# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
G.Yanaan
X.Song
J.Li
Y.Han
J.Yu
R.Xu
_publ_contact_author_name        'Jihong Yu'
_publ_contact_author_email       ihong@jlu.edu.cn

data_p-1
_database_code_depnum_ccdc_archive 'CCDC 817744'
#TrackingRef 'p-1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H8 Al3 Fe N4 O16 P4'
_chemical_formula_weight         652.83

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'
N N 0.0061 0.0033 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7558(15)
_cell_length_b                   9.0435(16)
_cell_length_c                   14.117(2)
_cell_angle_alpha                92.266(3)
_cell_angle_beta                 91.932(3)
_cell_angle_gamma                116.719(3)
_cell_volume                     996.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             650
_exptl_absorpt_coefficient_mu    1.303
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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_reflns_number            6435
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.1032
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         26.36
_reflns_number_total             4064
_reflns_number_gt                2623
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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^)+(0.0635P)^2^+5.8137P] 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         4064
_refine_ls_number_parameters     304
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.1789
_refine_ls_wR_factor_gt          0.1548
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.057
_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
Fe1 Fe 0.59148(15) 0.27812(15) 0.23374(8) 0.0209(3) Uani 1 1 d . . .
Al1 Al 1.1403(3) 0.4318(3) 0.40330(15) 0.0109(5) Uani 1 1 d . . .
Al2 Al 0.8083(3) 0.7892(3) 0.24825(15) 0.0096(5) Uani 1 1 d . . .
Al3 Al 0.1291(3) 0.4672(3) 0.12679(15) 0.0112(5) Uani 1 1 d . . .
P1 P 0.9003(2) 0.5937(2) 0.37918(13) 0.0112(4) Uani 1 1 d . . .
P2 P 0.8992(2) 0.1694(2) 0.24986(13) 0.0122(4) Uani 1 1 d . . .
P3 P 0.8334(2) 0.5530(2) 0.09221(13) 0.0117(4) Uani 1 1 d . . .
P4 P 0.4311(2) 0.5467(2) 0.26634(13) 0.0124(4) Uani 1 1 d . . .
O1 O 0.7200(6) 0.1485(7) 0.2407(4) 0.0184(12) Uani 1 1 d . . .
O2 O 0.4610(7) 0.4061(7) 0.2269(4) 0.0186(12) Uani 1 1 d . . .
O3 O 0.7057(7) 0.3812(6) 0.1161(4) 0.0180(12) Uani 1 1 d . . .
O4 O 0.9874(7) 0.2461(7) 0.3479(4) 0.0219(12) Uani 1 1 d . . .
O5 O 1.0688(6) 0.5825(7) 0.3900(4) 0.0199(12) Uani 1 1 d . . .
O6 O 0.8357(7) 0.5978(7) 0.4780(4) 0.0201(12) Uani 1 1 d . . .
O7 O 0.9365(6) 0.7570(6) 0.3353(4) 0.0170(12) Uani 1 1 d . . .
O8 O 0.8043(7) 0.6908(6) 0.1403(3) 0.0158(11) Uani 1 1 d . . .
O9 O 0.8208(7) 0.5700(7) -0.0147(3) 0.0220(13) Uani 1 1 d . . .
O10 O 1.0164(7) 0.5827(7) 0.1210(4) 0.0194(12) Uani 1 1 d . . .
O11 O 0.5981(6) 0.7075(6) 0.2857(4) 0.0156(11) Uani 1 1 d . . .
O12 O 0.3434(6) 0.5062(7) 0.3605(4) 0.0194(12) Uani 1 1 d . . .
O13 O 0.3153(7) 0.5824(7) 0.1966(4) 0.0200(12) Uani 1 1 d . . .
O14 O 0.7690(7) 0.4510(7) 0.3174(4) 0.0195(12) Uani 1 1 d . . .
O15 O 0.8945(7) -0.0005(6) 0.2360(4) 0.0175(12) Uani 1 1 d . . .
O16 O 1.0103(7) 0.2775(7) 0.1740(4) 0.0202(12) Uani 1 1 d . . .
N1 N 0.4108(8) 0.0925(8) 0.1417(5) 0.0211(15) Uani 1 1 d . . .
N2 N 0.3072(10) -0.1154(10) 0.0340(5) 0.038(2) Uani 1 1 d . . .
H2 H 0.2908 -0.2047 0.0020 0.045 Uiso 1 1 calc R . .
N3 N 0.4603(9) 0.1671(9) 0.3531(5) 0.0229(15) Uani 1 1 d . . .
N4 N 0.3771(14) 0.1367(14) 0.4988(6) 0.071(3) Uani 1 1 d . . .
H4 H 0.3697 0.1591 0.5578 0.085 Uiso 1 1 calc R . .
C1 C 0.2949(12) 0.1077(14) 0.0811(7) 0.042(3) Uani 1 1 d . . .
H1 H 0.2658 0.1947 0.0851 0.050 Uiso 1 1 calc R . .
C2 C 0.2287(13) -0.0178(14) 0.0155(7) 0.044(3) Uani 1 1 d . . .
H2A H 0.1463 -0.0354 -0.0327 0.053 Uiso 1 1 calc R . .
C3 C 0.4128(11) -0.0481(11) 0.1098(6) 0.030(2) Uani 1 1 d . . .
H3 H 0.4797 -0.0926 0.1373 0.036 Uiso 1 1 calc R . .
C4 C 0.4776(15) 0.2391(15) 0.4381(7) 0.050(3) Uani 1 1 d . . .
H4A H 0.5523 0.3500 0.4538 0.060 Uiso 1 1 calc R . .
C5 C 0.2917(13) -0.0055(13) 0.4511(7) 0.084(5) Uani 1 1 d U . .
H5 H 0.2086 -0.1014 0.4747 0.101 Uiso 1 1 calc R . .
C6 C 0.3424(13) 0.0092(13) 0.3639(7) 0.086(5) Uani 1 1 d RU . .
H6 H 0.3031 -0.0762 0.3167 0.104 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
Fe1 0.0190(6) 0.0217(7) 0.0226(6) 0.0007(5) 0.0014(5) 0.0096(5)
Al1 0.0094(11) 0.0159(12) 0.0080(10) 0.0012(8) 0.0007(8) 0.0062(9)
Al2 0.0087(11) 0.0109(11) 0.0105(10) 0.0012(8) 0.0012(8) 0.0057(9)
Al3 0.0107(11) 0.0147(11) 0.0097(10) 0.0024(9) 0.0002(8) 0.0070(9)
P1 0.0098(9) 0.0131(10) 0.0106(9) 0.0017(7) -0.0005(7) 0.0050(8)
P2 0.0124(10) 0.0107(10) 0.0144(9) 0.0008(7) -0.0002(7) 0.0060(8)
P3 0.0132(10) 0.0147(10) 0.0100(9) 0.0014(7) 0.0018(7) 0.0086(8)
P4 0.0092(9) 0.0155(10) 0.0138(9) 0.0012(8) 0.0007(7) 0.0068(8)
O1 0.013(3) 0.018(3) 0.025(3) 0.005(2) 0.002(2) 0.008(2)
O2 0.021(3) 0.020(3) 0.019(3) -0.003(2) 0.000(2) 0.013(2)
O3 0.020(3) 0.015(3) 0.019(3) 0.002(2) 0.006(2) 0.008(2)
O4 0.024(3) 0.022(3) 0.019(3) -0.005(2) -0.006(2) 0.011(3)
O5 0.010(3) 0.020(3) 0.029(3) 0.005(2) 0.001(2) 0.006(2)
O6 0.023(3) 0.030(3) 0.011(3) 0.004(2) 0.002(2) 0.015(3)
O7 0.018(3) 0.015(3) 0.017(3) 0.005(2) -0.004(2) 0.006(2)
O8 0.020(3) 0.020(3) 0.014(3) 0.000(2) 0.000(2) 0.015(2)
O9 0.038(3) 0.028(3) 0.006(3) 0.004(2) 0.005(2) 0.020(3)
O10 0.013(3) 0.018(3) 0.027(3) 0.002(2) 0.001(2) 0.007(2)
O11 0.008(3) 0.015(3) 0.022(3) 0.001(2) 0.003(2) 0.004(2)
O12 0.011(3) 0.026(3) 0.020(3) 0.007(2) 0.009(2) 0.007(2)
O13 0.017(3) 0.018(3) 0.023(3) 0.002(2) -0.007(2) 0.007(2)
O14 0.017(3) 0.018(3) 0.020(3) -0.004(2) -0.004(2) 0.005(2)
O15 0.020(3) 0.011(3) 0.022(3) 0.004(2) 0.005(2) 0.007(2)
O16 0.018(3) 0.017(3) 0.024(3) 0.008(2) 0.007(2) 0.005(2)
N1 0.015(3) 0.022(4) 0.025(4) -0.001(3) -0.002(3) 0.008(3)
N2 0.030(5) 0.028(5) 0.033(5) -0.005(4) 0.005(4) -0.006(4)
N3 0.024(4) 0.023(4) 0.019(4) 0.002(3) -0.001(3) 0.009(3)
N4 0.077(8) 0.086(9) 0.028(5) 0.012(5) 0.031(5) 0.016(7)
C1 0.040(6) 0.061(7) 0.036(5) -0.012(5) -0.019(5) 0.036(6)
C2 0.034(6) 0.053(7) 0.041(6) -0.025(5) -0.018(5) 0.019(5)
C3 0.026(5) 0.026(5) 0.036(5) 0.002(4) -0.004(4) 0.010(4)
C4 0.055(7) 0.047(7) 0.030(6) 0.001(5) 0.013(5) 0.007(6)
C5 0.068(7) 0.075(8) 0.050(6) 0.014(6) 0.024(6) -0.022(6)
C6 0.091(8) 0.061(7) 0.054(7) -0.001(6) 0.008(6) -0.013(6)

_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
Fe1 O14 1.950(5) . ?
Fe1 O1 1.959(5) . ?
Fe1 O2 1.961(5) . ?
Fe1 O3 2.006(5) . ?
Fe1 N1 2.075(7) . ?
Fe1 N3 2.096(7) . ?
Al1 O6 1.728(5) 2_766 ?
Al1 O12 1.734(5) 1_655 ?
Al1 O4 1.740(6) . ?
Al1 O5 1.751(6) . ?
Al2 O15 1.721(5) 1_565 ?
Al2 O8 1.726(5) . ?
Al2 O7 1.756(5) . ?
Al2 O11 1.757(5) . ?
Al3 O9 1.717(5) 2_665 ?
Al3 O13 1.732(6) . ?
Al3 O10 1.732(6) 1_455 ?
Al3 O16 1.733(5) 1_455 ?
P1 O14 1.502(5) . ?
P1 O5 1.527(5) . ?
P1 O7 1.527(5) . ?
P1 O6 1.528(5) . ?
P2 O1 1.494(5) . ?
P2 O15 1.523(5) . ?
P2 O16 1.531(5) . ?
P2 O4 1.538(5) . ?
P3 O3 1.511(5) . ?
P3 O8 1.520(5) . ?
P3 O9 1.528(5) . ?
P3 O10 1.537(5) . ?
P4 O2 1.500(5) . ?
P4 O12 1.531(5) . ?
P4 O13 1.534(5) . ?
P4 O11 1.536(5) . ?
O6 Al1 1.728(5) 2_766 ?
O9 Al3 1.717(5) 2_665 ?
O10 Al3 1.732(6) 1_655 ?
O12 Al1 1.734(5) 1_455 ?
O15 Al2 1.721(5) 1_545 ?
O16 Al3 1.733(5) 1_655 ?
N1 C3 1.341(11) . ?
N1 C1 1.363(11) . ?
N2 C3 1.321(11) . ?
N2 C2 1.369(13) . ?
N2 H2 0.8600 . ?
N3 C4 1.313(12) . ?
N3 C6 1.353(11) . ?
N4 C5 1.304(14) . ?
N4 C4 1.323(13) . ?
N4 H4 0.8600 . ?
C1 C2 1.330(13) . ?
C1 H1 0.9300 . ?
C2 H2A 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4A 0.9300 . ?
C5 C6 1.3131 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

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
O14 Fe1 O1 89.1(2) . . ?
O14 Fe1 O2 91.2(2) . . ?
O1 Fe1 O2 179.5(2) . . ?
O14 Fe1 O3 92.9(2) . . ?
O1 Fe1 O3 91.4(2) . . ?
O2 Fe1 O3 88.9(2) . . ?
O14 Fe1 N1 177.5(2) . . ?
O1 Fe1 N1 88.9(2) . . ?
O2 Fe1 N1 90.7(2) . . ?
O3 Fe1 N1 85.6(2) . . ?
O14 Fe1 N3 89.4(2) . . ?
O1 Fe1 N3 90.4(2) . . ?
O2 Fe1 N3 89.3(2) . . ?
O3 Fe1 N3 177.2(2) . . ?
N1 Fe1 N3 92.2(3) . . ?
O6 Al1 O12 105.8(3) 2_766 1_655 ?
O6 Al1 O4 108.6(3) 2_766 . ?
O12 Al1 O4 115.3(3) 1_655 . ?
O6 Al1 O5 110.7(3) 2_766 . ?
O12 Al1 O5 108.2(3) 1_655 . ?
O4 Al1 O5 108.2(3) . . ?
O15 Al2 O8 109.2(3) 1_565 . ?
O15 Al2 O7 107.3(3) 1_565 . ?
O8 Al2 O7 111.8(3) . . ?
O15 Al2 O11 112.0(3) 1_565 . ?
O8 Al2 O11 108.3(3) . . ?
O7 Al2 O11 108.4(3) . . ?
O9 Al3 O13 109.7(3) 2_665 . ?
O9 Al3 O10 109.6(3) 2_665 1_455 ?
O13 Al3 O10 107.6(3) . 1_455 ?
O9 Al3 O16 108.0(3) 2_665 1_455 ?
O13 Al3 O16 110.4(3) . 1_455 ?
O10 Al3 O16 111.7(3) 1_455 1_455 ?
O14 P1 O5 111.5(3) . . ?
O14 P1 O7 109.8(3) . . ?
O5 P1 O7 108.1(3) . . ?
O14 P1 O6 110.7(3) . . ?
O5 P1 O6 108.4(3) . . ?
O7 P1 O6 108.1(3) . . ?
O1 P2 O15 108.7(3) . . ?
O1 P2 O16 111.9(3) . . ?
O15 P2 O16 107.3(3) . . ?
O1 P2 O4 112.4(3) . . ?
O15 P2 O4 108.1(3) . . ?
O16 P2 O4 108.3(3) . . ?
O3 P3 O8 113.6(3) . . ?
O3 P3 O9 109.6(3) . . ?
O8 P3 O9 106.6(3) . . ?
O3 P3 O10 110.1(3) . . ?
O8 P3 O10 108.1(3) . . ?
O9 P3 O10 108.6(3) . . ?
O2 P4 O12 111.4(3) . . ?
O2 P4 O13 110.3(3) . . ?
O12 P4 O13 107.7(3) . . ?
O2 P4 O11 112.5(3) . . ?
O12 P4 O11 106.8(3) . . ?
O13 P4 O11 107.8(3) . . ?
P2 O1 Fe1 141.3(3) . . ?
P4 O2 Fe1 148.5(3) . . ?
P3 O3 Fe1 135.2(3) . . ?
P2 O4 Al1 141.2(4) . . ?
P1 O5 Al1 139.1(4) . . ?
P1 O6 Al1 145.3(4) . 2_766 ?
P1 O7 Al2 126.9(3) . . ?
P3 O8 Al2 144.3(3) . . ?
P3 O9 Al3 148.9(4) . 2_665 ?
P3 O10 Al3 137.5(4) . 1_655 ?
P4 O11 Al2 136.8(3) . . ?
P4 O12 Al1 139.8(4) . 1_455 ?
P4 O13 Al3 136.7(4) . . ?
P1 O14 Fe1 175.3(4) . . ?
P2 O15 Al2 153.9(4) . 1_545 ?
P2 O16 Al3 152.5(4) . 1_655 ?
C3 N1 C1 104.0(7) . . ?
C3 N1 Fe1 127.3(6) . . ?
C1 N1 Fe1 126.4(6) . . ?
C3 N2 C2 107.9(8) . . ?
C3 N2 H2 126.1 . . ?
C2 N2 H2 126.1 . . ?
C4 N3 C6 103.0(8) . . ?
C4 N3 Fe1 126.6(7) . . ?
C6 N3 Fe1 130.4(6) . . ?
C5 N4 C4 105.9(9) . . ?
C5 N4 H4 127.1 . . ?
C4 N4 H4 127.1 . . ?
C2 C1 N1 111.4(9) . . ?
C2 C1 H1 124.3 . . ?
N1 C1 H1 124.3 . . ?
C1 C2 N2 105.6(9) . . ?
C1 C2 H2A 127.2 . . ?
N2 C2 H2A 127.2 . . ?
N2 C3 N1 111.2(8) . . ?
N2 C3 H3 124.4 . . ?
N1 C3 H3 124.4 . . ?
N3 C4 N4 112.5(10) . . ?
N3 C4 H4A 123.7 . . ?
N4 C4 H4A 123.7 . . ?
N4 C5 C6 108.7(6) . . ?
N4 C5 H5 125.7 . . ?
C6 C5 H5 125.7 . . ?
C5 C6 N3 109.9(5) . . ?
C5 C6 H6 125.0 . . ?
N3 C6 H6 125.0 . . ?

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
N2 H2 O3 0.86 2.27 3.101(10) 161.8 2_655
N4 H4 O11 0.86 2.42 3.260(11) 165.4 2_666

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.955
_refine_diff_density_min         -1.238
_refine_diff_density_rms         0.175