 . . ?
C1 O14 C14 122.1(12) 5_565 . ?
C11 O15 C15 113.8(14) . . ?
C11 O15 K1 106.3(10) . . ?
C15 O15 K1 118.4(8) . . ?
C16 O16 K1 116.3(10) . . ?
C16 O16 H16 109.5 . . ?
K1 O16 H16 124.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -47.8(19) . . . . ?
C1 C2 C3 O3 174.9(14) . . . . ?
C1 C2 O2 K1 178.8(11) . . . 42_566 ?
C2 C1 O5 C5 -61(2) . . . . ?
C2 C3 C4 C5 39(2) . . . . ?
C2 C3 C4 O4 171.4(14) . . . . ?
C2 C3 O3 K1 -20.4(18) . . . 42_566 ?
C3 C2 O2 K1 -62.6(13) . . . 42_566 ?
C3 C4 C5 C6 -173.2(16) . . . . ?
C3 C4 C5 O5 -38(2) . . . . ?
C3 C4 O4 C11 110.5(17) . . . . ?
C4 C3 O3 K1 -156.6(10) . . . 42_566 ?
C4 C5 C6 O6 63(2) . . . . ?
C4 C5 O5 C1 49(2) . . . . ?
C5 C4 O4 C11 -115.0(15) . . . . ?
C6 C5 O5 C1 -169.3(13) . . . . ?
C11 C12 C13 C14 -51.3(16) . . . . ?
C11 C12 C13 O13 -170.2(12) . . . . ?
C12 C11 O4 C4 -118.0(14) . . . . ?
C12 C11 O15 C15 -52.7(19) . . . . ?
C12 C11 O15 K1 79.4(16) . . . . ?
C12 C13 C14 C15 60.6(17) . . . . ?
C12 C13 C14 O14 175.7(11) . . . . ?
C13 C14 C15 C16 179.7(14) . . . . ?
C13 C14 C15 O15 -61.6(18) . . . . ?
C13 C14 O14 C1 129.8(14) . . . 5_565 ?
C14 C15 C16 O16 59(2) . . . . ?
C14 C15 O15 C11 52.8(16) . . . . ?
C14 C15 O15 K1 -73.1(14) . . . . ?
C15 C14 O14 C1 -108.9(15) . . . 5_565 ?
C15 C16 O16 K1 42.0(17) . . . . ?
C16 C15 O15 C11 176.6(12) . . . . ?
C16 C15 O15 K1 50.7(14) . . . . ?
K1 C11 C12 C13 103.2(10) . . . . ?
K1 C11 C12 O12 -131.4(13) . . . . ?
K1 C11 O4 C4 69(3) . . . . ?
K1 C11 O15 C15 -132.1(12) . . . . ?
O2 C2 C3 C4 -169.9(13) . . . . ?
O2 C2 C3 O3 52.8(17) . . . . ?
O3 C3 C4 C5 175.7(15) . . . . ?
O3 C3 C4 O4 -51(2) . . . . ?
O4 C4 C5 C6 48(2) . . . . ?
O4 C4 C5 O5 -176.6(13) . . . . ?
O4 C11 C12 C13 -74.1(16) . . . . ?
O4 C11 C12 O12 51(2) . . . . ?
O4 C11 O15 C15 68.8(16) . . . . ?
O4 C11 O15 K1 -159.2(10) . . . . ?
O5 C1 C2 C3 60.5(19) . . . . ?
O5 C1 C2 O2 176.0(14) . . . . ?
O5 C5 C6 O6 -75.6(16) . . . . ?
O12 C12 C13 C14 175.5(12) . . . . ?
O12 C12 C13 O13 56.6(14) . . . . ?
O13 C13 C14 C15 174.4(13) . . . . ?
O13 C13 C14 O14 -70.4(15) . . . . ?
O14 C1 C2 C3 -71.1(19) 7_556 . . . ?
O14 C1 C2 O2 44(2) 7_556 . . . ?
O14 C1 O5 C5 71.5(17) 7_556 . . . ?
O14 C14 C15 C16 64.7(18) . . . . ?
O14 C14 C15 O15 -176.6(11) . . . . ?
O15 C11 C12 C13 51.7(19) . . . . ?
O15 C11 C12 O12 177.1(14) . . . . ?
O15 C11 O4 C4 112.4(16) . . . . ?
O15 C15 C16 O16 -60.5(17) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.018 -0.710 -0.791 14407.2 1731.0 ?


_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 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.832

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