# Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and 
# The Centre National de la Recherche Scientifique, 2002

data_ni
_database_code_CSD                  176796

_journal_coden_Cambridge      440


loop_
_publ_author_name
'Lu, Tongbu'

_publ_contact_author_name     	'Dr Tongbu Lu'  
_publ_contact_author_address 
;
Department of Chemistry, Zhongshan
Guangzhou
CHINA
;

_publ_contact_author_email       'CESLTB@ZSU.EDU.CN'

_publ_requested_journal       'New Journal of Chemistry'


_publ_section_title		
;
[NiL]3[BTC]214H2O (L =
3,10-bis(2-ethyl)-1,3,5,8,10,12-hexaazacyclo-tetradecane, BTC =
1,3,5-benzenetricarboxylate): synthesis, structure and unique selected guest
molecule absorption properties
;

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
'C54 H124 N18 Ni3 O26' 
_chemical_formula_weight          1617.9 

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                    8.541(2) 
_cell_length_b                    14.920(4) 
_cell_length_c                    17.352(5) 
_cell_angle_alpha                 115.233(4) 
_cell_angle_beta                  93.117(5) 
_cell_angle_gamma                 96.030(5) 
_cell_volume                      1977.0(10) 
_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        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.24 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.494 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              953 
_exptl_absorpt_coefficient_mu     0.798 
_exptl_absorpt_correction_type    ? 
_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   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             13265 
_diffrn_reflns_av_R_equivalents   0.0411 
_diffrn_reflns_av_sigmaI/netI     0.1150 
_diffrn_reflns_limit_h_min        -5 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -20 
_diffrn_reflns_limit_k_max        20 
_diffrn_reflns_limit_l_min        -24 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          2.61 
_diffrn_reflns_theta_max          29.87 
_reflns_number_total              9948 
_reflns_number_gt                 4745 
_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^)+(0.1000P)^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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          9948 
_refine_ls_number_parameters      460 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1538 
_refine_ls_R_factor_gt            0.0700 
_refine_ls_wR_factor_ref          0.2302 
_refine_ls_wR_factor_gt           0.1871 
_refine_ls_goodness_of_fit_ref    1.096 
_refine_ls_restrained_S_all       1.096 
_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 
Ni3 Ni 0.0000 0.5000 0.5000 0.0337(2) Uani 1 2 d S . . 
Ni1 Ni -1.0000 0.0000 0.0000 0.0362(2) Uani 1 2 d S . . 
Ni2 Ni -0.5000 0.0000 0.5000 0.0411(3) Uani 1 2 d S . . 
O1 O -0.8171(4) 0.0743(3) 0.1012(2) 0.0506(10) Uani 1 1 d . . . 
O3 O -0.1925(4) 0.3895(2) 0.4208(2) 0.0434(9) Uani 1 1 d . . . 
O5 O -0.5087(4) 0.0914(3) 0.4349(2) 0.0525(10) Uani 1 1 d . . . 
N8 N 0.0112(4) 0.5620(3) 0.4156(2) 0.0364(9) Uani 1 1 d . . . 
O4 O -0.2338(5) 0.4106(3) 0.3016(3) 0.0667(12) Uani 1 1 d . . . 
C27 C -0.6563(6) 0.1338(4) 0.2592(3) 0.0416(12) Uani 1 1 d . . . 
H27A H -0.7447 0.0848 0.2408 0.050 Uiso 1 1 calc R . . 
C22 C -0.3974(5) 0.2815(3) 0.3154(3) 0.0349(11) Uani 1 1 d . . . 
N9 N 0.1502(5) 0.3975(3) 0.4392(3) 0.0423(10) Uani 1 1 d . . . 
O6 O -0.7620(4) 0.0739(3) 0.3861(3) 0.0628(11) Uani 1 1 d . . . 
N3 N -1.0539(5) -0.0992(3) 0.0516(3) 0.0447(11) Uani 1 1 d . . . 
C26 C -0.6169(6) 0.1039(4) 0.3900(3) 0.0408(12) Uani 1 1 d . . . 
C20 C -0.6164(5) 0.1798(3) 0.2088(3) 0.0353(11) Uani 1 1 d . . . 
C25 C -0.5695(5) 0.1572(3) 0.3375(3) 0.0374(11) Uani 1 1 d . . . 
C24 C -0.4385(5) 0.2310(3) 0.3641(3) 0.0367(11) Uani 1 1 d . . . 
H24A H -0.3774 0.2468 0.4154 0.044 Uiso 1 1 calc R . . 
C23 C -0.2647(6) 0.3676(4) 0.3486(3) 0.0431(12) Uani 1 1 d . . . 
O2 O -0.6783(5) 0.1946(4) 0.0807(3) 0.0836(16) Uani 1 1 d . . . 
C21 C -0.4869(5) 0.2552(3) 0.2371(3) 0.0376(12) Uani 1 1 d . . . 
H21A H -0.4598 0.2882 0.2038 0.045 Uiso 1 1 calc R . . 
N5 N -0.7430(5) -0.0322(3) 0.4874(3) 0.0510(12) Uani 1 1 d . . . 
C19 C -0.7120(6) 0.1472(4) 0.1230(3) 0.0456(13) Uani 1 1 d . . . 
N7 N 0.2404(5) 0.4832(3) 0.3516(3) 0.0514(11) Uani 1 1 d . . . 
N2 N -1.1570(5) 0.0930(3) 0.0663(3) 0.0523(12) Uani 1 1 d . . . 
N6 N -0.4763(6) -0.1179(4) 0.3851(3) 0.0568(12) Uani 1 1 d . . . 
C15 C 0.1726(6) 0.5753(4) 0.3901(3) 0.0473(13) Uani 1 1 d . . . 
H15A H 0.1674 0.6043 0.3497 0.057 Uiso 1 1 calc R . . 
H15B H 0.2422 0.6222 0.4404 0.057 Uiso 1 1 calc R . . 
N4 N -0.7511(6) -0.1976(4) 0.3693(4) 0.0665(15) Uani 1 1 d . . . 
C18 C 0.2013(6) 0.3626(4) 0.5029(4) 0.0512(14) Uani 1 1 d . . . 
H18A H 0.2813 0.4126 0.5457 0.061 Uiso 1 1 calc R . . 
H18B H 0.2466 0.3012 0.4751 0.061 Uiso 1 1 calc R . . 
N1 N -1.1917(6) 0.0175(4) 0.1655(3) 0.0648(14) Uani 1 1 d . . . 
C4 C -1.0783(7) -0.0533(4) 0.1433(3) 0.0546(15) Uani 1 1 d . . . 
H4A H -1.1140 -0.1061 0.1595 0.066 Uiso 1 1 calc R . . 
H4B H -0.9773 -0.0191 0.1767 0.066 Uiso 1 1 calc R . . 
C16 C 0.2856(6) 0.4407(4) 0.4079(4) 0.0525(14) Uani 1 1 d . . . 
H16A H 0.3525 0.4920 0.4572 0.063 Uiso 1 1 calc R . . 
H16B H 0.3486 0.3882 0.3784 0.063 Uiso 1 1 calc R . . 
C17 C -0.0582(6) 0.6554(4) 0.4549(4) 0.0487(14) Uani 1 1 d . . . 
H17A H -0.0898 0.6765 0.4113 0.058 Uiso 1 1 calc R . . 
H17B H 0.0194 0.7079 0.4972 0.058 Uiso 1 1 calc R . . 
C14 C 0.1607(8) 0.4099(5) 0.2683(4) 0.0677(18) Uani 1 1 d . . . 
H14A H 0.0561 0.3850 0.2761 0.081 Uiso 1 1 calc R . . 
H14B H 0.2198 0.3537 0.2460 0.081 Uiso 1 1 calc R . . 
C10 C -0.5846(8) -0.2113(5) 0.3694(4) 0.075(2) Uani 1 1 d . . . 
H10A H -0.5689 -0.2641 0.3145 0.090 Uiso 1 1 calc R . . 
H10B H -0.5569 -0.2324 0.4134 0.090 Uiso 1 1 calc R . . 
C3 C -1.1508(8) 0.1078(5) 0.1569(4) 0.0648(17) Uani 1 1 d . . . 
H3A H -1.0446 0.1377 0.1850 0.078 Uiso 1 1 calc R . . 
H3B H -1.2227 0.1544 0.1861 0.078 Uiso 1 1 calc R . . 
C9 C -0.8003(7) -0.1402(5) 0.4508(5) 0.0643(18) Uani 1 1 d . . . 
H9A H -0.7636 -0.1658 0.4904 0.077 Uiso 1 1 calc R . . 
H9B H -0.9152 -0.1497 0.4457 0.077 Uiso 1 1 calc R . . 
C2 C -1.3606(8) -0.0283(7) 0.1362(5) 0.088(2) Uani 1 1 d . . . 
H2A H -1.3704 -0.0745 0.0759 0.105 Uiso 1 1 calc R . . 
H2B H -1.4246 0.0239 0.1424 0.105 Uiso 1 1 calc R . . 
C5 C -1.1107(8) 0.1880(4) 0.0583(4) 0.0691(18) Uani 1 1 d . . . 
H5A H -1.0183 0.2266 0.0983 0.083 Uiso 1 1 calc R . . 
H5B H -1.1966 0.2281 0.0717 0.083 Uiso 1 1 calc R . . 
C6 C -0.9258(7) -0.1620(5) 0.0328(4) 0.0631(17) Uani 1 1 d . . . 
H6A H -0.9586 -0.2227 0.0389 0.076 Uiso 1 1 calc R . . 
H6B H -0.8320 -0.1261 0.0727 0.076 Uiso 1 1 calc R . . 
C12 C -0.3036(8) -0.1279(5) 0.3880(4) 0.0718(19) Uani 1 1 d . . . 
H12A H -0.2793 -0.1628 0.4223 0.086 Uiso 1 1 calc R . . 
H12B H -0.2763 -0.1661 0.3306 0.086 Uiso 1 1 calc R . . 
C11 C -0.7904(7) 0.0236(5) 0.5728(4) 0.0687(18) Uani 1 1 d . . . 
H11A H -0.7695 -0.0101 0.6085 0.082 Uiso 1 1 calc R . . 
H11B H -0.9029 0.0278 0.5687 0.082 Uiso 1 1 calc R . . 
C13 C 0.1441(15) 0.4519(7) 0.2024(5) 0.151(5) Uani 1 1 d . . . 
H13A H 0.0903 0.4005 0.1495 0.227 Uiso 1 1 calc R . . 
H13B H 0.2473 0.4747 0.1928 0.227 Uiso 1 1 calc R . . 
H13C H 0.0841 0.5069 0.2234 0.227 Uiso 1 1 calc R . . 
C8 C -0.8196(10) -0.1853(6) 0.2958(5) 0.103(3) Uani 1 1 d . . . 
H8A H -0.7883 -0.1286 0.2877 0.124 Uiso 1 1 calc R . . 
C7 C -0.927(2) -0.2576(9) 0.2418(8) 0.251(9) Uani 1 1 d . . . 
H7A H -0.9616 -0.2415 0.1962 0.377 Uiso 1 1 calc R . . 
H7B H -1.0156 -0.2653 0.2712 0.377 Uiso 1 1 calc R . . 
H7C H -0.8822 -0.3189 0.2184 0.377 Uiso 1 1 calc R . . 
C1 C -1.4232(10) -0.0833(7) 0.1863(6) 0.115(3) Uani 1 1 d . . . 
H1A H -1.5315 -0.1121 0.1649 0.173 Uiso 1 1 calc R . . 
H1B H -1.4170 -0.0373 0.2458 0.173 Uiso 1 1 calc R . . 
H1C H -1.3608 -0.1354 0.1801 0.173 Uiso 1 1 calc R . . 
OW7 O -1.0195(6) 0.1578(4) 0.3523(3) 0.0922(16) Uani 1 1 d . . . 
OW6 O -0.4585(9) 0.5385(7) 0.2906(6) 0.186(4) Uani 1 1 d . . . 
OW5 O -0.5234(16) 0.3435(11) 0.0553(9) 0.149(6) Uani 0.50 1 d P . . 
OW4 O -0.394(2) 0.6375(15) 0.1764(10) 0.190(7) Uani 0.50 1 d P . . 
OW3 O -0.7781(19) 0.3581(14) -0.0454(11) 0.355(8) Uani 1 1 d . . . 
OW1 O -0.265(3) 0.4458(18) 0.1539(12) 0.229(9) Uani 0.50 1 d P . . 
OW2 O -0.647(2) 0.6560(17) 0.0832(13) 0.219(9) Uani 0.50 1 d P . . 

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 
Ni3 0.0303(5) 0.0270(4) 0.0377(5) 0.0116(4) -0.0104(4) -0.0034(3) 
Ni1 0.0362(5) 0.0341(5) 0.0299(5) 0.0096(4) -0.0118(4) -0.0022(4) 
Ni2 0.0350(5) 0.0434(5) 0.0491(6) 0.0286(5) -0.0120(4) -0.0059(4) 
O1 0.049(2) 0.050(2) 0.043(2) 0.0196(17) -0.0247(17) -0.0204(18) 
O3 0.0383(19) 0.0411(19) 0.0417(19) 0.0168(16) -0.0210(15) -0.0135(15) 
O5 0.040(2) 0.063(2) 0.068(2) 0.047(2) -0.0191(17) -0.0106(18) 
N8 0.033(2) 0.029(2) 0.042(2) 0.0127(18) -0.0026(17) -0.0035(17) 
O4 0.064(3) 0.076(3) 0.061(3) 0.046(2) -0.030(2) -0.041(2) 
C27 0.036(3) 0.037(3) 0.044(3) 0.017(2) -0.018(2) -0.010(2) 
C22 0.029(2) 0.032(2) 0.037(3) 0.012(2) -0.0095(19) -0.001(2) 
N9 0.040(2) 0.038(2) 0.049(3) 0.020(2) -0.0028(19) 0.0056(19) 
O6 0.039(2) 0.081(3) 0.089(3) 0.064(3) -0.016(2) -0.012(2) 
N3 0.043(2) 0.045(2) 0.042(2) 0.018(2) -0.0098(19) -0.002(2) 
C26 0.037(3) 0.040(3) 0.045(3) 0.023(2) -0.012(2) -0.010(2) 
C20 0.034(2) 0.035(2) 0.032(2) 0.014(2) -0.012(2) -0.003(2) 
C25 0.038(3) 0.033(2) 0.038(3) 0.016(2) -0.012(2) -0.003(2) 
C24 0.035(3) 0.031(2) 0.037(3) 0.014(2) -0.019(2) -0.004(2) 
C23 0.040(3) 0.036(3) 0.046(3) 0.015(2) -0.015(2) -0.007(2) 
O2 0.090(3) 0.097(3) 0.060(3) 0.050(3) -0.042(2) -0.051(3) 
C21 0.040(3) 0.035(2) 0.034(3) 0.015(2) -0.011(2) -0.004(2) 
N5 0.044(3) 0.056(3) 0.061(3) 0.039(2) -0.013(2) -0.011(2) 
C19 0.047(3) 0.049(3) 0.035(3) 0.020(2) -0.015(2) -0.013(3) 
N7 0.054(3) 0.049(3) 0.047(3) 0.019(2) -0.002(2) 0.004(2) 
N2 0.063(3) 0.051(3) 0.042(3) 0.016(2) 0.009(2) 0.019(2) 
N6 0.055(3) 0.058(3) 0.057(3) 0.027(2) -0.007(2) 0.000(2) 
C15 0.051(3) 0.038(3) 0.043(3) 0.015(2) -0.008(2) -0.013(2) 
N4 0.060(3) 0.059(3) 0.082(4) 0.043(3) -0.031(3) -0.021(3) 
C18 0.053(3) 0.042(3) 0.060(4) 0.022(3) 0.001(3) 0.015(3) 
N1 0.059(3) 0.083(4) 0.052(3) 0.032(3) -0.001(2) -0.001(3) 
C4 0.050(3) 0.065(4) 0.050(3) 0.030(3) -0.009(3) 0.000(3) 
C16 0.039(3) 0.060(4) 0.060(4) 0.025(3) 0.011(3) 0.014(3) 
C17 0.058(3) 0.035(3) 0.055(3) 0.023(3) -0.003(3) 0.005(3) 
C14 0.085(5) 0.059(4) 0.051(4) 0.016(3) 0.011(3) 0.012(4) 
C10 0.094(5) 0.045(3) 0.075(5) 0.022(3) -0.015(4) -0.009(4) 
C3 0.076(4) 0.065(4) 0.046(3) 0.015(3) 0.010(3) 0.015(3) 
C9 0.043(3) 0.071(4) 0.090(5) 0.055(4) -0.024(3) -0.018(3) 
C2 0.059(4) 0.134(7) 0.074(5) 0.051(5) 0.011(4) 0.004(4) 
C5 0.090(5) 0.051(4) 0.065(4) 0.020(3) 0.012(4) 0.024(3) 
C6 0.073(4) 0.056(4) 0.071(4) 0.037(3) -0.002(3) 0.012(3) 
C12 0.070(4) 0.078(5) 0.072(5) 0.035(4) 0.013(3) 0.021(4) 
C11 0.046(3) 0.096(5) 0.078(5) 0.053(4) -0.001(3) 0.002(3) 
C13 0.271(14) 0.097(7) 0.059(5) 0.030(5) -0.032(7) -0.045(8) 
C8 0.128(7) 0.083(5) 0.094(6) 0.055(5) -0.067(5) -0.040(5) 
C7 0.39(2) 0.158(12) 0.170(12) 0.076(10) -0.182(14) -0.031(13) 
C1 0.085(6) 0.147(8) 0.135(8) 0.086(7) 0.018(5) -0.015(6) 
OW7 0.093(4) 0.099(4) 0.064(3) 0.014(3) -0.002(3) 0.029(3) 
OW6 0.125(6) 0.246(9) 0.282(11) 0.203(9) 0.025(6) 0.039(6) 
OW5 0.142(11) 0.161(12) 0.178(13) 0.131(11) -0.035(9) -0.071(10) 
OW4 0.231(19) 0.223(19) 0.120(12) 0.067(13) 0.052(12) 0.060(15) 
OW3 0.309(17) 0.43(2) 0.343(18) 0.214(18) -0.035(14) -0.063(16) 
OW1 0.26(2) 0.29(2) 0.190(18) 0.162(19) -0.002(16) 0.04(2) 
OW2 0.23(2) 0.25(2) 0.201(19) 0.121(18) 0.071(16) 0.028(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 
Ni3 N8 2.040(4) 2_566 ? 
Ni3 N8 2.040(4) . ? 
Ni3 N9 2.069(4) . ? 
Ni3 N9 2.069(4) 2_566 ? 
Ni3 O3 2.136(3) 2_566 ? 
Ni3 O3 2.136(3) . ? 
Ni1 N2 2.060(4) 2_355 ? 
Ni1 N2 2.060(4) . ? 
Ni1 N3 2.058(4) 2_355 ? 
Ni1 N3 2.058(4) . ? 
Ni1 O1 2.105(3) 2_355 ? 
Ni1 O1 2.105(3) . ? 
Ni2 N5 2.059(4) 2_456 ? 
Ni2 N5 2.059(4) . ? 
Ni2 N6 2.059(5) . ? 
Ni2 N6 2.059(5) 2_456 ? 
Ni2 O5 2.114(3) . ? 
Ni2 O5 2.114(3) 2_456 ? 
O1 C19 1.241(6) . ? 
O3 C23 1.258(6) . ? 
O5 C26 1.256(5) . ? 
N8 C17 1.473(6) . ? 
N8 C15 1.489(6) . ? 
O4 C23 1.257(6) . ? 
C27 C20 1.359(7) . ? 
C27 C25 1.396(6) . ? 
C22 C24 1.389(7) . ? 
C22 C21 1.397(6) . ? 
C22 C23 1.503(7) . ? 
N9 C18 1.473(6) . ? 
N9 C16 1.502(7) . ? 
O6 C26 1.261(6) . ? 
N3 C6 1.475(7) . ? 
N3 C4 1.477(7) . ? 
C26 C25 1.490(7) . ? 
C20 C21 1.392(6) . ? 
C20 C19 1.513(6) . ? 
C25 C24 1.388(6) . ? 
O2 C19 1.242(6) . ? 
N5 C11 1.462(8) . ? 
N5 C9 1.472(7) . ? 
N7 C16 1.430(7) . ? 
N7 C15 1.448(7) . ? 
N7 C14 1.463(7) . ? 
N2 C3 1.488(7) . ? 
N2 C5 1.497(7) . ? 
N6 C10 1.499(8) . ? 
N6 C12 1.499(8) . ? 
N4 C9 1.421(8) . ? 
N4 C10 1.458(8) . ? 
N4 C8 1.464(8) . ? 
C18 C17 1.516(8) 2_566 ? 
N1 C3 1.427(8) . ? 
N1 C4 1.453(7) . ? 
N1 C2 1.491(8) . ? 
C17 C18 1.516(8) 2_566 ? 
C14 C13 1.527(10) . ? 
C2 C1 1.510(10) . ? 
C5 C6 1.518(8) 2_355 ? 
C6 C5 1.518(8) 2_355 ? 
C12 C11 1.518(9) 2_456 ? 
C11 C12 1.518(9) 2_456 ? 
C8 C7 1.311(12) . ? 

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 
N8 Ni3 N8 180.000(1) 2_566 . ? 
N8 Ni3 N9 86.11(16) 2_566 . ? 
N8 Ni3 N9 93.89(16) . . ? 
N8 Ni3 N9 93.89(16) 2_566 2_566 ? 
N8 Ni3 N9 86.11(16) . 2_566 ? 
N9 Ni3 N9 180.0(2) . 2_566 ? 
N8 Ni3 O3 91.36(14) 2_566 2_566 ? 
N8 Ni3 O3 88.64(14) . 2_566 ? 
N9 Ni3 O3 92.39(15) . 2_566 ? 
N9 Ni3 O3 87.61(15) 2_566 2_566 ? 
N8 Ni3 O3 88.64(14) 2_566 . ? 
N8 Ni3 O3 91.36(14) . . ? 
N9 Ni3 O3 87.61(15) . . ? 
N9 Ni3 O3 92.39(15) 2_566 . ? 
O3 Ni3 O3 180.00(17) 2_566 . ? 
N2 Ni1 N2 180.00(17) 2_355 . ? 
N2 Ni1 N3 93.46(18) 2_355 2_355 ? 
N2 Ni1 N3 86.54(18) . 2_355 ? 
N2 Ni1 N3 86.54(18) 2_355 . ? 
N2 Ni1 N3 93.46(18) . . ? 
N3 Ni1 N3 180.00(16) 2_355 . ? 
N2 Ni1 O1 92.10(17) 2_355 2_355 ? 
N2 Ni1 O1 87.90(17) . 2_355 ? 
N3 Ni1 O1 87.89(14) 2_355 2_355 ? 
N3 Ni1 O1 92.11(14) . 2_355 ? 
N2 Ni1 O1 87.90(17) 2_355 . ? 
N2 Ni1 O1 92.10(17) . . ? 
N3 Ni1 O1 92.11(14) 2_355 . ? 
N3 Ni1 O1 87.89(14) . . ? 
O1 Ni1 O1 180.00(16) 2_355 . ? 
N5 Ni2 N5 180.000(1) 2_456 . ? 
N5 Ni2 N6 85.86(19) 2_456 . ? 
N5 Ni2 N6 94.14(19) . . ? 
N5 Ni2 N6 94.14(19) 2_456 2_456 ? 
N5 Ni2 N6 85.86(19) . 2_456 ? 
N6 Ni2 N6 180.0(2) . 2_456 ? 
N5 Ni2 O5 87.43(15) 2_456 . ? 
N5 Ni2 O5 92.57(15) . . ? 
N6 Ni2 O5 88.55(17) . . ? 
N6 Ni2 O5 91.45(17) 2_456 . ? 
N5 Ni2 O5 92.57(15) 2_456 2_456 ? 
N5 Ni2 O5 87.43(15) . 2_456 ? 
N6 Ni2 O5 91.45(17) . 2_456 ? 
N6 Ni2 O5 88.55(17) 2_456 2_456 ? 
O5 Ni2 O5 180.000(1) . 2_456 ? 
C19 O1 Ni1 136.0(3) . . ? 
C23 O3 Ni3 134.5(3) . . ? 
C26 O5 Ni2 133.3(3) . . ? 
C17 N8 C15 114.0(4) . . ? 
C17 N8 Ni3 106.0(3) . . ? 
C15 N8 Ni3 114.0(3) . . ? 
C20 C27 C25 122.4(4) . . ? 
C24 C22 C21 119.2(4) . . ? 
C24 C22 C23 120.5(4) . . ? 
C21 C22 C23 120.2(5) . . ? 
C18 N9 C16 113.4(4) . . ? 
C18 N9 Ni3 104.5(3) . . ? 
C16 N9 Ni3 112.9(3) . . ? 
C6 N3 C4 113.1(4) . . ? 
C6 N3 Ni1 105.4(3) . . ? 
C4 N3 Ni1 115.3(3) . . ? 
O5 C26 O6 124.5(5) . . ? 
O5 C26 C25 117.4(4) . . ? 
O6 C26 C25 118.1(4) . . ? 
C27 C20 C21 119.0(4) . . ? 
C27 C20 C19 119.4(4) . . ? 
C21 C20 C19 121.5(5) . . ? 
C24 C25 C27 118.0(4) . . ? 
C24 C25 C26 121.6(4) . . ? 
C27 C25 C26 120.5(4) . . ? 
C22 C24 C25 121.0(4) . . ? 
O4 C23 O3 125.6(5) . . ? 
O4 C23 C22 117.5(4) . . ? 
O3 C23 C22 116.9(5) . . ? 
C20 C21 C22 120.4(5) . . ? 
C11 N5 C9 113.1(5) . . ? 
C11 N5 Ni2 105.8(3) . . ? 
C9 N5 Ni2 113.2(4) . . ? 
O1 C19 O2 126.0(5) . . ? 
O1 C19 C20 116.2(5) . . ? 
O2 C19 C20 117.8(5) . . ? 
C16 N7 C15 116.1(4) . . ? 
C16 N7 C14 114.1(5) . . ? 
C15 N7 C14 115.3(4) . . ? 
C3 N2 C5 113.0(5) . . ? 
C3 N2 Ni1 111.9(3) . . ? 
C5 N2 Ni1 104.5(4) . . ? 
C10 N6 C12 114.5(5) . . ? 
C10 N6 Ni2 112.5(4) . . ? 
C12 N6 Ni2 105.1(4) . . ? 
N7 C15 N8 113.8(4) . . ? 
C9 N4 C10 115.6(5) . . ? 
C9 N4 C8 117.8(6) . . ? 
C10 N4 C8 115.7(6) . . ? 
N9 C18 C17 108.5(4) . 2_566 ? 
C3 N1 C4 117.5(5) . . ? 
C3 N1 C2 114.2(5) . . ? 
C4 N1 C2 115.0(5) . . ? 
N1 C4 N3 114.5(4) . . ? 
N7 C16 N9 115.0(4) . . ? 
N8 C17 C18 108.9(4) . 2_566 ? 
N7 C14 C13 113.6(5) . . ? 
N4 C10 N6 112.7(5) . . ? 
N1 C3 N2 113.6(5) . . ? 
N4 C9 N5 114.7(5) . . ? 
N1 C2 C1 112.4(6) . . ? 
N2 C5 C6 108.8(5) . 2_355 ? 
N3 C6 C5 108.5(5) . 2_355 ? 
C11 C12 N6 108.2(5) 2_456 . ? 
N5 C11 C12 108.4(5) . 2_456 ? 
C7 C8 N4 117.2(8) . . ? 

_diffrn_measured_fraction_theta_max    0.872 
_diffrn_reflns_theta_full              29.87 
_diffrn_measured_fraction_theta_full   0.872 
_refine_diff_density_max    1.048 
_refine_diff_density_min   -1.002 
_refine_diff_density_rms    0.109