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

####################################################################### 
# 
# 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/. 
# 
# 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_130723c
_database_code_depnum_ccdc_archive 'CCDC 974277'
_audit_update_record             
;
2013-11-28 deposited with the CCDC.
2014-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H17 Al N2 O8 P2'
_chemical_formula_weight         322.13

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   8.8966(8)
_cell_length_b                   17.6602(16)
_cell_length_c                   8.3738(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.590(2)
_cell_angle_gamma                90.00
_cell_volume                     1284.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3316
_cell_measurement_theta_min      2.747
_cell_measurement_theta_max      28.289

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8262
_exptl_absorpt_correction_T_max  0.9169
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD 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            6321
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.75
_diffrn_reflns_theta_max         25.02
_reflns_number_total             2258
_reflns_number_gt                1880
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 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)+(0.0380P)²+0.8579P] 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_number_reflns         2258
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0890
_refine_ls_wR_factor_gt          0.0819
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.001
_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 0.23159(8) 0.27633(4) 0.88626(8) 0.01777(19) Uani 1 1 d . . .
N1 N 0.7248(2) 0.13797(12) 0.2657(3) 0.0287(5) Uani 1 1 d . . .
H1 H 0.7811 0.1391 0.1871 0.034 Uiso 1 1 calc R . .
N2 N 0.7626(2) 0.03256(12) 0.8232(2) 0.0266(5) Uani 1 1 d . . .
H2A H 0.8135 0.0705 0.8808 0.040 Uiso 1 1 calc R . .
H2B H 0.7842 -0.0105 0.8788 0.040 Uiso 1 1 calc R . .
H2C H 0.6618 0.0415 0.8053 0.040 Uiso 1 1 calc R . .
O1 O 0.09209(19) 0.23053(9) 0.9670(2) 0.0247(4) Uani 1 1 d . . .
O2 O 0.1288(2) 0.08977(9) 0.9766(2) 0.0280(4) Uani 1 1 d . . .
O3 O 0.1437(2) 0.16200(10) 1.2341(2) 0.0307(4) Uani 1 1 d . . .
O4 O -0.11009(19) 0.14758(10) 1.0376(2) 0.0297(4) Uani 1 1 d . . .
O5 O 0.35207(19) 0.21209(10) 0.8185(2) 0.0263(4) Uani 1 1 d . . .
O6 O 0.34944(19) 0.16793(10) 0.53451(19) 0.0253(4) Uani 1 1 d . . .
O7 O 0.1839(2) 0.10475(10) 0.6936(2) 0.0305(4) Uani 1 1 d . . .
H7 H 0.1733 0.0914 0.7843 0.046 Uiso 1 1 calc R . .
O8 O 0.4727(2) 0.08780(11) 0.7733(2) 0.0367(5) Uani 1 1 d . . .
P1 P 0.06130(7) 0.15606(3) 1.05195(7) 0.01951(18) Uani 1 1 d . . .
P2 P 0.34657(7) 0.14128(4) 0.70902(7) 0.01939(18) Uani 1 1 d . . .
C1 C 0.8146(3) 0.09180(17) 0.4021(3) 0.0370(7) Uani 1 1 d . . .
H1A H 0.9201 0.1098 0.4273 0.044 Uiso 1 1 calc R . .
H1B H 0.8159 0.0397 0.3657 0.044 Uiso 1 1 calc R . .
C2 C 0.7531(4) 0.09356(18) 0.5572(4) 0.0412(7) Uani 1 1 d . . .
H2D H 0.7863 0.1398 0.6169 0.049 Uiso 1 1 calc R . .
H2E H 0.6414 0.0934 0.5288 0.049 Uiso 1 1 calc R . .
C3 C 0.8095(3) 0.02617(15) 0.6647(3) 0.0307(6) Uani 1 1 d . . .
H3A H 0.7672 -0.0199 0.6096 0.037 Uiso 1 1 calc R . .
H3B H 0.9208 0.0233 0.6837 0.037 Uiso 1 1 calc R . .
C4 C 0.5739(4) 0.1035(2) 0.1880(4) 0.0543(9) Uani 1 1 d . . .
H4A H 0.5071 0.1045 0.2638 0.081 Uiso 1 1 calc R . .
H4B H 0.5895 0.0520 0.1583 0.081 Uiso 1 1 calc R . .
H4C H 0.5279 0.1317 0.0918 0.081 Uiso 1 1 calc R . .
C5 C 0.7059(4) 0.21775(16) 0.3118(4) 0.0419(7) Uani 1 1 d . . .
H5A H 0.6421 0.2198 0.3905 0.063 Uiso 1 1 calc R . .
H5B H 0.6584 0.2461 0.2163 0.063 Uiso 1 1 calc R . .
H5C H 0.8050 0.2391 0.3585 0.063 Uiso 1 1 calc R . .

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 0.0217(4) 0.0179(4) 0.0141(4) -0.0002(3) 0.0048(3) -0.0012(3)
N1 0.0331(13) 0.0311(12) 0.0252(12) -0.0002(9) 0.0137(10) -0.0032(10)
N2 0.0263(11) 0.0276(12) 0.0249(11) 0.0024(9) 0.0036(9) 0.0002(9)
O1 0.0268(9) 0.0212(9) 0.0282(10) 0.0021(7) 0.0111(7) -0.0026(7)
O2 0.0430(11) 0.0208(9) 0.0235(9) -0.0009(7) 0.0144(8) 0.0014(8)
O3 0.0421(11) 0.0295(10) 0.0181(9) -0.0043(8) 0.0013(8) -0.0046(8)
O4 0.0251(10) 0.0349(11) 0.0315(10) 0.0016(8) 0.0112(8) -0.0063(8)
O5 0.0241(9) 0.0298(10) 0.0265(9) -0.0081(8) 0.0089(7) -0.0012(7)
O6 0.0290(9) 0.0300(10) 0.0185(9) 0.0065(7) 0.0088(7) 0.0077(7)
O7 0.0334(10) 0.0371(11) 0.0229(9) -0.0044(8) 0.0102(8) -0.0106(8)
O8 0.0410(11) 0.0411(12) 0.0282(10) 0.0078(9) 0.0078(8) 0.0206(9)
P1 0.0234(3) 0.0194(3) 0.0164(3) -0.0011(2) 0.0059(3) -0.0034(2)
P2 0.0222(3) 0.0209(3) 0.0152(3) 0.0013(2) 0.0044(2) 0.0046(2)
C1 0.0408(16) 0.0398(17) 0.0335(16) 0.0064(13) 0.0150(13) 0.0095(13)
C2 0.0524(18) 0.0428(18) 0.0333(16) 0.0102(14) 0.0201(14) 0.0158(14)
C3 0.0355(15) 0.0287(14) 0.0293(14) 0.0009(12) 0.0101(12) 0.0030(12)
C4 0.052(2) 0.067(2) 0.0410(19) -0.0050(17) 0.0040(15) -0.0243(18)
C5 0.0529(19) 0.0298(16) 0.0447(18) 0.0039(14) 0.0144(15) 0.0039(13)

_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 O3 1.7284(18) 4_565 ?
Al1 O1 1.7369(17) . ?
Al1 O5 1.7385(18) . ?
Al1 O6 1.7442(17) 4_566 ?
N1 C5 1.480(3) . ?
N1 C1 1.487(3) . ?
N1 C4 1.488(4) . ?
N1 H1 0.9100 . ?
N2 C3 1.480(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
O1 P1 1.5479(17) . ?
O2 P1 1.5146(17) . ?
O3 P1 1.5450(18) . ?
O3 Al1 1.7284(18) 4_566 ?
O4 P1 1.5106(18) . ?
O5 P2 1.5451(17) . ?
O6 P2 1.5407(17) . ?
O6 Al1 1.7442(17) 4_565 ?
O7 P2 1.5642(18) . ?
O7 H7 0.8200 . ?
O8 P2 1.4755(18) . ?
C1 C2 1.515(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.510(4) . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?

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
O3 Al1 O1 109.48(9) 4_565 . ?
O3 Al1 O5 112.51(9) 4_565 . ?
O1 Al1 O5 111.52(9) . . ?
O3 Al1 O6 105.92(9) 4_565 4_566 ?
O1 Al1 O6 110.82(8) . 4_566 ?
O5 Al1 O6 106.43(9) . 4_566 ?
C5 N1 C1 113.2(2) . . ?
C5 N1 C4 111.2(2) . . ?
C1 N1 C4 113.2(2) . . ?
C5 N1 H1 106.2 . . ?
C1 N1 H1 106.2 . . ?
C4 N1 H1 106.2 . . ?
C3 N2 H2A 109.5 . . ?
C3 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C3 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
P1 O1 Al1 141.95(11) . . ?
P1 O3 Al1 144.26(12) . 4_566 ?
P2 O5 Al1 141.23(11) . . ?
P2 O6 Al1 135.71(11) . 4_565 ?
P2 O7 H7 109.5 . . ?
O4 P1 O2 112.03(10) . . ?
O4 P1 O3 109.79(10) . . ?
O2 P1 O3 108.54(10) . . ?
O4 P1 O1 108.92(10) . . ?
O2 P1 O1 109.84(9) . . ?
O3 P1 O1 107.62(10) . . ?
O8 P2 O6 111.89(10) . . ?
O8 P2 O5 112.24(11) . . ?
O6 P2 O5 108.11(10) . . ?
O8 P2 O7 112.49(11) . . ?
O6 P2 O7 104.72(10) . . ?
O5 P2 O7 106.96(9) . . ?
N1 C1 C2 114.4(2) . . ?
N1 C1 H1A 108.7 . . ?
C2 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
C2 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
C3 C2 C1 111.1(2) . . ?
C3 C2 H2D 109.4 . . ?
C1 C2 H2D 109.4 . . ?
C3 C2 H2E 109.4 . . ?
C1 C2 H2E 109.4 . . ?
H2D C2 H2E 108.0 . . ?
N2 C3 C2 110.7(2) . . ?
N2 C3 H3A 109.5 . . ?
C2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 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
O3 Al1 O1 P1 152.37(17) 4_565 . . . ?
O5 Al1 O1 P1 27.2(2) . . . . ?
O6 Al1 O1 P1 -91.16(19) 4_566 . . . ?
O3 Al1 O5 P2 -72.2(2) 4_565 . . . ?
O1 Al1 O5 P2 51.2(2) . . . . ?
O6 Al1 O5 P2 172.22(17) 4_566 . . . ?
Al1 O3 P1 O4 -104.0(2) 4_566 . . . ?
Al1 O3 P1 O2 133.2(2) 4_566 . . . ?
Al1 O3 P1 O1 14.4(2) 4_566 . . . ?
Al1 O1 P1 O4 -161.94(17) . . . . ?
Al1 O1 P1 O2 -38.9(2) . . . . ?
Al1 O1 P1 O3 79.1(2) . . . . ?
Al1 O6 P2 O8 174.78(15) 4_565 . . . ?
Al1 O6 P2 O5 -61.12(18) 4_565 . . . ?
Al1 O6 P2 O7 52.66(18) 4_565 . . . ?
Al1 O5 P2 O8 -145.48(18) . . . . ?
Al1 O5 P2 O6 90.63(19) . . . . ?
Al1 O5 P2 O7 -21.7(2) . . . . ?
C5 N1 C1 C2 54.3(3) . . . . ?
C4 N1 C1 C2 -73.4(3) . . . . ?
N1 C1 C2 C3 159.2(2) . . . . ?
C1 C2 C3 N2 174.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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/. 
# 
# 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_130723b
_database_code_depnum_ccdc_archive 'CCDC 974278'
_audit_update_record             
;
2013-11-28 deposited with the CCDC.
2014-12-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 H18 Al2 N2 O10 P2'
_chemical_formula_weight         382.11

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   15.5986(13)
_cell_length_b                   9.6662(7)
_cell_length_c                   10.0576(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.048(2)
_cell_angle_gamma                90.00
_cell_volume                     1493.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2761
_cell_measurement_theta_min      2.652
_cell_measurement_theta_max      28.142

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.37
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8032
_exptl_absorpt_correction_T_max  0.8487
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'CCD 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            3621
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         25.02
_reflns_number_total             1301
_reflns_number_gt                1150
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 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)+(0.0561P)²+5.3182P] 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     SHELXL
_refine_ls_extinction_coef       0.0086(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1301
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.1208
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
Al1 Al 0.28613(6) 0.37573(9) 0.34771(8) 0.0214(3) Uani 1 1 d . . .
N1 N 0.03913(18) 0.3009(3) 0.0232(3) 0.0342(7) Uani 1 1 d . . .
H1A H 0.0666 0.3804 0.0509 0.041 Uiso 1 1 calc R . .
H1B H -0.0144 0.3228 -0.0210 0.041 Uiso 1 1 calc R . .
O1 O 0.25769(14) 0.2017(2) 0.3368(2) 0.0281(5) Uani 1 1 d . . .
O2 O 0.24896(17) -0.0528(2) 0.3080(2) 0.0382(7) Uani 1 1 d . . .
O3 O 0.38966(16) 0.0539(3) 0.4103(3) 0.0522(8) Uani 1 1 d . . .
O4 O 0.2649(2) 0.0434(2) 0.5342(2) 0.0473(8) Uani 1 1 d . . .
O5 O 0.39313(14) 0.3936(3) 0.3888(3) 0.0436(7) Uani 1 1 d . . .
H5 H 0.4120 0.3113 0.4018 0.052 Uiso 1 1 d R . .
P1 P 0.29300(5) 0.06300(7) 0.39783(7) 0.0215(3) Uani 1 1 d . . .
C1 C 0.0302(3) 0.2177(4) 0.1432(4) 0.0414(9) Uani 1 1 d . . .
H1C H 0.0858 0.1760 0.1800 0.050 Uiso 1 1 calc R . .
H1D H -0.0114 0.1438 0.1169 0.050 Uiso 1 1 calc R . .
C2 C 0.0000 0.3058(5) 0.2500 0.0403(12) Uani 1 2 d S . .
H2A H -0.0474 0.3647 0.2081 0.048 Uiso 0.50 1 calc PR . .
H2B H 0.0474 0.3647 0.2919 0.048 Uiso 0.50 1 calc PR . .
C3 C 0.0876(3) 0.2309(5) -0.0727(5) 0.0551(11) Uani 1 1 d . . .
H3A H 0.1450 0.2075 -0.0269 0.083 Uiso 1 1 calc R . .
H3B H 0.0917 0.2919 -0.1467 0.083 Uiso 1 1 calc R . .
H3C H 0.0574 0.1481 -0.1064 0.083 Uiso 1 1 calc R . .

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 0.0261(5) 0.0191(5) 0.0177(5) 0.0017(3) -0.0002(3) 0.0000(3)
N1 0.0258(14) 0.0322(15) 0.0425(17) -0.0066(12) 0.0003(12) -0.0022(11)
O1 0.0335(12) 0.0200(11) 0.0280(12) 0.0023(8) -0.0026(9) 0.0003(9)
O2 0.0668(18) 0.0260(12) 0.0220(12) -0.0067(9) 0.0084(11) -0.0124(11)
O3 0.0298(14) 0.0329(14) 0.090(2) 0.0086(13) 0.0004(14) 0.0055(11)
O4 0.092(2) 0.0307(13) 0.0229(13) -0.0002(9) 0.0213(13) 0.0082(13)
O5 0.0172(11) 0.0328(13) 0.0738(19) 0.0047(12) -0.0116(11) -0.0065(9)
P1 0.0292(5) 0.0168(5) 0.0176(4) -0.0014(3) 0.0016(3) 0.0015(3)
C1 0.046(2) 0.0316(18) 0.043(2) -0.0023(15) -0.0024(16) 0.0034(15)
C2 0.045(3) 0.034(3) 0.041(3) 0.000 0.004(2) 0.000
C3 0.048(2) 0.055(3) 0.066(3) -0.015(2) 0.021(2) 0.000(2)

_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 O5 1.657(2) . ?
Al1 O2 1.712(2) 4 ?
Al1 O4 1.728(3) 7_556 ?
Al1 O1 1.738(2) . ?
Al1 H5 2.0415 . ?
N1 C1 1.477(5) . ?
N1 C3 1.488(5) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
O1 P1 1.536(2) . ?
O2 P1 1.525(2) . ?
O2 Al1 1.712(2) 4_545 ?
O3 P1 1.494(3) . ?
O4 P1 1.522(3) . ?
O4 Al1 1.728(3) 7_556 ?
O5 H5 0.8499 . ?
C1 C2 1.509(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 C1 1.509(5) 2 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

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
O5 Al1 O2 109.48(14) . 4 ?
O5 Al1 O4 110.28(15) . 7_556 ?
O2 Al1 O4 109.51(12) 4 7_556 ?
O5 Al1 O1 110.56(12) . . ?
O2 Al1 O1 107.20(11) 4 . ?
O4 Al1 O1 109.74(12) 7_556 . ?
O5 Al1 H5 23.8 . . ?
O2 Al1 H5 120.4 4 . ?
O4 Al1 H5 119.5 7_556 . ?
O1 Al1 H5 86.8 . . ?
C1 N1 C3 114.4(3) . . ?
C1 N1 H1A 108.7 . . ?
C3 N1 H1A 108.7 . . ?
C1 N1 H1B 108.7 . . ?
C3 N1 H1B 108.7 . . ?
H1A N1 H1B 107.6 . . ?
P1 O1 Al1 138.57(14) . . ?
P1 O2 Al1 151.37(16) . 4_545 ?
P1 O4 Al1 143.36(17) . 7_556 ?
Al1 O5 H5 104.4 . . ?
O3 P1 O4 111.21(17) . . ?
O3 P1 O2 110.50(16) . . ?
O4 P1 O2 105.79(14) . . ?
O3 P1 O1 111.80(14) . . ?
O4 P1 O1 109.20(13) . . ?
O2 P1 O1 108.11(13) . . ?
N1 C1 C2 111.1(3) . . ?
N1 C1 H1C 109.4 . . ?
C2 C1 H1C 109.4 . . ?
N1 C1 H1D 109.4 . . ?
C2 C1 H1D 109.4 . . ?
H1C C1 H1D 108.0 . . ?
C1 C2 C1 111.3(4) . 2 ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 2 . ?
C1 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 2 . ?
H2A C2 H2B 108.0 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 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
O5 Al1 O1 P1 27.9(3) . . . . ?
O2 Al1 O1 P1 147.2(2) 4 . . . ?
O4 Al1 O1 P1 -94.0(2) 7_556 . . . ?
Al1 O4 P1 O3 117.7(3) 7_556 . . . ?
Al1 O4 P1 O2 -122.3(3) 7_556 . . . ?
Al1 O4 P1 O1 -6.2(4) 7_556 . . . ?
Al1 O2 P1 O3 -77.4(4) 4_545 . . . ?
Al1 O2 P1 O4 162.1(4) 4_545 . . . ?
Al1 O2 P1 O1 45.2(4) 4_545 . . . ?
Al1 O1 P1 O3 -40.2(3) . . . . ?
Al1 O1 P1 O4 83.3(3) . . . . ?
Al1 O1 P1 O2 -162.0(2) . . . . ?
C3 N1 C1 C2 166.5(3) . . . . ?
N1 C1 C2 C1 166.1(3) . . . 2 ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.077
