# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Shuxia Liu'
_publ_contact_author_email       LIUSX@NENU.EDU.CN

_publ_section_title              
;
Microporous Pillared-layer Open Frameworks Based on
Mixed-Ligand Coordination of Nickel Ions
;
loop_
_publ_author_name
'Shuxia Liu.'
'Jianfang Cao.'
'Chaoying Gao.'
'Yuan-Hang Ren.'
;
Zhongming Su
;
'Chunyan Sun.'
'Linhua Xie.'
'Yongcun Zou.'

# Attachment '3.cif'

data_2
_database_code_depnum_ccdc_archive 'CCDC 665814'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H47 N9 Ni2 O11'
_chemical_formula_weight         1055.38

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           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.793(2)
_cell_length_b                   10.091(3)
_cell_length_c                   15.404(4)
_cell_angle_alpha                87.826(4)
_cell_angle_beta                 88.941(5)
_cell_angle_gamma                73.318(4)
_cell_volume                     1308.3(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1273
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      21.70

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             548
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.7574
_exptl_absorpt_correction_T_max  0.9522
_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  '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            7380
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0854
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.32
_diffrn_reflns_theta_max         26.09
_reflns_number_total             5052
_reflns_number_gt                3644
_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^)+(0.0627P)^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_number_reflns         5052
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1271
_refine_ls_wR_factor_gt          0.1195
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_restrained_S_all      0.923
_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
Ni1 Ni 0.94777(5) -0.07877(4) 0.64312(3) 0.02086(15) Uani 1 1 d . . .
O1 O 0.7871(3) -0.1901(2) 0.66471(15) 0.0276(5) Uani 1 1 d . . .
O2 O 0.7257(3) -0.3420(3) 0.58210(19) 0.0512(8) Uani 1 1 d . . .
O3 O 0.9351(3) -0.1135(2) 0.51367(14) 0.0236(5) Uani 1 1 d . . .
O4 O 0.8681(3) -0.0097(2) 0.38405(14) 0.0261(5) Uani 1 1 d . . .
N1 N 0.7637(3) 0.1125(3) 0.64504(18) 0.0260(7) Uani 1 1 d . . .
N2 N 0.1298(3) 0.7296(3) 0.65139(18) 0.0270(7) Uani 1 1 d . . .
N3 N 0.9732(3) -0.0539(3) 0.77574(18) 0.0279(7) Uani 1 1 d . . .
C1 C 0.6255(5) 0.1161(4) 0.6817(3) 0.0464(11) Uani 1 1 d . . .
H1 H 0.6127 0.0348 0.7070 0.056 Uiso 1 1 calc R . .
C2 C 0.4998(5) 0.2343(4) 0.6844(3) 0.0549(13) Uani 1 1 d . . .
H2 H 0.4046 0.2308 0.7103 0.066 Uiso 1 1 calc R . .
C3 C 0.5132(4) 0.3559(4) 0.6494(2) 0.0356(9) Uani 1 1 d . . .
C4 C 0.6563(5) 0.3540(4) 0.6136(3) 0.0656(16) Uani 1 1 d . . .
H4 H 0.6736 0.4354 0.5912 0.079 Uiso 1 1 calc R . .
C5 C 0.7758(5) 0.2304(4) 0.6105(3) 0.0549(13) Uani 1 1 d . . .
H5 H 0.8703 0.2306 0.5824 0.066 Uiso 1 1 calc R . .
C6 C 0.1185(6) 0.6195(4) 0.6087(3) 0.0636(14) Uani 1 1 d . . .
H6 H 0.0256 0.6256 0.5788 0.076 Uiso 1 1 calc R . .
C7 C 0.2415(6) 0.4960(4) 0.6076(3) 0.0637(14) Uani 1 1 d . . .
H7 H 0.2301 0.4217 0.5771 0.076 Uiso 1 1 calc R . .
C8 C 0.3792(4) 0.4845(4) 0.6515(2) 0.0347(9) Uani 1 1 d . . .
C9 C 0.3894(5) 0.5969(4) 0.6945(3) 0.0584(13) Uani 1 1 d . . .
H9 H 0.4813 0.5945 0.7242 0.070 Uiso 1 1 calc R . .
C10 C 0.2608(5) 0.7155(4) 0.6934(3) 0.0471(11) Uani 1 1 d . . .
H10 H 0.2690 0.7899 0.7249 0.056 Uiso 1 1 calc R . .
C11 C 0.9224(7) -0.1255(5) 0.8352(3) 0.0721(17) Uani 1 1 d . . .
H11 H 0.8772 -0.1927 0.8175 0.086 Uiso 1 1 calc R . .
C12 C 0.9316(8) -0.1079(6) 0.9225(3) 0.086(2) Uani 1 1 d . . .
H12 H 0.8932 -0.1633 0.9616 0.103 Uiso 1 1 calc R . .
C13 C 0.9950(5) -0.0118(4) 0.9532(2) 0.0370(9) Uani 1 1 d . . .
C14 C 1.0495(7) 0.0639(5) 0.8911(3) 0.0675(16) Uani 1 1 d . . .
H14 H 1.0954 0.1316 0.9070 0.081 Uiso 1 1 calc R . .
C15 C 1.0356(6) 0.0389(5) 0.8043(3) 0.0643(15) Uani 1 1 d . . .
H15 H 1.0735 0.0920 0.7634 0.077 Uiso 1 1 calc R . .
C16 C 0.7195(4) -0.2235(4) 0.6005(2) 0.0282(8) Uani 1 1 d . . .
C17 C 0.6124(4) -0.1076(3) 0.5461(2) 0.0241(7) Uani 1 1 d . . .
C18 C 0.4498(4) -0.0758(3) 0.5634(2) 0.0279(8) Uani 1 1 d . . .
H18 H 0.4149 -0.1281 0.6061 0.033 Uiso 1 1 calc R . .
C19 C 0.6614(4) -0.0290(3) 0.4797(2) 0.0244(8) Uani 1 1 d . . .
C20 C 0.8353(4) -0.0522(3) 0.4581(2) 0.0213(7) Uani 1 1 d . . .

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 0.0162(2) 0.0212(2) 0.0194(2) -0.00240(16) 0.00035(17) 0.00414(17)
O1 0.0232(13) 0.0279(13) 0.0287(14) 0.0025(11) -0.0013(11) -0.0031(11)
O2 0.0490(18) 0.0301(15) 0.073(2) -0.0006(14) -0.0226(16) -0.0087(14)
O3 0.0179(12) 0.0265(12) 0.0205(13) 0.0000(10) -0.0026(10) 0.0029(10)
O4 0.0188(12) 0.0334(13) 0.0230(13) 0.0003(10) 0.0008(10) -0.0028(11)
N1 0.0186(15) 0.0238(15) 0.0300(17) -0.0048(12) 0.0015(13) 0.0033(12)
N2 0.0179(15) 0.0253(15) 0.0303(17) -0.0062(13) -0.0015(13) 0.0065(13)
N3 0.0296(17) 0.0288(16) 0.0221(16) -0.0016(13) 0.0000(13) -0.0029(14)
C1 0.038(2) 0.028(2) 0.064(3) 0.007(2) 0.020(2) 0.0022(18)
C2 0.029(2) 0.036(2) 0.087(4) 0.007(2) 0.029(2) 0.0075(19)
C3 0.029(2) 0.0246(19) 0.041(2) 0.0016(17) 0.0012(18) 0.0107(17)
C4 0.047(3) 0.029(2) 0.105(4) 0.021(2) 0.033(3) 0.010(2)
C5 0.030(2) 0.030(2) 0.092(4) 0.008(2) 0.028(2) 0.0093(18)
C6 0.049(3) 0.047(3) 0.078(4) -0.023(2) -0.021(3) 0.018(2)
C7 0.059(3) 0.040(3) 0.078(4) -0.022(2) -0.014(3) 0.013(2)
C8 0.024(2) 0.0277(19) 0.043(2) -0.0021(17) 0.0029(18) 0.0072(17)
C9 0.041(3) 0.044(3) 0.073(3) -0.009(2) -0.018(2) 0.017(2)
C10 0.037(2) 0.034(2) 0.060(3) -0.014(2) -0.012(2) 0.0084(19)
C11 0.127(5) 0.093(4) 0.026(2) -0.005(2) -0.002(3) -0.077(4)
C12 0.162(6) 0.111(4) 0.022(2) 0.006(3) 0.003(3) -0.098(5)
C13 0.043(2) 0.045(2) 0.021(2) -0.0059(18) 0.0016(18) -0.010(2)
C14 0.113(5) 0.090(4) 0.026(2) -0.004(2) -0.005(3) -0.070(4)
C15 0.106(4) 0.087(4) 0.022(2) -0.002(2) 0.004(2) -0.064(3)
C16 0.0216(19) 0.0296(19) 0.032(2) 0.0021(16) 0.0008(16) -0.0060(16)
C17 0.0179(17) 0.0278(18) 0.0245(19) -0.0006(14) -0.0057(14) -0.0031(15)
C18 0.0193(18) 0.034(2) 0.028(2) 0.0055(16) 0.0013(15) -0.0043(16)
C19 0.0178(17) 0.0282(18) 0.0252(19) -0.0036(15) -0.0003(15) -0.0031(15)
C20 0.0183(17) 0.0212(16) 0.0228(19) -0.0050(14) -0.0007(14) -0.0025(14)

_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 O3 2.048(2) . ?
Ni1 O1 2.058(2) . ?
Ni1 O4 2.091(2) 2_756 ?
Ni1 N3 2.091(3) . ?
Ni1 N2 2.128(3) 1_645 ?
Ni1 N1 2.134(3) . ?
O1 C16 1.267(4) . ?
O2 C16 1.226(4) . ?
O3 C20 1.250(4) . ?
O4 C20 1.261(4) . ?
O4 Ni1 2.091(2) 2_756 ?
N1 C5 1.317(4) . ?
N1 C1 1.322(4) . ?
N2 C10 1.300(5) . ?
N2 C6 1.342(5) . ?
N2 Ni1 2.128(3) 1_465 ?
N3 C11 1.296(5) . ?
N3 C15 1.307(5) . ?
C1 C2 1.375(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.357(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.360(5) . ?
C3 C8 1.483(4) . ?
C4 C5 1.383(5) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.397(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.371(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.361(6) . ?
C9 C10 1.390(5) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.370(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.353(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.366(5) . ?
C13 C13 1.478(7) 2_757 ?
C14 C15 1.384(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.510(5) . ?
C17 C18 1.395(4) . ?
C17 C19 1.407(4) . ?
C18 C19 1.375(4) 2_656 ?
C18 H18 0.9300 . ?
C19 C18 1.375(4) 2_656 ?
C19 C20 1.511(4) . ?

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 Ni1 O1 87.31(9) . . ?
O3 Ni1 O4 89.61(9) . 2_756 ?
O1 Ni1 O4 172.41(9) . 2_756 ?
O3 Ni1 N3 176.44(10) . . ?
O1 Ni1 N3 93.03(10) . . ?
O4 Ni1 N3 89.62(10) 2_756 . ?
O3 Ni1 N2 86.95(10) . 1_645 ?
O1 Ni1 N2 87.42(10) . 1_645 ?
O4 Ni1 N2 85.48(10) 2_756 1_645 ?
N3 Ni1 N2 89.53(11) . 1_645 ?
O3 Ni1 N1 97.11(10) . . ?
O1 Ni1 N1 91.55(10) . . ?
O4 Ni1 N1 95.72(10) 2_756 . ?
N3 Ni1 N1 86.42(11) . . ?
N2 Ni1 N1 175.76(11) 1_645 . ?
C16 O1 Ni1 119.3(2) . . ?
C20 O3 Ni1 130.3(2) . . ?
C20 O4 Ni1 125.2(2) . 2_756 ?
C5 N1 C1 116.0(3) . . ?
C5 N1 Ni1 124.5(2) . . ?
C1 N1 Ni1 119.5(2) . . ?
C10 N2 C6 116.7(3) . . ?
C10 N2 Ni1 122.1(2) . 1_465 ?
C6 N2 Ni1 121.1(3) . 1_465 ?
C11 N3 C15 115.4(4) . . ?
C11 N3 Ni1 122.4(3) . . ?
C15 N3 Ni1 122.2(3) . . ?
N1 C1 C2 123.2(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 116.6(3) . . ?
C2 C3 C8 121.6(3) . . ?
C4 C3 C8 121.8(3) . . ?
C3 C4 C5 119.6(4) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
N1 C5 C4 123.8(4) . . ?
N1 C5 H5 118.1 . . ?
C4 C5 H5 118.1 . . ?
N2 C6 C7 122.2(4) . . ?
N2 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C8 C7 C6 119.9(4) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C9 C8 C7 117.4(4) . . ?
C9 C8 C3 121.6(4) . . ?
C7 C8 C3 121.0(4) . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N2 C10 C9 124.6(4) . . ?
N2 C10 H10 117.7 . . ?
C9 C10 H10 117.7 . . ?
N3 C11 C12 123.7(4) . . ?
N3 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C13 C12 C11 121.7(4) . . ?
C13 C12 H12 119.2 . . ?
C11 C12 H12 119.2 . . ?
C12 C13 C14 115.1(4) . . ?
C12 C13 C13 123.3(5) . 2_757 ?
C14 C13 C13 121.6(5) . 2_757 ?
C13 C14 C15 119.3(4) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N3 C15 C14 124.7(4) . . ?
N3 C15 H15 117.6 . . ?
C14 C15 H15 117.6 . . ?
O2 C16 O1 125.4(3) . . ?
O2 C16 C17 117.0(3) . . ?
O1 C16 C17 117.4(3) . . ?
C18 C17 C19 117.2(3) . . ?
C18 C17 C16 116.8(3) . . ?
C19 C17 C16 126.0(3) . . ?
C19 C18 C17 123.2(3) 2_656 . ?
C19 C18 H18 118.4 2_656 . ?
C17 C18 H18 118.4 . . ?
C18 C19 C17 119.6(3) 2_656 . ?
C18 C19 C20 119.2(3) 2_656 . ?
C17 C19 C20 121.1(3) . . ?
O3 C20 O4 125.0(3) . . ?
O3 C20 C19 118.2(3) . . ?
O4 C20 C19 116.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        26.09
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.082

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 -0.076 0.461 1.000 545 117 ' '


# Attachment '02-p.cif'

data_02-p
_database_code_depnum_ccdc_archive 'CCDC 666970'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H29 N5 Ni O9'
_chemical_formula_weight         566.21

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           Hexagonal
_symmetry_space_group_name_H-M   P-62c

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

_cell_length_a                   16.6361(8)
_cell_length_b                   16.6361(8)
_cell_length_c                   27.868(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6679.5(8)
_cell_formula_units_Z            12
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       platy
_exptl_crystal_colour            dark-green
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      .
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3552
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.941
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'

_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  '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            22836
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3946
_reflns_number_gt                2789
_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. Contributions of scattering
due to these disordered solvent molecules were removed with the SQUEEZE
routine of PLATON.
;

_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^)+(0.2000P)^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    ?
_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   0.00
_refine_ls_number_reflns         3946
_refine_ls_number_parameters     96
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.1658
_refine_ls_R_factor_gt           0.1472
_refine_ls_wR_factor_ref         0.4438
_refine_ls_wR_factor_gt          0.4233
_refine_ls_goodness_of_fit_ref   1.757
_refine_ls_restrained_S_all      1.751
_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 -0.01263(9) 0.33123(7) 0.37564(4) 0.0216(6) Uani 1 1 d D . .
C1 C -0.1588(9) 0.3369(7) 0.3742(3) 0.0281(18) Uiso 1 1 d . . .
C2 C -0.2486(9) 0.3328(7) 0.3718(4) 0.0281(18) Uiso 1 1 d . . .
C3 C -0.3346(7) 0.2546(9) 0.3692(4) 0.0281(18) Uiso 1 1 d . . .
H3 H -0.3352 0.1988 0.3651 0.034 Uiso 1 1 calc R . .
C4 C 0.0585(10) 0.1939(9) 0.3746(3) 0.0344(18) Uiso 1 1 d . . .
C5 C 0.0286(9) 0.0927(9) 0.3709(4) 0.0344(18) Uiso 1 1 d . . .
C6 C 0.0901(9) 0.0634(9) 0.3700(4) 0.0344(18) Uiso 1 1 d . . .
H6 H 0.1530 0.1072 0.3688 0.041 Uiso 1 1 calc R . .
C7 C 0.2016(9) 0.4754(10) 0.3756(3) 0.0385(19) Uiso 1 1 d . . .
C8 C 0.2702(10) 0.5750(10) 0.3720(4) 0.0385(19) Uiso 1 1 d . . .
C9 C 0.2395(10) 0.6371(10) 0.3719(3) 0.0385(19) Uiso 1 1 d . . .
H9 H 0.1763 0.6173 0.3718 0.046 Uiso 1 1 calc R . .
O1 O -0.0841(6) 0.4120(6) 0.3736(2) 0.033(2) Uiso 1 1 d . . .
O2 O -0.1593(5) 0.2538(5) 0.3765(2) 0.033(2) Uiso 1 1 d . . .
O3 O -0.0038(5) 0.2162(6) 0.3690(2) 0.0291(19) Uiso 1 1 d . . .
O4 O 0.1381(14) 0.2571(15) 0.3767(4) 0.153(7) Uiso 1 1 d . . .
O5 O 0.1130(6) 0.4472(7) 0.3748(2) 0.029(2) Uiso 1 1 d . . .
O6 O 0.2333(12) 0.4188(14) 0.3854(5) 0.156(7) Uiso 1 1 d . . .
N1 N -0.0145(5) 0.3320(4) 0.2984(3) 0.0283(16) Uiso 1 1 d D . .
N2 N -0.0038(5) 0.3337(4) 0.4499(3) 0.0178(14) Uiso 1 1 d D . .
C10 C 0.0100(12) 0.4102(9) 0.2737(3) 0.0283(16) Uiso 0.50 1 d PD . 1
H10 H 0.0272 0.4651 0.2901 0.034 Uiso 0.50 1 calc PR . 1
C11 C -0.0320(12) 0.2563(9) 0.2740(3) 0.0283(16) Uiso 0.50 1 d PD . 1
H11 H -0.0444 0.2027 0.2904 0.034 Uiso 0.50 1 calc PR . 1
C10' C 0.0632(9) 0.3543(12) 0.2741(3) 0.0283(16) Uiso 0.50 1 d PD . 2
H10' H 0.1176 0.3699 0.2907 0.034 Uiso 0.50 1 calc PR . 2
C11' C -0.0924(9) 0.3121(12) 0.2740(3) 0.0283(16) Uiso 0.50 1 d PD . 2
H11' H -0.1463 0.2982 0.2906 0.034 Uiso 0.50 1 calc PR . 2
C12 C -0.0565(11) 0.2537(12) 0.4762(6) 0.0178(14) Uiso 0.50 1 d PD . .
H12 H -0.0931 0.1989 0.4595 0.021 Uiso 0.50 1 calc PR . .
C13 C 0.0543(11) 0.4130(12) 0.4738(6) 0.0178(14) Uiso 0.50 1 d PD . .
H13 H 0.0914 0.4671 0.4567 0.021 Uiso 0.50 1 calc PR . .
C12' C 0.0583(12) 0.3085(10) 0.4799(6) 0.0178(14) Uiso 0.50 1 d PD . .
H12' H 0.0975 0.2919 0.4646 0.021 Uiso 0.50 1 calc PR . .
C13' C -0.0585(12) 0.3556(10) 0.4814(6) 0.0178(14) Uiso 0.50 1 d PD . .
H13' H -0.1011 0.3688 0.4671 0.021 Uiso 0.50 1 calc PR . .

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 0.0039(7) 0.0164(8) 0.0338(11) -0.0104(5) 0.0052(4) -0.0030(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
Ni1 O3 2.000(8) . ?
Ni1 O5 2.014(10) . ?
Ni1 N2 2.074(8) . ?
Ni1 O2 2.115(8) . ?
Ni1 N1 2.153(8) . ?
Ni1 O1 2.196(8) . ?
Ni1 C1 2.480(14) . ?
C1 O1 1.246(13) . ?
C1 O2 1.379(13) . ?
C1 C2 1.463(19) . ?
C2 C3 1.351(14) 2_565 ?
C2 C3 1.373(14) . ?
C3 C2 1.351(14) 3_455 ?
C4 O4 1.21(2) . ?
C4 O3 1.273(15) . ?
C4 C5 1.501(18) . ?
C5 C6 1.335(17) . ?
C5 C6 1.367(17) 2 ?
C6 C5 1.367(17) 3 ?
C7 O5 1.304(16) . ?
C7 O6 1.32(2) . ?
C7 C8 1.47(2) . ?
C8 C9 1.363(19) . ?
C8 C9 1.372(19) 2_665 ?
C9 C8 1.372(19) 3_565 ?
N1 C11 1.330(10) . ?
N1 C10' 1.337(11) . ?
N1 C10 1.342(10) . ?
N1 C11' 1.350(11) . ?
N2 C13 1.358(18) . ?
N2 C12 1.382(18) . ?
N2 C13' 1.437(18) . ?
N2 C12' 1.540(18) . ?
C10 C10 1.318(15) 4 ?
C11 C11 1.335(15) 4 ?
C10' C10' 1.343(15) 4 ?
C11' C11' 1.338(15) 4 ?
C12 C12' 1.22(2) 9_556 ?
C13 C13' 1.25(2) 9_556 ?
C12' C12 1.22(2) 9_556 ?
C12' C12' 2.02(3) 9_556 ?
C13' C13 1.25(2) 9_556 ?
C13' C13' 1.98(3) 9_556 ?

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 Ni1 O5 112.2(3) . . ?
O3 Ni1 N2 94.2(2) . . ?
O5 Ni1 N2 87.9(3) . . ?
O3 Ni1 O2 91.9(3) . . ?
O5 Ni1 O2 155.8(3) . . ?
N2 Ni1 O2 92.8(2) . . ?
O3 Ni1 N1 85.5(2) . . ?
O5 Ni1 N1 89.6(3) . . ?
N2 Ni1 N1 177.2(3) . . ?
O2 Ni1 N1 90.0(2) . . ?
O3 Ni1 O1 154.8(3) . . ?
O5 Ni1 O1 92.0(3) . . ?
N2 Ni1 O1 93.9(2) . . ?
O2 Ni1 O1 63.9(3) . . ?
N1 Ni1 O1 87.5(2) . . ?
O3 Ni1 C1 125.2(3) . . ?
O5 Ni1 C1 122.1(3) . . ?
N2 Ni1 C1 94.4(3) . . ?
O2 Ni1 C1 33.7(3) . . ?
N1 Ni1 C1 88.1(3) . . ?
O1 Ni1 C1 30.1(3) . . ?
O1 C1 O2 120.6(13) . . ?
O1 C1 C2 121.9(11) . . ?
O2 C1 C2 117.5(9) . . ?
O1 C1 Ni1 62.2(7) . . ?
O2 C1 Ni1 58.4(6) . . ?
C2 C1 Ni1 175.5(7) . . ?
C3 C2 C3 111.4(15) 2_565 . ?
C3 C2 C1 121.4(10) 2_565 . ?
C3 C2 C1 127.0(11) . . ?
C2 C3 C2 128.0(15) 3_455 . ?
O4 C4 O3 116.7(16) . . ?
O4 C4 C5 125.5(16) . . ?
O3 C4 C5 117.2(11) . . ?
C6 C5 C6 117.4(13) . 2 ?
C6 C5 C4 121.7(12) . . ?
C6 C5 C4 120.8(12) 2 . ?
C5 C6 C5 122.5(13) . 3 ?
O5 C7 O6 122.0(15) . . ?
O5 C7 C8 120.4(12) . . ?
O6 C7 C8 117.1(14) . . ?
C9 C8 C9 122.3(13) . 2_665 ?
C9 C8 C7 118.6(13) . . ?
C9 C8 C7 119.0(14) 2_665 . ?
C8 C9 C8 117.7(13) . 3_565 ?
C1 O1 Ni1 87.7(8) . . ?
C1 O2 Ni1 87.8(7) . . ?
C4 O3 Ni1 136.7(8) . . ?
C7 O5 Ni1 142.2(8) . . ?
C11 N1 C10' 74.1(9) . . ?
C11 N1 C10 118.1(8) . . ?
C10' N1 C10 71.8(10) . . ?
C11 N1 C11' 77.3(10) . . ?
C10' N1 C11' 119.3(8) . . ?
C10 N1 C11' 76.6(9) . . ?
C11 N1 Ni1 120.2(5) . . ?
C10' N1 Ni1 119.6(5) . . ?
C10 N1 Ni1 121.4(5) . . ?
C11' N1 Ni1 121.1(5) . . ?
C13 N2 C12 118.4(12) . . ?
C13 N2 C13' 71.7(9) . . ?
C12 N2 C13' 75.1(8) . . ?
C13 N2 C12' 75.5(8) . . ?
C12 N2 C12' 68.9(8) . . ?
C13' N2 C12' 109.4(11) . . ?
C13 N2 Ni1 121.2(8) . . ?
C12 N2 Ni1 120.4(8) . . ?
C13' N2 Ni1 124.6(8) . . ?
C12' N2 Ni1 126.0(7) . . ?
C10 C10 N1 120.9(4) 4 . ?
N1 C11 C11 120.8(4) . 4 ?
N1 C10' C10' 120.4(4) . 4 ?
C11' C11' N1 120.2(4) 4 . ?
C12' C12 N2 124.3(17) 9_556 . ?
C13' C13 N2 120.8(17) 9_556 . ?
C12 C12' N2 120.6(16) 9_556 . ?
C12 C12' C12' 55.2(11) 9_556 9_556 ?
N2 C12' C12' 79.5(9) . 9_556 ?
C13 C13' N2 126.3(17) 9_556 . ?
C13 C13' C13' 55.7(11) 9_556 9_556 ?
N2 C13' C13' 81.5(10) . 9_556 ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         5.050
_refine_diff_density_min         -1.528
_refine_diff_density_rms         0.260

# Attachment '2.cif'

data_191
_database_code_depnum_ccdc_archive 'CCDC 700659'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H29 N5 Ni O9'
_chemical_formula_weight         566.19

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           Hexagonal
_symmetry_space_group_name_H-M   P6/mmm

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

_cell_length_a                   9.6103(3)
_cell_length_b                   9.6103(3)
_cell_length_c                   6.9723(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     557.67(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    2347
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      26.47

_exptl_crystal_description       platy
_exptl_crystal_colour            dark-green
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      .
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             296
_exptl_absorpt_coefficient_mu    0.938
_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      183(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            3043
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0114
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         25.87
_reflns_number_total             260
_reflns_number_gt                260
_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^)+(0.0850P)^2^+0.2726P] 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_number_reflns         260
_refine_ls_number_parameters     43
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1237
_refine_ls_wR_factor_gt          0.1237
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_restrained_S_all      1.720
_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 1.0000 0.0000 0.0000 0.0423(8) Uani 1 24 d S . .
N1 N 1.0000 0.0000 0.3005(14) 0.043(2) Uani 1 12 d SD . .
C2 C 0.6573(7) 0.1852(9) 0.0000 0.084(12) Uani 0.33 2 d SPD . 2
O1 O 0.8819(7) 0.1181(9) 0.0000 0.041(3) Uani 0.33 4 d SPR . 2
C1 C 0.7197(7) 0.0702(9) 0.0000 0.092(6) Uani 0.17 2 d SPRD . 2
O2 O 0.7197(7) 0.0702(9) 0.0000 0.092(6) Uani 0.17 2 d SPR . 2
O3 O 0.7629(7) 0.0000(9) 0.0000 0.033(3) Uani 0.33 4 d SPR . 1
C4 C 0.7467(7) 0.2533(9) 0.0000 0.015(5) Uani 0.17 4 d SPRU . 1
C5 C 0.5825(7) 0.1648(9) 0.0000 0.042(12) Uani 0.17 4 d SPR . 1
H5 H 0.5254 0.0507 0.0000 0.051 Uiso 0.17 4 calc SPR . 1
C3 C 0.8296(7) 0.1704(9) 0.0000 0.040(7) Uani 0.17 4 d SPRU . 1
C6 C 1.0694(18) 0.139(4) 0.401(2) 0.056(12) Uani 0.17 2 d SPDU . .
C7 C 1.118(3) 0.118(3) 0.401(2) 0.042(7) Uani 0.17 2 d SPDU . .

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 0.0456(10) 0.0456(10) 0.0358(11) 0.000 0.000 0.0228(5)
N1 0.045(3) 0.045(3) 0.039(4) 0.000 0.000 0.0227(15)
C2 0.16(3) 0.036(10) 0.074(14) 0.000 0.000 0.063(14)
O1 0.031(5) 0.031(5) 0.052(7) 0.000 0.000 0.009(6)
C1 0.093(13) 0.024(6) 0.146(17) 0.000 0.000 0.019(7)
O2 0.093(13) 0.024(6) 0.146(17) 0.000 0.000 0.019(7)
O3 0.020(4) 0.015(6) 0.062(8) 0.000 0.000 0.008(3)
C4 0.012(8) 0.012(8) 0.026(11) 0.000 0.000 0.010(10)
C5 0.04(2) 0.03(2) 0.06(3) 0.000 0.000 0.016(12)
C3 0.045(10) 0.045(10) 0.055(13) 0.000 0.000 0.041(12)
C6 0.059(17) 0.058(15) 0.051(15) 0.004(11) 0.002(6) 0.029(7)
C7 0.041(8) 0.041(8) 0.043(13) 0.001(8) 0.001(8) 0.018(11)

_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 O1 1.966(7) 15_665 ?
Ni1 O1 1.966(7) 14_765 ?
Ni1 O1 1.966(7) 2_545 ?
Ni1 O1 1.966(7) 3_645 ?
Ni1 O1 1.966(7) 13_755 ?
Ni1 O1 1.966(7) . ?
Ni1 N1 2.095(9) . ?
Ni1 N1 2.095(9) 13_755 ?
Ni1 O3 2.278(6) 14_765 ?
Ni1 O3 2.278(6) 2_545 ?
Ni1 O3 2.278(6) 15_665 ?
Ni1 O3 2.278(6) . ?
N1 C7 1.34(2) . ?
N1 C7 1.34(2) 2_545 ?
N1 C7 1.34(2) 6_665 ?
N1 C7 1.34(2) 3_645 ?
N1 C7 1.34(2) 4_755 ?
N1 C7 1.34(2) 5_765 ?
N1 C6 1.35(3) 6_665 ?
N1 C6 1.35(3) . ?
N1 C6 1.35(3) 2_545 ?
N1 C6 1.35(3) 3_645 ?
N1 C6 1.35(3) 5_765 ?
N1 C6 1.35(3) 4_755 ?
C2 C2 1.243(12) 11_655 ?
C2 C1 1.4980 . ?
C2 O2 1.4980 . ?
C2 C2 1.514(13) 7_665 ?
O1 O2 1.3874 . ?
O1 C1 1.3874 . ?
O1 O2 1.387(9) 7_665 ?
O1 C1 1.387(9) 7_665 ?
C1 O2 1.168(15) 8 ?
C1 C1 1.168(15) 8 ?
O2 O2 1.168(15) 8 ?
O2 C1 1.168(15) 8 ?
O3 C3 1.429(8) 2_545 ?
O3 C3 1.4299 . ?
C4 C5 1.3684 . ?
C4 C5 1.369(14) 3_655 ?
C4 C3 1.3791 . ?
C5 C4 1.369(14) 14_665 ?
C5 H5 0.9500 . ?
C3 O3 1.429(8) 15_665 ?
C6 C7 0.594(8) 2_545 ?
C6 C7 0.594(8) . ?
C6 C6 1.16(3) 2_545 ?
C6 C6 1.16(3) 6_665 ?
C6 C6 1.39(3) 16_556 ?
C6 C7 1.505(17) 16_556 ?
C6 C7 1.505(17) 17_546 ?
C6 C7 1.62(2) 3_645 ?
C6 C7 1.62(2) 6_665 ?
C6 C6 1.80(3) 15_666 ?
C6 C6 1.80(3) 17_546 ?
C7 C6 0.594(8) 6_665 ?
C7 C7 1.14(3) 2_545 ?
C7 C7 1.14(3) 6_665 ?
C7 C7 1.38(3) 16_556 ?
C7 C6 1.505(17) 16_556 ?
C7 C6 1.505(17) 15_666 ?
C7 C6 1.62(2) 2_545 ?
C7 C6 1.62(2) 5_765 ?
C7 C7 1.79(3) 17_546 ?
C7 C7 1.79(3) 15_666 ?

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
O1 Ni1 O1 60.0 15_665 14_765 ?
O1 Ni1 O1 120.0 15_665 2_545 ?
O1 Ni1 O1 180.0(5) 14_765 2_545 ?
O1 Ni1 O1 180.0(4) 15_665 3_645 ?
O1 Ni1 O1 120.0 14_765 3_645 ?
O1 Ni1 O1 60.0 2_545 3_645 ?
O1 Ni1 O1 120.0 15_665 13_755 ?
O1 Ni1 O1 60.0 14_765 13_755 ?
O1 Ni1 O1 120.0 2_545 13_755 ?
O1 Ni1 O1 60.0 3_645 13_755 ?
O1 Ni1 O1 60.0 15_665 . ?
O1 Ni1 O1 120.0 14_765 . ?
O1 Ni1 O1 60.0 2_545 . ?
O1 Ni1 O1 120.0 3_645 . ?
O1 Ni1 O1 180.0(2) 13_755 . ?
O1 Ni1 N1 90.000(1) 15_665 . ?
O1 Ni1 N1 90.0 14_765 . ?
O1 Ni1 N1 90.0 2_545 . ?
O1 Ni1 N1 90.000(1) 3_645 . ?
O1 Ni1 N1 90.0 13_755 . ?
O1 Ni1 N1 90.0 . . ?
O1 Ni1 N1 90.000(1) 15_665 13_755 ?
O1 Ni1 N1 90.0 14_765 13_755 ?
O1 Ni1 N1 90.0 2_545 13_755 ?
O1 Ni1 N1 90.000(1) 3_645 13_755 ?
O1 Ni1 N1 90.0 13_755 13_755 ?
O1 Ni1 N1 90.0 . 13_755 ?
N1 Ni1 N1 180.0 . 13_755 ?
O1 Ni1 O3 29.99(9) 15_665 14_765 ?
O1 Ni1 O3 30.01(9) 14_765 14_765 ?
O1 Ni1 O3 149.99(9) 2_545 14_765 ?
O1 Ni1 O3 150.01(9) 3_645 14_765 ?
O1 Ni1 O3 90.01(9) 13_755 14_765 ?
O1 Ni1 O3 89.99(9) . 14_765 ?
N1 Ni1 O3 90.0 . 14_765 ?
N1 Ni1 O3 90.0 13_755 14_765 ?
O1 Ni1 O3 150.01(9) 15_665 2_545 ?
O1 Ni1 O3 149.99(9) 14_765 2_545 ?
O1 Ni1 O3 30.01(9) 2_545 2_545 ?
O1 Ni1 O3 29.99(9) 3_645 2_545 ?
O1 Ni1 O3 89.99(9) 13_755 2_545 ?
O1 Ni1 O3 90.01(9) . 2_545 ?
N1 Ni1 O3 90.0 . 2_545 ?
N1 Ni1 O3 90.0 13_755 2_545 ?
O3 Ni1 O3 180.0(3) 14_765 2_545 ?
O1 Ni1 O3 30.01(9) 15_665 15_665 ?
O1 Ni1 O3 90.01(9) 14_765 15_665 ?
O1 Ni1 O3 89.99(9) 2_545 15_665 ?
O1 Ni1 O3 149.99(9) 3_645 15_665 ?
O1 Ni1 O3 150.01(9) 13_755 15_665 ?
O1 Ni1 O3 29.99(9) . 15_665 ?
N1 Ni1 O3 90.0 . 15_665 ?
N1 Ni1 O3 90.0 13_755 15_665 ?
O3 Ni1 O3 60.0 14_765 15_665 ?
O3 Ni1 O3 120.0 2_545 15_665 ?
O1 Ni1 O3 90.01(9) 15_665 . ?
O1 Ni1 O3 150.01(9) 14_765 . ?
O1 Ni1 O3 29.99(9) 2_545 . ?
O1 Ni1 O3 89.99(9) 3_645 . ?
O1 Ni1 O3 149.99(9) 13_755 . ?
O1 Ni1 O3 30.01(9) . . ?
N1 Ni1 O3 90.0 . . ?
N1 Ni1 O3 90.0 13_755 . ?
O3 Ni1 O3 120.0 14_765 . ?
O3 Ni1 O3 60.0 2_545 . ?
O3 Ni1 O3 60.0 15_665 . ?
C7 N1 C7 50.4(5) . 2_545 ?
C7 N1 C7 50.4(5) . 6_665 ?
C7 N1 C7 95.0(12) 2_545 6_665 ?
C7 N1 C7 95.0(12) . 3_645 ?
C7 N1 C7 50.4(5) 2_545 3_645 ?
C7 N1 C7 116.7(18) 6_665 3_645 ?
C7 N1 C7 116.7(18) . 4_755 ?
C7 N1 C7 95.0(12) 2_545 4_755 ?
C7 N1 C7 95.0(12) 6_665 4_755 ?
C7 N1 C7 50.4(5) 3_645 4_755 ?
C7 N1 C7 95.0(12) . 5_765 ?
C7 N1 C7 116.7(18) 2_545 5_765 ?
C7 N1 C7 50.4(5) 6_665 5_765 ?
C7 N1 C7 95.0(12) 3_645 5_765 ?
C7 N1 C7 50.4(5) 4_755 5_765 ?
C7 N1 C6 25.53(18) . 6_665 ?
C7 N1 C6 74.3(6) 2_545 6_665 ?
C7 N1 C6 25.53(18) 6_665 6_665 ?
C7 N1 C6 111.1(11) 3_645 6_665 ?
C7 N1 C6 111.1(11) 4_755 6_665 ?
C7 N1 C6 74.3(6) 5_765 6_665 ?
C7 N1 C6 25.53(18) . . ?
C7 N1 C6 25.53(18) 2_545 . ?
C7 N1 C6 74.3(6) 6_665 . ?
C7 N1 C6 74.3(6) 3_645 . ?
C7 N1 C6 111.1(11) 4_755 . ?
C7 N1 C6 111.1(11) 5_765 . ?
C6 N1 C6 50.7(6) 6_665 . ?
C7 N1 C6 74.3(6) . 2_545 ?
C7 N1 C6 25.53(18) 2_545 2_545 ?
C7 N1 C6 111.1(11) 6_665 2_545 ?
C7 N1 C6 25.53(18) 3_645 2_545 ?
C7 N1 C6 74.3(6) 4_755 2_545 ?
C7 N1 C6 111.1(11) 5_765 2_545 ?
C6 N1 C6 95.6(13) 6_665 2_545 ?
C6 N1 C6 50.7(6) . 2_545 ?
C7 N1 C6 111.1(11) . 3_645 ?
C7 N1 C6 74.3(6) 2_545 3_645 ?
C7 N1 C6 111.1(11) 6_665 3_645 ?
C7 N1 C6 25.53(18) 3_645 3_645 ?
C7 N1 C6 25.53(18) 4_755 3_645 ?
C7 N1 C6 74.3(6) 5_765 3_645 ?
C6 N1 C6 118(2) 6_665 3_645 ?
C6 N1 C6 95.6(13) . 3_645 ?
C6 N1 C6 50.7(6) 2_545 3_645 ?
C7 N1 C6 74.3(6) . 5_765 ?
C7 N1 C6 111.1(11) 2_545 5_765 ?
C7 N1 C6 25.53(18) 6_665 5_765 ?
C7 N1 C6 111.1(11) 3_645 5_765 ?
C7 N1 C6 74.3(6) 4_755 5_765 ?
C7 N1 C6 25.53(18) 5_765 5_765 ?
C6 N1 C6 50.7(6) 6_665 5_765 ?
C6 N1 C6 95.6(13) . 5_765 ?
C6 N1 C6 118(2) 2_545 5_765 ?
C6 N1 C6 95.6(13) 3_645 5_765 ?
C7 N1 C6 111.1(11) . 4_755 ?
C7 N1 C6 111.1(11) 2_545 4_755 ?
C7 N1 C6 74.3(6) 6_665 4_755 ?
C7 N1 C6 74.3(6) 3_645 4_755 ?
C7 N1 C6 25.53(18) 4_755 4_755 ?
C7 N1 C6 25.53(18) 5_765 4_755 ?
C6 N1 C6 95.6(13) 6_665 4_755 ?
C6 N1 C6 118(2) . 4_755 ?
C6 N1 C6 95.6(13) 2_545 4_755 ?
C6 N1 C6 50.7(6) 3_645 4_755 ?
C6 N1 C6 50.7(6) 5_765 4_755 ?
C2 C2 C1 140.288(1) 11_655 . ?
C2 C2 O2 140.288(1) 11_655 . ?
C1 C2 O2 0.0(3) . . ?
C2 C2 C2 120.0 11_655 7_665 ?
C1 C2 C2 99.712(1) . 7_665 ?
O2 C2 C2 99.712(1) . 7_665 ?
O2 O1 C1 0.0(7) . . ?
O2 O1 O2 93.4(4) . 7_665 ?
C1 O1 O2 93.4(4) . 7_665 ?
O2 O1 C1 93.4(4) . 7_665 ?
C1 O1 C1 93.4(4) . 7_665 ?
O2 O1 C1 0.0(7) 7_665 7_665 ?
O2 O1 Ni1 133.29(19) . . ?
C1 O1 Ni1 133.29(19) . . ?
O2 O1 Ni1 133.3(6) 7_665 . ?
C1 O1 Ni1 133.3(6) 7_665 . ?
O2 C1 C1 0.0(6) 8 8 ?
O2 C1 O1 106.7 8 . ?
C1 C1 O1 106.7 8 . ?
O2 C1 C2 129.7 8 . ?
C1 C1 C2 129.7 8 . ?
O1 C1 C2 123.6 . . ?
O2 O2 C1 0.0(6) 8 8 ?
O2 O2 O1 106.7 8 . ?
C1 O2 O1 106.7 8 . ?
O2 O2 C2 129.7 8 . ?
C1 O2 C2 129.7 8 . ?
O1 O2 C2 123.6 . . ?
C3 O3 C3 165.6(2) 2_545 . ?
C3 O3 Ni1 97.19(14) 2_545 . ?
C3 O3 Ni1 97.18(19) . . ?
C5 C4 C5 125.1(4) . 3_655 ?
C5 C4 C3 117.5 . . ?
C5 C4 C3 117.5(4) 3_655 . ?
C4 C5 C4 114.9(4) . 14_665 ?
C4 C5 H5 122.5 . . ?
C4 C5 H5 122.5 14_665 . ?
C4 C3 O3 127.2(2) . 15_665 ?
C4 C3 O3 127.2 . . ?
O3 C3 O3 105.6(2) 15_665 . ?
C7 C6 C7 147(9) 2_545 . ?
C7 C6 C6 13(4) 2_545 2_545 ?
C7 C6 C6 133(4) . 2_545 ?
C7 C6 C6 133(4) 2_545 6_665 ?
C7 C6 C6 13(4) . 6_665 ?
C6 C6 C6 120.000(7) 2_545 6_665 ?
C7 C6 N1 76(4) 2_545 . ?
C7 C6 N1 76(4) . . ?
C6 C6 N1 64.7(3) 2_545 . ?
C6 C6 N1 64.7(3) 6_665 . ?
C7 C6 C6 90(2) 2_545 16_556 ?
C7 C6 C6 90(2) . 16_556 ?
C6 C6 C6 90.000(4) 2_545 16_556 ?
C6 C6 C6 90.0 6_665 16_556 ?
N1 C6 C6 121.2(10) . 16_556 ?
C7 C6 C7 109(3) 2_545 16_556 ?
C7 C6 C7 67(2) . 16_556 ?
C6 C6 C7 105.7(13) 2_545 16_556 ?
C6 C6 C7 67.4(6) 6_665 16_556 ?
N1 C6 C7 112(2) . 16_556 ?
C6 C6 C7 23.2(4) 16_556 16_556 ?
C7 C6 C7 67(2) 2_545 17_546 ?
C7 C6 C7 109(3) . 17_546 ?
C6 C6 C7 67.4(6) 2_545 17_546 ?
C6 C6 C7 105.7(12) 6_665 17_546 ?
N1 C6 C7 112(2) . 17_546 ?
C6 C6 C7 23.2(4) 16_556 17_546 ?
C7 C6 C7 44.4(11) 16_556 17_546 ?
C7 C6 C7 29(3) 2_545 3_645 ?
C7 C6 C7 118(5) . 3_645 ?
C6 C6 C7 15.4(12) 2_545 3_645 ?
C6 C6 C7 104.6(12) 6_665 3_645 ?
N1 C6 C7 52.5(12) . 3_645 ?
C6 C6 C7 89.9(8) 16_556 3_645 ?
C7 C6 C7 101(2) 16_556 3_645 ?
C7 C6 C7 69.7(12) 17_546 3_645 ?
C7 C6 C7 118(5) 2_545 6_665 ?
C7 C6 C7 29(3) . 6_665 ?
C6 C6 C7 104.6(12) 2_545 6_665 ?
C6 C6 C7 15.4(12) 6_665 6_665 ?
N1 C6 C7 52.5(12) . 6_665 ?
C6 C6 C7 89.9(8) 16_556 6_665 ?
C7 C6 C7 69.7(12) 16_556 6_665 ?
C7 C6 C7 101(2) 17_546 6_665 ?
C7 C6 C7 89(2) 3_645 6_665 ?
C7 C6 C6 116(3) 2_545 15_666 ?
C7 C6 C6 51(2) . 15_666 ?
C6 C6 C6 108.7(3) 2_545 15_666 ?
C6 C6 C6 50.2(9) 6_665 15_666 ?
N1 C6 C6 97.1(11) . 15_666 ?
C6 C6 C6 39.8(9) 16_556 15_666 ?
C7 C6 C6 17.9(6) 16_556 15_666 ?
C7 C6 C6 57.8(10) 17_546 15_666 ?
C7 C6 C6 99.2(10) 3_645 15_666 ?
C7 C6 C6 51.8(7) 6_665 15_666 ?
C7 C6 C6 51(2) 2_545 17_546 ?
C7 C6 C6 116(3) . 17_546 ?
C6 C6 C6 50.2(9) 2_545 17_546 ?
C6 C6 C6 108.7(4) 6_665 17_546 ?
N1 C6 C6 97.1(11) . 17_546 ?
C6 C6 C6 39.8(9) 16_556 17_546 ?
C7 C6 C6 57.8(10) 16_556 17_546 ?
C7 C6 C6 17.9(6) 17_546 17_546 ?
C7 C6 C6 51.8(7) 3_645 17_546 ?
C7 C6 C6 99.2(10) 6_665 17_546 ?
C6 C6 C6 67.4(14) 15_666 17_546 ?
C6 C7 C6 153(9) . 6_665 ?
C6 C7 C7 17(4) . 2_545 ?
C6 C7 C7 137(4) 6_665 2_545 ?
C6 C7 C7 137(4) . 6_665 ?
C6 C7 C7 17(4) 6_665 6_665 ?
C7 C7 C7 120.000(4) 2_545 6_665 ?
C6 C7 N1 78(4) . . ?
C6 C7 N1 78(4) 6_665 . ?
C7 C7 N1 64.8(3) 2_545 . ?
C7 C7 N1 64.8(3) 6_665 . ?
C6 C7 C7 90(2) . 16_556 ?
C6 C7 C7 90(2) 6_665 16_556 ?
C7 C7 C7 90.000(2) 2_545 16_556 ?
C7 C7 C7 90.000(2) 6_665 16_556 ?
N1 C7 C7 121.6(9) . 16_556 ?
C6 C7 C6 67(2) . 16_556 ?
C6 C7 C6 111(3) 6_665 16_556 ?
C7 C7 C6 67.8(6) 2_545 16_556 ?
C7 C7 C6 106.7(13) 6_665 16_556 ?
N1 C7 C6 114(2) . 16_556 ?
C7 C7 C6 23.2(4) 16_556 16_556 ?
C6 C7 C6 111(3) . 15_666 ?
C6 C7 C6 67(2) 6_665 15_666 ?
C7 C7 C6 106.7(13) 2_545 15_666 ?
C7 C7 C6 67.8(6) 6_665 15_666 ?
N1 C7 C6 114(2) . 15_666 ?
C7 C7 C6 23.2(4) 16_556 15_666 ?
C6 C7 C6 45.1(12) 16_556 15_666 ?
C6 C7 C6 31(3) . 2_545 ?
C6 C7 C6 122(5) 6_665 2_545 ?
C7 C7 C6 14.6(12) 2_545 2_545 ?
C7 C7 C6 105.4(12) 6_665 2_545 ?
N1 C7 C6 53.2(11) . 2_545 ?
C7 C7 C6 90.1(8) 16_556 2_545 ?
C6 C7 C6 70.4(11) 16_556 2_545 ?
C6 C7 C6 102(2) 15_666 2_545 ?
C6 C7 C6 122(5) . 5_765 ?
C6 C7 C6 31(3) 6_665 5_765 ?
C7 C7 C6 105.4(12) 2_545 5_765 ?
C7 C7 C6 14.6(12) 6_665 5_765 ?
N1 C7 C6 53.2(11) . 5_765 ?
C7 C7 C6 90.1(8) 16_556 5_765 ?
C6 C7 C6 102(2) 16_556 5_765 ?
C6 C7 C6 70.4(11) 15_666 5_765 ?
C6 C7 C6 91(2) 2_545 5_765 ?
C6 C7 C7 53(2) . 17_546 ?
C6 C7 C7 118(3) 6_665 17_546 ?
C7 C7 C7 50.5(8) 2_545 17_546 ?
C7 C7 C7 108.5(3) 6_665 17_546 ?
N1 C7 C7 97.7(10) . 17_546 ?
C7 C7 C7 39.5(8) 16_556 17_546 ?
C6 C7 C7 18.3(7) 16_556 17_546 ?
C6 C7 C7 58.2(10) 15_666 17_546 ?
C6 C7 C7 52.1(7) 2_545 17_546 ?
C6 C7 C7 99.8(10) 5_765 17_546 ?
C6 C7 C7 118(3) . 15_666 ?
C6 C7 C7 53(2) 6_665 15_666 ?
C7 C7 C7 108.5(3) 2_545 15_666 ?
C7 C7 C7 50.5(8) 6_665 15_666 ?
N1 C7 C7 97.7(10) . 15_666 ?
C7 C7 C7 39.5(8) 16_556 15_666 ?
C6 C7 C7 58.2(10) 16_556 15_666 ?
C6 C7 C7 18.3(7) 15_666 15_666 ?
C6 C7 C7 99.8(10) 2_545 15_666 ?
C6 C7 C7 52.1(7) 5_765 15_666 ?
C7 C7 C7 66.8(12) 17_546 15_666 ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.87
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.065

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 -0.019 0.480 0.500 193 58 ' '