Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2003

data_global

_publ_contact_author_email       SARAH.HEATH@MAN.AC.UK

_publ_contact_author_name        'Dr Sarah Louise Heath'
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_publ_contact_author_address     
;
Department of Chemistry
University of Manchester
Oxford Road
Manchester
M13 9PL
UNITED KINGDOM
;

_publ_section_title              
;
Synthesis and Structure of a new Aluminum citrate
trimer from aqueous solution at very low pH
;

loop_
_publ_author_name
'Sarah Louise Heath'
'Paul Cooper'
'Simon A. Malone'

data_s1579m
_database_code_depnum_ccdc_archive 'CCDC 220850'
_chemical_name_common            'Al Trimer (1)'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H60 Al7 N O55'
_chemical_formula_weight         1431.59

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   10.3785(12)
_cell_length_b                   12.4967(15)
_cell_length_c                   20.839(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.624(2)
_cell_angle_gamma                90.00
_cell_volume                     2656.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1953
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      23.39

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1484
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_correction_T_min  0.9461
_exptl_absorpt_correction_T_max  0.9944
_exptl_absorpt_process_details   'repeated and equivalent reflections'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Bruker-AXS Apex area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11645
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0799
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         23.31
_reflns_number_total             3830
_reflns_number_gt                2344
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1231P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         3830
_refine_ls_number_parameters     478
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0630
_refine_ls_wR_factor_ref         0.1972
_refine_ls_wR_factor_gt          0.1773
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.014
_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 0.49292(17) 0.95372(14) 0.13924(9) 0.0154(5) Uani 1 1 d . . .
Al2 Al 0.26115(17) 0.95738(14) 0.19348(10) 0.0191(5) Uani 1 1 d . . .
Al3 Al 0.54909(17) 0.94906(14) 0.30729(9) 0.0154(5) Uani 1 1 d . . .
O1 O 0.5936(4) 0.8431(3) 0.1130(2) 0.0194(10) Uani 1 1 d . . .
O2 O 0.7169(4) 0.7000(4) 0.1284(2) 0.0308(12) Uani 1 1 d . . .
O3 O 0.5991(4) 0.9534(3) 0.22424(19) 0.0159(9) Uani 1 1 d . . .
O4 O 0.5973(4) 1.0620(3) 0.1133(2) 0.0184(10) Uani 1 1 d . . .
O5 O 0.7495(5) 1.1867(4) 0.1209(2) 0.0395(14) Uani 1 1 d . . .
O6 O 0.7291(4) 0.9474(3) 0.34209(19) 0.0177(10) Uani 1 1 d . . .
O7 O 0.9267(4) 0.9455(3) 0.3149(2) 0.0231(11) Uani 1 1 d . . .
O8 O 0.1587(4) 1.0663(3) 0.2209(2) 0.0225(11) Uani 1 1 d . . .
O9 O 0.0709(4) 1.1704(3) 0.2852(2) 0.0243(11) Uani 1 1 d . . .
O10 O 0.3690(4) 0.9536(3) 0.2802(2) 0.0191(10) Uani 1 1 d . . .
O11 O 0.5216(4) 0.9424(3) 0.3932(2) 0.0199(10) Uani 1 1 d . . .
O12 O 0.3672(4) 0.9370(4) 0.4542(2) 0.0275(11) Uani 1 1 d . . .
O13 O 0.1501(4) 0.8512(3) 0.2149(2) 0.0220(11) Uani 1 1 d . . .
O14 O 0.0655(4) 0.7324(3) 0.2732(2) 0.0237(11) Uani 1 1 d . . .
O15 O 0.3734(4) 1.0496(2) 0.1609(2) 0.0176(10) Uani 1 1 d D . .
H15 H 0.381(6) 1.1220(17) 0.179(3) 0.021 Uiso 1 1 d D . .
O16 O 0.3693(4) 0.8628(3) 0.1604(2) 0.0191(10) Uani 1 1 d D . .
H16 H 0.377(6) 0.7858(9) 0.169(3) 0.023 Uiso 1 1 d D . .
O17 O 0.1428(2) 0.9648(3) 0.1104(2) 0.0296(12) Uani 1 1 d D . .
H17A H 0.0469(3) 0.961(4) 0.103(3) 0.044 Uiso 1 1 d D . .
H17B H 0.160(4) 1.028(3) 0.085(3) 0.044 Uiso 1 1 d D . .
O18 O 0.4063(4) 0.9532(2) 0.0476(2) 0.0209(10) Uani 1 1 d D . .
H18A H 0.364(3) 1.0147(17) 0.0230(18) 0.031 Uiso 1 1 d D . .
H18B H 0.377(5) 0.8922(18) 0.0191(18) 0.031 Uiso 1 1 d D . .
O19 O 0.5513(3) 0.7941(3) 0.3067(2) 0.0211(10) Uani 1 1 d D . .
H19A H 0.498(5) 0.747(4) 0.275(2) 0.032 Uiso 1 1 d D . .
H19B H 0.611(5) 0.749(4) 0.337(2) 0.032 Uiso 1 1 d D . .
O20 O 0.5574(3) 1.1040(3) 0.3158(2) 0.0199(10) Uani 1 1 d D . .
H20A H 0.503(5) 1.153(4) 0.286(2) 0.030 Uiso 1 1 d D . .
H20B H 0.636(3) 1.144(4) 0.335(3) 0.030 Uiso 1 1 d D . .
C1 C 0.6917(6) 0.7930(5) 0.1440(3) 0.0189(15) Uani 1 1 d . . .
C2 C 0.7791(6) 0.8422(5) 0.2013(3) 0.0250(16) Uani 1 1 d . . .
H2A H 0.8663 0.8527 0.1895 0.030 Uiso 1 1 calc R . .
H2B H 0.7902 0.7896 0.2375 0.030 Uiso 1 1 calc R . .
C3 C 0.7376(5) 0.9491(5) 0.2279(3) 0.0190(14) Uani 1 1 d . . .
C4 C 0.7892(6) 1.0501(5) 0.2003(3) 0.0280(17) Uani 1 1 d . . .
H4A H 0.8047 1.1040 0.2357 0.034 Uiso 1 1 calc R . .
H4B H 0.8755 1.0327 0.1892 0.034 Uiso 1 1 calc R . .
C5 C 0.7073(6) 1.1025(5) 0.1412(3) 0.0255(16) Uani 1 1 d . . .
C6 C 0.8062(6) 0.9476(5) 0.3008(3) 0.0212(15) Uani 1 1 d . . .
C7 C 0.1444(6) 1.0961(5) 0.2771(3) 0.0191(15) Uani 1 1 d . . .
C8 C 0.2219(6) 1.0484(5) 0.3380(3) 0.0263(16) Uani 1 1 d . . .
H8A H 0.1601 1.0341 0.3680 0.032 Uiso 1 1 calc R . .
H8B H 0.2837 1.1039 0.3590 0.032 Uiso 1 1 calc R . .
C9 C 0.3003(6) 0.9468(5) 0.3341(3) 0.0239(16) Uani 1 1 d . . .
C10 C 0.2288(6) 0.8405(5) 0.3317(3) 0.0257(16) Uani 1 1 d . . .
H10A H 0.2956 0.7836 0.3432 0.031 Uiso 1 1 calc R . .
H10B H 0.1751 0.8413 0.3663 0.031 Uiso 1 1 calc R . .
C11 C 0.1408(6) 0.8084(5) 0.2688(3) 0.0195(15) Uani 1 1 d . . .
C12 C 0.4033(6) 0.9429(5) 0.4005(3) 0.0252(16) Uani 1 1 d . . .
Al4 Al 0.5000 1.5000 0.0000 0.0184(6) Uani 1 2 d S . .
O1W O 0.6866(3) 1.4961(2) 0.0236(2) 0.0218(10) Uani 1 1 d D . .
H1A H 0.6954(8) 1.4188(7) 0.031(3) 0.033 Uiso 1 1 d D . .
H1B H 0.760(4) 1.513(3) 0.002(3) 0.033 Uiso 1 1 d D . .
O2W O 0.5047(3) 1.3845(2) -0.0578(2) 0.0204(10) Uani 1 1 d D . .
H2C H 0.5649(5) 1.3256(12) -0.042(2) 0.031 Uiso 1 1 d D . .
H2D H 0.432(3) 1.349(2) -0.087(2) 0.031 Uiso 1 1 d D . .
O3W O 0.5131(4) 1.5944(2) -0.0661(2) 0.0233(11) Uani 1 1 d D . .
H3A H 0.469(5) 1.568(5) -0.1088(14) 0.035 Uiso 1 1 d D . .
H3B H 0.512(6) 1.6723(6) -0.061(3) 0.035 Uiso 1 1 d D . .
O4W O 0.7002(4) 1.2417(4) -0.0121(2) 0.0402(13) Uani 1 1 d D . .
H4C H 0.707(7) 1.218(6) 0.0332(12) 0.060 Uiso 1 1 d D . .
H4D H 0.726(7) 1.263(6) -0.0532(19) 0.060 Uiso 1 1 d D . .
O5W O 0.5661(3) 1.7927(3) -0.0366(3) 0.0521(15) Uani 1 1 d D . .
H5A H 0.653(4) 1.826(6) -0.024(4) 0.078 Uiso 1 1 d D . .
H5B H 0.518(7) 1.856(4) -0.056(4) 0.078 Uiso 1 1 d D . .
O6W O 0.5515(4) 0.8038(4) 0.5342(3) 0.074(2) Uani 1 1 d D . .
H6A H 0.526(9) 0.753(6) 0.498(3) 0.112 Uiso 1 1 d D . .
H6B H 0.499(8) 0.829(8) 0.566(4) 0.112 Uiso 1 1 d D . .
N1 N -0.1519(13) 0.9227(15) 0.0302(9) 0.071(5) Uani 0.50 1 d PD . .
O21 O -0.1256(10) 1.0058(12) 0.0562(8) 0.082(5) Uani 0.50 1 d PD . .
O22 O -0.1817(12) 0.8703(9) -0.0255(5) 0.080(5) Uani 0.50 1 d PD . .
O23 O -0.0875(9) 0.8602(8) 0.0785(5) 0.040(3) Uani 0.50 1 d PD . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Al1 0.0141(10) 0.0131(10) 0.0183(10) 0.0013(8) 0.0006(8) 0.0013(7)
Al2 0.0097(10) 0.0191(11) 0.0274(12) 0.0001(9) 0.0001(8) 0.0012(8)
Al3 0.0132(10) 0.0156(10) 0.0157(10) -0.0004(8) -0.0017(8) 0.0007(8)
O1 0.015(2) 0.020(2) 0.022(2) -0.0036(19) -0.0011(19) 0.0053(18)
O2 0.023(3) 0.026(3) 0.037(3) -0.014(2) -0.012(2) 0.008(2)
O3 0.011(2) 0.016(2) 0.021(2) 0.0007(18) 0.0017(18) 0.0032(17)
O4 0.012(2) 0.021(2) 0.021(2) 0.0029(19) 0.0003(18) -0.0011(18)
O5 0.040(3) 0.035(3) 0.038(3) 0.016(2) -0.007(2) -0.018(2)
O6 0.020(2) 0.018(2) 0.013(2) -0.0038(18) -0.0019(19) 0.0014(18)
O7 0.014(2) 0.032(3) 0.022(3) 0.000(2) 0.0004(19) -0.0003(19)
O8 0.009(2) 0.025(3) 0.032(3) 0.004(2) 0.000(2) 0.0057(18)
O9 0.020(2) 0.019(3) 0.032(3) -0.003(2) 0.000(2) 0.000(2)
O10 0.013(2) 0.022(2) 0.022(2) -0.0022(19) 0.0030(18) 0.0006(18)
O11 0.017(2) 0.024(2) 0.016(2) -0.0001(19) -0.0026(18) -0.0008(19)
O12 0.024(3) 0.039(3) 0.021(3) 0.000(2) 0.008(2) -0.001(2)
O13 0.013(2) 0.026(3) 0.025(3) 0.001(2) -0.0025(19) -0.0042(19)
O14 0.020(2) 0.018(3) 0.031(3) 0.003(2) -0.001(2) -0.001(2)
O15 0.012(2) 0.013(2) 0.027(3) -0.0026(19) 0.0027(18) 0.0008(18)
O16 0.014(2) 0.016(2) 0.026(3) 0.0010(19) -0.0001(18) 0.0001(18)
O17 0.013(2) 0.042(3) 0.032(3) 0.000(2) -0.003(2) -0.003(2)
O18 0.021(2) 0.019(2) 0.020(2) 0.0004(19) -0.0051(19) 0.0017(18)
O19 0.020(2) 0.017(2) 0.024(3) 0.0010(19) -0.0050(19) 0.0005(18)
O20 0.015(2) 0.018(2) 0.024(3) -0.002(2) -0.0030(19) -0.0010(18)
C1 0.016(4) 0.019(4) 0.022(4) -0.003(3) 0.004(3) 0.001(3)
C2 0.012(3) 0.024(4) 0.036(4) -0.007(3) -0.002(3) 0.003(3)
C3 0.010(3) 0.021(4) 0.027(4) -0.002(3) 0.005(3) 0.000(3)
C4 0.018(4) 0.032(4) 0.032(4) 0.004(3) -0.001(3) -0.002(3)
C5 0.026(4) 0.027(4) 0.024(4) 0.003(3) 0.004(3) -0.002(3)
C6 0.023(4) 0.018(4) 0.022(4) -0.002(3) 0.003(3) 0.004(3)
C7 0.011(3) 0.018(4) 0.027(4) 0.002(3) 0.000(3) -0.008(3)
C8 0.024(4) 0.029(4) 0.026(4) -0.002(3) 0.004(3) -0.002(3)
C9 0.016(3) 0.029(4) 0.027(4) 0.001(3) 0.006(3) 0.000(3)
C10 0.019(4) 0.028(4) 0.030(4) -0.003(3) 0.004(3) 0.000(3)
C11 0.011(3) 0.016(4) 0.030(4) -0.006(3) 0.001(3) 0.007(3)
C12 0.015(4) 0.026(4) 0.031(4) 0.000(3) -0.006(3) -0.003(3)
Al4 0.0175(14) 0.0194(14) 0.0170(15) 0.0000(12) -0.0005(11) 0.0003(12)
O1W 0.020(2) 0.021(2) 0.022(3) 0.001(2) 0.0007(19) -0.0010(19)
O2W 0.023(2) 0.019(2) 0.018(2) 0.0001(19) -0.0023(19) -0.0007(19)
O3W 0.024(2) 0.024(3) 0.019(2) 0.001(2) -0.0043(19) 0.000(2)
O4W 0.046(3) 0.032(3) 0.038(3) 0.002(3) -0.005(3) 0.005(2)
O5W 0.073(4) 0.034(3) 0.049(4) 0.014(3) 0.009(3) 0.010(3)
O6W 0.082(5) 0.081(5) 0.058(5) 0.011(4) 0.007(4) 0.027(4)
N1 0.038(9) 0.090(14) 0.090(14) 0.060(12) 0.028(9) -0.017(9)
O21 0.013(6) 0.088(10) 0.153(14) -0.083(10) 0.036(7) -0.008(6)
O22 0.123(11) 0.058(8) 0.022(6) 0.045(6) -0.085(7) -0.084(7)
O23 0.030(6) 0.050(7) 0.039(6) -0.001(5) 0.006(5) -0.028(5)

_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
Al1 O16 1.827(4) . ?
Al1 O15 1.840(4) . ?
Al1 O1 1.874(4) . ?
Al1 O4 1.875(4) . ?
Al1 O3 1.906(4) . ?
Al1 O18 1.956(4) . ?
Al1 Al2 2.840(3) . ?
Al2 O16 1.849(4) . ?
Al2 O15 1.853(4) . ?
Al2 O13 1.865(4) . ?
Al2 O8 1.880(5) . ?
Al2 O17 1.931(4) . ?
Al2 O10 1.943(4) . ?
Al3 O10 1.851(4) . ?
Al3 O11 1.866(4) . ?
Al3 O6 1.875(4) . ?
Al3 O3 1.897(4) . ?
Al3 O19 1.937(4) . ?
Al3 O20 1.945(4) . ?
O1 C1 1.266(7) . ?
O2 C1 1.248(7) . ?
O3 C3 1.426(7) . ?
O4 C5 1.286(7) . ?
O5 C5 1.243(8) . ?
O6 C6 1.280(8) . ?
O7 C6 1.232(7) . ?
O8 C7 1.263(8) . ?
O9 C7 1.233(7) . ?
O10 C9 1.441(8) . ?
O11 C12 1.264(7) . ?
O12 C12 1.247(8) . ?
O13 C11 1.264(7) . ?
O14 C11 1.243(7) . ?
C1 C2 1.493(8) . ?
C2 C3 1.538(8) . ?
C3 C4 1.525(8) . ?
C3 C6 1.554(9) . ?
C4 C5 1.510(9) . ?
C7 C8 1.496(9) . ?
C8 C9 1.518(9) . ?
C9 C10 1.518(9) . ?
C9 C12 1.584(9) . ?
C10 C11 1.507(8) . ?
Al4 O3W 1.837(4) . ?
Al4 O3W 1.837(4) 3_685 ?
Al4 O2W 1.887(4) . ?
Al4 O2W 1.887(4) 3_685 ?
Al4 O1W 1.909(3) 3_685 ?
Al4 O1W 1.909(3) . ?
N1 O21 1.18(2) . ?
N1 O22 1.32(2) . ?
N1 O23 1.351(17) . ?

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
O16 Al1 O15 79.06(18) . . ?
O16 Al1 O1 93.79(19) . . ?
O15 Al1 O1 171.63(19) . . ?
O16 Al1 O4 170.8(2) . . ?
O15 Al1 O4 93.01(18) . . ?
O1 Al1 O4 93.7(2) . . ?
O16 Al1 O3 94.92(19) . . ?
O15 Al1 O3 94.25(19) . . ?
O1 Al1 O3 90.67(18) . . ?
O4 Al1 O3 90.22(18) . . ?
O16 Al1 O18 90.97(18) . . ?
O15 Al1 O18 91.86(18) . . ?
O1 Al1 O18 83.86(17) . . ?
O4 Al1 O18 84.64(17) . . ?
O3 Al1 O18 172.2(2) . . ?
O16 Al1 Al2 39.68(13) . . ?
O15 Al1 Al2 39.90(12) . . ?
O1 Al1 Al2 133.38(16) . . ?
O4 Al1 Al2 132.84(15) . . ?
O3 Al1 Al2 91.00(14) . . ?
O18 Al1 Al2 96.79(14) . . ?
O16 Al2 O15 78.17(18) . . ?
O16 Al2 O13 94.51(19) . . ?
O15 Al2 O13 171.0(2) . . ?
O16 Al2 O8 173.0(2) . . ?
O15 Al2 O8 95.17(18) . . ?
O13 Al2 O8 91.9(2) . . ?
O16 Al2 O17 91.48(18) . . ?
O15 Al2 O17 88.89(18) . . ?
O13 Al2 O17 85.97(18) . . ?
O8 Al2 O17 86.34(18) . . ?
O16 Al2 O10 92.63(18) . . ?
O15 Al2 O10 93.59(19) . . ?
O13 Al2 O10 92.04(19) . . ?
O8 Al2 O10 89.77(19) . . ?
O17 Al2 O10 175.6(2) . . ?
O16 Al2 Al1 39.13(13) . . ?
O15 Al2 Al1 39.55(11) . . ?
O13 Al2 Al1 133.60(16) . . ?
O8 Al2 Al1 134.47(16) . . ?
O17 Al2 Al1 95.11(14) . . ?
O10 Al2 Al1 89.13(14) . . ?
O10 Al3 O11 88.26(19) . . ?
O10 Al3 O6 175.0(2) . . ?
O11 Al3 O6 86.92(19) . . ?
O10 Al3 O3 98.72(19) . . ?
O11 Al3 O3 172.99(19) . . ?
O6 Al3 O3 86.13(19) . . ?
O10 Al3 O19 92.35(17) . . ?
O11 Al3 O19 88.04(19) . . ?
O6 Al3 O19 88.83(17) . . ?
O3 Al3 O19 90.96(19) . . ?
O10 Al3 O20 91.30(16) . . ?
O11 Al3 O20 88.23(19) . . ?
O6 Al3 O20 87.21(16) . . ?
O3 Al3 O20 92.29(18) . . ?
O19 Al3 O20 174.70(19) . . ?
C1 O1 Al1 130.9(4) . . ?
C3 O3 Al3 113.1(3) . . ?
C3 O3 Al1 117.0(3) . . ?
Al3 O3 Al1 129.7(2) . . ?
C5 O4 Al1 131.8(4) . . ?
C6 O6 Al3 116.2(4) . . ?
C7 O8 Al2 131.7(4) . . ?
C9 O10 Al3 112.2(4) . . ?
C9 O10 Al2 116.4(3) . . ?
Al3 O10 Al2 131.4(2) . . ?
C12 O11 Al3 116.0(4) . . ?
C11 O13 Al2 131.7(4) . . ?
Al1 O15 Al2 100.55(16) . . ?
Al1 O16 Al2 101.19(19) . . ?
O2 C1 O1 121.0(5) . . ?
O2 C1 C2 117.8(5) . . ?
O1 C1 C2 121.2(5) . . ?
C1 C2 C3 118.5(5) . . ?
O3 C3 C4 111.7(5) . . ?
O3 C3 C2 111.1(5) . . ?
C4 C3 C2 116.2(5) . . ?
O3 C3 C6 109.2(5) . . ?
C4 C3 C6 104.4(5) . . ?
C2 C3 C6 103.5(5) . . ?
C5 C4 C3 118.9(5) . . ?
O5 C5 O4 121.3(6) . . ?
O5 C5 C4 117.6(6) . . ?
O4 C5 C4 121.1(6) . . ?
O7 C6 O6 125.0(6) . . ?
O7 C6 C3 119.7(6) . . ?
O6 C6 C3 115.3(5) . . ?
O9 C7 O8 122.0(6) . . ?
O9 C7 C8 115.7(6) . . ?
O8 C7 C8 122.2(6) . . ?
C7 C8 C9 119.8(6) . . ?
O10 C9 C8 109.9(5) . . ?
O10 C9 C10 109.5(5) . . ?
C8 C9 C10 118.1(5) . . ?
O10 C9 C12 109.3(5) . . ?
C8 C9 C12 105.1(5) . . ?
C10 C9 C12 104.4(5) . . ?
C11 C10 C9 118.4(6) . . ?
O14 C11 O13 122.7(6) . . ?
O14 C11 C10 115.3(6) . . ?
O13 C11 C10 121.8(6) . . ?
O12 C12 O11 124.5(6) . . ?
O12 C12 C9 121.3(6) . . ?
O11 C12 C9 114.2(6) . . ?
O3W Al4 O3W 180.00(17) . 3_685 ?
O3W Al4 O2W 89.89(16) . . ?
O3W Al4 O2W 90.11(16) 3_685 . ?
O3W Al4 O2W 90.11(16) . 3_685 ?
O3W Al4 O2W 89.89(16) 3_685 3_685 ?
O2W Al4 O2W 180.00(19) . 3_685 ?
O3W Al4 O1W 90.10(17) . 3_685 ?
O3W Al4 O1W 89.90(17) 3_685 3_685 ?
O2W Al4 O1W 89.98(14) . 3_685 ?
O2W Al4 O1W 90.02(14) 3_685 3_685 ?
O3W Al4 O1W 89.90(17) . . ?
O3W Al4 O1W 90.10(17) 3_685 . ?
O2W Al4 O1W 90.02(14) . . ?
O2W Al4 O1W 89.98(14) 3_685 . ?
O1W Al4 O1W 180.0(3) 3_685 . ?
O21 N1 O22 147.1(16) . . ?
O21 N1 O23 97.2(17) . . ?
O22 N1 O23 111.8(15) . . ?

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
O15 Al1 Al2 O16 168.1(3) . . . . ?
O1 Al1 Al2 O16 -4.6(3) . . . . ?
O4 Al1 Al2 O16 172.3(3) . . . . ?
O3 Al1 Al2 O16 -96.5(2) . . . . ?
O18 Al1 Al2 O16 83.3(2) . . . . ?
O16 Al1 Al2 O15 -168.1(3) . . . . ?
O1 Al1 Al2 O15 -172.7(3) . . . . ?
O4 Al1 Al2 O15 4.2(3) . . . . ?
O3 Al1 Al2 O15 95.4(2) . . . . ?
O18 Al1 Al2 O15 -84.8(2) . . . . ?
O16 Al1 Al2 O13 3.3(3) . . . . ?
O15 Al1 Al2 O13 171.3(3) . . . . ?
O1 Al1 Al2 O13 -1.4(3) . . . . ?
O4 Al1 Al2 O13 175.5(3) . . . . ?
O3 Al1 Al2 O13 -93.2(2) . . . . ?
O18 Al1 Al2 O13 86.6(2) . . . . ?
O16 Al1 Al2 O8 -175.9(3) . . . . ?
O15 Al1 Al2 O8 -7.9(3) . . . . ?
O1 Al1 Al2 O8 179.4(3) . . . . ?
O4 Al1 Al2 O8 -3.7(3) . . . . ?
O3 Al1 Al2 O8 87.6(2) . . . . ?
O18 Al1 Al2 O8 -92.6(2) . . . . ?
O16 Al1 Al2 O17 -86.0(2) . . . . ?
O15 Al1 Al2 O17 82.0(2) . . . . ?
O1 Al1 Al2 O17 -90.7(2) . . . . ?
O4 Al1 Al2 O17 86.2(2) . . . . ?
O3 Al1 Al2 O17 177.45(17) . . . . ?
O18 Al1 Al2 O17 -2.74(16) . . . . ?
O16 Al1 Al2 O10 95.2(2) . . . . ?
O15 Al1 Al2 O10 -96.7(2) . . . . ?
O1 Al1 Al2 O10 90.6(2) . . . . ?
O4 Al1 Al2 O10 -92.5(2) . . . . ?
O3 Al1 Al2 O10 -1.26(18) . . . . ?
O18 Al1 Al2 O10 178.55(16) . . . . ?
O16 Al1 O1 C1 -94.5(5) . . . . ?
O15 Al1 O1 C1 -125.6(14) . . . . ?
O4 Al1 O1 C1 90.7(5) . . . . ?
O3 Al1 O1 C1 0.4(5) . . . . ?
O18 Al1 O1 C1 174.9(5) . . . . ?
Al2 Al1 O1 C1 -91.6(5) . . . . ?
O10 Al3 O3 C3 -179.0(3) . . . . ?
O11 Al3 O3 C3 -4.8(18) . . . . ?
O6 Al3 O3 C3 2.3(4) . . . . ?
O19 Al3 O3 C3 -86.5(3) . . . . ?
O20 Al3 O3 C3 89.3(3) . . . . ?
O10 Al3 O3 Al1 -3.2(3) . . . . ?
O11 Al3 O3 Al1 171.0(15) . . . . ?
O6 Al3 O3 Al1 178.1(3) . . . . ?
O19 Al3 O3 Al1 89.3(3) . . . . ?
O20 Al3 O3 Al1 -94.9(3) . . . . ?
O16 Al1 O3 C3 139.0(4) . . . . ?
O15 Al1 O3 C3 -141.6(4) . . . . ?
O1 Al1 O3 C3 45.2(4) . . . . ?
O4 Al1 O3 C3 -48.6(4) . . . . ?
O18 Al1 O3 C3 0.0(15) . . . . ?
Al2 Al1 O3 C3 178.6(3) . . . . ?
O16 Al1 O3 Al3 -36.6(3) . . . . ?
O15 Al1 O3 Al3 42.7(3) . . . . ?
O1 Al1 O3 Al3 -130.5(3) . . . . ?
O4 Al1 O3 Al3 135.8(3) . . . . ?
O18 Al1 O3 Al3 -175.7(11) . . . . ?
Al2 Al1 O3 Al3 2.9(3) . . . . ?
O16 Al1 O4 C5 134.0(13) . . . . ?
O15 Al1 O4 C5 104.1(6) . . . . ?
O1 Al1 O4 C5 -80.9(6) . . . . ?
O3 Al1 O4 C5 9.8(6) . . . . ?
O18 Al1 O4 C5 -164.4(6) . . . . ?
Al2 Al1 O4 C5 101.4(5) . . . . ?
O10 Al3 O6 C6 -167(2) . . . . ?
O11 Al3 O6 C6 177.9(4) . . . . ?
O3 Al3 O6 C6 -1.2(4) . . . . ?
O19 Al3 O6 C6 89.8(4) . . . . ?
O20 Al3 O6 C6 -93.7(4) . . . . ?
O16 Al2 O8 C7 -129.2(16) . . . . ?
O15 Al2 O8 C7 -112.5(5) . . . . ?
O13 Al2 O8 C7 73.1(5) . . . . ?
O17 Al2 O8 C7 158.9(5) . . . . ?
O10 Al2 O8 C7 -19.0(5) . . . . ?
Al1 Al2 O8 C7 -107.5(5) . . . . ?
O11 Al3 O10 C9 -1.7(4) . . . . ?
O6 Al3 O10 C9 -17(2) . . . . ?
O3 Al3 O10 C9 177.6(4) . . . . ?
O19 Al3 O10 C9 86.2(4) . . . . ?
O20 Al3 O10 C9 -89.9(4) . . . . ?
O11 Al3 O10 Al2 -177.7(3) . . . . ?
O6 Al3 O10 Al2 167(2) . . . . ?
O3 Al3 O10 Al2 1.6(3) . . . . ?
O19 Al3 O10 Al2 -89.7(3) . . . . ?
O20 Al3 O10 Al2 94.1(3) . . . . ?
O16 Al2 O10 C9 -137.1(4) . . . . ?
O15 Al2 O10 C9 144.6(4) . . . . ?
O13 Al2 O10 C9 -42.4(4) . . . . ?
O8 Al2 O10 C9 49.5(4) . . . . ?
O17 Al2 O10 C9 21(3) . . . . ?
Al1 Al2 O10 C9 -176.0(4) . . . . ?
O16 Al2 O10 Al3 38.8(3) . . . . ?
O15 Al2 O10 Al3 -39.5(3) . . . . ?
O13 Al2 O10 Al3 133.4(3) . . . . ?
O8 Al2 O10 Al3 -134.7(3) . . . . ?
O17 Al2 O10 Al3 -163(2) . . . . ?
Al1 Al2 O10 Al3 -0.2(3) . . . . ?
O10 Al3 O11 C12 0.2(4) . . . . ?
O6 Al3 O11 C12 178.9(4) . . . . ?
O3 Al3 O11 C12 -174.1(15) . . . . ?
O19 Al3 O11 C12 -92.2(4) . . . . ?
O20 Al3 O11 C12 91.6(4) . . . . ?
O16 Al2 O13 C11 102.4(5) . . . . ?
O15 Al2 O13 C11 138.1(12) . . . . ?
O8 Al2 O13 C11 -80.2(5) . . . . ?
O17 Al2 O13 C11 -166.4(5) . . . . ?
O10 Al2 O13 C11 9.6(5) . . . . ?
Al1 Al2 O13 C11 100.4(5) . . . . ?
O16 Al1 O15 Al2 7.7(2) . . . . ?
O1 Al1 O15 Al2 39.4(15) . . . . ?
O4 Al1 O15 Al2 -176.9(2) . . . . ?
O3 Al1 O15 Al2 -86.5(2) . . . . ?
O18 Al1 O15 Al2 98.37(19) . . . . ?
O16 Al2 O15 Al1 -7.67(19) . . . . ?
O13 Al2 O15 Al1 -44.1(13) . . . . ?
O8 Al2 O15 Al1 174.4(2) . . . . ?
O17 Al2 O15 Al1 -99.4(2) . . . . ?
O10 Al2 O15 Al1 84.3(2) . . . . ?
O15 Al1 O16 Al2 -7.8(2) . . . . ?
O1 Al1 O16 Al2 176.62(19) . . . . ?
O4 Al1 O16 Al2 -38.3(14) . . . . ?
O3 Al1 O16 Al2 85.6(2) . . . . ?
O18 Al1 O16 Al2 -99.48(19) . . . . ?
O15 Al2 O16 Al1 7.74(19) . . . . ?
O13 Al2 O16 Al1 -177.6(2) . . . . ?
O8 Al2 O16 Al1 24.7(18) . . . . ?
O17 Al2 O16 Al1 96.3(2) . . . . ?
O10 Al2 O16 Al1 -85.4(2) . . . . ?
Al1 O1 C1 O2 153.7(5) . . . . ?
Al1 O1 C1 C2 -24.9(9) . . . . ?
O2 C1 C2 C3 -170.5(6) . . . . ?
O1 C1 C2 C3 8.1(9) . . . . ?
Al3 O3 C3 C4 -117.7(5) . . . . ?
Al1 O3 C3 C4 65.9(5) . . . . ?
Al3 O3 C3 C2 110.8(5) . . . . ?
Al1 O3 C3 C2 -65.6(6) . . . . ?
Al3 O3 C3 C6 -2.7(5) . . . . ?
Al1 O3 C3 C6 -179.1(3) . . . . ?
C1 C2 C3 O3 36.8(8) . . . . ?
C1 C2 C3 C4 -92.3(7) . . . . ?
C1 C2 C3 C6 153.8(6) . . . . ?
O3 C3 C4 C5 -37.2(8) . . . . ?
C2 C3 C4 C5 91.6(7) . . . . ?
C6 C3 C4 C5 -155.1(6) . . . . ?
Al1 O4 C5 O5 -167.3(5) . . . . ?
Al1 O4 C5 C4 11.9(9) . . . . ?
C3 C4 C5 O5 177.7(6) . . . . ?
C3 C4 C5 O4 -1.6(10) . . . . ?
Al3 O6 C6 O7 -179.1(5) . . . . ?
Al3 O6 C6 C3 -0.1(6) . . . . ?
O3 C3 C6 O7 -179.0(5) . . . . ?
C4 C3 C6 O7 -59.5(7) . . . . ?
C2 C3 C6 O7 62.6(7) . . . . ?
O3 C3 C6 O6 1.9(7) . . . . ?
C4 C3 C6 O6 121.4(6) . . . . ?
C2 C3 C6 O6 -116.5(6) . . . . ?
Al2 O8 C7 O9 -179.7(4) . . . . ?
Al2 O8 C7 C8 4.3(8) . . . . ?
O9 C7 C8 C9 171.3(6) . . . . ?
O8 C7 C8 C9 -12.5(9) . . . . ?
Al3 O10 C9 C8 117.5(4) . . . . ?
Al2 O10 C9 C8 -65.9(5) . . . . ?
Al3 O10 C9 C10 -111.3(4) . . . . ?
Al2 O10 C9 C10 65.3(5) . . . . ?
Al3 O10 C9 C12 2.6(6) . . . . ?
Al2 O10 C9 C12 179.2(4) . . . . ?
C7 C8 C9 O10 43.8(8) . . . . ?
C7 C8 C9 C10 -82.8(8) . . . . ?
C7 C8 C9 C12 161.3(6) . . . . ?
O10 C9 C10 C11 -51.6(7) . . . . ?
C8 C9 C10 C11 75.1(8) . . . . ?
C12 C9 C10 C11 -168.7(5) . . . . ?
Al2 O13 C11 O14 -175.0(4) . . . . ?
Al2 O13 C11 C10 -0.1(8) . . . . ?
C9 C10 C11 O14 -166.1(5) . . . . ?
C9 C10 C11 O13 18.6(9) . . . . ?
Al3 O11 C12 O12 178.6(5) . . . . ?
Al3 O11 C12 C9 1.2(7) . . . . ?
O10 C9 C12 O12 180.0(6) . . . . ?
C8 C9 C12 O12 62.1(7) . . . . ?
C10 C9 C12 O12 -62.9(7) . . . . ?
O10 C9 C12 O11 -2.5(7) . . . . ?
C8 C9 C12 O11 -120.4(6) . . . . ?
C10 C9 C12 O11 114.6(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.31
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.119