# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
'Wenxu Zheng'
'Wei Yongqin'
'Xueying Xiao'
'Wu Kechen'
_publ_contact_author_name        'Zheng, Wenxu'
_publ_contact_author_email       wkc@fjirsm.ac.cn

data_a
_database_code_depnum_ccdc_archive 'CCDC 842119'
#TrackingRef '- a.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H12 N3 Ni1.50 O10'
_chemical_formula_weight         350.23

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   P3(1)21

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

_cell_length_a                   11.92450(10)
_cell_length_b                   11.92450(10)
_cell_length_c                   16.3020(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2007.48(7)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5263
_cell_measurement_theta_min      3.1836
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1074
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8247
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  Saturn70
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15752
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3077
_reflns_number_gt                2908
_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^)+(0.0860P)^2^+1.1088P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_number_reflns         3077
_refine_ls_number_parameters     168
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1249
_refine_ls_wR_factor_gt          0.1223
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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
Ni1 Ni 0.62675(6) 0.62675(6) 0.0000 0.01644(18) Uani 1 2 d S . .
Ni2 Ni 0.45662(6) 0.50488(5) 0.19226(3) 0.02117(16) Uani 1 1 d . . .
N3 N 0.5745(3) 0.7195(3) 0.07986(19) 0.0182(7) Uani 1 1 d . . .
O1 O 0.4568(3) 0.9319(3) 0.24863(17) 0.0231(6) Uani 1 1 d . . .
O3 O 0.6984(4) 0.8094(3) -0.05657(18) 0.0295(8) Uani 1 1 d . . .
O2 O 0.4303(4) 0.7532(3) 0.3110(2) 0.0371(9) Uani 1 1 d . . .
N1 N 0.5723(4) 0.8952(4) 0.1183(2) 0.0240(8) Uani 1 1 d . . .
O3W O 0.2872(4) 0.4355(4) 0.1248(2) 0.0410(9) Uani 1 1 d . . .
O1W O 0.6270(4) 0.5757(4) 0.2587(3) 0.0485(10) Uani 1 1 d . . .
N2 N 0.5127(4) 0.6909(3) 0.1537(2) 0.0190(7) Uani 1 1 d . . .
C2 C 0.5139(4) 0.8003(4) 0.1750(2) 0.0201(8) Uani 1 1 d . . .
C3 C 0.6065(4) 0.8388(4) 0.0610(2) 0.0211(8) Uani 1 1 d . . .
C1 C 0.4616(5) 0.8265(4) 0.2519(3) 0.0219(9) Uani 1 1 d . . .
O2W O 0.3504(5) 0.5033(4) 0.2894(2) 0.0488(12) Uani 1 1 d . . .
O4 O 0.7192(6) 1.0045(4) -0.0388(3) 0.0611(16) Uani 1 1 d . . .
C4 C 0.6801(6) 0.8908(5) -0.0172(3) 0.0312(11) Uani 1 1 d . . .
O4W O 0.8416(5) 0.8002(6) 0.2089(3) 0.0604(13) Uani 1 1 d . . .
O5W O 0.6347(11) 0.5464(13) 0.4276(5) 0.152(5) Uani 1 1 d . . .
O6W O 0.1371(14) 0.1732(9) 0.0979(7) 0.225(7) Uani 1 1 d . . .
H5WB H 0.6865 0.6278 0.4271 0.269 Uiso 1 1 d R . .
H2WA H 0.3039 0.4562 0.3288 0.269 Uiso 1 1 d R . .
H2WB H 0.4268 0.5313 0.3074 0.269 Uiso 1 1 d R . .
H6WB H 0.1464 0.1964 0.1479 0.269 Uiso 1 1 d R . .
H3WB H 0.3008 0.4888 0.0863 0.269 Uiso 1 1 d R . .
H1WA H 0.6001 0.5950 0.3019 0.269 Uiso 1 1 d R . .
H4WB H 0.8977 0.7861 0.2313 0.269 Uiso 1 1 d R . .
H6WA H 0.0578 0.1414 0.0854 0.269 Uiso 1 1 d R . .
H3WA H 0.2468 0.3623 0.1015 0.269 Uiso 1 1 d R . .
H4WA H 0.8125 0.7462 0.1698 0.269 Uiso 1 1 d R . .
H5WA H 0.6344 0.5057 0.4710 0.269 Uiso 1 1 d R . .
H1WB H 0.6897 0.6498 0.2457 0.269 Uiso 1 1 d 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
Ni1 0.0189(3) 0.0189(3) 0.0156(3) -0.00106(12) 0.00106(12) 0.0125(3)
Ni2 0.0309(3) 0.0170(3) 0.0205(2) 0.0033(2) 0.0051(2) 0.0156(2)
N3 0.0207(17) 0.0181(16) 0.0173(14) 0.0006(12) 0.0046(13) 0.0109(14)
O1 0.0359(18) 0.0172(14) 0.0198(12) 0.0037(11) 0.0088(12) 0.0160(14)
O3 0.044(2) 0.0236(15) 0.0267(14) 0.0052(13) 0.0156(14) 0.0212(15)
O2 0.067(3) 0.0269(18) 0.0248(15) 0.0080(14) 0.0144(17) 0.0293(19)
N1 0.032(2) 0.0164(18) 0.0267(16) 0.0032(14) 0.0062(15) 0.0142(16)
O3W 0.034(2) 0.042(2) 0.0443(19) 0.0038(18) -0.0066(16) 0.0170(18)
O1W 0.051(3) 0.044(2) 0.048(2) 0.0031(19) -0.017(2) 0.022(2)
N2 0.0285(19) 0.0183(17) 0.0159(14) 0.0028(13) 0.0037(14) 0.0160(15)
C2 0.027(2) 0.0148(19) 0.0203(18) 0.0051(15) 0.0070(16) 0.0123(17)
C3 0.025(2) 0.021(2) 0.0204(17) 0.0014(15) 0.0050(16) 0.0131(17)
C1 0.031(2) 0.0168(19) 0.0214(18) -0.0012(15) 0.0026(16) 0.0151(17)
O2W 0.079(3) 0.030(2) 0.045(2) 0.0119(17) 0.035(2) 0.033(2)
O4 0.110(4) 0.031(2) 0.055(2) 0.0234(19) 0.053(3) 0.044(3)
C4 0.049(3) 0.026(2) 0.0237(19) 0.0048(18) 0.013(2) 0.023(2)
O4W 0.053(3) 0.081(4) 0.044(2) -0.008(2) -0.006(2) 0.032(3)
O5W 0.169(9) 0.270(15) 0.101(5) 0.014(7) -0.011(6) 0.172(11)
O6W 0.265(15) 0.098(7) 0.283(14) -0.052(9) -0.186(12) 0.071(9)

_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
Ni1 N3 1.999(3) . ?
Ni1 N3 1.999(3) 6 ?
Ni1 O1 2.090(3) 3_564 ?
Ni1 O1 2.090(3) 5_655 ?
Ni1 O3 2.112(3) 6 ?
Ni1 O3 2.112(3) . ?
Ni2 O2W 2.022(3) . ?
Ni2 N1 2.054(4) 5_655 ?
Ni2 N2 2.068(3) . ?
Ni2 O1W 2.073(4) . ?
Ni2 O3W 2.075(4) . ?
Ni2 O1 2.153(3) 5_655 ?
Ni2 H2WB 1.9642 . ?
N3 C3 1.313(6) . ?
N3 N2 1.364(4) . ?
O1 C1 1.287(5) . ?
O1 Ni1 2.090(3) 2_665 ?
O1 Ni2 2.153(3) 5_665 ?
O3 C4 1.271(6) . ?
O2 C1 1.227(5) . ?
N1 C3 1.329(5) . ?
N1 C2 1.353(5) . ?
N1 Ni2 2.054(4) 5_665 ?
O3W H3WB 0.8493 . ?
O3W H3WA 0.8471 . ?
O1W H1WA 0.8518 . ?
O1W H1WB 0.8509 . ?
N2 C2 1.343(5) . ?
C2 C1 1.502(5) . ?
C3 C4 1.495(6) . ?
O2W H2WA 0.8509 . ?
O2W H2WB 0.8501 . ?
O4 C4 1.244(6) . ?
O4W H4WB 0.8493 . ?
O4W H4WA 0.8478 . ?
O5W H5WB 0.8509 . ?
O5W H5WA 0.8572 . ?
O6W H6WB 0.8498 . ?
O6W H6WA 0.8500 . ?

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
N3 Ni1 N3 166.1(2) . 6 ?
N3 Ni1 O1 105.02(13) . 3_564 ?
N3 Ni1 O1 84.42(12) 6 3_564 ?
N3 Ni1 O1 84.42(12) . 5_655 ?
N3 Ni1 O1 105.02(13) 6 5_655 ?
O1 Ni1 O1 95.73(18) 3_564 5_655 ?
N3 Ni1 O3 92.02(13) . 6 ?
N3 Ni1 O3 77.97(13) 6 6 ?
O1 Ni1 O3 162.29(11) 3_564 6 ?
O1 Ni1 O3 90.60(13) 5_655 6 ?
N3 Ni1 O3 77.97(12) . . ?
N3 Ni1 O3 92.02(13) 6 . ?
O1 Ni1 O3 90.60(13) 3_564 . ?
O1 Ni1 O3 162.29(11) 5_655 . ?
O3 Ni1 O3 88.3(2) 6 . ?
O2W Ni2 N1 94.30(15) . 5_655 ?
O2W Ni2 N2 96.49(14) . . ?
N1 Ni2 N2 168.97(15) 5_655 . ?
O2W Ni2 O1W 94.38(19) . . ?
N1 Ni2 O1W 87.06(16) 5_655 . ?
N2 Ni2 O1W 89.81(16) . . ?
O2W Ni2 O3W 86.04(19) . . ?
N1 Ni2 O3W 93.35(17) 5_655 . ?
N2 Ni2 O3W 89.71(15) . . ?
O1W Ni2 O3W 179.39(18) . . ?
O2W Ni2 O1 170.52(16) . 5_655 ?
N1 Ni2 O1 79.26(13) 5_655 5_655 ?
N2 Ni2 O1 90.30(12) . 5_655 ?
O1W Ni2 O1 92.25(16) . 5_655 ?
O3W Ni2 O1 87.39(14) . 5_655 ?
O2W Ni2 H2WB 24.6 . . ?
N1 Ni2 H2WB 92.8 5_655 . ?
N2 Ni2 H2WB 96.0 . . ?
O1W Ni2 H2WB 69.8 . . ?
O3W Ni2 H2WB 110.6 . . ?
O1 Ni2 H2WB 160.9 5_655 . ?
C3 N3 N2 107.8(3) . . ?
C3 N3 Ni1 116.4(3) . . ?
N2 N3 Ni1 135.8(3) . . ?
C1 O1 Ni1 127.9(3) . 2_665 ?
C1 O1 Ni2 115.0(3) . 5_665 ?
Ni1 O1 Ni2 117.12(13) 2_665 5_665 ?
C4 O3 Ni1 115.6(3) . . ?
C3 N1 C2 102.5(3) . . ?
C3 N1 Ni2 143.8(3) . 5_665 ?
C2 N1 Ni2 112.0(3) . 5_665 ?
Ni2 O3W H3WB 108.1 . . ?
Ni2 O3W H3WA 126.0 . . ?
H3WB O3W H3WA 103.7 . . ?
Ni2 O1W H1WA 96.7 . . ?
Ni2 O1W H1WB 117.7 . . ?
H1WA O1W H1WB 100.3 . . ?
C2 N2 N3 104.1(3) . . ?
C2 N2 Ni2 143.6(3) . . ?
N3 N2 Ni2 112.4(2) . . ?
N2 C2 N1 112.8(4) . . ?
N2 C2 C1 127.9(4) . . ?
N1 C2 C1 119.3(4) . . ?
N3 C3 N1 112.8(4) . . ?
N3 C3 C4 116.2(4) . . ?
N1 C3 C4 130.9(4) . . ?
O2 C1 O1 125.6(4) . . ?
O2 C1 C2 121.2(4) . . ?
O1 C1 C2 113.2(4) . . ?
Ni2 O2W H2WA 142.8 . . ?
Ni2 O2W H2WB 73.9 . . ?
H2WA O2W H2WB 102.5 . . ?
O4 C4 O3 125.2(4) . . ?
O4 C4 C3 121.1(4) . . ?
O3 C4 C3 113.8(4) . . ?
H4WB O4W H4WA 103.7 . . ?
H5WB O5W H5WA 116.8 . . ?
H6WB O6W H6WA 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.986
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.130