Electronic Supplementary Material for CrystEngComm
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Shuxia Liu'
_publ_contact_author_address     
;
Key Laboratory of Polyoxometalates Science of Ministry of Education,
Northeast Normal Universit
College of Chemistry
Changchun City
JiLin
130024
CHINA
;

_publ_contact_author_email       LIUSX@NENU.EDU.CN

_publ_section_title              
;
Design and construction of a microporous metal-organic
framework based on the pillared-layer motif
;
loop_
_publ_author_name
'Shuxia Liu'
'Jianfang Cao'
'Chaoying Gao'
'Yuan-Hang Ren'
;
Chunyan Sun
;
'Linhua Xie'

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 636900'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H99 N15 Ni3 O27'
_chemical_formula_weight         1232.70

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   P-62m

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'

_cell_length_a                   16.634(2)
_cell_length_b                   16.634(2)
_cell_length_c                   11.234(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2691.9(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.760
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             612
_exptl_absorpt_coefficient_mu    0.560
_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      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  'multiwire proportional'
_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            21183
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_sigmaI/netI    0.0372
_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       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1774
_reflns_number_gt                1678
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_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^)+(0.0778P)^2^+0.3251P] 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   0.07(3)
_refine_ls_number_reflns         1774
_refine_ls_number_parameters     114
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0472
_refine_ls_wR_factor_ref         0.1206
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.089
_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
C1 C 0.1742(4) 0.1742(4) 0.0000 0.0287(16) Uani 1 4 d S A .
C2 C 0.0838(4) 0.0838(4) 0.0000 0.0254(15) Uani 1 4 d S . .
C3 C 0.0000 0.0830(4) 0.0000 0.0308(16) Uani 1 4 d S . .
H3 H 0.0000 0.1389 0.0000 0.037 Uiso 1 4 calc SR . .
C4 C 0.5306(3) 0.3923(3) 0.0000 0.0419(14) Uani 1 2 d S A .
C5 C 0.6013(3) 0.3626(4) 0.0000 0.0406(14) Uani 1 2 d S . .
C6 C 0.5724(3) 0.2684(3) 0.0000 0.0423(15) Uani 1 2 d S . .
H6 H 0.5093 0.2249 0.0000 0.051 Uiso 1 2 calc SR . .
C7 C 0.3210(3) 0.3210(3) 0.4342(5) 0.0539(12) Uani 1 2 d SD . .
C8 C 0.2853(10) 0.3625(10) 0.3684(7) 0.115(6) Uani 0.774(12) 1 d PD A 1
H8 H 0.2555 0.3900 0.4066 0.138 Uiso 0.774(12) 1 calc PR A 1
C9 C 0.2910(10) 0.3660(10) 0.2462(7) 0.101(5) Uani 0.774(12) 1 d P A 1
H9 H 0.2716 0.4021 0.2055 0.122 Uiso 0.774(12) 1 calc PR A 1
C10 C 0.3923(15) 0.3923(15) 0.374(3) 0.063(17) Uani 0.151(8) 2 d SPD A 2
H10 H 0.4410 0.4410 0.4145 0.075 Uiso 0.151(8) 2 calc SPR A 2
C11 C 0.3905(14) 0.3905(14) 0.255(3) 0.12(3) Uani 0.151(8) 2 d SPD A 2
H11 H 0.4395 0.4395 0.2154 0.146 Uiso 0.151(8) 2 calc SPR A 2
C12 C 0.2438(14) 0.2709(15) 0.371(2) 0.10(3) Uani 0.151(8) 1 d PD A 2
H12 H 0.1879 0.2344 0.4106 0.116 Uiso 0.151(8) 1 calc PR A 2
C13 C 0.2456(13) 0.2724(14) 0.2505(18) 0.06(2) Uani 0.151(8) 1 d PD A 2
H13 H 0.1899 0.2365 0.2103 0.075 Uiso 0.151(8) 1 calc PR A 2
N1 N 0.3217(2) 0.3217(2) 0.1861(3) 0.0412(8) Uani 1 2 d SD . .
Ni1 Ni 0.31981(4) 0.31981(4) 0.0000 0.0232(2) Uani 1 4 d S . .
O1 O 0.2498(2) 0.17319(19) 0.0000 0.0333(8) Uani 1 2 d S . .
O2 O 0.4492(2) 0.3340(2) 0.0000 0.0415(11) Uani 1 2 d S . .
O3 O 0.5615(3) 0.4786(3) 0.0000 0.104(2) Uani 1 2 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 0.022(2) 0.022(2) 0.034(4) 0.000 0.000 0.005(3)
C2 0.020(2) 0.020(2) 0.035(4) 0.000 0.000 0.009(3)
C3 0.030(4) 0.024(3) 0.041(5) 0.000 0.000 0.0148(18)
C4 0.023(3) 0.022(3) 0.080(4) 0.000 0.000 0.011(2)
C5 0.023(2) 0.020(2) 0.080(4) 0.000 0.000 0.012(2)
C6 0.017(2) 0.015(2) 0.092(5) 0.000 0.000 0.006(2)
C7 0.062(3) 0.062(3) 0.043(3) -0.003(2) -0.003(2) 0.035(3)
C8 0.221(16) 0.176(14) 0.046(4) -0.013(8) -0.004(8) 0.173(14)
C9 0.192(13) 0.148(11) 0.048(4) 0.015(7) 0.014(8) 0.147(11)
C10 0.046(16) 0.046(16) 0.000(14) -0.002(9) -0.002(9) -0.050(17)
C11 0.05(2) 0.05(2) 0.11(5) 0.018(15) 0.018(15) -0.09(3)
C12 0.037(16) 0.08(4) 0.08(2) 0.02(2) 0.018(14) -0.04(2)
C13 0.018(10) 0.08(3) 0.019(11) 0.006(15) 0.003(8) -0.031(19)
N1 0.0452(16) 0.0452(16) 0.039(2) 0.0004(14) 0.0004(14) 0.027(2)
Ni1 0.0151(3) 0.0151(3) 0.0380(4) 0.000 0.000 0.0065(3)
O1 0.0161(18) 0.0252(15) 0.058(2) 0.000 0.000 0.0098(15)
O2 0.0189(17) 0.029(2) 0.079(3) 0.000 0.000 0.0139(16)
O3 0.024(2) 0.021(2) 0.271(7) 0.000 0.000 0.0152(18)

_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 O1 1.267(5) . ?
C1 O1 1.267(5) 7 ?
C1 C2 1.505(8) . ?
C2 C3 1.387(4) 2 ?
C2 C3 1.387(4) . ?
C3 C2 1.387(4) 3 ?
C3 H3 0.9300 . ?
C4 O2 1.209(6) . ?
C4 O3 1.260(6) . ?
C4 C5 1.486(7) . ?
C5 C6 1.390(7) . ?
C5 C6 1.396(6) 2_665 ?
C6 C5 1.396(6) 3_655 ?
C6 H6 0.9300 . ?
C7 C12 1.33(2) 7 ?
C7 C12 1.33(2) . ?
C7 C8 1.337(8) 7 ?
C7 C8 1.337(8) . ?
C7 C10 1.37(3) . ?
C7 C7 1.478(10) 4_556 ?
C8 C9 1.375(11) . ?
C8 H8 0.9300 . ?
C9 N1 1.280(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.33(4) . ?
C10 H10 0.9300 . ?
C11 N1 1.38(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.36(3) . ?
C12 H12 0.9300 . ?
C13 N1 1.33(2) . ?
C13 H13 0.9300 . ?
N1 C9 1.280(7) 7 ?
N1 C13 1.33(2) 7 ?
N1 Ni1 2.090(4) . ?
Ni1 O2 2.045(3) . ?
Ni1 O2 2.045(3) 7 ?
Ni1 N1 2.090(4) 4 ?
Ni1 O1 2.113(3) . ?
Ni1 O1 2.113(3) 7 ?

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 C1 O1 121.3(6) . 7 ?
O1 C1 C2 119.3(3) . . ?
O1 C1 C2 119.3(3) 7 . ?
C3 C2 C3 119.0(6) 2 . ?
C3 C2 C1 120.5(3) 2 . ?
C3 C2 C1 120.5(3) . . ?
C2 C3 C2 121.0(6) 3 . ?
C2 C3 H3 119.5 3 . ?
C2 C3 H3 119.5 . . ?
O2 C4 O3 124.8(5) . . ?
O2 C4 C5 119.2(4) . . ?
O3 C4 C5 116.1(4) . . ?
C6 C5 C6 119.5(5) . 2_665 ?
C6 C5 C4 119.4(4) . . ?
C6 C5 C4 121.1(4) 2_665 . ?
C5 C6 C5 120.5(5) . 3_655 ?
C5 C6 H6 119.8 . . ?
C5 C6 H6 119.8 3_655 . ?
C12 C7 C12 34.1(14) 7 . ?
C12 C7 C8 59.4(10) 7 7 ?
C12 C7 C8 88.8(10) . 7 ?
C12 C7 C8 88.8(10) 7 . ?
C12 C7 C8 59.4(10) . . ?
C8 C7 C8 112.7(7) 7 . ?
C12 C7 C10 115.2(15) 7 . ?
C12 C7 C10 115.2(15) . . ?
C8 C7 C10 72.2(9) 7 . ?
C8 C7 C10 72.2(9) . . ?
C12 C7 C7 122.1(10) 7 4_556 ?
C12 C7 C7 122.1(10) . 4_556 ?
C8 C7 C7 123.6(4) 7 4_556 ?
C8 C7 C7 123.6(4) . 4_556 ?
C10 C7 C7 119.8(13) . 4_556 ?
C7 C8 C9 122.4(6) . . ?
C7 C8 H8 118.8 . . ?
C9 C8 H8 118.8 . . ?
N1 C9 C8 122.8(6) . . ?
N1 C9 H9 118.6 . . ?
C8 C9 H9 118.6 . . ?
C11 C10 C7 118(2) . . ?
C11 C10 H10 120.8 . . ?
C7 C10 H10 120.8 . . ?
C10 C11 N1 125(2) . . ?
C10 C11 H11 117.3 . . ?
N1 C11 H11 117.3 . . ?
C7 C12 C13 121.0(17) . . ?
C7 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
N1 C13 C12 124.1(16) . . ?
N1 C13 H13 117.9 . . ?
C12 C13 H13 117.9 . . ?
C9 N1 C9 115.3(7) 7 . ?
C9 N1 C13 62.3(10) 7 7 ?
C9 N1 C13 91.6(9) . 7 ?
C9 N1 C13 91.6(9) 7 . ?
C9 N1 C13 62.3(10) . . ?
C13 N1 C13 33.8(14) 7 . ?
C9 N1 C11 68.4(9) 7 . ?
C9 N1 C11 68.4(9) . . ?
C13 N1 C11 110.2(15) 7 . ?
C13 N1 C11 110.2(15) . . ?
C9 N1 Ni1 121.9(3) 7 . ?
C9 N1 Ni1 121.9(3) . . ?
C13 N1 Ni1 122.2(9) 7 . ?
C13 N1 Ni1 122.2(9) . . ?
C11 N1 Ni1 125.0(13) . . ?
O2 Ni1 O2 108.57(19) . 7 ?
O2 Ni1 N1 89.49(6) . . ?
O2 Ni1 N1 89.49(6) 7 . ?
O2 Ni1 N1 89.49(6) . 4 ?
O2 Ni1 N1 89.49(6) 7 4 ?
N1 Ni1 N1 178.3(2) . 4 ?
O2 Ni1 O1 94.21(14) . . ?
O2 Ni1 O1 157.22(13) 7 . ?
N1 Ni1 O1 90.75(8) . . ?
N1 Ni1 O1 90.75(8) 4 . ?
O2 Ni1 O1 157.22(13) . 7 ?
O2 Ni1 O1 94.21(14) 7 7 ?
N1 Ni1 O1 90.75(8) . 7 ?
N1 Ni1 O1 90.75(8) 4 7 ?
O1 Ni1 O1 63.0(2) . 7 ?
C1 O1 Ni1 87.8(3) . . ?
C4 O2 Ni1 141.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.079


data_compound1
_database_code_depnum_ccdc_archive 'CCDC 636901'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H17 N2 Ni O8'
_chemical_formula_weight         412.02

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   P6(3)/mcm

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

_cell_length_a                   16.609(2)
_cell_length_b                   16.609(2)
_cell_length_c                   14.325(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3422.2(10)
_cell_formula_units_Z            6
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       hexagon
_exptl_crystal_colour            yellow-green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1278
_exptl_absorpt_coefficient_mu    0.886
_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      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  'multiwire proportional'
_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            25128
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1115
_reflns_number_gt                992
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_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^)+(0.0726P)^2^+3.5333P] 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         1115
_refine_ls_number_parameters     84
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.1469
_refine_ls_wR_factor_gt          0.1416
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_restrained_S_all      1.193
_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 0.67976(4) 0.0000 0.2500 0.0383(4) Uani 1 4 d S . .
C1 C 0.8257(4) 0.0000 0.2500 0.0324(14) Uani 1 4 d S . .
C2 C 0.9166(3) 0.0000 0.2500 0.0261(12) Uani 1 4 d S . .
C3 C 1.0000 0.0836(3) 0.2500 0.0291(13) Uani 1 4 d S . .
H3 H 1.0000 0.1396 0.2500 0.035 Uiso 1 4 calc SR . .
C4 C 0.6091(3) 0.1377(3) 0.2500 0.0413(12) Uani 1 2 d S . .
C5 C 0.6389(3) 0.2398(3) 0.2500 0.0342(11) Uani 1 2 d S . .
C6 C 0.7319(3) 0.3056(3) 0.2500 0.0384(11) Uani 1 2 d S . .
H6 H 0.7762 0.2869 0.2500 0.046 Uiso 1 2 calc SR . .
C7 C 0.6728(7) -0.0298(7) 0.0593(11) 0.078(3) Uani 0.50 1 d P . .
H7 H 0.6532 -0.0851 0.0270 0.093 Uiso 0.50 1 calc PR . .
C8 C 0.7439(13) 0.0835(12) -0.1089(11) 0.288(9) Uani 1 1 d . . .
H8A H 0.7315 0.0631 -0.1727 0.431 Uiso 1 1 calc R . .
H8B H 0.8090 0.1093 -0.0961 0.431 Uiso 1 1 calc R . .
H8C H 0.7266 0.1300 -0.0985 0.431 Uiso 1 1 calc R . .
N1 N 0.6869(6) 0.0000 -0.0436(7) 0.153(5) Uani 1 2 d S . .
O1 O 0.8259(2) 0.0752(2) 0.2500 0.0509(10) Uani 1 2 d S . .
O2 O 0.6676(2) 0.1148(2) 0.2500 0.0873(19) Uani 1 2 d S . .
O3 O 0.5236(2) 0.0829(2) 0.2500 0.0866(19) Uani 1 2 d S . .
O4 O 0.6741(6) 0.0000 0.1144(6) 0.141(4) Uani 1 2 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
Ni1 0.0173(4) 0.0187(4) 0.0792(7) 0.000 0.000 0.0094(2)
C1 0.026(2) 0.024(3) 0.047(4) 0.000 0.000 0.0118(15)
C2 0.019(2) 0.018(3) 0.041(3) 0.000 0.000 0.0092(13)
C3 0.031(3) 0.023(2) 0.036(3) 0.000 0.000 0.0154(16)
C4 0.024(2) 0.022(2) 0.077(3) 0.000 0.000 0.0109(19)
C5 0.021(2) 0.019(2) 0.064(3) 0.000 0.000 0.0103(16)
C6 0.022(2) 0.024(2) 0.073(3) 0.000 0.000 0.0139(18)
C7 0.048(5) 0.053(6) 0.131(11) -0.007(6) -0.010(7) 0.024(4)
C8 0.33(2) 0.35(2) 0.153(14) 0.040(11) 0.051(12) 0.139(18)
N1 0.143(6) 0.268(15) 0.089(6) 0.000 -0.019(4) 0.134(8)
O1 0.0217(16) 0.0249(16) 0.110(3) 0.000 0.000 0.0146(13)
O2 0.0269(19) 0.0194(17) 0.220(6) 0.000 0.000 0.0146(15)
O3 0.026(2) 0.0177(17) 0.215(6) 0.000 0.000 0.0098(15)
O4 0.156(7) 0.200(11) 0.081(5) 0.000 -0.037(4) 0.100(5)

_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 O4 1.945(8) . ?
Ni1 O4 1.945(8) 16_556 ?
Ni1 O2 2.015(3) 8 ?
Ni1 O2 2.015(3) . ?
Ni1 O1 2.102(3) . ?
Ni1 O1 2.102(3) 8 ?
C1 O1 1.248(4) 8 ?
C1 O1 1.248(4) . ?
C1 C2 1.509(8) . ?
C2 C3 1.387(4) . ?
C2 C3 1.387(4) 2_645 ?
C3 C2 1.387(4) 3_765 ?
C4 O2 1.207(5) . ?
C4 O3 1.246(6) . ?
C4 C5 1.510(5) . ?
C5 C6 1.376(6) . ?
C5 C6 1.379(6) 3_665 ?
C6 C5 1.379(6) 2_655 ?
C7 C7 0.86(2) 23 ?
C7 O4 0.926(14) . ?
C7 N1 1.535(16) . ?
C8 N1 1.543(15) . ?
N1 C7 1.535(16) 23 ?
N1 C8 1.543(15) 23 ?
O4 C7 0.926(14) 23 ?

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
O4 Ni1 O4 174.5(6) . 16_556 ?
O4 Ni1 O2 88.42(17) . 8 ?
O4 Ni1 O2 88.42(17) 16_556 8 ?
O4 Ni1 O2 88.42(17) . . ?
O4 Ni1 O2 88.42(17) 16_556 . ?
O2 Ni1 O2 110.03(19) 8 . ?
O4 Ni1 O1 92.4(3) . . ?
O4 Ni1 O1 92.4(3) 16_556 . ?
O2 Ni1 O1 155.97(12) 8 . ?
O2 Ni1 O1 94.00(13) . . ?
O4 Ni1 O1 92.4(3) . 8 ?
O4 Ni1 O1 92.4(3) 16_556 8 ?
O2 Ni1 O1 94.00(13) 8 8 ?
O2 Ni1 O1 155.97(12) . 8 ?
O1 Ni1 O1 61.97(16) . 8 ?
O1 C1 O1 120.2(5) 8 . ?
O1 C1 C2 119.9(3) 8 . ?
O1 C1 C2 119.9(3) . . ?
C3 C2 C3 120.2(6) . 2_645 ?
C3 C2 C1 119.9(3) . . ?
C3 C2 C1 119.9(3) 2_645 . ?
C2 C3 C2 119.8(6) . 3_765 ?
O2 C4 O3 125.0(4) . . ?
O2 C4 C5 119.3(4) . . ?
O3 C4 C5 115.7(4) . . ?
C6 C5 C6 119.4(4) . 3_665 ?
C6 C5 C4 119.9(3) . . ?
C6 C5 C4 120.7(4) 3_665 . ?
C5 C6 C5 120.6(4) . 2_655 ?
C7 C7 O4 62.4(7) 23 . ?
C7 C7 N1 73.8(4) 23 . ?
O4 C7 N1 133.3(10) . . ?
C7 N1 C7 32.4(8) . 23 ?
C7 N1 C8 111.3(8) . 23 ?
C7 N1 C8 142.9(9) 23 23 ?
C7 N1 C8 142.9(9) . . ?
C7 N1 C8 111.3(8) 23 . ?
C8 N1 C8 102.2(14) 23 . ?
C1 O1 Ni1 88.9(3) . . ?
C4 O2 Ni1 140.8(3) . . ?
C7 O4 C7 55.2(14) 23 . ?
C7 O4 Ni1 147.1(9) 23 . ?
C7 O4 Ni1 147.1(9) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.084


