# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Kajal Rajak'
_publ_contact_author_email       KAJALRAJAK@REDIFFMAIL.COM

_publ_section_title              
;
Mixed bridged binuclear Ni(II) complexes: Synthesis,
Structure, Magnetic properties and DFT study
;
loop_
_publ_author_name
'Kajal Rajak'
'Atanu Banerjee'
'Deepak Chopra'
'E. Colacio'
'Reena Singh'

# Attachment 'CIF__ESI_.txt'

data_[Ni2(L)(Cl)(H2O)].C4H10O
_database_code_depnum_ccdc_archive 'CCDC 689422'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H53 Cl N4 Ni2 O5'
_chemical_formula_weight         762.64

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'
Cl Cl 0.1484 0.1585 '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           Triclinic
_symmetry_space_group_name_H-M   p-1

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

_cell_length_a                   10.539(8)
_cell_length_b                   11.245(9)
_cell_length_c                   16.988(13)
_cell_angle_alpha                91.738(13)
_cell_angle_beta                 97.871(13)
_cell_angle_gamma                114.220(12)
_cell_volume                     1810(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      25.00

_exptl_crystal_description       parallopiped
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    1.160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_process_details   (SADABAS,SHELDRICK-1997)

_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            17111
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6351
_reflns_number_gt                4561
_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.

We have rechecked the structure and found that the anisotropy solution of carbon
atoms of ether molecule generates large thermal parameter which is probably
due to thermal agitation. Moreover, solving the carbon atoms of the solvent
ether molecule anisotropically no significant change in the residual electron
density has been observed.
Thus the carbon atoms of ether modelled isotropically.
;

_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^)+(0.0771P)^2^+6.3089P] 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    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6351
_refine_ls_number_parameters     404
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0824
_refine_ls_wR_factor_ref         0.2164
_refine_ls_wR_factor_gt          0.2049
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.098
_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 0.7955(7) 0.6355(6) 0.1781(4) 0.0385(15) Uani 1 1 d . . .
C2 C 0.9171(7) 0.6195(6) 0.1641(4) 0.0399(16) Uani 1 1 d . . .
C3 C 0.9016(9) 0.5217(7) 0.1065(4) 0.0494(18) Uani 1 1 d . . .
H3 H 0.9816 0.5116 0.0969 0.059 Uiso 1 1 calc R . .
C4 C 0.7726(9) 0.4391(7) 0.0630(4) 0.0518(19) Uani 1 1 d . . .
C5 C 0.6540(9) 0.4549(7) 0.0775(4) 0.053(2) Uani 1 1 d . . .
H5 H 0.5660 0.3993 0.0493 0.063 Uiso 1 1 calc R . .
C6 C 0.6644(8) 0.5526(6) 0.1337(4) 0.0411(16) Uani 1 1 d . . .
C7 C 1.0583(8) 0.7065(6) 0.2078(4) 0.0463(17) Uani 1 1 d . . .
H7A H 1.1277 0.6853 0.1860 0.056 Uiso 1 1 calc R . .
H7B H 1.0626 0.6871 0.2631 0.056 Uiso 1 1 calc R . .
C8 C 1.0765(8) 0.8799(7) 0.1208(4) 0.0483(18) Uani 1 1 d . . .
H8A H 1.1409 0.8608 0.0925 0.058 Uiso 1 1 calc R . .
H8B H 0.9814 0.8208 0.0964 0.058 Uiso 1 1 calc R . .
C9 C 1.0957(8) 1.0176(7) 0.1092(4) 0.0462(17) Uani 1 1 d . . .
C10 C 1.0129(8) 1.0691(7) 0.1435(4) 0.0489(18) Uani 1 1 d . . .
C11 C 1.0239(10) 1.1927(7) 0.1233(4) 0.064(2) Uani 1 1 d . . .
H11 H 0.9683 1.2281 0.1440 0.077 Uiso 1 1 calc R . .
C12 C 1.1134(10) 1.2620(8) 0.0742(5) 0.069(3) Uani 1 1 d . . .
H12 H 1.1179 1.3437 0.0621 0.083 Uiso 1 1 calc R . .
C13 C 1.1968(10) 1.2140(9) 0.0422(5) 0.071(3) Uani 1 1 d . . .
H13 H 1.2592 1.2632 0.0096 0.085 Uiso 1 1 calc R . .
C14 C 1.1871(9) 1.0884(8) 0.0591(4) 0.060(2) Uani 1 1 d . . .
H14 H 1.2418 1.0536 0.0367 0.072 Uiso 1 1 calc R . .
C15 C 1.2484(8) 0.9218(7) 0.2457(5) 0.0538(19) Uani 1 1 d . . .
H15A H 1.3108 0.9316 0.2070 0.065 Uiso 1 1 calc R . .
H15B H 1.2693 0.8718 0.2870 0.065 Uiso 1 1 calc R . .
C16 C 1.2735(8) 1.0558(7) 0.2824(4) 0.057(2) Uani 1 1 d . . .
H16A H 1.3674 1.0972 0.3137 0.069 Uiso 1 1 calc R . .
H16B H 1.2671 1.1107 0.2405 0.069 Uiso 1 1 calc R . .
C17 C 0.5321(8) 0.5707(7) 0.1414(4) 0.0467(17) Uani 1 1 d . . .
H17A H 0.5414 0.6534 0.1215 0.056 Uiso 1 1 calc R . .
H17B H 0.4531 0.5016 0.1075 0.056 Uiso 1 1 calc R . .
C18 C 0.3623(8) 0.5822(7) 0.2175(4) 0.0540(19) Uani 1 1 d . . .
H18A H 0.2916 0.5090 0.1820 0.065 Uiso 1 1 calc R . .
H18B H 0.3731 0.6615 0.1925 0.065 Uiso 1 1 calc R . .
C19 C 0.3071(8) 0.5864(7) 0.2938(5) 0.0511(18) Uani 1 1 d . . .
C20 C 0.3867(9) 0.6893(8) 0.3531(5) 0.055(2) Uani 1 1 d . . .
C21 C 0.3230(11) 0.6990(9) 0.4197(5) 0.067(2) Uani 1 1 d . . .
H21 H 0.3721 0.7679 0.4593 0.080 Uiso 1 1 calc R . .
C22 C 0.1915(11) 0.6100(10) 0.4275(6) 0.072(3) Uani 1 1 d . . .
H22 H 0.1535 0.6190 0.4724 0.087 Uiso 1 1 calc R . .
C23 C 0.1125(10) 0.5050(10) 0.3691(6) 0.076(3) Uani 1 1 d . . .
H23 H 0.0229 0.4442 0.3745 0.091 Uiso 1 1 calc R . .
C24 C 0.1737(9) 0.4950(8) 0.3023(5) 0.061(2) Uani 1 1 d . . .
H24 H 0.1241 0.4258 0.2630 0.074 Uiso 1 1 calc R . .
C25 C 0.4880(8) 0.4478(6) 0.2597(4) 0.0483(18) Uani 1 1 d . . .
H25A H 0.5510 0.4165 0.2388 0.058 Uiso 1 1 calc R . .
H25B H 0.3925 0.3808 0.2451 0.058 Uiso 1 1 calc R . .
C26 C 0.5255(9) 0.4715(8) 0.3484(5) 0.061(2) Uani 1 1 d . . .
H26A H 0.5318 0.3946 0.3697 0.073 Uiso 1 1 calc R . .
H26B H 0.4516 0.4853 0.3701 0.073 Uiso 1 1 calc R . .
C27 C 1.1600(10) 1.1717(7) 0.3488(5) 0.068(2) Uani 1 1 d . . .
H27A H 1.1351 1.2001 0.2987 0.102 Uiso 1 1 calc R . .
H27B H 1.2505 1.2351 0.3750 0.102 Uiso 1 1 calc R . .
H27C H 1.0903 1.1628 0.3819 0.102 Uiso 1 1 calc R . .
C28 C 1.2040(10) 0.9974(10) 0.4119(5) 0.077(3) Uani 1 1 d . . .
H28A H 1.2062 0.9138 0.4024 0.115 Uiso 1 1 calc R . .
H28B H 1.1349 0.9895 0.4453 0.115 Uiso 1 1 calc R . .
H28C H 1.2951 1.0597 0.4380 0.115 Uiso 1 1 calc R . .
C29 C 0.6684(11) 0.6314(9) 0.4587(4) 0.076(3) Uani 1 1 d . . .
H29A H 0.5893 0.6516 0.4629 0.115 Uiso 1 1 calc R . .
H29B H 0.7544 0.7079 0.4762 0.115 Uiso 1 1 calc R . .
H29C H 0.6651 0.5625 0.4916 0.115 Uiso 1 1 calc R . .
C30 C 0.7833(10) 0.5573(9) 0.3700(5) 0.075(3) Uani 1 1 d . . .
H30A H 0.7817 0.5289 0.3159 0.113 Uiso 1 1 calc R . .
H30B H 0.7787 0.4888 0.4034 0.113 Uiso 1 1 calc R . .
H30C H 0.8689 0.6340 0.3881 0.113 Uiso 1 1 calc R . .
C31 C 0.7648(11) 0.3316(8) 0.0023(5) 0.082(3) Uani 1 1 d . . .
H31A H 0.8580 0.3378 0.0008 0.122 Uiso 1 1 calc R . .
H31B H 0.7242 0.3425 -0.0497 0.122 Uiso 1 1 calc R . .
H31C H 0.7073 0.2473 0.0177 0.122 Uiso 1 1 calc R . .
C32 C 0.712(3) 0.147(3) 0.3849(11) 0.289(14) Uiso 1 1 d D . .
H32A H 0.7901 0.1967 0.4258 0.434 Uiso 1 1 calc R . .
H32B H 0.6894 0.0554 0.3863 0.434 Uiso 1 1 calc R . .
H32C H 0.6313 0.1625 0.3937 0.434 Uiso 1 1 calc R . .
C33 C 0.748(2) 0.187(2) 0.3072(12) 0.251(12) Uiso 1 1 d D . .
H33A H 0.8243 0.1669 0.2952 0.301 Uiso 1 1 calc R . .
H33B H 0.7743 0.2804 0.3050 0.301 Uiso 1 1 calc R . .
C34 C 0.644(2) 0.169(2) 0.1823(11) 0.226(10) Uiso 1 1 d D . .
H34A H 0.7314 0.1704 0.1697 0.271 Uiso 1 1 calc R . .
H34B H 0.6562 0.2591 0.1908 0.271 Uiso 1 1 calc R . .
C35 C 0.535(2) 0.105(2) 0.1170(10) 0.250(11) Uiso 1 1 d D . .
H35A H 0.5590 0.1492 0.0703 0.375 Uiso 1 1 calc R . .
H35B H 0.4486 0.1051 0.1287 0.375 Uiso 1 1 calc R . .
H35C H 0.5233 0.0158 0.1078 0.375 Uiso 1 1 calc R . .
Cl1 Cl 0.8511(2) 0.91143(19) 0.37384(11) 0.0642(6) Uani 1 1 d . . .
N1 N 1.0999(6) 0.8508(5) 0.2060(3) 0.0416(13) Uani 1 1 d . . .
N2 N 1.1663(7) 1.0429(6) 0.3348(3) 0.0509(15) Uani 1 1 d . . .
N3 N 0.4987(6) 0.5699(5) 0.2241(3) 0.0423(14) Uani 1 1 d . . .
N4 N 0.6628(6) 0.5880(6) 0.3741(3) 0.0463(14) Uani 1 1 d . . .
Ni1 Ni 0.97490(10) 0.90047(8) 0.27081(5) 0.0425(3) Uani 1 1 d . . .
Ni2 Ni 0.65197(10) 0.73160(8) 0.29480(5) 0.0431(3) Uani 1 1 d . . .
O1 O 0.9254(6) 1.0042(5) 0.1917(3) 0.0537(13) Uani 1 1 d . . .
O2 O 0.8068(5) 0.7275(4) 0.2346(2) 0.0441(11) Uani 1 1 d . . .
O3 O 0.5149(6) 0.7739(5) 0.3466(3) 0.0612(14) Uani 1 1 d . . .
O4 O 0.6417(6) 0.8673(5) 0.2088(3) 0.0613(14) Uani 1 1 d . . .
H4A H 0.5754 0.8389 0.1648 0.074 Uiso 1 1 d R . .
H4B H 0.7037 0.9520 0.2172 0.074 Uiso 1 1 d R . .
O5 O 0.6164(12) 0.1098(12) 0.2513(8) 0.179(5) Uani 1 1 d 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
C1 0.054(4) 0.029(3) 0.031(3) 0.008(3) 0.007(3) 0.016(3)
C2 0.055(4) 0.031(3) 0.037(3) 0.006(3) 0.011(3) 0.021(3)
C3 0.068(5) 0.042(4) 0.043(4) 0.005(3) 0.020(4) 0.025(4)
C4 0.081(6) 0.037(4) 0.041(4) 0.001(3) 0.021(4) 0.025(4)
C5 0.081(6) 0.037(4) 0.030(4) 0.000(3) 0.009(4) 0.015(4)
C6 0.065(5) 0.027(3) 0.034(3) 0.009(3) 0.009(3) 0.021(3)
C7 0.063(5) 0.036(4) 0.045(4) 0.008(3) 0.014(3) 0.023(4)
C8 0.067(5) 0.043(4) 0.040(4) 0.007(3) 0.014(3) 0.026(4)
C9 0.061(5) 0.040(4) 0.032(3) 0.007(3) 0.003(3) 0.016(4)
C10 0.059(5) 0.045(4) 0.037(4) 0.006(3) 0.002(3) 0.017(4)
C11 0.096(7) 0.048(4) 0.044(4) 0.010(4) 0.001(4) 0.030(5)
C12 0.084(7) 0.050(5) 0.057(5) 0.009(4) -0.012(5) 0.019(5)
C13 0.067(6) 0.070(6) 0.048(5) 0.032(4) -0.001(4) 0.003(5)
C14 0.062(5) 0.068(5) 0.040(4) 0.018(4) 0.006(4) 0.017(4)
C15 0.057(5) 0.055(5) 0.052(4) 0.007(4) 0.010(4) 0.026(4)
C16 0.057(5) 0.052(5) 0.047(4) 0.003(3) 0.001(4) 0.009(4)
C17 0.052(4) 0.048(4) 0.038(4) -0.003(3) 0.000(3) 0.021(4)
C18 0.059(5) 0.048(4) 0.052(4) 0.004(3) 0.003(4) 0.022(4)
C19 0.052(5) 0.045(4) 0.055(4) 0.007(3) 0.008(4) 0.020(4)
C20 0.071(6) 0.055(5) 0.057(5) 0.015(4) 0.018(4) 0.040(5)
C21 0.093(7) 0.068(5) 0.060(5) 0.016(4) 0.023(5) 0.051(5)
C22 0.088(7) 0.079(7) 0.075(6) 0.028(5) 0.032(6) 0.052(6)
C23 0.071(6) 0.073(6) 0.104(8) 0.048(6) 0.037(6) 0.041(5)
C24 0.061(5) 0.059(5) 0.074(6) 0.018(4) 0.014(4) 0.033(4)
C25 0.062(5) 0.033(4) 0.051(4) 0.010(3) 0.016(4) 0.019(3)
C26 0.074(6) 0.054(5) 0.056(5) 0.018(4) 0.018(4) 0.024(4)
C27 0.085(6) 0.036(4) 0.066(5) -0.008(4) 0.011(5) 0.010(4)
C28 0.084(7) 0.093(7) 0.040(4) 0.008(4) 0.001(4) 0.027(5)
C29 0.106(8) 0.086(6) 0.038(4) 0.010(4) 0.017(5) 0.039(6)
C30 0.083(7) 0.086(7) 0.072(6) 0.041(5) 0.023(5) 0.045(6)
C31 0.119(8) 0.061(6) 0.064(5) -0.019(4) 0.035(5) 0.031(6)
Cl1 0.0757(14) 0.0523(11) 0.0475(10) -0.0118(8) 0.0210(10) 0.0076(10)
N1 0.049(4) 0.038(3) 0.035(3) 0.005(2) 0.006(3) 0.015(3)
N2 0.062(4) 0.049(4) 0.038(3) 0.001(3) 0.003(3) 0.021(3)
N3 0.054(4) 0.039(3) 0.036(3) 0.007(2) 0.005(3) 0.021(3)
N4 0.055(4) 0.048(3) 0.036(3) 0.010(3) 0.010(3) 0.021(3)
Ni1 0.0563(6) 0.0338(5) 0.0328(5) 0.0014(3) 0.0108(4) 0.0134(4)
Ni2 0.0589(6) 0.0345(5) 0.0345(5) 0.0032(4) 0.0115(4) 0.0169(4)
O1 0.069(4) 0.051(3) 0.048(3) 0.011(2) 0.012(3) 0.030(3)
O2 0.059(3) 0.037(2) 0.032(2) 0.0003(19) 0.011(2) 0.014(2)
O3 0.064(4) 0.050(3) 0.064(3) -0.003(3) 0.018(3) 0.016(3)
O4 0.074(4) 0.046(3) 0.058(3) 0.006(2) 0.002(3) 0.022(3)
O5 0.166(11) 0.188(12) 0.217(13) 0.081(10) 0.058(10) 0.094(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
C1 O2 1.348(7) . ?
C1 C6 1.400(9) . ?
C1 C2 1.414(10) . ?
C2 C3 1.392(9) . ?
C2 C7 1.477(10) . ?
C3 C4 1.380(11) . ?
C4 C5 1.385(11) . ?
C4 C31 1.533(9) . ?
C5 C6 1.393(9) . ?
C6 C17 1.511(10) . ?
C7 N1 1.500(8) . ?
C8 C9 1.500(9) . ?
C8 N1 1.503(8) . ?
C9 C14 1.387(10) . ?
C9 C10 1.405(10) . ?
C10 O1 1.320(8) . ?
C10 C11 1.404(10) . ?
C11 C12 1.358(12) . ?
C12 C13 1.364(13) . ?
C13 C14 1.415(12) . ?
C15 N1 1.481(9) . ?
C15 C16 1.516(10) . ?
C16 N2 1.495(10) . ?
C17 N3 1.493(8) . ?
C18 N3 1.490(9) . ?
C18 C19 1.498(11) . ?
C19 C24 1.390(11) . ?
C19 C20 1.400(11) . ?
C20 O3 1.317(9) . ?
C20 C21 1.416(11) . ?
C21 C22 1.363(13) . ?
C22 C23 1.402(13) . ?
C23 C24 1.403(12) . ?
C25 N3 1.485(8) . ?
C25 C26 1.491(10) . ?
C26 N4 1.496(10) . ?
C27 N2 1.491(10) . ?
C28 N2 1.483(10) . ?
C29 N4 1.490(9) . ?
C30 N4 1.455(10) . ?
C32 C33 1.457(17) . ?
C33 O5 1.474(15) . ?
C34 O5 1.372(15) . ?
C34 C35 1.411(16) . ?
Cl1 Ni1 2.351(2) . ?
Cl1 Ni2 2.424(2) . ?
N1 Ni1 2.055(6) . ?
N2 Ni1 2.111(6) . ?
N3 Ni2 2.070(6) . ?
N4 Ni2 2.162(6) . ?
Ni1 O1 1.960(5) . ?
Ni1 O2 2.025(5) . ?
Ni2 O3 1.993(6) . ?
Ni2 O2 2.056(5) . ?
Ni2 O4 2.168(5) . ?

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
O2 C1 C6 121.2(6) . . ?
O2 C1 C2 119.8(6) . . ?
C6 C1 C2 119.0(6) . . ?
C3 C2 C1 118.5(7) . . ?
C3 C2 C7 120.4(7) . . ?
C1 C2 C7 121.1(6) . . ?
C4 C3 C2 122.8(7) . . ?
C3 C4 C5 118.3(6) . . ?
C3 C4 C31 119.3(8) . . ?
C5 C4 C31 122.4(8) . . ?
C4 C5 C6 121.0(7) . . ?
C5 C6 C1 120.4(7) . . ?
C5 C6 C17 117.9(7) . . ?
C1 C6 C17 121.6(6) . . ?
C2 C7 N1 116.1(6) . . ?
C9 C8 N1 115.7(6) . . ?
C14 C9 C10 120.8(7) . . ?
C14 C9 C8 119.2(7) . . ?
C10 C9 C8 119.8(6) . . ?
O1 C10 C11 120.5(7) . . ?
O1 C10 C9 122.2(6) . . ?
C11 C10 C9 117.3(7) . . ?
C12 C11 C10 121.8(9) . . ?
C11 C12 C13 121.2(8) . . ?
C12 C13 C14 119.2(8) . . ?
C9 C14 C13 119.6(8) . . ?
N1 C15 C16 110.3(6) . . ?
N2 C16 C15 110.0(6) . . ?
N3 C17 C6 115.3(6) . . ?
N3 C18 C19 116.6(6) . . ?
C24 C19 C20 120.8(8) . . ?
C24 C19 C18 120.0(7) . . ?
C20 C19 C18 119.0(7) . . ?
O3 C20 C19 121.2(7) . . ?
O3 C20 C21 121.7(8) . . ?
C19 C20 C21 117.1(8) . . ?
C22 C21 C20 121.8(9) . . ?
C21 C22 C23 121.3(9) . . ?
C22 C23 C24 117.5(9) . . ?
C19 C24 C23 121.4(9) . . ?
N3 C25 C26 110.8(6) . . ?
C25 C26 N4 111.6(6) . . ?
C32 C33 O5 103.6(15) . . ?
O5 C34 C35 112.5(16) . . ?
Ni1 Cl1 Ni2 85.35(8) . . ?
C15 N1 C7 108.6(5) . . ?
C15 N1 C8 113.0(6) . . ?
C7 N1 C8 108.9(5) . . ?
C15 N1 Ni1 108.2(4) . . ?
C7 N1 Ni1 107.9(4) . . ?
C8 N1 Ni1 110.1(4) . . ?
C28 N2 C27 110.0(6) . . ?
C28 N2 C16 109.8(6) . . ?
C27 N2 C16 109.7(6) . . ?
C28 N2 Ni1 110.6(5) . . ?
C27 N2 Ni1 111.9(5) . . ?
C16 N2 Ni1 104.7(4) . . ?
C25 N3 C18 110.9(6) . . ?
C25 N3 C17 111.6(5) . . ?
C18 N3 C17 106.4(5) . . ?
C25 N3 Ni2 110.1(4) . . ?
C18 N3 Ni2 108.1(4) . . ?
C17 N3 Ni2 109.7(4) . . ?
C30 N4 C29 108.0(7) . . ?
C30 N4 C26 112.2(7) . . ?
C29 N4 C26 107.7(6) . . ?
C30 N4 Ni2 113.3(4) . . ?
C29 N4 Ni2 111.6(5) . . ?
C26 N4 Ni2 103.8(4) . . ?
O1 Ni1 O2 97.5(2) . . ?
O1 Ni1 N1 96.1(2) . . ?
O2 Ni1 N1 92.2(2) . . ?
O1 Ni1 N2 101.0(2) . . ?
O2 Ni1 N2 161.5(2) . . ?
N1 Ni1 N2 85.5(2) . . ?
O1 Ni1 Cl1 103.16(17) . . ?
O2 Ni1 Cl1 84.40(14) . . ?
N1 Ni1 Cl1 160.69(16) . . ?
N2 Ni1 Cl1 91.80(18) . . ?
O3 Ni2 O2 167.9(2) . . ?
O3 Ni2 N3 94.6(2) . . ?
O2 Ni2 N3 92.1(2) . . ?
O3 Ni2 N4 96.0(2) . . ?
O2 Ni2 N4 94.7(2) . . ?
N3 Ni2 N4 83.8(2) . . ?
O3 Ni2 O4 87.0(2) . . ?
O2 Ni2 O4 82.5(2) . . ?
N3 Ni2 O4 93.6(2) . . ?
N4 Ni2 O4 176.2(2) . . ?
O3 Ni2 Cl1 91.90(17) . . ?
O2 Ni2 Cl1 81.89(14) . . ?
N3 Ni2 Cl1 173.30(17) . . ?
N4 Ni2 Cl1 93.79(18) . . ?
O4 Ni2 Cl1 88.46(16) . . ?
C10 O1 Ni1 121.6(5) . . ?
C1 O2 Ni1 127.2(4) . . ?
C1 O2 Ni2 127.6(4) . . ?
Ni1 O2 Ni2 105.0(2) . . ?
C20 O3 Ni2 125.0(5) . . ?
C34 O5 C33 101.9(12) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.108

##=======End

data_[Ni2(L)(N3)(H2O)].H2O.CH3OH
_database_code_depnum_ccdc_archive 'CCDC 689423'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H49 N7 Ni2 O6'
_chemical_formula_weight         745.16

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                   10.4736(13)
_cell_length_b                   11.0275(13)
_cell_length_c                   17.238(2)
_cell_angle_alpha                91.438(2)
_cell_angle_beta                 99.001(2)
_cell_angle_gamma                114.755(2)
_cell_volume                     1776.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.04
_cell_measurement_theta_max      26.00

_exptl_crystal_description       parallopiped
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_process_details   (SADABAS,SHELDRICK-1997)

_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            18586
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6943
_reflns_number_gt                5327
_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^)+(0.0673P)^2^+1.1274P] 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    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6943
_refine_ls_number_parameters     424
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1244
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 -0.1870(3) 0.6442(3) 0.17583(19) 0.0325(7) Uani 1 1 d . . .
C2 C -0.0691(4) 0.6248(3) 0.1592(2) 0.0374(8) Uani 1 1 d . . .
C3 C -0.0911(4) 0.5193(3) 0.1054(2) 0.0425(8) Uani 1 1 d . . .
H3A H -0.0121 0.5085 0.0945 0.051 Uiso 1 1 calc R . .
C4 C -0.2261(4) 0.4294(3) 0.0674(2) 0.0457(9) Uani 1 1 d . . .
C5 C -0.3412(4) 0.4507(3) 0.0837(2) 0.0432(9) Uani 1 1 d . . .
H5A H -0.4330 0.3916 0.0589 0.052 Uiso 1 1 calc R . .
C6 C -0.3250(4) 0.5563(3) 0.13550(19) 0.0363(8) Uani 1 1 d . . .
C7 C 0.0803(4) 0.7165(3) 0.2006(2) 0.0405(8) Uani 1 1 d . . .
H7A H 0.0901 0.6994 0.2556 0.049 Uiso 1 1 calc R . .
H7B H 0.1474 0.6938 0.1777 0.049 Uiso 1 1 calc R . .
C8 C 0.0920(4) 0.8897(4) 0.1129(2) 0.0417(8) Uani 1 1 d . . .
H8A H -0.0068 0.8309 0.0903 0.050 Uiso 1 1 calc R . .
H8B H 0.1520 0.8664 0.0837 0.050 Uiso 1 1 calc R . .
C9 C 0.1167(4) 1.0319(4) 0.1008(2) 0.0399(8) Uani 1 1 d . . .
C10 C 0.0381(4) 1.0885(4) 0.1349(2) 0.0403(8) Uani 1 1 d . . .
C11 C 0.0556(4) 1.2178(4) 0.1165(2) 0.0513(10) Uani 1 1 d . . .
H11A H 0.0042 1.2572 0.1379 0.062 Uiso 1 1 calc R . .
C12 C 0.1471(5) 1.2864(4) 0.0675(2) 0.0590(12) Uani 1 1 d . . .
H12A H 0.1569 1.3716 0.0563 0.071 Uiso 1 1 calc R . .
C13 C 0.2238(4) 1.2317(4) 0.0350(2) 0.0606(12) Uani 1 1 d . . .
H13A H 0.2858 1.2792 0.0020 0.073 Uiso 1 1 calc R . .
C14 C 0.2084(4) 1.1042(4) 0.0517(2) 0.0518(10) Uani 1 1 d . . .
H14A H 0.2607 1.0667 0.0294 0.062 Uiso 1 1 calc R . .
C15 C 0.2752(4) 0.9394(4) 0.2335(2) 0.0476(9) Uani 1 1 d . . .
H15A H 0.3337 0.9504 0.1935 0.057 Uiso 1 1 calc R . .
H15B H 0.3017 0.8893 0.2734 0.057 Uiso 1 1 calc R . .
C16 C 0.3035(4) 1.0758(4) 0.2709(2) 0.0452(9) Uani 1 1 d . . .
H16A H 0.3998 1.1179 0.3016 0.054 Uiso 1 1 calc R . .
H16B H 0.2961 1.1325 0.2300 0.054 Uiso 1 1 calc R . .
C17 C -0.4539(4) 0.5786(4) 0.1445(2) 0.0403(8) Uani 1 1 d . . .
H17A H -0.4455 0.6605 0.1217 0.048 Uiso 1 1 calc R . .
H17B H -0.5379 0.5053 0.1140 0.048 Uiso 1 1 calc R . .
C18 C -0.6152(4) 0.6025(4) 0.2216(2) 0.0439(9) Uani 1 1 d . . .
H18A H -0.6063 0.6810 0.1947 0.053 Uiso 1 1 calc R . .
H18B H -0.6907 0.5248 0.1893 0.053 Uiso 1 1 calc R . .
C19 C -0.6591(4) 0.6149(4) 0.2986(2) 0.0432(9) Uani 1 1 d . . .
C20 C -0.5713(4) 0.7263(4) 0.3545(2) 0.0434(9) Uani 1 1 d . . .
C21 C -0.6224(4) 0.7411(4) 0.4231(2) 0.0541(10) Uani 1 1 d . . .
H21A H -0.5669 0.8139 0.4606 0.065 Uiso 1 1 calc R . .
C22 C -0.7546(5) 0.6486(5) 0.4359(3) 0.0662(13) Uani 1 1 d . . .
H22A H -0.7870 0.6603 0.4815 0.079 Uiso 1 1 calc R . .
C23 C -0.8384(5) 0.5391(5) 0.3810(3) 0.0634(12) Uani 1 1 d . . .
H23A H -0.9264 0.4766 0.3898 0.076 Uiso 1 1 calc R . .
C24 C -0.7904(4) 0.5237(4) 0.3134(3) 0.0520(10) Uani 1 1 d . . .
H24A H -0.8471 0.4503 0.2766 0.062 Uiso 1 1 calc R . .
C25 C -0.4828(4) 0.4703(3) 0.2670(2) 0.0425(8) Uani 1 1 d . . .
H25A H -0.4237 0.4351 0.2452 0.051 Uiso 1 1 calc R . .
H25B H -0.5803 0.4010 0.2567 0.051 Uiso 1 1 calc R . .
C26 C -0.4311(4) 0.5040(4) 0.3552(3) 0.0586(11) Uani 1 1 d . . .
H26A H -0.5026 0.5183 0.3787 0.070 Uiso 1 1 calc R . .
H26B H -0.4195 0.4286 0.3777 0.070 Uiso 1 1 calc R . .
C27 C 0.1996(4) 1.1952(4) 0.3390(2) 0.0523(10) Uani 1 1 d . . .
H27A H 0.2921 1.2565 0.3675 0.078 Uiso 1 1 calc R . .
H27B H 0.1283 1.1865 0.3701 0.078 Uiso 1 1 calc R . .
H27C H 0.1791 1.2287 0.2900 0.078 Uiso 1 1 calc R . .
C28 C 0.2350(5) 1.0129(5) 0.3989(2) 0.0631(12) Uani 1 1 d . . .
H28A H 0.3250 1.0783 0.4277 0.095 Uiso 1 1 calc R . .
H28B H 0.2415 0.9299 0.3887 0.095 Uiso 1 1 calc R . .
H28C H 0.1617 0.9987 0.4296 0.095 Uiso 1 1 calc R . .
C29 C -0.1701(5) 0.5958(5) 0.3738(3) 0.0727(14) Uani 1 1 d . . .
H29A H -0.1678 0.5353 0.4125 0.109 Uiso 1 1 calc R . .
H29B H -0.0842 0.6779 0.3859 0.109 Uiso 1 1 calc R . .
H29C H -0.1769 0.5555 0.3224 0.109 Uiso 1 1 calc R . .
C30 C -0.2814(6) 0.6804(5) 0.4563(3) 0.0760(14) Uani 1 1 d . . .
H30A H -0.2731 0.6187 0.4928 0.114 Uiso 1 1 calc R . .
H30B H -0.3648 0.6944 0.4603 0.114 Uiso 1 1 calc R . .
H30C H -0.1979 0.7645 0.4685 0.114 Uiso 1 1 calc R . .
C31 C -0.2481(5) 0.3134(4) 0.0097(3) 0.0700(13) Uani 1 1 d . . .
H31A H -0.1571 0.3147 0.0058 0.105 Uiso 1 1 calc R . .
H31B H -0.2943 0.3216 -0.0412 0.105 Uiso 1 1 calc R . .
H31C H -0.3069 0.2303 0.0281 0.105 Uiso 1 1 calc R . .
C32 C -0.2245(11) 1.2356(8) 0.2493(6) 0.181(4) Uani 1 1 d . . .
H32A H -0.2429 1.2958 0.2148 0.272 Uiso 1 1 calc R . .
H32B H -0.1614 1.2049 0.2293 0.272 Uiso 1 1 calc R . .
H32C H -0.1807 1.2816 0.3012 0.272 Uiso 1 1 calc R . .
N1 N 0.1213(3) 0.8627(3) 0.19688(17) 0.0357(6) Uani 1 1 d . . .
N2 N 0.1988(3) 1.0621(3) 0.32281(17) 0.0410(7) Uani 1 1 d . . .
N3 N -0.4776(3) 0.5886(3) 0.22734(16) 0.0342(6) Uani 1 1 d . . .
N4 N -0.2944(3) 0.6245(3) 0.37469(17) 0.0409(7) Uani 1 1 d . . .
N5 N -0.1196(3) 0.9256(3) 0.3469(2) 0.0411(7) Uani 1 1 d . . .
N6 N -0.1065(3) 1.0050(4) 0.3898(2) 0.0567(9) Uani 1 1 d . . .
N7 N -0.0909(5) 1.0923(5) 0.4392(3) 0.0932(16) Uani 1 1 d . . .
O1 O -0.0484(3) 1.0249(2) 0.18401(15) 0.0441(6) Uani 1 1 d . . .
O2 O -0.1686(2) 0.7424(2) 0.22935(14) 0.0359(5) Uani 1 1 d . . .
O3 O -0.4437(3) 0.8128(2) 0.34349(16) 0.0484(6) Uani 1 1 d . . .
O4 O -0.3325(3) 0.8888(3) 0.19904(16) 0.0521(7) Uani 1 1 d . . .
H4A H -0.3402 0.8622 0.1480 0.063 Uiso 1 1 d R . .
H4B H -0.3329 0.9680 0.2124 0.063 Uiso 1 1 d R . .
O5 O -0.3603(6) 1.1196(6) 0.2532(4) 0.160(2) Uani 1 1 d . . .
H5B H -0.4350 1.1345 0.2210 0.192 Uiso 1 1 d R . .
O6 O -0.3892(4) 1.0639(4) 0.3959(3) 0.1126(14) Uani 1 1 d . . .
H6A H -0.3194 1.1131 0.4366 0.135 Uiso 1 1 d R . .
H6B H -0.4686 0.9950 0.4050 0.135 Uiso 1 1 d R . .
Ni1 Ni 0.00216(4) 0.91923(4) 0.26143(2) 0.03223(14) Uani 1 1 d . . .
Ni2 Ni -0.31346(4) 0.76051(4) 0.28988(2) 0.03386(14) 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
C1 0.0368(18) 0.0241(16) 0.0347(17) 0.0026(13) 0.0113(14) 0.0096(14)
C2 0.0413(19) 0.0305(17) 0.0419(19) 0.0053(15) 0.0104(16) 0.0159(15)
C3 0.047(2) 0.0375(19) 0.050(2) 0.0057(17) 0.0169(17) 0.0221(17)
C4 0.061(2) 0.0326(19) 0.044(2) -0.0007(16) 0.0162(18) 0.0194(18)
C5 0.047(2) 0.0341(19) 0.0376(19) -0.0043(15) 0.0055(16) 0.0078(16)
C6 0.0371(18) 0.0340(18) 0.0336(18) 0.0014(14) 0.0079(15) 0.0108(15)
C7 0.0409(19) 0.0387(19) 0.048(2) 0.0089(16) 0.0122(16) 0.0213(16)
C8 0.043(2) 0.043(2) 0.039(2) 0.0016(16) 0.0124(16) 0.0167(17)
C9 0.0363(18) 0.0400(19) 0.0347(18) 0.0044(15) 0.0047(15) 0.0087(16)
C10 0.0387(19) 0.0391(19) 0.0340(18) 0.0051(15) -0.0026(15) 0.0111(16)
C11 0.058(2) 0.044(2) 0.048(2) 0.0088(18) 0.0001(19) 0.0201(19)
C12 0.065(3) 0.042(2) 0.049(2) 0.0138(19) -0.009(2) 0.009(2)
C13 0.051(2) 0.058(3) 0.045(2) 0.021(2) 0.0032(19) -0.002(2)
C14 0.044(2) 0.061(3) 0.041(2) 0.0097(19) 0.0086(17) 0.0132(19)
C15 0.0268(17) 0.054(2) 0.058(2) -0.0021(19) 0.0044(16) 0.0149(17)
C16 0.0293(17) 0.046(2) 0.048(2) -0.0004(17) 0.0051(16) 0.0055(16)
C17 0.0348(18) 0.042(2) 0.0353(19) -0.0011(15) 0.0026(15) 0.0091(16)
C18 0.0321(18) 0.047(2) 0.050(2) 0.0021(17) 0.0024(16) 0.0163(16)
C19 0.0348(18) 0.047(2) 0.053(2) 0.0109(18) 0.0124(17) 0.0214(17)
C20 0.042(2) 0.047(2) 0.050(2) 0.0093(18) 0.0116(17) 0.0257(18)
C21 0.056(2) 0.064(3) 0.053(2) 0.010(2) 0.019(2) 0.033(2)
C22 0.075(3) 0.084(3) 0.067(3) 0.028(3) 0.039(3) 0.050(3)
C23 0.049(2) 0.062(3) 0.092(4) 0.034(3) 0.037(2) 0.027(2)
C24 0.043(2) 0.048(2) 0.070(3) 0.015(2) 0.015(2) 0.0227(19)
C25 0.046(2) 0.0316(18) 0.046(2) 0.0053(16) 0.0119(17) 0.0119(16)
C26 0.056(2) 0.050(2) 0.067(3) 0.016(2) 0.014(2) 0.018(2)
C27 0.052(2) 0.035(2) 0.056(2) -0.0081(18) 0.0171(19) 0.0036(17)
C28 0.059(3) 0.073(3) 0.044(2) 0.014(2) -0.001(2) 0.019(2)
C29 0.064(3) 0.090(4) 0.088(4) 0.041(3) 0.028(3) 0.048(3)
C30 0.099(4) 0.092(4) 0.050(3) 0.011(3) 0.014(3) 0.053(3)
C31 0.083(3) 0.057(3) 0.068(3) -0.020(2) 0.013(3) 0.029(3)
C32 0.174(9) 0.103(6) 0.254(12) 0.036(7) 0.100(9) 0.025(6)
N1 0.0304(14) 0.0338(15) 0.0399(16) 0.0010(12) 0.0035(12) 0.0119(12)
N2 0.0345(15) 0.0418(17) 0.0382(16) 0.0039(13) 0.0055(13) 0.0087(13)
N3 0.0281(14) 0.0331(15) 0.0403(16) 0.0017(12) 0.0062(12) 0.0121(12)
N4 0.0386(16) 0.0429(17) 0.0394(16) 0.0056(13) 0.0060(13) 0.0160(14)
N5 0.0287(15) 0.0272(15) 0.058(2) -0.0022(15) 0.0103(14) 0.0029(12)
N6 0.0349(18) 0.074(3) 0.052(2) 0.012(2) 0.0141(16) 0.0124(18)
N7 0.077(3) 0.087(3) 0.090(3) -0.038(3) 0.031(3) 0.008(2)
O1 0.0433(14) 0.0461(14) 0.0477(15) 0.0146(12) 0.0123(12) 0.0220(12)
O2 0.0306(12) 0.0306(12) 0.0426(13) -0.0016(10) 0.0092(10) 0.0088(10)
O3 0.0402(14) 0.0433(14) 0.0612(17) -0.0029(13) 0.0146(12) 0.0160(12)
O4 0.0538(16) 0.0441(15) 0.0591(17) 0.0080(13) 0.0060(13) 0.0231(13)
O5 0.106(4) 0.161(5) 0.233(7) -0.012(5) 0.025(4) 0.079(4)
O6 0.090(3) 0.088(3) 0.155(4) -0.011(3) 0.027(3) 0.034(2)
Ni1 0.0291(2) 0.0302(2) 0.0338(2) 0.00229(18) 0.00636(18) 0.00910(18)
Ni2 0.0307(2) 0.0310(2) 0.0374(3) 0.00039(18) 0.00665(18) 0.01092(19)

_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 O2 1.335(4) . ?
C1 C2 1.408(5) . ?
C1 C6 1.411(4) . ?
C2 C3 1.386(5) . ?
C2 C7 1.507(5) . ?
C3 C4 1.384(5) . ?
C4 C5 1.389(5) . ?
C4 C31 1.515(5) . ?
C5 C6 1.384(5) . ?
C6 C17 1.500(5) . ?
C7 N1 1.490(4) . ?
C8 N1 1.496(4) . ?
C8 C9 1.504(5) . ?
C9 C14 1.387(5) . ?
C9 C10 1.405(5) . ?
C10 O1 1.329(4) . ?
C10 C11 1.411(5) . ?
C11 C12 1.371(6) . ?
C12 C13 1.361(6) . ?
C13 C14 1.389(6) . ?
C15 N1 1.492(4) . ?
C15 C16 1.511(5) . ?
C16 N2 1.484(4) . ?
C17 N3 1.496(4) . ?
C18 C19 1.493(5) . ?
C18 N3 1.500(4) . ?
C19 C24 1.390(5) . ?
C19 C20 1.414(5) . ?
C20 O3 1.324(4) . ?
C20 C21 1.405(5) . ?
C21 C22 1.388(6) . ?
C22 C23 1.386(7) . ?
C23 C24 1.371(6) . ?
C25 N3 1.473(4) . ?
C25 C26 1.514(5) . ?
C26 N4 1.471(5) . ?
C27 N2 1.484(5) . ?
C28 N2 1.487(5) . ?
C29 N4 1.465(5) . ?
C30 N4 1.484(5) . ?
C32 O5 1.475(8) . ?
N1 Ni1 2.058(3) . ?
N2 Ni1 2.088(3) . ?
N3 Ni2 2.073(3) . ?
N4 Ni2 2.167(3) . ?
N5 N6 1.080(4) . ?
N5 Ni1 2.111(3) . ?
N5 Ni2 2.143(3) . ?
N6 N7 1.210(5) . ?
O1 Ni1 1.948(2) . ?
O2 Ni1 2.005(2) . ?
O2 Ni2 2.042(2) . ?
O3 Ni2 2.018(2) . ?
O4 Ni2 2.178(3) . ?

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
O2 C1 C2 120.6(3) . . ?
O2 C1 C6 120.8(3) . . ?
C2 C1 C6 118.5(3) . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 C7 119.9(3) . . ?
C1 C2 C7 120.4(3) . . ?
C4 C3 C2 122.6(3) . . ?
C3 C4 C5 117.1(3) . . ?
C3 C4 C31 121.8(4) . . ?
C5 C4 C31 121.2(4) . . ?
C6 C5 C4 122.7(3) . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 C17 119.1(3) . . ?
C1 C6 C17 121.4(3) . . ?
N1 C7 C2 115.2(3) . . ?
N1 C8 C9 115.4(3) . . ?
C14 C9 C10 119.6(3) . . ?
C14 C9 C8 120.6(3) . . ?
C10 C9 C8 119.6(3) . . ?
O1 C10 C9 122.0(3) . . ?
O1 C10 C11 120.2(4) . . ?
C9 C10 C11 117.7(3) . . ?
C12 C11 C10 121.1(4) . . ?
C13 C12 C11 121.1(4) . . ?
C12 C13 C14 119.3(4) . . ?
C9 C14 C13 121.2(4) . . ?
N1 C15 C16 111.0(3) . . ?
N2 C16 C15 110.1(3) . . ?
N3 C17 C6 115.6(3) . . ?
C19 C18 N3 115.2(3) . . ?
C24 C19 C20 119.7(4) . . ?
C24 C19 C18 120.6(4) . . ?
C20 C19 C18 119.6(3) . . ?
O3 C20 C21 120.8(4) . . ?
O3 C20 C19 121.3(3) . . ?
C21 C20 C19 117.9(4) . . ?
C22 C21 C20 121.0(4) . . ?
C23 C22 C21 120.3(4) . . ?
C24 C23 C22 119.4(4) . . ?
C23 C24 C19 121.7(4) . . ?
N3 C25 C26 111.8(3) . . ?
N4 C26 C25 112.0(3) . . ?
C7 N1 C15 109.0(3) . . ?
C7 N1 C8 109.6(3) . . ?
C15 N1 C8 111.8(3) . . ?
C7 N1 Ni1 109.0(2) . . ?
C15 N1 Ni1 108.0(2) . . ?
C8 N1 Ni1 109.3(2) . . ?
C27 N2 C16 108.8(3) . . ?
C27 N2 C28 109.0(3) . . ?
C16 N2 C28 111.4(3) . . ?
C27 N2 Ni1 113.1(2) . . ?
C16 N2 Ni1 105.6(2) . . ?
C28 N2 Ni1 109.0(2) . . ?
C25 N3 C17 111.1(3) . . ?
C25 N3 C18 111.9(3) . . ?
C17 N3 C18 106.3(3) . . ?
C25 N3 Ni2 109.5(2) . . ?
C17 N3 Ni2 109.3(2) . . ?
C18 N3 Ni2 108.6(2) . . ?
C29 N4 C26 113.0(3) . . ?
C29 N4 C30 106.9(3) . . ?
C26 N4 C30 107.8(3) . . ?
C29 N4 Ni2 113.6(2) . . ?
C26 N4 Ni2 104.6(2) . . ?
C30 N4 Ni2 110.9(3) . . ?
N6 N5 Ni1 131.8(3) . . ?
N6 N5 Ni2 128.4(3) . . ?
Ni1 N5 Ni2 95.61(13) . . ?
N5 N6 N7 178.4(5) . . ?
C10 O1 Ni1 121.4(2) . . ?
C1 O2 Ni1 128.44(19) . . ?
C1 O2 Ni2 128.94(19) . . ?
Ni1 O2 Ni2 102.31(10) . . ?
C20 O3 Ni2 123.6(2) . . ?
O1 Ni1 O2 99.06(10) . . ?
O1 Ni1 N1 96.74(11) . . ?
O2 Ni1 N1 91.59(10) . . ?
O1 Ni1 N2 101.10(11) . . ?
O2 Ni1 N2 159.83(11) . . ?
N1 Ni1 N2 85.51(11) . . ?
O1 Ni1 N5 100.57(11) . . ?
O2 Ni1 N5 80.28(10) . . ?
N1 Ni1 N5 161.82(11) . . ?
N2 Ni1 N5 96.51(11) . . ?
O3 Ni2 O2 169.46(10) . . ?
O3 Ni2 N3 94.57(10) . . ?
O2 Ni2 N3 91.69(10) . . ?
O3 Ni2 N5 95.34(11) . . ?
O2 Ni2 N5 78.72(11) . . ?
N3 Ni2 N5 170.00(11) . . ?
O3 Ni2 N4 95.18(11) . . ?
O2 Ni2 N4 93.89(10) . . ?
N3 Ni2 N4 84.16(11) . . ?
N5 Ni2 N4 93.60(11) . . ?
O3 Ni2 O4 87.63(11) . . ?
O2 Ni2 O4 83.51(10) . . ?
N3 Ni2 O4 93.56(10) . . ?
N5 Ni2 O4 88.20(11) . . ?
N4 Ni2 O4 176.51(11) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.073

#Additional comments:

#a) The accuracy of the hydrogen atom positions on the water
#and solvent hydroxyl groups is not great as they
#have not been placed for potentially strong hydrogen bonds.
#b) The void space as well as the unaccounted electron density were solved
#using SQUEEZE command and have now been included in the CIF (ESI).