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


data_global
_journal_name_full               J.Mater.Chem.
_journal_coden_cambridge         1145

_publ_contact_author_name        'Guojian Ren'
_publ_contact_author_address     
;
Key Lab for Polyoxometalate Science of Ministry of Education
College of Chemistry
Northeast Normal University
Changchun 130024
P.R.China
;
_publ_contact_author_email       rengj974@nenu.edu.cn
_publ_contact_author_phone       +86-431-85099328
_publ_contact_author_fax         +86-431-85099328
loop_
_publ_author_name
'Guojian Ren'
'Shuxia Liu'
'Fengji Ma'
'Feng Wei'
'Qun Tang'
'Yuan Yang'
;
Dadong Liang
;
'Shujun Li'

#===========================================================================
data_p1
_database_code_depnum_ccdc_archive 'CCDC 808418'
#TrackingRef 'p1.cif'

# SQUEEZE RESULTS (APPEND TO CIF)
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 -0.102 -0.043 -0.030 5271 1625 ' '
_platon_squeeze_details          
;
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H18 N3 Ni3 O13'
_chemical_formula_weight         804.54

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'
Ni Ni 0.3393 1.1124 '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           cubic
_symmetry_space_group_name_H-M   'I -4 3 m'

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

_cell_length_a                   21.6623(19)
_cell_length_b                   21.6623(19)
_cell_length_c                   21.6623(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10165.1(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1755
_cell_measurement_theta_min      1.33
_cell_measurement_theta_max      28.35

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.192
_exptl_crystal_density_meas      1.051
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3256
_exptl_absorpt_coefficient_mu    1.145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            31197
_diffrn_reflns_av_R_equivalents  0.1512
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         28.35
_reflns_number_total             2340
_reflns_number_gt                1849
_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 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^)+(0.0235P)^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    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   0.01(2)
_refine_ls_number_reflns         2340
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.0610
_refine_ls_wR_factor_gt          0.0580
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_restrained_S_all      0.903
_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
C1 C 0.70314(13) 0.70314(13) 0.91426(18) 0.0347(9) Uani 1 2 d S . .
C2 C 0.67137(14) 0.74796(14) 0.94634(13) 0.0483(10) Uani 1 1 d . . .
H2 H 0.6397 0.7699 0.9274 0.071(10) Uiso 1 1 calc R . .
C3 C 0.54525(12) 0.7529(2) 0.54525(12) 0.0556(15) Uani 1 2 d S . .
C4 C 0.68688(12) 0.75969(15) 1.00616(13) 0.0448(8) Uani 1 1 d . . .
H4 H 0.6639 0.7890 1.0274 0.19(2) Uiso 1 1 calc R . .
C5 C 0.56149(15) 0.7566(2) 0.48403(15) 0.1017(18) Uani 1 1 d . . .
H5 H 0.6029 0.7591 0.4730 0.066(10) Uiso 1 1 calc R . .
C6 C 0.69189(12) 0.69189(12) 0.84608(17) 0.0273(9) Uani 1 2 d S . .
C7 C 0.59479(12) 0.7453(2) 0.59479(12) 0.0437(12) Uani 1 2 d S . .
N1 N 0.73226(10) 0.73226(10) 1.03583(11) 0.0293(6) Uani 1 2 d S . .
Ni1 Ni 0.618802(18) 0.731960(14) 0.731960(14) 0.01851(10) Uani 1 2 d S . .
O1 O 0.65252(8) 0.72567(10) 0.82121(8) 0.0431(5) Uani 1 1 d . . .
O3 O 0.57662(9) 0.74112(12) 0.64816(9) 0.0658(8) Uani 1 1 d . . .
O2 O 0.69929(11) 0.69929(11) 0.69929(11) 0.0255(10) Uani 1 6 d S . .

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
C1 0.0380(15) 0.0380(15) 0.028(2) -0.0080(14) -0.0080(14) 0.011(2)
C2 0.048(2) 0.068(3) 0.0290(17) -0.0114(15) -0.0172(14) 0.0306(17)
C3 0.0286(15) 0.110(5) 0.0286(15) 0.0023(16) -0.0152(19) 0.0023(16)
C4 0.0436(18) 0.061(2) 0.0297(16) -0.0208(15) -0.0127(13) 0.0263(16)
C5 0.034(2) 0.237(6) 0.035(2) 0.010(3) -0.0127(15) -0.015(3)
C6 0.0304(14) 0.0304(14) 0.021(2) -0.0068(12) -0.0068(12) 0.0025(17)
C7 0.0366(15) 0.058(3) 0.0366(15) -0.0063(13) -0.017(2) -0.0063(13)
N1 0.0346(10) 0.0346(10) 0.0189(15) -0.0015(10) -0.0015(10) 0.0053(19)
Ni1 0.0159(2) 0.01983(15) 0.01983(15) -0.0007(2) -0.00113(13) -0.00113(13)
O1 0.0414(12) 0.0645(15) 0.0232(11) -0.0048(10) -0.0099(8) 0.0278(11)
O3 0.0418(13) 0.134(2) 0.0213(11) -0.0025(14) -0.0109(10) 0.0096(15)
O2 0.0255(10) 0.0255(10) 0.0255(10) 0.0046(12) 0.0046(12) 0.0046(12)

_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
C1 C2 1.378(3) 8 ?
C1 C2 1.378(3) . ?
C1 C6 1.516(5) . ?
C2 C4 1.362(4) . ?
C3 C5 1.374(4) 18 ?
C3 C5 1.374(4) . ?
C3 C7 1.527(5) . ?
C4 N1 1.316(3) . ?
C5 C5 1.395(6) 21_656 ?
C6 O1 1.246(2) 8 ?
C6 O1 1.246(2) . ?
C7 O3 1.225(2) 18 ?
C7 O3 1.225(2) . ?
N1 C4 1.316(3) 8 ?
N1 Ni1 2.105(3) 44_665 ?
Ni1 O2 2.0104(6) . ?
Ni1 O3 2.0419(18) . ?
Ni1 O3 2.0419(18) 16 ?
Ni1 O1 2.0712(17) 16 ?
Ni1 O1 2.0712(17) . ?
Ni1 N1 2.105(3) 37_466 ?
Ni1 Ni1 3.4666(8) 17 ?
Ni1 Ni1 3.4666(8) 8 ?
O2 Ni1 2.0104(6) 17 ?
O2 Ni1 2.0104(6) 8 ?

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
C2 C1 C2 116.7(4) 8 . ?
C2 C1 C6 121.61(18) 8 . ?
C2 C1 C6 121.61(18) . . ?
C4 C2 C1 119.2(3) . . ?
C5 C3 C5 119.4(4) 18 . ?
C5 C3 C7 120.3(2) 18 . ?
C5 C3 C7 120.3(2) . . ?
N1 C4 C2 124.4(3) . . ?
C3 C5 C5 120.08(19) . 21_656 ?
O1 C6 O1 128.1(3) 8 . ?
O1 C6 C1 115.89(17) 8 . ?
O1 C6 C1 115.89(17) . . ?
O3 C7 O3 127.0(4) 18 . ?
O3 C7 C3 116.47(19) 18 . ?
O3 C7 C3 116.47(19) . . ?
C4 N1 C4 115.8(3) 8 . ?
C4 N1 Ni1 121.71(16) 8 44_665 ?
C4 N1 Ni1 121.71(16) . 44_665 ?
O2 Ni1 O3 96.28(10) . . ?
O2 Ni1 O3 96.28(10) . 16 ?
O3 Ni1 O3 88.42(15) . 16 ?
O2 Ni1 O1 89.98(10) . 16 ?
O3 Ni1 O1 90.50(9) . 16 ?
O3 Ni1 O1 173.73(8) 16 16 ?
O2 Ni1 O1 89.98(10) . . ?
O3 Ni1 O1 173.73(8) . . ?
O3 Ni1 O1 90.50(9) 16 . ?
O1 Ni1 O1 89.91(12) 16 . ?
O2 Ni1 N1 178.48(15) . 37_466 ?
O3 Ni1 N1 84.81(9) . 37_466 ?
O3 Ni1 N1 84.81(9) 16 37_466 ?
O1 Ni1 N1 88.95(7) 16 37_466 ?
O1 Ni1 N1 88.95(7) . 37_466 ?
O2 Ni1 Ni1 30.44(2) . 17 ?
O3 Ni1 Ni1 71.81(6) . 17 ?
O3 Ni1 Ni1 112.65(7) 16 17 ?
O1 Ni1 Ni1 72.79(5) 16 17 ?
O1 Ni1 Ni1 114.25(5) . 17 ?
N1 Ni1 Ni1 149.772(9) 37_466 17 ?
O2 Ni1 Ni1 30.44(2) . 8 ?
O3 Ni1 Ni1 112.65(7) . 8 ?
O3 Ni1 Ni1 71.81(6) 16 8 ?
O1 Ni1 Ni1 114.25(5) 16 8 ?
O1 Ni1 Ni1 72.79(5) . 8 ?
N1 Ni1 Ni1 149.772(9) 37_466 8 ?
Ni1 Ni1 Ni1 60.0 17 8 ?
C6 O1 Ni1 133.1(2) . . ?
C7 O3 Ni1 134.6(2) . . ?
Ni1 O2 Ni1 119.12(4) 17 . ?
Ni1 O2 Ni1 119.12(4) 17 8 ?
Ni1 O2 Ni1 119.12(4) . 8 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.046