# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H30 Al2 O6'
_chemical_formula_weight         420.40

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.3154(12)
_cell_length_b                   9.5003(8)
_cell_length_c                   16.2703(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2367.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    70
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      19.85

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             896
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_T_max  1.033


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36478
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         26.60
_reflns_number_total             2474
_reflns_number_gt                1450
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


_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 > 2σ(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0781P)²+0.4812P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2474
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1636
_refine_ls_wR_factor_gt          0.1421
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C2 C 0.6358(2) 0.0708(4) 0.6150(2) 0.0649(9) Uani 1 1 d . . .
H2A H 0.6788 0.1470 0.6127 0.097 Uiso 1 1 calc R . .
H2B H 0.6619 -0.0160 0.5938 0.097 Uiso 1 1 calc R . .
H2C H 0.6173 0.0564 0.6721 0.097 Uiso 1 1 calc R . .
Al1 Al 0.53492(5) 0.12062(8) 0.54840(5) 0.0431(3) Uani 1 1 d . . .
O1 O 0.54614(12) 0.03009(19) 0.44551(10) 0.0454(5) Uani 1 1 d . . .
O2 O 0.54288(15) -0.1225(2) 0.31014(13) 0.0644(6) Uani 1 1 d . . .
O3 O 0.64878(15) 0.2477(2) 0.46193(14) 0.0714(7) Uani 1 1 d . . .
C1 C 0.4703(2) 0.2969(3) 0.5363(2) 0.0651(9) Uani 1 1 d . . .
H1A H 0.5115 0.3757 0.5331 0.098 Uiso 1 1 calc R . .
H1B H 0.4317 0.3099 0.5837 0.098 Uiso 1 1 calc R . .
H1C H 0.4353 0.2936 0.4859 0.098 Uiso 1 1 calc R . .
C11 C 0.60192(16) 0.0628(3) 0.38267(15) 0.0395(6) Uani 1 1 d . . .
C13 C 0.60185(17) -0.0155(3) 0.31065(16) 0.0436(6) Uani 1 1 d . . .
C5 C 0.6585(2) 0.0174(3) 0.24705(19) 0.0588(8) Uani 1 1 d . . .
H5 H 0.6589 -0.0366 0.1979 0.071 Uiso 1 1 calc R . .
C6 C 0.7141(2) 0.1301(4) 0.2566(2) 0.0713(10) Uani 1 1 d . . .
H6 H 0.7533 0.1530 0.2134 0.086 Uiso 1 1 calc R . .
C7 C 0.7145(2) 0.2105(3) 0.3271(2) 0.0645(9) Uani 1 1 d . . .
H7 H 0.7537 0.2874 0.3326 0.077 Uiso 1 1 calc R . .
C12 C 0.65700(18) 0.1773(3) 0.38970(18) 0.0480(7) Uani 1 1 d . . .
C9 C 0.6993(3) 0.3709(4) 0.4763(3) 0.0964(14) Uani 1 1 d . . .
H9A H 0.6858 0.4084 0.5310 0.145 Uiso 1 1 calc R . .
H9B H 0.6854 0.4418 0.4345 0.145 Uiso 1 1 calc R . .
H9C H 0.7615 0.3474 0.4733 0.145 Uiso 1 1 calc R . .
C10 C 0.5281(3) -0.1982(5) 0.2362(2) 0.0934(13) Uani 1 1 d . . .
H10A H 0.4837 -0.2707 0.2457 0.140 Uiso 1 1 calc R . .
H10B H 0.5826 -0.2428 0.2184 0.140 Uiso 1 1 calc R . .
H10C H 0.5077 -0.1333 0.1935 0.140 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C2 Al1 1.945(3) . ?
Al1 O1 1.8976(18) 5_656 ?
Al1 O1 1.8900(19) . ?
Al1 C1 1.956(3) . ?
Al1 Al1 2.9796(15) 5_656 ?
O1 C11 1.368(3) . ?
O1 Al1 1.8976(18) 5_656 ?
O2 C13 1.359(3) . ?
O2 C10 1.419(4) . ?
O3 C12 1.358(3) . ?
O3 C9 1.423(4) . ?
C11 C13 1.388(4) . ?
C11 C12 1.382(4) . ?
C13 C5 1.386(4) . ?
C5 C6 1.377(5) . ?
C6 C7 1.378(5) . ?
C7 C12 1.383(4) . ?

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
O1 Al1 O1 76.25(9) 5_656 . ?
O1 Al1 C2 107.87(13) 5_656 . ?
O1 Al1 C2 108.10(12) . . ?
O1 Al1 C1 108.70(12) 5_656 . ?
O1 Al1 C1 110.26(13) . . ?
C2 Al1 C1 131.79(14) . . ?
O1 Al1 Al1 38.03(6) 5_656 5_656 ?
O1 Al1 Al1 38.22(5) . 5_656 ?
C2 Al1 Al1 113.11(11) . 5_656 ?
C1 Al1 Al1 115.07(11) . 5_656 ?
C11 O1 Al1 128.23(16) . 5_656 ?
C11 O1 Al1 127.98(16) . . ?
Al1 O1 Al1 103.75(9) 5_656 . ?
C13 O2 C10 119.3(3) . . ?
C12 O3 C9 119.8(3) . . ?
O1 C11 C13 120.6(2) . . ?
O1 C11 C12 119.9(2) . . ?
C13 C11 C12 119.5(2) . . ?
C11 C13 C5 120.6(3) . . ?
C11 C13 O2 114.0(2) . . ?
C5 C13 O2 125.4(3) . . ?
C6 C5 C13 118.6(3) . . ?
C5 C6 C7 121.9(3) . . ?
C6 C7 C12 118.9(3) . . ?
O3 C12 C7 125.8(3) . . ?
O3 C12 C11 113.7(2) . . ?
C7 C12 C11 120.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.60
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.048
_database_code_depnum_ccdc_archive 'CCDC 993198'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H48 Al2 Na2 O12'
_chemical_formula_weight         772.68

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_Int_Tables_number      18

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   13.7778(16)
_cell_length_b                   14.062(3)
_cell_length_c                   10.594(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2052.4(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    49
_cell_measurement_theta_min      3.25
_cell_measurement_theta_max      27.52
_cell_measurement_wavelength     0.71073

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_T_max  0.965

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35554
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         27.51
_reflns_number_total             4697
_reflns_number_gt                3338
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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 > 2σ(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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0992P)²+0.1149P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_number_reflns         4697
_refine_ls_number_parameters     236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1577
_refine_ls_wR_factor_gt          0.1392
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.95590(7) 0.82889(6) 0.70716(8) 0.0365(2) Uani 1 1 d . . .
Na1 Na 0.87195(10) 1.02743(10) 0.58860(14) 0.0561(4) Uani 1 1 d . . .
O1 O 0.85346(16) 0.90634(14) 0.7290(2) 0.0425(5) Uani 1 1 d . . .
O2 O 0.98571(18) 0.89354(14) 0.56195(17) 0.0411(5) Uani 1 1 d . . .
O3 O 0.72175(19) 1.03774(16) 0.6845(2) 0.0555(6) Uani 1 1 d . . .
O4 O 0.84215(18) 0.78641(16) 0.9230(2) 0.0508(6) Uani 1 1 d . . .
O5 O 0.86187(17) 0.95631(15) 0.3876(2) 0.0497(6) Uani 1 1 d . . .
O6 O 1.12859(18) 0.7751(2) 0.5088(2) 0.0588(7) Uani 1 1 d . . .
C1 C 0.9256(3) 0.6950(2) 0.6696(4) 0.0610(10) Uani 1 1 d . . .
H1A H 0.9862 0.6592 0.6594 0.092 Uiso 1 1 calc R . .
H1B H 0.8878 0.6913 0.5915 0.092 Uiso 1 1 calc R . .
H1C H 0.8879 0.6678 0.7393 0.092 Uiso 1 1 calc R . .
C2 C 1.0613(3) 0.8570(3) 0.8262(3) 0.0548(9) Uani 1 1 d . . .
H2A H 1.1154 0.8132 0.8113 0.082 Uiso 1 1 calc R . .
H2B H 1.0377 0.8493 0.9128 0.082 Uiso 1 1 calc R . .
H2C H 1.0834 0.9226 0.8138 0.082 Uiso 1 1 calc R . .
C11 C 0.7808(2) 0.9138(2) 0.8087(3) 0.0358(6) Uani 1 1 d . . .
C12 C 0.7079(2) 0.9821(2) 0.7893(3) 0.0438(7) Uani 1 1 d . . .
C13 C 0.6288(2) 0.9902(3) 0.8695(4) 0.0557(9) Uani 1 1 d . . .
H13 H 0.5804 1.0370 0.8547 0.067 Uiso 1 1 calc R . .
C14 C 0.6216(3) 0.9291(3) 0.9710(4) 0.0628(11) Uani 1 1 d . . .
H14 H 0.5683 0.9352 1.0272 0.075 Uiso 1 1 calc R . .
C15 C 0.6898(2) 0.8599(3) 0.9924(3) 0.0503(8) Uani 1 1 d . . .
H15 H 0.6830 0.8177 1.0619 0.060 Uiso 1 1 calc R . .
C16 C 0.7694(2) 0.8519(2) 0.9113(3) 0.0395(7) Uani 1 1 d . . .
C17 C 0.6474(4) 1.1032(4) 0.6525(5) 0.0947(17) Uani 1 1 d . . .
H17A H 0.6660 1.1383 0.5764 0.142 Uiso 1 1 calc R . .
H17B H 0.6379 1.1480 0.7224 0.142 Uiso 1 1 calc R . .
H17C H 0.5868 1.0687 0.6369 0.142 Uiso 1 1 calc R . .
C18 C 0.8192(3) 0.6983(3) 0.9824(4) 0.0664(11) Uani 1 1 d . . .
H18A H 0.8771 0.6579 0.9844 0.100 Uiso 1 1 calc R . .
H18B H 0.7677 0.6663 0.9347 0.100 Uiso 1 1 calc R . .
H18C H 0.7969 0.7102 1.0688 0.100 Uiso 1 1 calc R . .
C21 C 0.9927(2) 0.8593(2) 0.4431(2) 0.0348(6) Uani 1 1 d . . .
C22 C 0.9309(2) 0.8908(2) 0.3490(3) 0.0386(7) Uani 1 1 d . . .
C23 C 0.9392(3) 0.8576(2) 0.2265(3) 0.0462(8) Uani 1 1 d . . .
H23 H 0.8967 0.8796 0.1622 0.055 Uiso 1 1 calc R . .
C24 C 1.0107(3) 0.7918(3) 0.1997(3) 0.0542(9) Uani 1 1 d . . .
H24 H 1.0159 0.7679 0.1161 0.065 Uiso 1 1 calc R . .
C25 C 1.0747(3) 0.7594(2) 0.2901(3) 0.0524(8) Uani 1 1 d . . .
H25 H 1.1231 0.7138 0.2697 0.063 Uiso 1 1 calc R . .
C26 C 1.0664(2) 0.7954(2) 0.4117(3) 0.0426(7) Uani 1 1 d . . .
C27 C 1.1876(4) 0.6918(4) 0.4987(5) 0.0855(15) Uani 1 1 d . . .
H27A H 1.2280 0.6856 0.5744 0.128 Uiso 1 1 calc R . .
H27B H 1.2293 0.6970 0.4241 0.128 Uiso 1 1 calc R . .
H27C H 1.1459 0.6356 0.4905 0.128 Uiso 1 1 calc R . .
C28 C 0.8043(3) 1.0000(3) 0.2915(5) 0.0727(11) Uani 1 1 d . . .
H28A H 0.7586 1.0446 0.3304 0.109 Uiso 1 1 calc R . .
H28B H 0.7683 0.9510 0.2454 0.109 Uiso 1 1 calc R . .
H28C H 0.8467 1.0344 0.2329 0.109 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
Al1 O1 1.798(2) . ?
Al1 O2 1.833(2) . ?
Al1 C2 1.963(4) . ?
Al1 C1 1.970(3) . ?
Al1 Na1 3.2725(17) . ?
Al1 Na1 3.3593(18) 2_775 ?
Na1 O2 2.272(3) 2_775 ?
Na1 O1 2.275(2) . ?
Na1 O3 2.310(3) . ?
Na1 O5 2.357(3) . ?
Na1 O2 2.466(3) . ?
Na1 C21 2.897(3) 2_775 ?
Na1 O6 2.903(3) 2_775 ?
Na1 C11 3.093(3) . ?
Na1 Al1 3.3593(18) 2_775 ?
Na1 Na1 3.612(3) 2_775 ?
O1 C11 1.314(4) . ?
O2 C21 1.351(3) . ?
O2 Na1 2.272(3) 2_775 ?
O3 C12 1.372(4) . ?
O3 C17 1.419(5) . ?
O4 C16 1.367(4) . ?
O4 C18 1.424(4) . ?
O5 C22 1.386(4) . ?
O5 C28 1.429(5) . ?
O6 C26 1.369(4) . ?
O6 C27 1.430(5) . ?
O6 Na1 2.903(3) 2_775 ?
C11 C12 1.405(4) . ?
C11 C16 1.401(4) . ?
C12 C13 1.385(5) . ?
C13 C14 1.379(6) . ?
C14 C15 1.372(6) . ?
C15 C16 1.397(5) . ?
C21 C22 1.385(4) . ?
C21 C26 1.396(4) . ?
C21 Na1 2.897(3) 2_775 ?
C22 C23 1.384(4) . ?
C23 C24 1.381(5) . ?
C24 C25 1.379(6) . ?
C25 C26 1.388(5) . ?

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
O1 Al1 O2 89.06(10) . . ?
O1 Al1 C2 112.09(15) . . ?
O2 Al1 C2 105.87(14) . . ?
O1 Al1 C1 116.04(17) . . ?
O2 Al1 C1 110.62(14) . . ?
C2 Al1 C1 118.60(18) . . ?
O1 Al1 Na1 41.85(7) . . ?
O2 Al1 Na1 48.25(7) . . ?
C2 Al1 Na1 109.65(12) . . ?
C1 Al1 Na1 131.56(14) . . ?
O1 Al1 Na1 103.78(8) . 2_775 ?
O2 Al1 Na1 39.64(8) . 2_775 ?
C2 Al1 Na1 66.23(11) . 2_775 ?
C1 Al1 Na1 130.47(13) . 2_775 ?
Na1 Al1 Na1 65.99(5) . 2_775 ?
O2 Na1 O1 122.95(10) 2_775 . ?
O2 Na1 O3 142.88(11) 2_775 . ?
O1 Na1 O3 70.08(9) . . ?
O2 Na1 O5 98.40(9) 2_775 . ?
O1 Na1 O5 105.47(10) . . ?
O3 Na1 O5 111.79(11) . . ?
O2 Na1 O2 79.08(9) 2_775 . ?
O1 Na1 O2 64.83(8) . . ?
O3 Na1 O2 131.90(10) . . ?
O5 Na1 O2 67.05(8) . . ?
O2 Na1 C21 27.01(7) 2_775 2_775 ?
O1 Na1 C21 146.26(10) . 2_775 ?
O3 Na1 C21 140.91(10) . 2_775 ?
O5 Na1 C21 77.92(9) . 2_775 ?
O2 Na1 C21 87.13(9) . 2_775 ?
O2 Na1 O6 59.87(8) 2_775 2_775 ?
O1 Na1 O6 154.95(10) . 2_775 ?
O3 Na1 O6 93.76(9) . 2_775 ?
O5 Na1 O6 98.21(9) . 2_775 ?
O2 Na1 O6 134.32(9) . 2_775 ?
C21 Na1 O6 47.20(8) 2_775 2_775 ?
O2 Na1 C11 134.18(9) 2_775 . ?
O1 Na1 C11 22.35(8) . . ?
O3 Na1 C11 48.49(8) . . ?
O5 Na1 C11 115.99(9) . . ?
O2 Na1 C11 87.14(8) . . ?
C21 Na1 C11 161.18(9) 2_775 . ?
O6 Na1 C11 135.44(9) 2_775 . ?
O2 Na1 Al1 99.20(7) 2_775 . ?
O1 Na1 Al1 31.82(6) . . ?
O3 Na1 Al1 101.63(7) . . ?
O5 Na1 Al1 90.32(7) . . ?
O2 Na1 Al1 33.69(5) . . ?
C21 Na1 Al1 116.48(8) 2_775 . ?
O6 Na1 Al1 158.24(7) 2_775 . ?
C11 Na1 Al1 54.10(6) . . ?
O2 Na1 Al1 30.99(5) 2_775 2_775 ?
O1 Na1 Al1 106.54(8) . 2_775 ?
O3 Na1 Al1 115.50(8) . 2_775 ?
O5 Na1 Al1 129.39(8) . 2_775 ?
O2 Na1 Al1 93.05(7) . 2_775 ?
C21 Na1 Al1 54.09(6) 2_775 2_775 ?
O6 Na1 Al1 62.30(6) 2_775 2_775 ?
C11 Na1 Al1 108.39(7) . 2_775 ?
Al1 Na1 Al1 96.89(5) . 2_775 ?
O2 Na1 Na1 42.36(6) 2_775 2_775 ?
O1 Na1 Na1 87.11(7) . 2_775 ?
O3 Na1 Na1 152.71(7) . 2_775 ?
O5 Na1 Na1 88.10(7) . 2_775 ?
O2 Na1 Na1 38.37(6) . 2_775 ?
C21 Na1 Na1 59.24(7) 2_775 2_775 ?
O6 Na1 Na1 101.93(7) 2_775 2_775 ?
C11 Na1 Na1 106.64(7) . 2_775 ?
Al1 Na1 Na1 58.16(4) . 2_775 ?
Al1 Na1 Na1 55.85(4) 2_775 2_775 ?
C11 O1 Al1 136.84(19) . . ?
C11 O1 Na1 116.47(18) . . ?
Al1 O1 Na1 106.33(11) . . ?
C21 O2 Al1 128.36(18) . . ?
C21 O2 Na1 103.22(19) . 2_775 ?
Al1 O2 Na1 109.37(11) . 2_775 ?
C21 O2 Na1 115.11(18) . . ?
Al1 O2 Na1 98.05(9) . . ?
Na1 O2 Na1 99.27(9) 2_775 . ?
C12 O3 C17 117.5(3) . . ?
C12 O3 Na1 116.44(19) . . ?
C17 O3 Na1 125.7(3) . . ?
C16 O4 C18 117.5(3) . . ?
C22 O5 C28 117.2(3) . . ?
C22 O5 Na1 120.56(19) . . ?
C28 O5 Na1 119.6(2) . . ?
C26 O6 C27 118.0(3) . . ?
C26 O6 Na1 91.02(19) . 2_775 ?
C27 O6 Na1 143.8(3) . 2_775 ?
O1 C11 C12 120.3(3) . . ?
O1 C11 C16 122.3(3) . . ?
C12 C11 C16 117.3(3) . . ?
O1 C11 Na1 41.18(13) . . ?
C12 C11 Na1 80.02(19) . . ?
C16 C11 Na1 162.0(2) . . ?
O3 C12 C13 124.0(3) . . ?
O3 C12 C11 114.1(3) . . ?
C13 C12 C11 121.9(3) . . ?
C14 C13 C12 118.9(3) . . ?
C13 C14 C15 121.4(4) . . ?
C14 C15 C16 119.5(4) . . ?
O4 C16 C15 125.0(3) . . ?
O4 C16 C11 114.0(3) . . ?
C15 C16 C11 121.0(3) . . ?
O2 C21 C22 120.8(3) . . ?
O2 C21 C26 120.3(3) . . ?
C22 C21 C26 118.8(3) . . ?
O2 C21 Na1 49.77(15) . 2_775 ?
C22 C21 Na1 127.1(2) . 2_775 ?
C26 C21 Na1 90.7(2) . 2_775 ?
C21 C22 O5 115.0(3) . . ?
C21 C22 C23 121.1(3) . . ?
O5 C22 C23 123.9(3) . . ?
C24 C23 C22 118.5(3) . . ?
C23 C24 C25 122.3(3) . . ?
C24 C25 C26 118.1(3) . . ?
O6 C26 C21 114.2(3) . . ?
O6 C26 C25 124.7(3) . . ?
C21 C26 C25 121.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.058
_database_code_depnum_ccdc_archive 'CCDC 993199'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3c.C4H8O

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H32 Al K O7'
_chemical_formula_weight         474.56

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'
Al Al 0.0645 0.0514 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.4801(13)
_cell_length_b                   7.311(2)
_cell_length_c                   25.671(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.860(17)
_cell_angle_gamma                90.00
_cell_volume                     2339.5(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    50
_cell_measurement_theta_max      21.04
_cell_measurement_theta_min      3.45

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.37
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;

_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_T_max  1.425

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42907
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5351
_reflns_number_gt                3859
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0593P)²+7.1015P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5351
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0835
_refine_ls_wR_factor_ref         0.2258
_refine_ls_wR_factor_gt          0.2144
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.104
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 -0.029 0.500 254 29 ' '
2 0.500 -0.054 0.000 254 29 ' '
_platon_squeeze_details          
;
;
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.98958(7) 0.56452(14) 0.24707(4) 0.0397(3) Uani 1 1 d . . .
Al1 Al 0.78733(9) 0.83577(19) 0.18308(5) 0.0352(3) Uani 1 1 d . . .
O1 O 0.8273(2) 0.8538(5) 0.25164(10) 0.0428(8) Uani 1 1 d . . .
O2 O 0.9295(2) 0.8486(5) 0.17108(10) 0.0414(7) Uani 1 1 d . . .
O4 O 0.6140(2) 0.8349(6) 0.25238(13) 0.0583(10) Uani 1 1 d . . .
O5 O 1.1356(2) 0.7997(5) 0.18828(12) 0.0458(8) Uani 1 1 d . . .
O3 O 0.9531(2) 0.8023(5) 0.33554(10) 0.0420(7) Uani 1 1 d . . .
O6 O 0.8326(3) 0.8276(6) 0.07662(12) 0.0606(10) Uani 1 1 d . . .
C11 C 0.7806(3) 0.8147(6) 0.29594(15) 0.0351(9) Uani 1 1 d . . .
C12 C 0.8441(3) 0.7874(6) 0.34120(16) 0.0398(10) Uani 1 1 d . . .
C13 C 0.7972(4) 0.7459(8) 0.38805(18) 0.0583(14) Uani 1 1 d . . .
H13 H 0.8398 0.7256 0.4183 0.070 Uiso 1 1 calc R . .
C14 C 0.6877(5) 0.7355(10) 0.3889(2) 0.0709(17) Uani 1 1 d . . .
H14 H 0.6567 0.7095 0.4202 0.085 Uiso 1 1 calc R . .
C15 C 0.6221(4) 0.7624(8) 0.3449(2) 0.0560(13) Uani 1 1 d . . .
H15 H 0.5480 0.7539 0.3463 0.067 Uiso 1 1 calc R . .
C16 C 0.6688(3) 0.8020(7) 0.29869(17) 0.0434(10) Uani 1 1 d . . .
C17 C 0.5003(4) 0.8249(9) 0.2505(3) 0.0660(15) Uani 1 1 d . . .
H17A H 0.4727 0.8507 0.2157 0.099 Uiso 1 1 calc R . .
H17B H 0.4727 0.9128 0.2741 0.099 Uiso 1 1 calc R . .
H17C H 0.4786 0.7043 0.2603 0.099 Uiso 1 1 calc R . .
C21 C 0.9874(3) 0.8110(6) 0.12976(15) 0.0348(9) Uani 1 1 d . . .
C26 C 0.9406(4) 0.7959(7) 0.07937(16) 0.0427(10) Uani 1 1 d . . .
C23 C 1.0012(4) 0.7547(7) 0.03734(17) 0.0525(12) Uani 1 1 d . . .
H23 H 0.9693 0.7439 0.0040 0.063 Uiso 1 1 calc R . .
C24 C 1.1103(4) 0.7300(8) 0.0460(2) 0.0615(15) Uani 1 1 d . . .
H24 H 1.1519 0.7040 0.0178 0.074 Uiso 1 1 calc R . .
C25 C 1.1595(4) 0.7426(8) 0.0952(2) 0.0537(13) Uani 1 1 d . . .
H25 H 1.2330 0.7246 0.1003 0.064 Uiso 1 1 calc R . .
C22 C 1.0968(3) 0.7829(6) 0.13720(17) 0.0413(10) Uani 1 1 d . . .
C27 C 0.7761(5) 0.8111(11) 0.0279(2) 0.0759(19) Uani 1 1 d . . .
H27A H 0.7017 0.8380 0.0318 0.114 Uiso 1 1 calc R . .
H27B H 0.7832 0.6886 0.0151 0.114 Uiso 1 1 calc R . .
H27C H 0.8050 0.8955 0.0036 0.114 Uiso 1 1 calc R . .
C28 C 1.2503(3) 0.7960(8) 0.1972(2) 0.0532(13) Uani 1 1 d . . .
H28A H 1.2680 0.8089 0.2338 0.080 Uiso 1 1 calc R . .
H28B H 1.2816 0.8949 0.1786 0.080 Uiso 1 1 calc R . .
H28C H 1.2778 0.6819 0.1851 0.080 Uiso 1 1 calc R . .
C2 C 0.7046(4) 1.0456(7) 0.15752(19) 0.0531(12) Uani 1 1 d . . .
H20A H 0.6855 1.0295 0.1211 0.080 Uiso 1 1 calc R . .
H20B H 0.7468 1.1546 0.1622 0.080 Uiso 1 1 calc R . .
H20C H 0.6406 1.0563 0.1766 0.080 Uiso 1 1 calc R . .
C1 C 0.7361(4) 0.5882(7) 0.1696(2) 0.0575(13) Uani 1 1 d . . .
H10A H 0.7145 0.5760 0.1333 0.086 Uiso 1 1 calc R . .
H10B H 0.6759 0.5638 0.1904 0.086 Uiso 1 1 calc R . .
H10C H 0.7925 0.5027 0.1783 0.086 Uiso 1 1 calc R . .
C18 C 1.0213(4) 0.7953(7) 0.38222(17) 0.0488(11) Uani 1 1 d . . .
H18A H 1.0948 0.8072 0.3734 0.073 Uiso 1 1 calc R . .
H18B H 1.0115 0.6805 0.3995 0.073 Uiso 1 1 calc R . .
H18C H 1.0031 0.8935 0.4050 0.073 Uiso 1 1 calc R . .


_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
K1 O1 2.755(3) 2_745 ?
K1 O2 2.778(3) 2_745 ?
K1 O3 2.914(3) . ?
K1 O2 2.922(3) . ?
K1 O1 2.935(3) . ?
K1 O5 2.971(3) . ?
K1 O3 2.973(3) 2_745 ?
K1 O5 3.034(3) 2_745 ?
K1 C11 3.471(4) . ?
K1 C12 3.497(4) . ?
K1 C21 3.508(4) . ?
K1 Al1 3.5480(16) . ?
Al1 O1 1.810(3) . ?
Al1 O2 1.819(3) . ?
Al1 C1 1.945(5) . ?
Al1 C2 1.945(5) . ?
Al1 K1 3.6423(16) 2_755 ?
O1 C11 1.335(4) . ?
O1 K1 2.755(3) 2_755 ?
O2 C21 1.341(4) . ?
O2 K1 2.778(3) 2_755 ?
O4 C16 1.363(5) . ?
O4 C17 1.419(5) . ?
O5 C22 1.380(5) . ?
O5 C28 1.439(5) . ?
O5 K1 3.034(3) 2_755 ?
O3 C12 1.379(5) . ?
O3 C18 1.436(5) . ?
O3 K1 2.973(3) 2_755 ?
O6 C26 1.365(5) . ?
O6 C27 1.409(5) . ?
C11 C12 1.388(6) . ?
C11 C16 1.403(6) . ?
C12 C13 1.397(6) . ?
C13 C14 1.370(8) . ?
C14 C15 1.375(8) . ?
C15 C16 1.378(6) . ?
C21 C22 1.385(6) . ?
C21 C26 1.397(6) . ?
C26 C23 1.382(6) . ?
C23 C24 1.380(7) . ?
C24 C25 1.380(7) . ?
C25 C22 1.394(6) . ?

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
O1 K1 O2 53.35(8) 2_745 2_745 ?
O1 K1 O3 119.07(9) 2_745 . ?
O2 K1 O3 79.30(9) 2_745 . ?
O1 K1 O2 126.20(9) 2_745 . ?
O2 K1 O2 168.71(11) 2_745 . ?
O3 K1 O2 92.95(9) . . ?
O1 K1 O1 167.48(11) 2_745 . ?
O2 K1 O1 127.22(9) 2_745 . ?
O3 K1 O1 53.41(8) . . ?
O2 K1 O1 50.19(8) . . ?
O1 K1 O5 78.48(9) 2_745 . ?
O2 K1 O5 120.28(9) 2_745 . ?
O3 K1 O5 100.04(9) . . ?
O2 K1 O5 52.61(8) . . ?
O1 K1 O5 92.59(9) . . ?
O1 K1 O3 54.47(8) 2_745 2_745 ?
O2 K1 O3 94.69(9) 2_745 2_745 ?
O3 K1 O3 173.39(7) . 2_745 ?
O2 K1 O3 92.58(9) . 2_745 ?
O1 K1 O3 133.20(8) . 2_745 ?
O5 K1 O3 80.52(9) . 2_745 ?
O1 K1 O5 94.93(9) 2_745 2_745 ?
O2 K1 O5 53.19(8) 2_745 2_745 ?
O3 K1 O5 81.35(9) . 2_745 ?
O2 K1 O5 134.21(8) . 2_745 ?
O1 K1 O5 93.62(9) . 2_745 ?
O5 K1 O5 173.12(8) . 2_745 ?
O3 K1 O5 97.32(9) 2_745 2_745 ?
O1 K1 C11 158.14(9) 2_745 . ?
O2 K1 C11 106.10(9) 2_745 . ?
O3 K1 C11 41.79(9) . . ?
O2 K1 C11 72.21(9) . . ?
O1 K1 C11 22.08(8) . . ?
O5 K1 C11 111.69(10) . . ?
O3 K1 C11 144.06(9) 2_745 . ?
O5 K1 C11 73.86(10) 2_745 . ?
O1 K1 C12 135.33(10) 2_745 . ?
O2 K1 C12 85.62(10) 2_745 . ?
O3 K1 C12 22.59(9) . . ?
O2 K1 C12 90.31(10) . . ?
O1 K1 C12 41.71(9) . . ?
O5 K1 C12 115.72(10) . . ?
O3 K1 C12 160.95(10) 2_745 . ?
O5 K1 C12 67.68(10) 2_745 . ?
C11 K1 C12 22.97(9) . . ?
O1 K1 C21 105.58(9) 2_745 . ?
O2 K1 C21 158.17(9) 2_745 . ?
O3 K1 C21 111.58(10) . . ?
O2 K1 C21 21.71(8) . . ?
O1 K1 C21 71.84(9) . . ?
O5 K1 C21 41.02(9) . . ?
O3 K1 C21 73.19(9) 2_745 . ?
O5 K1 C21 144.62(9) 2_745 . ?
C11 K1 C21 93.77(10) . . ?
C12 K1 C21 111.82(10) . . ?
O1 K1 Al1 152.71(7) 2_745 . ?
O2 K1 Al1 153.03(7) 2_745 . ?
O3 K1 Al1 83.81(7) . . ?
O2 K1 Al1 30.75(6) . . ?
O1 K1 Al1 30.60(6) . . ?
O5 K1 Al1 83.19(7) . . ?
O3 K1 Al1 102.78(7) 2_745 . ?
O5 K1 Al1 103.67(7) 2_745 . ?
C11 K1 Al1 48.92(7) . . ?
C12 K1 Al1 71.19(8) . . ?
C21 K1 Al1 48.74(7) . . ?
O1 Al1 O2 86.39(13) . . ?
O1 Al1 C1 108.3(2) . . ?
O2 Al1 C1 109.4(2) . . ?
O1 Al1 C2 112.7(2) . . ?
O2 Al1 C2 114.1(2) . . ?
C1 Al1 C2 120.6(2) . . ?
O1 Al1 K1 55.62(11) . . ?
O2 Al1 K1 55.23(11) . . ?
C1 Al1 K1 77.44(17) . . ?
C2 Al1 K1 161.90(17) . . ?
O1 Al1 K1 47.23(10) . 2_755 ?
O2 Al1 K1 48.04(9) . 2_755 ?
C1 Al1 K1 138.73(17) . 2_755 ?
C2 Al1 K1 100.59(17) . 2_755 ?
K1 Al1 K1 61.32(2) . 2_755 ?
C11 O1 Al1 134.6(3) . . ?
C11 O1 K1 120.5(2) . 2_755 ?
Al1 O1 K1 103.93(12) . 2_755 ?
C11 O1 K1 102.2(2) . . ?
Al1 O1 K1 93.77(13) . . ?
K1 O1 K1 80.20(7) 2_755 . ?
C21 O2 Al1 133.8(3) . . ?
C21 O2 K1 121.7(2) . 2_755 ?
Al1 O2 K1 102.83(12) . 2_755 ?
C21 O2 K1 104.6(2) . . ?
Al1 O2 K1 94.02(12) . . ?
K1 O2 K1 80.06(7) 2_755 . ?
C16 O4 C17 118.6(4) . . ?
C22 O5 C28 116.6(3) . . ?
C22 O5 K1 103.7(2) . . ?
C28 O5 K1 122.6(3) . . ?
C22 O5 K1 114.3(2) . 2_755 ?
C28 O5 K1 117.4(3) . 2_755 ?
K1 O5 K1 75.28(7) . 2_755 ?
C12 O3 C18 117.1(3) . . ?
C12 O3 K1 103.2(2) . . ?
C18 O3 K1 121.4(3) . . ?
C12 O3 K1 113.6(2) . 2_755 ?
C18 O3 K1 117.7(3) . 2_755 ?
K1 O3 K1 77.07(7) . 2_755 ?
C26 O6 C27 118.7(4) . . ?
O1 C11 C12 119.3(3) . . ?
O1 C11 C16 122.3(4) . . ?
C12 C11 C16 118.4(4) . . ?
O1 C11 K1 55.7(2) . . ?
C12 C11 K1 79.6(2) . . ?
C16 C11 K1 138.6(3) . . ?
O3 C12 C11 115.2(3) . . ?
O3 C12 C13 124.4(4) . . ?
C11 C12 C13 120.4(4) . . ?
O3 C12 K1 54.22(19) . . ?
C11 C12 K1 77.5(2) . . ?
C13 C12 K1 138.4(4) . . ?
C14 C13 C12 119.1(5) . . ?
C13 C14 C15 122.2(4) . . ?
C14 C15 C16 118.5(4) . . ?
O4 C16 C15 124.9(4) . . ?
O4 C16 C11 113.7(4) . . ?
C15 C16 C11 121.4(4) . . ?
O2 C21 C22 119.2(4) . . ?
O2 C21 C26 122.1(4) . . ?
C22 C21 C26 118.7(4) . . ?
O2 C21 K1 53.7(2) . . ?
C22 C21 K1 80.8(2) . . ?
C26 C21 K1 137.7(3) . . ?
O6 C26 C23 125.1(4) . . ?
O6 C26 C21 113.6(4) . . ?
C23 C26 C21 121.3(4) . . ?
C24 C23 C26 118.5(4) . . ?
C25 C24 C23 121.9(4) . . ?
C24 C25 C22 118.8(4) . . ?
O5 C22 C21 114.5(4) . . ?
O5 C22 C25 124.7(4) . . ?
C21 C22 C25 120.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.082
_database_code_depnum_ccdc_archive 'CCDC 993200'
