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

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#                                CCDC 
# 
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# 
#  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.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H20 Al O10 P3'
_chemical_formula_weight         444.17

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   35.285(3)
_cell_length_b                   35.285(3)
_cell_length_c                   12.398(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13367(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.15
_cell_measurement_theta_max      24.99

_exptl_crystal_description       cubic
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4140
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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            10451
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_sigmaI/netI    0.1108
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.15
_diffrn_reflns_theta_max         24.99
_reflns_number_total             5187
_reflns_number_gt                2985
_reflns_threshold_expression     >2sigma(I)

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

_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^)+(0.0618P)^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         5187
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1495
_refine_ls_wR_factor_gt          0.1223
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_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 0.02308(4) 0.70867(4) 0.25457(9) 0.0235(3) Uani 1 1 d . . .
O1W O -0.00001(9) 0.71804(9) 0.1159(2) 0.0325(7) Uani 1 1 d . . .
H1W H -0.0275 0.7050 0.1259 0.039 Uiso 1 1 d R . .
H2W H -0.0052 0.6992 0.0669 0.039 Uiso 1 1 d R . .
O1 O 0.08201(9) 0.74419(9) 0.5432(2) 0.0332(7) Uani 1 1 d . . .
H1A H 0.0920 0.7618 0.4934 0.050 Uiso 1 1 calc R . .
O2 O 0.04187(9) 0.69684(9) 0.3836(2) 0.0286(7) Uani 1 1 d . . .
O3 O 0.02033(9) 0.66922(9) 0.5748(2) 0.0278(7) Uani 1 1 d . . .
O4 O 0.21548(9) 0.85873(9) 0.2601(2) 0.0322(7) Uani 1 1 d . . .
O5 O 0.19705(9) 0.85023(9) 0.4579(2) 0.0338(8) Uani 1 1 d . . .
H5A H 0.1727 0.8360 0.4309 0.051 Uiso 1 1 calc R . .
O6 O 0.27456(9) 0.89704(9) 0.4000(2) 0.0327(7) Uani 1 1 d . . .
O7 O 0.11867(10) 0.76177(9) 0.0475(2) 0.0392(8) Uani 1 1 d . . .
H7C H 0.1231 0.7767 0.1018 0.059 Uiso 1 1 calc R . .
O8 O 0.07002(9) 0.68870(9) -0.0217(2) 0.0288(7) Uani 1 1 d . . .
O9 O 0.06452(8) 0.70414(9) 0.1742(2) 0.0275(7) Uani 1 1 d . . .
P1 P 0.05678(4) 0.69682(4) 0.49686(8) 0.0258(3) Uani 1 1 d . . .
P2 P 0.23232(4) 0.85723(4) 0.37317(9) 0.0288(3) Uani 1 1 d . . .
P3 P 0.09341(4) 0.71243(4) 0.07884(9) 0.0269(3) Uani 1 1 d . . .
C1 C 0.13243(13) 0.70311(13) 0.4190(3) 0.0267(10) Uani 1 1 d . . .
C2 C 0.17032(13) 0.74282(14) 0.4421(3) 0.0281(10) Uani 1 1 d . . .
C3 C 0.19883(13) 0.76713(13) 0.3576(3) 0.0263(10) Uani 1 1 d . . .
C4 C 0.18845(14) 0.75189(14) 0.2505(3) 0.0275(10) Uani 1 1 d . . .
C5 C 0.15024(13) 0.71181(14) 0.2290(3) 0.0268(10) Uani 1 1 d . . .
C6 C 0.12402(13) 0.68620(13) 0.3140(3) 0.0273(10) Uani 1 1 d . . .
C7 C 0.09655(13) 0.67905(14) 0.5029(3) 0.0310(11) Uani 1 1 d . . .
H7A H 0.1095 0.6847 0.5743 0.037 Uiso 1 1 calc R . .
H7B H 0.0822 0.6478 0.4897 0.037 Uiso 1 1 calc R . .
C8 C 0.18116(15) 0.75854(15) 0.5579(3) 0.0404(12) Uani 1 1 d . . .
H8A H 0.1583 0.7382 0.6046 0.061 Uiso 1 1 calc R . .
H8B H 0.1836 0.7868 0.5642 0.061 Uiso 1 1 calc R . .
H8C H 0.2084 0.7606 0.5780 0.061 Uiso 1 1 calc R . .
C9 C 0.23996(13) 0.81065(13) 0.3814(3) 0.0310(11) Uani 1 1 d . . .
H9A H 0.2626 0.8146 0.3307 0.037 Uiso 1 1 calc R . .
H9B H 0.2502 0.8094 0.4532 0.037 Uiso 1 1 calc R . .
C10 C 0.21845(15) 0.77766(15) 0.1582(4) 0.0441(13) Uani 1 1 d . . .
H10A H 0.2429 0.8040 0.1856 0.066 Uiso 1 1 calc R . .
H10B H 0.2026 0.7850 0.1072 0.066 Uiso 1 1 calc R . .
H10C H 0.2288 0.7603 0.1232 0.066 Uiso 1 1 calc R . .
C11 C 0.13424(14) 0.69791(14) 0.1141(3) 0.0336(11) Uani 1 1 d . . .
H11A H 0.1218 0.6665 0.1072 0.040 Uiso 1 1 calc R . .
H11B H 0.1588 0.7121 0.0647 0.040 Uiso 1 1 calc R . .
C12 C 0.08679(14) 0.64012(14) 0.2953(4) 0.0415(12) Uani 1 1 d . . .
H12A H 0.0852 0.6331 0.2200 0.062 Uiso 1 1 calc R . .
H12B H 0.0598 0.6381 0.3177 0.062 Uiso 1 1 calc R . .
H12C H 0.0918 0.6199 0.3363 0.062 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 0.0225(7) 0.0279(7) 0.0197(6) -0.0001(6) -0.0001(5) 0.0124(6)
O1W 0.0353(18) 0.0396(19) 0.0235(16) -0.0042(14) -0.0033(14) 0.0195(16)
O1 0.0375(19) 0.0335(18) 0.0259(16) -0.0046(14) -0.0020(14) 0.0156(15)
O2 0.0292(17) 0.0380(18) 0.0201(15) 0.0006(13) -0.0036(13) 0.0180(15)
O3 0.0263(17) 0.0359(18) 0.0228(15) 0.0008(13) 0.0021(13) 0.0167(15)
O4 0.0304(17) 0.0308(18) 0.0310(17) 0.0036(14) -0.0019(14) 0.0120(15)
O5 0.0258(17) 0.0328(18) 0.0354(17) -0.0085(14) -0.0041(14) 0.0091(15)
O6 0.0270(17) 0.0262(17) 0.0361(17) -0.0022(14) -0.0032(14) 0.0067(14)
O7 0.047(2) 0.0268(18) 0.0312(17) -0.0036(14) 0.0066(15) 0.0089(16)
O8 0.0273(17) 0.0305(17) 0.0205(15) -0.0022(13) 0.0002(13) 0.0084(14)
O9 0.0267(17) 0.0323(17) 0.0243(15) 0.0011(13) 0.0039(13) 0.0155(14)
P1 0.0247(6) 0.0329(7) 0.0213(6) 0.0009(5) 0.0001(5) 0.0157(6)
P2 0.0274(7) 0.0272(7) 0.0292(6) -0.0036(5) -0.0030(5) 0.0116(6)
P3 0.0246(6) 0.0281(7) 0.0234(6) -0.0020(5) 0.0020(5) 0.0098(6)
C1 0.025(2) 0.029(3) 0.030(2) 0.000(2) 0.000(2) 0.016(2)
C2 0.029(3) 0.029(3) 0.029(2) -0.005(2) -0.002(2) 0.017(2)
C3 0.026(2) 0.025(2) 0.030(2) -0.003(2) -0.002(2) 0.015(2)
C4 0.026(2) 0.033(3) 0.031(2) 0.001(2) 0.000(2) 0.020(2)
C5 0.024(2) 0.028(3) 0.030(2) -0.007(2) -0.003(2) 0.015(2)
C6 0.024(2) 0.024(2) 0.037(3) -0.004(2) -0.003(2) 0.014(2)
C7 0.030(3) 0.034(3) 0.032(2) 0.003(2) -0.001(2) 0.018(2)
C8 0.040(3) 0.046(3) 0.025(2) -0.004(2) -0.005(2) 0.015(3)
C9 0.027(3) 0.031(3) 0.033(3) -0.001(2) -0.002(2) 0.014(2)
C10 0.035(3) 0.047(3) 0.035(3) -0.004(2) 0.009(2) 0.010(3)
C11 0.028(3) 0.037(3) 0.032(3) -0.007(2) 0.000(2) 0.013(2)
C12 0.036(3) 0.034(3) 0.046(3) -0.005(2) 0.003(2) 0.011(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 O9 1.841(3) . ?
Al1 O8 1.848(3) 5_565 ?
Al1 O2 1.857(3) . ?
Al1 O6 1.878(3) 16_565 ?
Al1 O3 1.942(3) 9_454 ?
Al1 O1W 1.999(3) . ?
O1 P1 1.558(3) . ?
O2 P1 1.500(3) . ?
O3 P1 1.511(3) . ?
O3 Al1 1.942(3) 5_565 ?
O4 P2 1.534(3) . ?
O5 P2 1.551(3) . ?
O6 P2 1.487(3) . ?
O6 Al1 1.878(3) 16_565 ?
O7 P3 1.557(3) . ?
O8 P3 1.499(3) . ?
O8 Al1 1.848(3) 9_454 ?
O9 P3 1.491(3) . ?
P1 C7 1.803(4) . ?
P2 C9 1.797(4) . ?
P3 C11 1.808(4) . ?
C1 C2 1.399(5) . ?
C1 C6 1.401(6) . ?
C1 C7 1.526(5) . ?
C2 C3 1.408(6) . ?
C2 C8 1.517(6) . ?
C3 C4 1.410(6) . ?
C3 C9 1.524(6) . ?
C4 C5 1.408(6) . ?
C4 C10 1.515(6) . ?
C5 C6 1.395(6) . ?
C5 C11 1.521(5) . ?
C6 C12 1.512(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
O9 Al1 O8 169.69(13) . 5_565 ?
O9 Al1 O2 93.34(13) . . ?
O8 Al1 O2 96.95(13) 5_565 . ?
O9 Al1 O6 92.04(13) . 16_565 ?
O8 Al1 O6 87.79(13) 5_565 16_565 ?
O2 Al1 O6 94.49(13) . 16_565 ?
O9 Al1 O3 91.63(13) . 9_454 ?
O8 Al1 O3 88.13(13) 5_565 9_454 ?
O2 Al1 O3 87.92(12) . 9_454 ?
O6 Al1 O3 175.49(14) 16_565 9_454 ?
O9 Al1 O1W 87.47(12) . . ?
O8 Al1 O1W 82.21(12) 5_565 . ?
O2 Al1 O1W 176.83(14) . . ?
O6 Al1 O1W 88.55(13) 16_565 . ?
O3 Al1 O1W 89.00(12) 9_454 . ?
P1 O2 Al1 166.22(19) . . ?
P1 O3 Al1 137.53(17) . 5_565 ?
P2 O6 Al1 151.8(2) . 16_565 ?
P3 O8 Al1 145.82(18) . 9_454 ?
P3 O9 Al1 155.05(19) . . ?
O2 P1 O3 114.43(16) . . ?
O2 P1 O1 110.92(16) . . ?
O3 P1 O1 107.54(15) . . ?
O2 P1 C7 111.90(18) . . ?
O3 P1 C7 108.00(17) . . ?
O1 P1 C7 103.37(18) . . ?
O6 P2 O4 113.23(16) . . ?
O6 P2 O5 110.14(16) . . ?
O4 P2 O5 109.34(16) . . ?
O6 P2 C9 108.27(18) . . ?
O4 P2 C9 108.72(18) . . ?
O5 P2 C9 106.94(18) . . ?
O9 P3 O8 114.73(16) . . ?
O9 P3 O7 111.71(16) . . ?
O8 P3 O7 105.36(16) . . ?
O9 P3 C11 108.46(18) . . ?
O8 P3 C11 109.69(18) . . ?
O7 P3 C11 106.58(19) . . ?
C2 C1 C6 120.6(4) . . ?
C2 C1 C7 121.9(4) . . ?
C6 C1 C7 117.1(4) . . ?
C1 C2 C3 119.4(4) . . ?
C1 C2 C8 120.0(4) . . ?
C3 C2 C8 120.6(4) . . ?
C2 C3 C4 119.9(4) . . ?
C2 C3 C9 120.0(4) . . ?
C4 C3 C9 120.1(4) . . ?
C5 C4 C3 119.8(4) . . ?
C5 C4 C10 119.4(4) . . ?
C3 C4 C10 120.8(4) . . ?
C6 C5 C4 120.0(4) . . ?
C6 C5 C11 118.7(4) . . ?
C4 C5 C11 121.1(4) . . ?
C5 C6 C1 119.7(4) . . ?
C5 C6 C12 121.3(4) . . ?
C1 C6 C12 119.0(4) . . ?
C1 C7 P1 110.6(3) . . ?
C3 C9 P2 114.1(3) . . ?
C5 C11 P3 110.8(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O4 0.82 1.78 2.585(4) 168.4 16_565
O5 H5A O4 0.82 1.70 2.504(4) 165.4 16_565
O7 H7C O5 0.82 1.81 2.627(4) 171.8 16_565
O1W H2W O2 0.85 2.53 3.210(4) 138.0 9_454
O1W H2W O3 0.85 2.05 2.818(4) 149.9 5_564

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.070
_database_code_depnum_ccdc_archive 'CCDC 969636'