# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Jose Garcia-Vazquez'
_publ_contact_author_email       JOSEARTURO.GARCIA@USC.ES

_publ_section_title              
;
Electrochemical Synthesis and Structural Characterization of
Co(II), Ni(II) and Cu(II) Complexes of
N,N-Bis(4,5-dimethyl-2-hydroxybenzyl)-N-(2-pyridylmethyl)amine
;
loop_
_publ_author_name
'Jose Garcia-Vazquez'
'Ernesto Cano'
'Elena Labisbal'
'Francisco Orallo'
'Jose Real'
;
L.Rodriguez
;
'Jaime Romero'
'Antonio Sousa'
'A Sousa-Pedrares'
'Oscar Souto'
'Matilde Yanez'

# Attachment 'DALTON.cif'

data_Compound1
_database_code_depnum_ccdc_archive 'CCDC 710317'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
;
bis-(m2-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine-di-cobalt(ii) monohydrate.
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H54 Co2 N4 O5'
_chemical_formula_weight         884.81

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'
Co Co 0.3494 0.9721 '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                   10.886(4)
_cell_length_b                   11.807(4)
_cell_length_c                   20.893(7)
_cell_angle_alpha                85.537(6)
_cell_angle_beta                 75.688(5)
_cell_angle_gamma                63.367(5)
_cell_volume                     2324.3(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    973
_cell_measurement_theta_min      2.192
_cell_measurement_theta_max      28.124

_exptl_crystal_description       Prism
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7021
_exptl_absorpt_correction_T_max  0.8444
_exptl_absorpt_process_details   
;
Sheldrick, G.M. SADABS: Program for absorption correction
using area detector data. University of G\"ottingen, Germany, 1996.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29164
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         27.48
_reflns_number_total             10551
_reflns_number_gt                8484
_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, 1997)'
_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^)+(0.0415P)^2^+0.5521P] 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         10551
_refine_ls_number_parameters     546
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0836
_refine_ls_wR_factor_gt          0.0799
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.002
_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
Co1 Co 0.52323(2) 0.053746(19) 0.806264(10) 0.01422(6) Uani 1 1 d . . .
Co2 Co 0.32782(2) 0.197544(19) 0.710703(10) 0.01508(6) Uani 1 1 d . . .
O1 O 0.48500(11) 0.02442(10) 0.72303(5) 0.0185(2) Uani 1 1 d . . .
O2 O 0.66356(11) 0.11451(10) 0.80047(5) 0.0187(2) Uani 1 1 d D . .
O3 O 0.33967(11) 0.21789(10) 0.80264(5) 0.0173(2) Uani 1 1 d . . .
O4 O 0.42853(12) 0.26430(11) 0.64220(6) 0.0217(3) Uani 1 1 d D . .
N1 N 0.68563(13) -0.14409(12) 0.80041(6) 0.0154(3) Uani 1 1 d . . .
N2 N 0.45469(14) -0.00751(12) 0.89856(6) 0.0160(3) Uani 1 1 d . . .
N3 N 0.13502(14) 0.37324(12) 0.71933(6) 0.0175(3) Uani 1 1 d . . .
N4 N 0.19598(14) 0.13215(13) 0.68745(7) 0.0193(3) Uani 1 1 d . . .
C1 C 0.57488(16) -0.06568(15) 0.67526(8) 0.0173(3) Uani 1 1 d . . .
C2 C 0.65466(17) -0.18921(15) 0.69272(8) 0.0176(3) Uani 1 1 d . . .
C3 C 0.74851(17) -0.27928(15) 0.64228(8) 0.0203(3) Uani 1 1 d . . .
H3 H 0.8040 -0.3630 0.6540 0.024 Uiso 1 1 calc R . .
C4 C 0.76411(17) -0.25181(16) 0.57598(8) 0.0216(4) Uani 1 1 d . . .
C5 C 0.68300(18) -0.12760(16) 0.55891(8) 0.0220(3) Uani 1 1 d . . .
C6 C 0.59027(18) -0.03671(16) 0.60849(8) 0.0215(3) Uani 1 1 d . . .
H6 H 0.5359 0.0473 0.5967 0.026 Uiso 1 1 calc R . .
C7 C 0.86747(19) -0.35288(18) 0.52382(9) 0.0282(4) Uani 1 1 d . . .
H7A H 0.9135 -0.4330 0.5450 0.042 Uiso 1 1 calc R . .
H7B H 0.9392 -0.3273 0.4987 0.042 Uiso 1 1 calc R . .
H7C H 0.8169 -0.3641 0.4939 0.042 Uiso 1 1 calc R . .
C8 C 0.6981(2) -0.09242(19) 0.48725(8) 0.0310(4) Uani 1 1 d . . .
H8A H 0.6312 -0.0037 0.4843 0.047 Uiso 1 1 calc R . .
H8B H 0.6779 -0.1471 0.4627 0.047 Uiso 1 1 calc R . .
H8C H 0.7948 -0.1037 0.4683 0.047 Uiso 1 1 calc R . .
C9 C 0.64574(17) -0.22171(15) 0.76391(8) 0.0181(3) Uani 1 1 d . . .
H9A H 0.5479 -0.2077 0.7854 0.022 Uiso 1 1 calc R . .
H9B H 0.7094 -0.3127 0.7667 0.022 Uiso 1 1 calc R . .
C10 C 0.82740(16) -0.15478(15) 0.76586(8) 0.0178(3) Uani 1 1 d . . .
H10A H 0.8250 -0.1248 0.7204 0.021 Uiso 1 1 calc R . .
H10B H 0.8974 -0.2451 0.7625 0.021 Uiso 1 1 calc R . .
C11 C 0.79140(17) 0.05148(15) 0.81314(7) 0.0169(3) Uani 1 1 d . . .
C12 C 0.84717(18) 0.11716(16) 0.84059(8) 0.0196(3) Uani 1 1 d . . .
H12 H 0.7941 0.2063 0.8480 0.024 Uiso 1 1 calc R . .
C13 C 0.97749(18) 0.05687(17) 0.85744(8) 0.0213(3) Uani 1 1 d . . .
C14 C 1.05866(18) -0.07392(17) 0.84509(8) 0.0232(4) Uani 1 1 d . . .
C15 C 1.00528(17) -0.13914(16) 0.81696(8) 0.0206(3) Uani 1 1 d . . .
H15 H 1.0600 -0.2280 0.8087 0.025 Uiso 1 1 calc R . .
C16 C 0.87455(16) -0.08005(15) 0.80022(8) 0.0172(3) Uani 1 1 d . . .
C17 C 1.2033(2) -0.14208(19) 0.86060(11) 0.0345(5) Uani 1 1 d . . .
H17A H 1.2442 -0.2326 0.8489 0.052 Uiso 1 1 calc R . .
H17B H 1.1935 -0.1312 0.9079 0.052 Uiso 1 1 calc R . .
H17C H 1.2654 -0.1065 0.8350 0.052 Uiso 1 1 calc R . .
C18 C 1.0266(2) 0.13299(18) 0.89031(9) 0.0289(4) Uani 1 1 d . . .
H18A H 0.9544 0.2215 0.8966 0.043 Uiso 1 1 calc R . .
H18B H 1.1153 0.1289 0.8623 0.043 Uiso 1 1 calc R . .
H18C H 1.0420 0.0981 0.9333 0.043 Uiso 1 1 calc R . .
C19 C 0.68492(17) -0.18908(15) 0.86804(8) 0.0186(3) Uani 1 1 d . . .
H19A H 0.7538 -0.1735 0.8848 0.022 Uiso 1 1 calc R . .
H19B H 0.7154 -0.2817 0.8673 0.022 Uiso 1 1 calc R . .
C20 C 0.54142(17) -0.12424(15) 0.91403(8) 0.0178(3) Uani 1 1 d . . .
C21 C 0.50546(19) -0.17938(17) 0.97172(8) 0.0258(4) Uani 1 1 d . . .
H21 H 0.5686 -0.2623 0.9811 0.031 Uiso 1 1 calc R . .
C22 C 0.3772(2) -0.11343(18) 1.01564(9) 0.0283(4) Uani 1 1 d . . .
H22 H 0.3510 -0.1500 1.0556 0.034 Uiso 1 1 calc R . .
C23 C 0.28713(18) 0.00741(16) 1.00035(8) 0.0226(4) Uani 1 1 d . . .
H23 H 0.1980 0.0550 1.0296 0.027 Uiso 1 1 calc R . .
C24 C 0.32970(17) 0.05682(16) 0.94182(8) 0.0184(3) Uani 1 1 d . . .
H24 H 0.2683 0.1397 0.9315 0.022 Uiso 1 1 calc R . .
C25 C 0.26866(17) 0.32690(15) 0.83991(7) 0.0180(3) Uani 1 1 d . . .
C26 C 0.13002(18) 0.41164(15) 0.83682(8) 0.0203(3) Uani 1 1 d . . .
C27 C 0.05829(19) 0.51888(16) 0.87925(8) 0.0250(4) Uani 1 1 d . . .
H27 H -0.0366 0.5750 0.8781 0.030 Uiso 1 1 calc R . .
C28 C 0.1183(2) 0.54774(16) 0.92302(8) 0.0268(4) Uani 1 1 d . . .
C29 C 0.2602(2) 0.46728(16) 0.92253(8) 0.0245(4) Uani 1 1 d . . .
C30 C 0.33256(19) 0.35812(15) 0.88150(8) 0.0216(4) Uani 1 1 d . . .
H30 H 0.4282 0.3033 0.8818 0.026 Uiso 1 1 calc R . .
C31 C 0.0311(2) 0.66259(17) 0.96963(9) 0.0372(5) Uani 1 1 d . . .
H31A H -0.0654 0.7048 0.9632 0.056 Uiso 1 1 calc R . .
H31B H 0.0738 0.7215 0.9606 0.056 Uiso 1 1 calc R . .
H31C H 0.0285 0.6360 1.0154 0.056 Uiso 1 1 calc R . .
C32 C 0.3339(2) 0.50041(18) 0.96509(9) 0.0345(5) Uani 1 1 d . . .
H32A H 0.4340 0.4390 0.9558 0.052 Uiso 1 1 calc R . .
H32B H 0.2897 0.4981 1.0118 0.052 Uiso 1 1 calc R . .
H32C H 0.3258 0.5857 0.9553 0.052 Uiso 1 1 calc R . .
C33 C 0.05627(17) 0.39058(16) 0.79009(8) 0.0211(3) Uani 1 1 d . . .
H33A H 0.0411 0.3145 0.8032 0.025 Uiso 1 1 calc R . .
H33B H -0.0379 0.4641 0.7946 0.025 Uiso 1 1 calc R . .
C34 C 0.16653(18) 0.48236(15) 0.69743(8) 0.0209(3) Uani 1 1 d . . .
H34A H 0.2234 0.4908 0.7255 0.025 Uiso 1 1 calc R . .
H34B H 0.0766 0.5611 0.7038 0.025 Uiso 1 1 calc R . .
C35 C 0.37122(18) 0.35809(16) 0.60260(8) 0.0204(3) Uani 1 1 d . . .
C36 C 0.43891(19) 0.34680(19) 0.53528(8) 0.0260(4) Uani 1 1 d . . .
H36 H 0.5216 0.2710 0.5188 0.031 Uiso 1 1 calc R . .
C37 C 0.3891(2) 0.4428(2) 0.49183(9) 0.0307(4) Uani 1 1 d . . .
C38 C 0.2685(2) 0.5549(2) 0.51583(9) 0.0318(4) Uani 1 1 d . . .
C39 C 0.19768(19) 0.56425(18) 0.58212(9) 0.0265(4) Uani 1 1 d . . .
H39 H 0.1133 0.6391 0.5980 0.032 Uiso 1 1 calc R . .
C40 C 0.24585(18) 0.46789(16) 0.62604(8) 0.0205(3) Uani 1 1 d . . .
C41 C 0.2116(2) 0.6623(2) 0.47052(12) 0.0496(6) Uani 1 1 d . . .
H41A H 0.1304 0.7346 0.4964 0.074 Uiso 1 1 calc R . .
H41B H 0.1818 0.6342 0.4368 0.074 Uiso 1 1 calc R . .
H41C H 0.2857 0.6878 0.4491 0.074 Uiso 1 1 calc R . .
C42 C 0.4634(2) 0.4215(2) 0.41937(9) 0.0436(6) Uani 1 1 d . . .
H42A H 0.5492 0.3406 0.4127 0.065 Uiso 1 1 calc R . .
H42B H 0.4890 0.4906 0.4047 0.065 Uiso 1 1 calc R . .
H42C H 0.4002 0.4194 0.3937 0.065 Uiso 1 1 calc R . .
C43 C 0.05015(17) 0.35605(16) 0.67933(8) 0.0204(3) Uani 1 1 d . . .
H43A H 0.0783 0.3788 0.6333 0.025 Uiso 1 1 calc R . .
H43B H -0.0511 0.4138 0.6970 0.025 Uiso 1 1 calc R . .
C44 C 0.06977(17) 0.22135(16) 0.67975(8) 0.0201(3) Uani 1 1 d . . .
C45 C -0.03261(19) 0.19080(18) 0.66890(8) 0.0250(4) Uani 1 1 d . . .
H45 H -0.1219 0.2556 0.6647 0.030 Uiso 1 1 calc R . .
C46 C -0.0027(2) 0.06444(19) 0.66428(9) 0.0294(4) Uani 1 1 d . . .
H46 H -0.0711 0.0413 0.6567 0.035 Uiso 1 1 calc R . .
C47 C 0.1280(2) -0.02800(18) 0.67088(9) 0.0285(4) Uani 1 1 d . . .
H47 H 0.1515 -0.1154 0.6671 0.034 Uiso 1 1 calc R . .
C48 C 0.22347(19) 0.00962(16) 0.68311(8) 0.0240(4) Uani 1 1 d . . .
H48 H 0.3123 -0.0537 0.6887 0.029 Uiso 1 1 calc R . .
O1S O 0.62914(19) 0.28314(18) 0.69777(9) 0.0553(5) Uani 1 1 d . . .
H1S H 0.633(3) 0.238(3) 0.7304(13) 0.083 Uiso 1 1 d D . .
H2S H 0.587(3) 0.261(3) 0.6725(14) 0.083 Uiso 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
Co1 0.01343(11) 0.01336(11) 0.01317(11) 0.00070(8) -0.00391(8) -0.00325(9)
Co2 0.01397(11) 0.01469(11) 0.01362(11) 0.00107(8) -0.00430(8) -0.00338(9)
O1 0.0162(6) 0.0155(5) 0.0156(5) -0.0022(4) -0.0046(4) 0.0009(5)
O2 0.0161(6) 0.0155(5) 0.0229(6) 0.0022(4) -0.0069(5) -0.0049(5)
O3 0.0175(6) 0.0135(5) 0.0152(5) -0.0013(4) -0.0052(4) -0.0009(5)
O4 0.0186(6) 0.0212(6) 0.0208(6) 0.0037(5) -0.0026(5) -0.0065(5)
N1 0.0141(6) 0.0160(6) 0.0149(6) 0.0019(5) -0.0041(5) -0.0055(5)
N2 0.0157(7) 0.0150(6) 0.0164(6) 0.0002(5) -0.0053(5) -0.0052(5)
N3 0.0160(7) 0.0174(7) 0.0162(7) 0.0038(5) -0.0054(5) -0.0048(6)
N4 0.0188(7) 0.0206(7) 0.0173(7) 0.0022(5) -0.0044(5) -0.0078(6)
C1 0.0139(7) 0.0176(8) 0.0175(8) -0.0040(6) -0.0036(6) -0.0039(6)
C2 0.0161(8) 0.0163(8) 0.0197(8) -0.0009(6) -0.0066(6) -0.0052(6)
C3 0.0177(8) 0.0151(8) 0.0263(9) -0.0041(6) -0.0071(7) -0.0041(7)
C4 0.0159(8) 0.0230(9) 0.0237(9) -0.0089(7) -0.0043(7) -0.0055(7)
C5 0.0202(8) 0.0248(9) 0.0196(8) -0.0027(7) -0.0051(7) -0.0082(7)
C6 0.0217(8) 0.0191(8) 0.0193(8) -0.0013(6) -0.0069(7) -0.0038(7)
C7 0.0225(9) 0.0283(10) 0.0270(9) -0.0124(7) -0.0028(7) -0.0048(8)
C8 0.0330(10) 0.0346(10) 0.0174(9) -0.0031(7) -0.0017(8) -0.0096(9)
C9 0.0195(8) 0.0139(7) 0.0206(8) 0.0005(6) -0.0062(6) -0.0066(7)
C10 0.0134(7) 0.0171(8) 0.0183(8) -0.0014(6) -0.0012(6) -0.0038(6)
C11 0.0170(8) 0.0203(8) 0.0127(7) 0.0037(6) -0.0036(6) -0.0083(7)
C12 0.0228(8) 0.0205(8) 0.0164(8) 0.0015(6) -0.0030(6) -0.0112(7)
C13 0.0240(9) 0.0296(9) 0.0152(8) 0.0034(7) -0.0048(7) -0.0165(8)
C14 0.0185(8) 0.0313(10) 0.0213(8) 0.0057(7) -0.0073(7) -0.0117(8)
C15 0.0171(8) 0.0202(8) 0.0207(8) 0.0018(6) -0.0036(6) -0.0056(7)
C16 0.0149(8) 0.0196(8) 0.0161(8) 0.0013(6) -0.0022(6) -0.0076(7)
C17 0.0251(10) 0.0356(11) 0.0476(12) 0.0066(9) -0.0188(9) -0.0133(9)
C18 0.0358(11) 0.0356(10) 0.0268(9) 0.0063(8) -0.0142(8) -0.0232(9)
C19 0.0169(8) 0.0174(8) 0.0175(8) 0.0040(6) -0.0058(6) -0.0038(7)
C20 0.0181(8) 0.0176(8) 0.0181(8) 0.0006(6) -0.0057(6) -0.0075(7)
C21 0.0255(9) 0.0219(9) 0.0230(9) 0.0064(7) -0.0041(7) -0.0064(8)
C22 0.0303(10) 0.0297(10) 0.0195(9) 0.0063(7) -0.0009(7) -0.0120(8)
C23 0.0190(8) 0.0252(9) 0.0193(8) -0.0035(7) 0.0001(7) -0.0078(7)
C24 0.0163(8) 0.0197(8) 0.0186(8) -0.0017(6) -0.0056(6) -0.0063(7)
C25 0.0220(8) 0.0130(7) 0.0130(7) 0.0014(6) -0.0035(6) -0.0031(7)
C26 0.0210(8) 0.0173(8) 0.0153(8) 0.0011(6) -0.0025(6) -0.0032(7)
C27 0.0260(9) 0.0174(8) 0.0181(8) 0.0012(6) -0.0026(7) 0.0006(7)
C28 0.0381(11) 0.0142(8) 0.0179(8) 0.0009(6) -0.0045(7) -0.0040(8)
C29 0.0368(10) 0.0176(8) 0.0164(8) 0.0029(6) -0.0082(7) -0.0091(8)
C30 0.0258(9) 0.0171(8) 0.0170(8) 0.0020(6) -0.0073(7) -0.0043(7)
C31 0.0518(13) 0.0197(9) 0.0231(9) -0.0047(7) -0.0048(9) -0.0025(9)
C32 0.0559(13) 0.0227(9) 0.0285(10) 0.0012(7) -0.0195(9) -0.0159(9)
C33 0.0160(8) 0.0210(8) 0.0175(8) 0.0029(6) -0.0021(6) -0.0017(7)
C34 0.0211(8) 0.0157(8) 0.0222(8) 0.0035(6) -0.0063(7) -0.0050(7)
C35 0.0210(8) 0.0248(9) 0.0202(8) 0.0043(7) -0.0066(7) -0.0140(7)
C36 0.0252(9) 0.0379(10) 0.0214(9) 0.0005(7) -0.0034(7) -0.0205(8)
C37 0.0348(11) 0.0540(13) 0.0199(9) 0.0085(8) -0.0100(8) -0.0335(10)
C38 0.0340(11) 0.0476(12) 0.0309(10) 0.0217(9) -0.0195(8) -0.0300(10)
C39 0.0254(9) 0.0285(10) 0.0317(10) 0.0126(8) -0.0146(8) -0.0151(8)
C40 0.0217(8) 0.0231(9) 0.0205(8) 0.0058(6) -0.0082(7) -0.0123(7)
C41 0.0454(13) 0.0741(17) 0.0478(13) 0.0425(12) -0.0284(11) -0.0399(13)
C42 0.0532(14) 0.0790(17) 0.0211(10) 0.0102(10) -0.0098(9) -0.0497(13)
C43 0.0164(8) 0.0231(9) 0.0202(8) 0.0052(6) -0.0077(6) -0.0064(7)
C44 0.0199(8) 0.0258(9) 0.0138(8) 0.0054(6) -0.0049(6) -0.0099(7)
C45 0.0209(9) 0.0376(10) 0.0186(8) 0.0071(7) -0.0066(7) -0.0148(8)
C46 0.0326(10) 0.0432(11) 0.0238(9) 0.0060(8) -0.0088(8) -0.0264(9)
C47 0.0365(11) 0.0296(10) 0.0251(9) 0.0034(7) -0.0063(8) -0.0205(9)
C48 0.0264(9) 0.0231(9) 0.0219(9) 0.0024(7) -0.0056(7) -0.0107(8)
O1S 0.0566(11) 0.0795(13) 0.0656(12) 0.0515(10) -0.0435(9) -0.0539(10)

_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
Co1 O2 1.9341(12) . ?
Co1 O1 1.9744(12) . ?
Co1 O3 2.0820(12) . ?
Co1 N2 2.0865(14) . ?
Co1 N1 2.1982(14) . ?
Co2 O4 1.9222(12) . ?
Co2 O3 1.9965(12) . ?
Co2 O1 2.0427(12) . ?
Co2 N4 2.0710(15) . ?
Co2 N3 2.1699(14) . ?
O1 C1 1.3544(18) . ?
O2 C11 1.3355(19) . ?
O3 C25 1.3515(18) . ?
O4 C35 1.339(2) . ?
N1 C19 1.470(2) . ?
N1 C10 1.486(2) . ?
N1 C9 1.496(2) . ?
N2 C20 1.346(2) . ?
N2 C24 1.348(2) . ?
N3 C43 1.473(2) . ?
N3 C34 1.488(2) . ?
N3 C33 1.492(2) . ?
N4 C44 1.345(2) . ?
N4 C48 1.345(2) . ?
C1 C6 1.397(2) . ?
C1 C2 1.397(2) . ?
C2 C3 1.398(2) . ?
C2 C9 1.497(2) . ?
C3 C4 1.384(2) . ?
C4 C5 1.404(2) . ?
C4 C7 1.507(2) . ?
C5 C6 1.389(2) . ?
C5 C8 1.511(2) . ?
C10 C16 1.498(2) . ?
C11 C12 1.401(2) . ?
C11 C16 1.410(2) . ?
C12 C13 1.395(2) . ?
C13 C14 1.399(2) . ?
C13 C18 1.508(2) . ?
C14 C15 1.384(2) . ?
C14 C17 1.519(2) . ?
C15 C16 1.397(2) . ?
C19 C20 1.500(2) . ?
C20 C21 1.379(2) . ?
C21 C22 1.378(2) . ?
C22 C23 1.389(3) . ?
C23 C24 1.379(2) . ?
C25 C30 1.398(2) . ?
C25 C26 1.403(2) . ?
C26 C27 1.395(2) . ?
C26 C33 1.505(2) . ?
C27 C28 1.386(3) . ?
C28 C29 1.403(3) . ?
C28 C31 1.511(2) . ?
C29 C30 1.394(2) . ?
C29 C32 1.509(3) . ?
C34 C40 1.507(2) . ?
C35 C40 1.402(2) . ?
C35 C36 1.403(2) . ?
C36 C37 1.391(3) . ?
C37 C38 1.395(3) . ?
C37 C42 1.510(3) . ?
C38 C39 1.394(3) . ?
C38 C41 1.512(3) . ?
C39 C40 1.397(2) . ?
C43 C44 1.506(2) . ?
C44 C45 1.386(2) . ?
C45 C46 1.383(3) . ?
C46 C47 1.384(3) . ?
C47 C48 1.380(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 Co1 O1 117.83(5) . . ?
O2 Co1 O3 103.79(5) . . ?
O1 Co1 O3 78.10(5) . . ?
O2 Co1 N2 115.89(5) . . ?
O1 Co1 N2 125.17(5) . . ?
O3 Co1 N2 99.28(5) . . ?
O2 Co1 N1 91.02(5) . . ?
O1 Co1 N1 89.75(5) . . ?
O3 Co1 N1 164.01(5) . . ?
N2 Co1 N1 79.14(5) . . ?
O4 Co2 O3 116.10(5) . . ?
O4 Co2 O1 101.70(5) . . ?
O3 Co2 O1 78.54(4) . . ?
O4 Co2 N4 119.18(6) . . ?
O3 Co2 N4 124.21(5) . . ?
O1 Co2 N4 96.99(6) . . ?
O4 Co2 N3 91.02(5) . . ?
O3 Co2 N3 92.78(5) . . ?
O1 Co2 N3 166.80(5) . . ?
N4 Co2 N3 79.57(6) . . ?
C1 O1 Co1 126.65(10) . . ?
C1 O1 Co2 126.79(10) . . ?
Co1 O1 Co2 101.86(5) . . ?
C11 O2 Co1 127.66(10) . . ?
C25 O3 Co2 125.34(9) . . ?
C25 O3 Co1 132.34(10) . . ?
Co2 O3 Co1 99.75(5) . . ?
C35 O4 Co2 126.17(10) . . ?
C19 N1 C10 110.80(12) . . ?
C19 N1 C9 108.57(13) . . ?
C10 N1 C9 110.21(12) . . ?
C19 N1 Co1 108.17(9) . . ?
C10 N1 Co1 110.91(9) . . ?
C9 N1 Co1 108.10(9) . . ?
C20 N2 C24 118.04(14) . . ?
C20 N2 Co1 116.12(11) . . ?
C24 N2 Co1 125.75(11) . . ?
C43 N3 C34 111.52(12) . . ?
C43 N3 C33 108.27(13) . . ?
C34 N3 C33 111.32(13) . . ?
C43 N3 Co2 107.37(10) . . ?
C34 N3 Co2 111.32(10) . . ?
C33 N3 Co2 106.82(9) . . ?
C44 N4 C48 118.34(15) . . ?
C44 N4 Co2 116.13(12) . . ?
C48 N4 Co2 125.43(12) . . ?
O1 C1 C6 120.93(14) . . ?
O1 C1 C2 119.79(14) . . ?
C6 C1 C2 119.28(14) . . ?
C1 C2 C3 118.34(15) . . ?
C1 C2 C9 120.53(14) . . ?
C3 C2 C9 121.03(14) . . ?
C4 C3 C2 122.88(15) . . ?
C3 C4 C5 118.37(15) . . ?
C3 C4 C7 120.44(16) . . ?
C5 C4 C7 121.19(16) . . ?
C6 C5 C4 119.45(16) . . ?
C6 C5 C8 120.21(16) . . ?
C4 C5 C8 120.34(15) . . ?
C5 C6 C1 121.69(16) . . ?
N1 C9 C2 112.31(13) . . ?
N1 C10 C16 113.00(13) . . ?
O2 C11 C12 119.48(15) . . ?
O2 C11 C16 122.91(14) . . ?
C12 C11 C16 117.61(15) . . ?
C13 C12 C11 122.64(16) . . ?
C12 C13 C14 119.34(16) . . ?
C12 C13 C18 119.49(16) . . ?
C14 C13 C18 121.14(16) . . ?
C15 C14 C13 118.33(15) . . ?
C15 C14 C17 120.81(17) . . ?
C13 C14 C17 120.84(16) . . ?
C14 C15 C16 122.90(16) . . ?
C15 C16 C11 119.13(15) . . ?
C15 C16 C10 120.11(15) . . ?
C11 C16 C10 120.68(14) . . ?
N1 C19 C20 112.10(13) . . ?
N2 C20 C21 122.16(15) . . ?
N2 C20 C19 116.95(14) . . ?
C21 C20 C19 120.74(15) . . ?
C22 C21 C20 119.56(16) . . ?
C21 C22 C23 118.79(16) . . ?
C24 C23 C22 118.64(16) . . ?
N2 C24 C23 122.80(15) . . ?
O3 C25 C30 120.69(14) . . ?
O3 C25 C26 120.52(15) . . ?
C30 C25 C26 118.79(15) . . ?
C27 C26 C25 118.24(16) . . ?
C27 C26 C33 119.18(15) . . ?
C25 C26 C33 122.58(14) . . ?
C28 C27 C26 123.38(16) . . ?
C27 C28 C29 118.01(15) . . ?
C27 C28 C31 120.09(17) . . ?
C29 C28 C31 121.90(17) . . ?
C30 C29 C28 119.31(16) . . ?
C30 C29 C32 120.64(17) . . ?
C28 C29 C32 120.04(16) . . ?
C29 C30 C25 122.03(16) . . ?
N3 C33 C26 114.05(14) . . ?
N3 C34 C40 112.65(14) . . ?
O4 C35 C40 122.34(15) . . ?
O4 C35 C36 119.08(16) . . ?
C40 C35 C36 118.58(16) . . ?
C37 C36 C35 122.27(18) . . ?
C36 C37 C38 119.17(17) . . ?
C36 C37 C42 119.3(2) . . ?
C38 C37 C42 121.47(19) . . ?
C39 C38 C37 118.63(17) . . ?
C39 C38 C41 120.3(2) . . ?
C37 C38 C41 120.97(19) . . ?
C38 C39 C40 122.61(18) . . ?
C39 C40 C35 118.59(16) . . ?
C39 C40 C34 120.86(16) . . ?
C35 C40 C34 120.54(15) . . ?
N3 C43 C44 111.54(13) . . ?
N4 C44 C45 122.11(16) . . ?
N4 C44 C43 115.76(15) . . ?
C45 C44 C43 122.02(15) . . ?
C46 C45 C44 118.93(17) . . ?
C45 C46 C47 119.30(17) . . ?
C48 C47 C46 118.52(17) . . ?
N4 C48 C47 122.78(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S O2 0.83(2) 1.96(2) 2.7879(19) 173(3) .
O1S H2S O4 0.89(2) 1.97(2) 2.810(2) 157(3) .

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.057

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
1 0.000 0.000 0.500 82.8 1.5
2 0.459 0.453 0.209 111.1 18.9
3 0.541 0.547 0.791 111.1 19.2
_platon_squeeze_details          
;
;

#===END

data_Compound2
_database_code_depnum_ccdc_archive 'CCDC 710318'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
;
m2-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine, m3-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine, (m2, m3)-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine-tri-nickel(ii)
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H78 N6 Ni3 O6'
_chemical_formula_weight         1299.53

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           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   51.673(9)
_cell_length_b                   13.205(2)
_cell_length_c                   21.820(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.747(3)
_cell_angle_gamma                90.00
_cell_volume                     14577(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1004
_cell_measurement_theta_min      2.915
_cell_measurement_theta_max      26.195

_exptl_crystal_description       Prism
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5472
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7464
_exptl_absorpt_correction_T_max  0.7915
_exptl_absorpt_process_details   
;
Sheldrick, G.M. SADABS: Program for absorption correction
using area detector data. University of G\"ottingen, Germany, 1996.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            62460
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         26.42
_reflns_number_total             14836
_reflns_number_gt                11217
_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, 1997)'
_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^)+(0.0483P)^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         14836
_refine_ls_number_parameters     797
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0922
_refine_ls_wR_factor_gt          0.0875
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.006
_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 0.628529(5) 0.884095(19) 0.661564(12) 0.01792(7) Uani 1 1 d . . .
Ni2 Ni 0.620481(5) 1.108704(19) 0.585337(12) 0.01787(7) Uani 1 1 d . . .
Ni3 Ni 0.659431(5) 1.067438(19) 0.693100(12) 0.01835(7) Uani 1 1 d . . .
O1 O 0.59078(3) 0.88292(11) 0.61168(7) 0.0246(3) Uani 1 1 d . . .
O2 O 0.66200(3) 0.92142(10) 0.72193(6) 0.0211(3) Uani 1 1 d . . .
O3 O 0.58806(3) 1.02705(11) 0.54793(7) 0.0267(3) Uani 1 1 d . . .
O4 O 0.64636(2) 0.98737(10) 0.60407(6) 0.0188(3) Uani 1 1 d . . .
O5 O 0.61934(2) 1.04246(10) 0.67919(6) 0.0195(3) Uani 1 1 d . . .
O6 O 0.65243(3) 1.18566(10) 0.63437(6) 0.0222(3) Uani 1 1 d . . .
N1 N 0.61738(3) 0.78209(12) 0.72691(7) 0.0194(4) Uani 1 1 d . . .
N2 N 0.63217(3) 0.74961(13) 0.61625(8) 0.0218(4) Uani 1 1 d . . .
N3 N 0.62841(3) 1.13213(12) 0.49729(8) 0.0201(4) Uani 1 1 d . . .
N4 N 0.59784(3) 1.23646(13) 0.56568(8) 0.0232(4) Uani 1 1 d . . .
N5 N 0.65845(3) 1.15286(13) 0.77166(8) 0.0233(4) Uani 1 1 d . . .
N6 N 0.69879(3) 1.10605(13) 0.71098(8) 0.0234(4) Uani 1 1 d . . .
C1 C 0.57403(4) 0.80272(15) 0.60528(10) 0.0226(4) Uani 1 1 d . . .
C2 C 0.57234(4) 0.74727(16) 0.65904(10) 0.0228(4) Uani 1 1 d . . .
C3 C 0.55448(4) 0.66755(16) 0.65237(11) 0.0275(5) Uani 1 1 d . . .
H3 H 0.5532 0.6287 0.6883 0.033 Uiso 1 1 calc R . .
C4 C 0.53839(4) 0.64211(16) 0.59556(11) 0.0290(5) Uani 1 1 d . . .
C5 C 0.54070(4) 0.69707(17) 0.54212(11) 0.0299(5) Uani 1 1 d . . .
C6 C 0.55886(4) 0.77621(16) 0.54769(10) 0.0255(5) Uani 1 1 d . . .
H6 H 0.5609 0.8126 0.5114 0.031 Uiso 1 1 calc R . .
C7 C 0.51755(5) 0.56090(19) 0.59206(13) 0.0421(6) Uani 1 1 d . . .
H7A H 0.5201 0.5249 0.6321 0.063 Uiso 1 1 calc R . .
H7B H 0.5190 0.5130 0.5587 0.063 Uiso 1 1 calc R . .
H7C H 0.5000 0.5921 0.5831 0.063 Uiso 1 1 calc R . .
C8 C 0.52325(5) 0.6750(2) 0.47869(12) 0.0438(6) Uani 1 1 d . . .
H8A H 0.5261 0.6052 0.4665 0.066 Uiso 1 1 calc R . .
H8B H 0.5277 0.7217 0.4475 0.066 Uiso 1 1 calc R . .
H8C H 0.5047 0.6839 0.4812 0.066 Uiso 1 1 calc R . .
C9 C 0.58796(4) 0.78060(17) 0.72150(10) 0.0245(5) Uani 1 1 d . . .
H9A H 0.5821 0.8495 0.7303 0.029 Uiso 1 1 calc R . .
H9B H 0.5838 0.7348 0.7541 0.029 Uiso 1 1 calc R . .
C10 C 0.62921(4) 0.81323(16) 0.79255(9) 0.0227(4) Uani 1 1 d . . .
H10A H 0.6229 0.7659 0.8215 0.027 Uiso 1 1 calc R . .
H10B H 0.6224 0.8814 0.7998 0.027 Uiso 1 1 calc R . .
C11 C 0.67355(4) 0.87673(15) 0.77567(9) 0.0214(4) Uani 1 1 d . . .
C12 C 0.70054(4) 0.89035(16) 0.79995(10) 0.0246(5) Uani 1 1 d . . .
H12 H 0.7106 0.9306 0.7773 0.030 Uiso 1 1 calc R . .
C13 C 0.71318(4) 0.84669(17) 0.85638(10) 0.0277(5) Uani 1 1 d . . .
C14 C 0.69904(4) 0.78235(17) 0.88819(10) 0.0279(5) Uani 1 1 d . . .
C15 C 0.67235(4) 0.76815(16) 0.86341(10) 0.0260(5) Uani 1 1 d . . .
H15 H 0.6627 0.7233 0.8844 0.031 Uiso 1 1 calc R . .
C16 C 0.65897(4) 0.81624(16) 0.80928(9) 0.0220(4) Uani 1 1 d . . .
C17 C 0.71173(5) 0.7341(2) 0.94991(11) 0.0397(6) Uani 1 1 d . . .
H17A H 0.6989 0.6900 0.9641 0.060 Uiso 1 1 calc R . .
H17B H 0.7175 0.7871 0.9812 0.060 Uiso 1 1 calc R . .
H17C H 0.7270 0.6939 0.9444 0.060 Uiso 1 1 calc R . .
C18 C 0.74178(5) 0.87425(19) 0.88316(12) 0.0395(6) Uani 1 1 d . . .
H18A H 0.7487 0.9157 0.8529 0.059 Uiso 1 1 calc R . .
H18B H 0.7523 0.8123 0.8919 0.059 Uiso 1 1 calc R . .
H18C H 0.7428 0.9125 0.9221 0.059 Uiso 1 1 calc R . .
C19 C 0.62711(4) 0.67931(16) 0.71478(10) 0.0241(5) Uani 1 1 d . . .
H19A H 0.6156 0.6274 0.7283 0.029 Uiso 1 1 calc R . .
H19B H 0.6453 0.6700 0.7394 0.029 Uiso 1 1 calc R . .
C20 C 0.62708(4) 0.66570(16) 0.64650(10) 0.0223(4) Uani 1 1 d . . .
C21 C 0.62286(4) 0.57269(17) 0.61670(11) 0.0298(5) Uani 1 1 d . . .
H21 H 0.6197 0.5139 0.6391 0.036 Uiso 1 1 calc R . .
C22 C 0.62338(5) 0.56716(19) 0.55390(12) 0.0391(6) Uani 1 1 d . . .
H22 H 0.6208 0.5040 0.5327 0.047 Uiso 1 1 calc R . .
C23 C 0.62756(5) 0.65310(19) 0.52219(11) 0.0351(6) Uani 1 1 d . . .
H23 H 0.6276 0.6508 0.4787 0.042 Uiso 1 1 calc R . .
C24 C 0.63177(4) 0.74284(17) 0.55465(10) 0.0269(5) Uani 1 1 d . . .
H24 H 0.6345 0.8026 0.5326 0.032 Uiso 1 1 calc R . .
C25 C 0.57258(4) 1.05412(15) 0.49210(10) 0.0238(5) Uani 1 1 d . . .
C26 C 0.54550(4) 1.06672(17) 0.48546(10) 0.0272(5) Uani 1 1 d . . .
H26 H 0.5374 1.0522 0.5199 0.033 Uiso 1 1 calc R . .
C27 C 0.52997(4) 1.10017(17) 0.42955(11) 0.0298(5) Uani 1 1 d . . .
C28 C 0.54188(4) 1.12177(18) 0.37884(11) 0.0335(5) Uani 1 1 d . . .
C29 C 0.56888(5) 1.10680(17) 0.38557(11) 0.0318(5) Uani 1 1 d . . .
H29 H 0.5770 1.1202 0.3511 0.038 Uiso 1 1 calc R . .
C30 C 0.58437(4) 1.07256(16) 0.44166(10) 0.0241(5) Uani 1 1 d . . .
C31 C 0.50080(5) 1.1152(2) 0.42511(13) 0.0446(7) Uani 1 1 d . . .
H31A H 0.4964 1.1015 0.4659 0.067 Uiso 1 1 calc R . .
H31B H 0.4910 1.0688 0.3938 0.067 Uiso 1 1 calc R . .
H31C H 0.4961 1.1852 0.4127 0.067 Uiso 1 1 calc R . .
C32 C 0.52582(5) 1.1606(3) 0.31753(13) 0.0576(8) Uani 1 1 d . . .
H32A H 0.5370 1.1642 0.2864 0.086 Uiso 1 1 calc R . .
H32B H 0.5190 1.2283 0.3238 0.086 Uiso 1 1 calc R . .
H32C H 0.5110 1.1146 0.3027 0.086 Uiso 1 1 calc R . .
C33 C 0.61383(4) 1.06011(17) 0.45000(10) 0.0254(5) Uani 1 1 d . . .
H33A H 0.6187 0.9899 0.4634 0.031 Uiso 1 1 calc R . .
H33B H 0.6191 1.0716 0.4094 0.031 Uiso 1 1 calc R . .
C34 C 0.65718(4) 1.12104(15) 0.49997(10) 0.0221(4) Uani 1 1 d . . .
H34A H 0.6665 1.1724 0.5294 0.027 Uiso 1 1 calc R . .
H34B H 0.6606 1.1372 0.4580 0.027 Uiso 1 1 calc R . .
C35 C 0.66548(4) 0.96374(15) 0.57149(9) 0.0180(4) Uani 1 1 d . . .
C36 C 0.68250(4) 0.88200(15) 0.59157(9) 0.0195(4) Uani 1 1 d . . .
H36 H 0.6806 0.8462 0.6282 0.023 Uiso 1 1 calc R . .
C37 C 0.70185(4) 0.85160(15) 0.56021(10) 0.0212(4) Uani 1 1 d . . .
C38 C 0.70503(4) 0.90327(16) 0.50613(10) 0.0232(5) Uani 1 1 d . . .
C39 C 0.68876(4) 0.98602(16) 0.48750(10) 0.0231(4) Uani 1 1 d . . .
H39 H 0.6909 1.0222 0.4512 0.028 Uiso 1 1 calc R . .
C40 C 0.66931(4) 1.01904(15) 0.51941(9) 0.0193(4) Uani 1 1 d . . .
C41 C 0.71946(4) 0.76274(17) 0.58398(11) 0.0287(5) Uani 1 1 d . . .
H41A H 0.7159 0.7404 0.6243 0.043 Uiso 1 1 calc R . .
H41B H 0.7380 0.7832 0.5893 0.043 Uiso 1 1 calc R . .
H41C H 0.7159 0.7070 0.5538 0.043 Uiso 1 1 calc R . .
C42 C 0.72575(4) 0.87162(18) 0.47021(11) 0.0317(5) Uani 1 1 d . . .
H42A H 0.7247 0.9155 0.4335 0.047 Uiso 1 1 calc R . .
H42B H 0.7227 0.8012 0.4565 0.047 Uiso 1 1 calc R . .
H42C H 0.7433 0.8777 0.4972 0.047 Uiso 1 1 calc R . .
C43 C 0.62050(4) 1.23802(15) 0.47910(10) 0.0237(5) Uani 1 1 d . . .
H43A H 0.6146 1.2417 0.4330 0.028 Uiso 1 1 calc R . .
H43B H 0.6360 1.2829 0.4913 0.028 Uiso 1 1 calc R . .
C44 C 0.59860(4) 1.27523(16) 0.50937(10) 0.0241(5) Uani 1 1 d . . .
C45 C 0.58121(5) 1.35008(19) 0.48224(12) 0.0378(6) Uani 1 1 d . . .
H45 H 0.5817 1.3751 0.4417 0.045 Uiso 1 1 calc R . .
C46 C 0.56318(5) 1.3876(2) 0.51508(14) 0.0529(8) Uani 1 1 d . . .
H46 H 0.5513 1.4401 0.4979 0.063 Uiso 1 1 calc R . .
C47 C 0.56254(5) 1.3482(2) 0.57313(14) 0.0502(8) Uani 1 1 d . . .
H47 H 0.5502 1.3728 0.5964 0.060 Uiso 1 1 calc R . .
C48 C 0.58005(4) 1.27256(18) 0.59704(11) 0.0336(5) Uani 1 1 d . . .
H48 H 0.5795 1.2451 0.6370 0.040 Uiso 1 1 calc R . .
C49 C 0.60342(4) 1.06716(15) 0.71954(10) 0.0209(4) Uani 1 1 d . . .
C50 C 0.61325(4) 1.09423(16) 0.78227(10) 0.0242(5) Uani 1 1 d . . .
C51 C 0.59533(5) 1.12054(16) 0.81921(11) 0.0287(5) Uani 1 1 d . . .
H51 H 0.6021 1.1398 0.8614 0.034 Uiso 1 1 calc R . .
C52 C 0.56821(5) 1.12021(17) 0.79804(11) 0.0317(5) Uani 1 1 d . . .
C53 C 0.55828(4) 1.09455(17) 0.73486(12) 0.0315(5) Uani 1 1 d . . .
C54 C 0.57605(4) 1.06797(16) 0.69755(11) 0.0260(5) Uani 1 1 d . . .
H54 H 0.5693 1.0495 0.6552 0.031 Uiso 1 1 calc R . .
C55 C 0.54998(5) 1.1497(2) 0.84147(13) 0.0486(7) Uani 1 1 d . . .
H55A H 0.5605 1.1711 0.8819 0.073 Uiso 1 1 calc R . .
H55B H 0.5391 1.0913 0.8477 0.073 Uiso 1 1 calc R . .
H55C H 0.5385 1.2055 0.8229 0.073 Uiso 1 1 calc R . .
C56 C 0.52918(5) 1.0979(2) 0.70718(14) 0.0500(7) Uani 1 1 d . . .
H56A H 0.5263 1.0833 0.6623 0.075 Uiso 1 1 calc R . .
H56B H 0.5223 1.1653 0.7135 0.075 Uiso 1 1 calc R . .
H56C H 0.5200 1.0471 0.7277 0.075 Uiso 1 1 calc R . .
C57 C 0.64250(4) 1.09946(16) 0.81122(10) 0.0253(5) Uani 1 1 d . . .
H57A H 0.6448 1.1345 0.8521 0.030 Uiso 1 1 calc R . .
H57B H 0.6494 1.0297 0.8192 0.030 Uiso 1 1 calc R . .
C58 C 0.64652(4) 1.25541(16) 0.75405(10) 0.0256(5) Uani 1 1 d . . .
H58A H 0.6278 1.2463 0.7328 0.031 Uiso 1 1 calc R . .
H58B H 0.6467 1.2946 0.7928 0.031 Uiso 1 1 calc R . .
C59 C 0.66111(4) 1.27959(15) 0.65212(10) 0.0221(4) Uani 1 1 d . . .
C60 C 0.67250(4) 1.34159(16) 0.61324(10) 0.0269(5) Uani 1 1 d . . .
H60 H 0.6732 1.3181 0.5724 0.032 Uiso 1 1 calc R . .
C61 C 0.68294(4) 1.43657(16) 0.63167(11) 0.0279(5) Uani 1 1 d . . .
C62 C 0.68236(4) 1.47148(16) 0.69187(11) 0.0270(5) Uani 1 1 d . . .
C63 C 0.67099(4) 1.41024(16) 0.73065(11) 0.0268(5) Uani 1 1 d . . .
H63 H 0.6705 1.4338 0.7715 0.032 Uiso 1 1 calc R . .
C64 C 0.66029(4) 1.31552(16) 0.71226(10) 0.0234(4) Uani 1 1 d . . .
C65 C 0.69381(5) 1.57292(17) 0.71424(12) 0.0355(6) Uani 1 1 d . . .
H65A H 0.6913 1.5850 0.7569 0.053 Uiso 1 1 calc R . .
H65B H 0.6849 1.6262 0.6865 0.053 Uiso 1 1 calc R . .
H65C H 0.7127 1.5736 0.7139 0.053 Uiso 1 1 calc R . .
C66 C 0.69402(5) 1.50085(18) 0.58621(12) 0.0391(6) Uani 1 1 d . . .
H66A H 0.6943 1.4617 0.5482 0.059 Uiso 1 1 calc R . .
H66B H 0.7121 1.5216 0.6054 0.059 Uiso 1 1 calc R . .
H66C H 0.6830 1.5611 0.5755 0.059 Uiso 1 1 calc R . .
C67 C 0.68599(4) 1.16314(18) 0.80566(10) 0.0287(5) Uani 1 1 d . . .
H67A H 0.6904 1.1057 0.8351 0.034 Uiso 1 1 calc R . .
H67B H 0.6878 1.2264 0.8305 0.034 Uiso 1 1 calc R . .
C68 C 0.70507(4) 1.16525(16) 0.76225(10) 0.0266(5) Uani 1 1 d . . .
C69 C 0.72841(4) 1.22038(18) 0.77538(11) 0.0342(5) Uani 1 1 d . . .
H69 H 0.7323 1.2629 0.8112 0.041 Uiso 1 1 calc R . .
C70 C 0.74587(5) 1.21246(19) 0.73560(12) 0.0388(6) Uani 1 1 d . . .
H70 H 0.7620 1.2494 0.7437 0.047 Uiso 1 1 calc R . .
C71 C 0.73969(4) 1.15057(18) 0.68416(12) 0.0338(5) Uani 1 1 d . . .
H71 H 0.7517 1.1428 0.6569 0.041 Uiso 1 1 calc R . .
C72 C 0.71581(4) 1.09955(17) 0.67236(11) 0.0290(5) Uani 1 1 d . . .
H72 H 0.7114 1.0588 0.6359 0.035 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01900(13) 0.01982(14) 0.01499(13) 0.00035(10) 0.00354(10) -0.00138(10)
Ni2 0.01865(13) 0.01872(13) 0.01621(14) 0.00074(10) 0.00349(10) 0.00111(10)
Ni3 0.01861(13) 0.02012(14) 0.01616(13) 0.00002(11) 0.00315(10) -0.00104(10)
O1 0.0230(7) 0.0241(8) 0.0241(8) 0.0030(6) -0.0013(6) -0.0060(6)
O2 0.0213(7) 0.0230(7) 0.0178(7) 0.0027(6) 0.0011(6) -0.0020(6)
O3 0.0225(8) 0.0309(8) 0.0231(8) 0.0072(7) -0.0041(6) -0.0039(6)
O4 0.0179(7) 0.0233(7) 0.0168(7) 0.0008(6) 0.0070(6) 0.0011(6)
O5 0.0192(7) 0.0241(8) 0.0163(7) -0.0016(6) 0.0066(6) -0.0009(6)
O6 0.0256(7) 0.0197(7) 0.0201(7) -0.0004(6) 0.0017(6) -0.0029(6)
N1 0.0190(8) 0.0230(9) 0.0159(9) -0.0004(7) 0.0029(7) -0.0005(7)
N2 0.0189(8) 0.0257(9) 0.0209(9) -0.0006(7) 0.0044(7) -0.0020(7)
N3 0.0230(9) 0.0190(9) 0.0180(9) 0.0030(7) 0.0037(7) 0.0025(7)
N4 0.0237(9) 0.0229(9) 0.0230(10) -0.0006(8) 0.0051(7) 0.0015(7)
N5 0.0244(9) 0.0261(9) 0.0179(9) 0.0005(8) 0.0008(7) -0.0012(7)
N6 0.0217(9) 0.0233(9) 0.0238(10) 0.0034(8) 0.0011(7) 0.0001(7)
C1 0.0185(10) 0.0216(11) 0.0276(12) -0.0007(9) 0.0043(9) -0.0017(8)
C2 0.0179(10) 0.0239(11) 0.0264(12) 0.0003(9) 0.0039(9) 0.0010(8)
C3 0.0239(11) 0.0221(11) 0.0370(13) 0.0049(10) 0.0072(10) -0.0018(9)
C4 0.0212(11) 0.0238(12) 0.0405(14) 0.0001(10) 0.0026(10) -0.0021(9)
C5 0.0247(11) 0.0280(12) 0.0352(13) -0.0045(10) 0.0017(10) -0.0008(9)
C6 0.0243(11) 0.0253(11) 0.0261(12) 0.0015(9) 0.0031(9) -0.0020(9)
C7 0.0293(13) 0.0361(14) 0.0587(18) 0.0003(13) 0.0039(12) -0.0087(11)
C8 0.0402(14) 0.0435(16) 0.0428(16) -0.0020(12) -0.0026(12) -0.0107(12)
C9 0.0235(11) 0.0283(12) 0.0238(11) 0.0043(9) 0.0097(9) 0.0010(9)
C10 0.0295(11) 0.0246(11) 0.0146(10) 0.0008(8) 0.0058(9) -0.0022(9)
C11 0.0246(11) 0.0233(11) 0.0156(10) -0.0031(8) 0.0027(8) 0.0045(8)
C12 0.0230(11) 0.0260(11) 0.0240(11) -0.0013(9) 0.0025(9) 0.0022(9)
C13 0.0256(11) 0.0317(12) 0.0230(11) -0.0068(10) -0.0017(9) 0.0071(9)
C14 0.0338(12) 0.0303(12) 0.0174(11) -0.0009(9) 0.0000(9) 0.0101(10)
C15 0.0354(12) 0.0245(11) 0.0190(11) 0.0006(9) 0.0077(9) 0.0058(9)
C16 0.0256(11) 0.0248(11) 0.0148(10) -0.0025(8) 0.0025(8) 0.0030(9)
C17 0.0432(14) 0.0474(15) 0.0235(12) 0.0031(11) -0.0050(11) 0.0120(12)
C18 0.0311(13) 0.0457(15) 0.0361(14) -0.0025(12) -0.0066(11) 0.0089(11)
C19 0.0243(11) 0.0238(11) 0.0236(11) 0.0021(9) 0.0032(9) 0.0012(9)
C20 0.0172(10) 0.0248(11) 0.0243(11) 0.0000(9) 0.0028(8) 0.0017(8)
C21 0.0320(12) 0.0243(11) 0.0310(13) -0.0044(10) 0.0019(10) -0.0030(10)
C22 0.0462(15) 0.0329(14) 0.0384(15) -0.0144(12) 0.0092(12) -0.0058(11)
C23 0.0407(14) 0.0405(14) 0.0254(12) -0.0092(11) 0.0098(10) -0.0035(11)
C24 0.0255(11) 0.0339(13) 0.0230(11) -0.0049(10) 0.0087(9) -0.0050(9)
C25 0.0226(11) 0.0212(11) 0.0241(11) -0.0005(9) -0.0038(9) -0.0016(8)
C26 0.0257(11) 0.0294(12) 0.0253(12) -0.0008(10) 0.0027(9) -0.0025(9)
C27 0.0230(11) 0.0303(12) 0.0330(13) -0.0036(10) -0.0018(10) 0.0019(9)
C28 0.0309(12) 0.0406(14) 0.0245(12) 0.0008(10) -0.0046(10) 0.0011(10)
C29 0.0349(13) 0.0368(13) 0.0215(12) -0.0009(10) 0.0008(10) -0.0014(10)
C30 0.0262(11) 0.0241(11) 0.0202(11) -0.0010(9) 0.0002(9) -0.0011(9)
C31 0.0293(13) 0.0546(17) 0.0469(16) 0.0016(13) 0.0002(12) 0.0064(12)
C32 0.0425(16) 0.087(2) 0.0370(16) 0.0170(16) -0.0069(12) 0.0039(16)
C33 0.0289(11) 0.0295(12) 0.0172(11) -0.0012(9) 0.0030(9) 0.0026(9)
C34 0.0228(11) 0.0246(11) 0.0209(11) 0.0027(9) 0.0089(9) 0.0003(8)
C35 0.0166(10) 0.0213(10) 0.0162(10) -0.0038(8) 0.0035(8) -0.0013(8)
C36 0.0205(10) 0.0196(10) 0.0186(10) 0.0002(8) 0.0043(8) -0.0018(8)
C37 0.0186(10) 0.0220(11) 0.0230(11) -0.0004(9) 0.0040(8) -0.0005(8)
C38 0.0214(10) 0.0259(11) 0.0231(11) -0.0034(9) 0.0065(9) -0.0005(8)
C39 0.0247(11) 0.0270(12) 0.0190(11) 0.0011(9) 0.0081(9) -0.0013(9)
C40 0.0198(10) 0.0201(10) 0.0177(10) 0.0001(8) 0.0035(8) 0.0001(8)
C41 0.0280(12) 0.0303(12) 0.0297(12) 0.0048(10) 0.0104(10) 0.0065(9)
C42 0.0343(13) 0.0364(13) 0.0273(12) 0.0034(10) 0.0137(10) 0.0059(10)
C43 0.0275(11) 0.0212(11) 0.0221(11) 0.0039(9) 0.0045(9) 0.0037(9)
C44 0.0257(11) 0.0200(11) 0.0257(12) 0.0007(9) 0.0031(9) -0.0001(8)
C45 0.0424(14) 0.0377(14) 0.0346(14) 0.0087(11) 0.0112(11) 0.0134(11)
C46 0.0488(17) 0.0532(18) 0.0600(19) 0.0255(15) 0.0192(15) 0.0310(14)
C47 0.0523(17) 0.0510(17) 0.0562(18) 0.0135(14) 0.0320(15) 0.0296(14)
C48 0.0368(13) 0.0332(13) 0.0344(13) 0.0043(11) 0.0153(11) 0.0071(10)
C49 0.0235(10) 0.0190(10) 0.0225(11) -0.0013(9) 0.0104(9) -0.0030(8)
C50 0.0297(11) 0.0233(11) 0.0210(11) 0.0014(9) 0.0087(9) 0.0000(9)
C51 0.0417(13) 0.0247(12) 0.0230(12) 0.0006(9) 0.0147(10) 0.0010(10)
C52 0.0366(13) 0.0278(12) 0.0369(14) 0.0001(10) 0.0216(11) 0.0000(10)
C53 0.0278(12) 0.0305(13) 0.0404(14) -0.0030(10) 0.0167(11) -0.0004(9)
C54 0.0229(11) 0.0279(12) 0.0287(12) -0.0004(10) 0.0088(9) -0.0010(9)
C55 0.0529(17) 0.0504(17) 0.0518(17) -0.0042(14) 0.0328(14) 0.0016(13)
C56 0.0294(14) 0.0593(18) 0.066(2) -0.0183(15) 0.0216(13) -0.0052(12)
C57 0.0321(12) 0.0258(12) 0.0182(11) -0.0021(9) 0.0054(9) 0.0004(9)
C58 0.0294(11) 0.0241(11) 0.0240(11) -0.0032(9) 0.0071(9) 0.0013(9)
C59 0.0204(10) 0.0198(11) 0.0244(11) 0.0013(9) 0.0007(8) 0.0001(8)
C60 0.0330(12) 0.0248(12) 0.0229(11) 0.0014(9) 0.0056(9) -0.0016(9)
C61 0.0245(11) 0.0243(12) 0.0339(13) 0.0048(10) 0.0036(9) -0.0022(9)
C62 0.0229(11) 0.0199(11) 0.0357(13) -0.0012(10) 0.0001(9) -0.0004(9)
C63 0.0269(11) 0.0248(12) 0.0266(12) -0.0041(9) 0.0004(9) 0.0014(9)
C64 0.0228(10) 0.0213(11) 0.0248(11) -0.0002(9) 0.0015(9) 0.0000(8)
C65 0.0346(13) 0.0250(12) 0.0448(15) -0.0041(11) 0.0035(11) -0.0054(10)
C66 0.0471(15) 0.0279(13) 0.0430(15) 0.0035(11) 0.0107(12) -0.0080(11)
C67 0.0296(12) 0.0304(12) 0.0235(12) -0.0037(10) -0.0008(9) -0.0031(10)
C68 0.0242(11) 0.0251(12) 0.0265(12) 0.0047(9) -0.0040(9) -0.0002(9)
C69 0.0282(12) 0.0343(13) 0.0347(13) 0.0001(11) -0.0064(10) -0.0048(10)
C70 0.0243(12) 0.0350(14) 0.0531(17) 0.0092(12) -0.0019(11) -0.0063(10)
C71 0.0251(12) 0.0371(14) 0.0393(14) 0.0073(11) 0.0071(10) -0.0022(10)
C72 0.0260(12) 0.0291(12) 0.0314(13) 0.0040(10) 0.0046(10) -0.0002(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.0103(14) . ?
Ni1 O1 2.0313(14) . ?
Ni1 N2 2.0598(17) . ?
Ni1 N1 2.1245(16) . ?
Ni1 O4 2.1801(13) . ?
Ni1 O5 2.1956(14) . ?
Ni1 Ni3 2.9047(5) . ?
Ni2 O3 2.0195(14) . ?
Ni2 O6 2.0452(14) . ?
Ni2 N4 2.0480(17) . ?
Ni2 N3 2.0676(17) . ?
Ni2 O4 2.0734(13) . ?
Ni2 O5 2.2386(14) . ?
Ni2 Ni3 2.8195(5) . ?
Ni3 O6 2.0053(14) . ?
Ni3 O2 2.0241(14) . ?
Ni3 N6 2.0555(17) . ?
Ni3 O5 2.0582(13) . ?
Ni3 N5 2.0612(17) . ?
Ni3 O4 2.1939(14) . ?
O1 C1 1.357(2) . ?
O2 C11 1.340(2) . ?
O3 C25 1.362(2) . ?
O4 C35 1.366(2) . ?
O5 C49 1.361(2) . ?
O6 C59 1.349(2) . ?
N1 C19 1.490(3) . ?
N1 C10 1.496(2) . ?
N1 C9 1.501(2) . ?
N2 C24 1.343(3) . ?
N2 C20 1.343(3) . ?
N3 C34 1.483(2) . ?
N3 C43 1.488(2) . ?
N3 C33 1.490(3) . ?
N4 C44 1.339(3) . ?
N4 C48 1.341(3) . ?
N5 C67 1.471(3) . ?
N5 C57 1.487(3) . ?
N5 C58 1.505(3) . ?
N6 C72 1.339(3) . ?
N6 C68 1.349(3) . ?
C1 C6 1.384(3) . ?
C1 C2 1.400(3) . ?
C2 C3 1.388(3) . ?
C2 C9 1.501(3) . ?
C3 C4 1.386(3) . ?
C4 C5 1.399(3) . ?
C4 C7 1.511(3) . ?
C5 C6 1.393(3) . ?
C5 C8 1.518(3) . ?
C10 C16 1.507(3) . ?
C11 C12 1.399(3) . ?
C11 C16 1.403(3) . ?
C12 C13 1.396(3) . ?
C13 C14 1.394(3) . ?
C13 C18 1.519(3) . ?
C14 C15 1.387(3) . ?
C14 C17 1.513(3) . ?
C15 C16 1.394(3) . ?
C19 C20 1.500(3) . ?
C20 C21 1.386(3) . ?
C21 C22 1.378(3) . ?
C22 C23 1.369(3) . ?
C23 C24 1.375(3) . ?
C25 C30 1.384(3) . ?
C25 C26 1.387(3) . ?
C26 C27 1.389(3) . ?
C27 C28 1.401(3) . ?
C27 C31 1.504(3) . ?
C28 C29 1.387(3) . ?
C28 C32 1.513(3) . ?
C29 C30 1.394(3) . ?
C30 C33 1.505(3) . ?
C34 C40 1.509(3) . ?
C35 C40 1.398(3) . ?
C35 C36 1.405(3) . ?
C36 C37 1.381(3) . ?
C37 C38 1.401(3) . ?
C37 C41 1.511(3) . ?
C38 C39 1.388(3) . ?
C38 C42 1.509(3) . ?
C39 C40 1.404(3) . ?
C43 C44 1.504(3) . ?
C44 C45 1.385(3) . ?
C45 C46 1.378(3) . ?
C46 C47 1.376(4) . ?
C47 C48 1.377(3) . ?
C49 C54 1.398(3) . ?
C49 C50 1.406(3) . ?
C50 C51 1.390(3) . ?
C50 C57 1.516(3) . ?
C51 C52 1.383(3) . ?
C52 C53 1.411(3) . ?
C52 C55 1.517(3) . ?
C53 C54 1.390(3) . ?
C53 C56 1.503(3) . ?
C58 C64 1.494(3) . ?
C59 C60 1.393(3) . ?
C59 C64 1.404(3) . ?
C60 C61 1.392(3) . ?
C61 C62 1.398(3) . ?
C61 C66 1.505(3) . ?
C62 C63 1.385(3) . ?
C62 C65 1.505(3) . ?
C63 C64 1.393(3) . ?
C67 C68 1.500(3) . ?
C68 C69 1.388(3) . ?
C69 C70 1.377(3) . ?
C70 C71 1.373(3) . ?
C71 C72 1.383(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 Ni1 O1 163.18(6) . . ?
O2 Ni1 N2 112.05(6) . . ?
O1 Ni1 N2 84.71(6) . . ?
O2 Ni1 N1 91.74(6) . . ?
O1 Ni1 N1 89.58(6) . . ?
N2 Ni1 N1 80.75(6) . . ?
O2 Ni1 O4 79.38(5) . . ?
O1 Ni1 O4 99.71(5) . . ?
N2 Ni1 O4 99.93(6) . . ?
N1 Ni1 O4 170.71(6) . . ?
O2 Ni1 O5 80.77(5) . . ?
O1 Ni1 O5 83.27(5) . . ?
N2 Ni1 O5 161.70(6) . . ?
N1 Ni1 O5 112.86(6) . . ?
O4 Ni1 O5 68.70(5) . . ?
O2 Ni1 Ni3 44.14(4) . . ?
O1 Ni1 Ni3 123.71(4) . . ?
N2 Ni1 Ni3 137.12(5) . . ?
N1 Ni1 Ni3 125.49(5) . . ?
O4 Ni1 Ni3 48.59(4) . . ?
O5 Ni1 Ni3 44.98(3) . . ?
O3 Ni2 O6 172.50(6) . . ?
O3 Ni2 N4 87.92(6) . . ?
O6 Ni2 N4 93.79(6) . . ?
O3 Ni2 N3 90.54(6) . . ?
O6 Ni2 N3 96.90(6) . . ?
N4 Ni2 N3 83.97(7) . . ?
O3 Ni2 O4 96.64(6) . . ?
O6 Ni2 O4 82.03(5) . . ?
N4 Ni2 O4 174.71(6) . . ?
N3 Ni2 O4 93.26(6) . . ?
O3 Ni2 O5 89.25(5) . . ?
O6 Ni2 O5 83.36(5) . . ?
N4 Ni2 O5 113.15(6) . . ?
N3 Ni2 O5 162.85(6) . . ?
O4 Ni2 O5 69.74(5) . . ?
O3 Ni2 Ni3 128.79(4) . . ?
O6 Ni2 Ni3 45.31(4) . . ?
N4 Ni2 Ni3 127.89(5) . . ?
N3 Ni2 Ni3 124.12(5) . . ?
O4 Ni2 Ni3 50.51(4) . . ?
O5 Ni2 Ni3 46.28(3) . . ?
O6 Ni3 O2 158.75(6) . . ?
O6 Ni3 N6 88.34(6) . . ?
O2 Ni3 N6 100.23(6) . . ?
O6 Ni3 O5 89.15(5) . . ?
O2 Ni3 O5 83.89(5) . . ?
N6 Ni3 O5 174.25(6) . . ?
O6 Ni3 N5 94.22(6) . . ?
O2 Ni3 N5 105.90(6) . . ?
N6 Ni3 N5 84.11(7) . . ?
O5 Ni3 N5 90.91(6) . . ?
O6 Ni3 O4 80.00(5) . . ?
O2 Ni3 O4 78.76(5) . . ?
N6 Ni3 O4 113.70(6) . . ?
O5 Ni3 O4 70.91(5) . . ?
N5 Ni3 O4 160.86(6) . . ?
O6 Ni3 Ni2 46.47(4) . . ?
O2 Ni3 Ni2 115.71(4) . . ?
N6 Ni3 Ni2 128.39(5) . . ?
O5 Ni3 Ni2 51.82(4) . . ?
N5 Ni3 Ni2 116.97(5) . . ?
O4 Ni3 Ni2 46.83(4) . . ?
O6 Ni3 Ni1 118.58(4) . . ?
O2 Ni3 Ni1 43.76(4) . . ?
N6 Ni3 Ni1 136.61(5) . . ?
O5 Ni3 Ni1 48.95(4) . . ?
N5 Ni3 Ni1 123.21(5) . . ?
O4 Ni3 Ni1 48.18(3) . . ?
Ni2 Ni3 Ni1 72.474(12) . . ?
C1 O1 Ni1 125.72(12) . . ?
C11 O2 Ni1 129.49(13) . . ?
C11 O2 Ni3 132.92(13) . . ?
Ni1 O2 Ni3 92.10(6) . . ?
C25 O3 Ni2 120.62(12) . . ?
C35 O4 Ni2 125.44(12) . . ?
C35 O4 Ni1 126.29(12) . . ?
Ni2 O4 Ni1 105.41(5) . . ?
C35 O4 Ni3 116.49(11) . . ?
Ni2 O4 Ni3 82.66(5) . . ?
Ni1 O4 Ni3 83.22(5) . . ?
C49 O5 Ni3 126.08(12) . . ?
C49 O5 Ni1 121.47(12) . . ?
Ni3 O5 Ni1 86.07(5) . . ?
C49 O5 Ni2 129.04(12) . . ?
Ni3 O5 Ni2 81.90(5) . . ?
Ni1 O5 Ni2 99.50(5) . . ?
C59 O6 Ni3 121.75(12) . . ?
C59 O6 Ni2 142.48(12) . . ?
Ni3 O6 Ni2 88.22(5) . . ?
C19 N1 C10 109.49(15) . . ?
C19 N1 C9 110.32(16) . . ?
C10 N1 C9 106.79(15) . . ?
C19 N1 Ni1 108.12(12) . . ?
C10 N1 Ni1 110.76(12) . . ?
C9 N1 Ni1 111.37(12) . . ?
C24 N2 C20 118.19(18) . . ?
C24 N2 Ni1 123.61(15) . . ?
C20 N2 Ni1 115.41(13) . . ?
C34 N3 C43 108.79(15) . . ?
C34 N3 C33 109.02(15) . . ?
C43 N3 C33 110.01(16) . . ?
C34 N3 Ni2 109.60(12) . . ?
C43 N3 Ni2 107.02(12) . . ?
C33 N3 Ni2 112.33(12) . . ?
C44 N4 C48 118.94(18) . . ?
C44 N4 Ni2 112.64(13) . . ?
C48 N4 Ni2 127.43(15) . . ?
C67 N5 C57 110.15(16) . . ?
C67 N5 C58 110.46(17) . . ?
C57 N5 C58 109.17(16) . . ?
C67 N5 Ni3 106.55(13) . . ?
C57 N5 Ni3 109.49(12) . . ?
C58 N5 Ni3 110.99(12) . . ?
C72 N6 C68 118.75(18) . . ?
C72 N6 Ni3 128.03(15) . . ?
C68 N6 Ni3 111.27(14) . . ?
O1 C1 C6 121.50(19) . . ?
O1 C1 C2 117.98(18) . . ?
C6 C1 C2 120.52(19) . . ?
C3 C2 C1 117.5(2) . . ?
C3 C2 C9 122.71(19) . . ?
C1 C2 C9 119.57(18) . . ?
C4 C3 C2 122.9(2) . . ?
C3 C4 C5 118.8(2) . . ?
C3 C4 C7 120.6(2) . . ?
C5 C4 C7 120.5(2) . . ?
C6 C5 C4 119.1(2) . . ?
C6 C5 C8 119.2(2) . . ?
C4 C5 C8 121.6(2) . . ?
C1 C6 C5 121.1(2) . . ?
N1 C9 C2 115.07(16) . . ?
N1 C10 C16 115.92(16) . . ?
O2 C11 C12 120.46(19) . . ?
O2 C11 C16 121.17(18) . . ?
C12 C11 C16 118.36(19) . . ?
C13 C12 C11 122.2(2) . . ?
C14 C13 C12 119.5(2) . . ?
C14 C13 C18 121.5(2) . . ?
C12 C13 C18 119.0(2) . . ?
C15 C14 C13 117.93(19) . . ?
C15 C14 C17 120.4(2) . . ?
C13 C14 C17 121.6(2) . . ?
C14 C15 C16 123.4(2) . . ?
C15 C16 C11 118.42(19) . . ?
C15 C16 C10 119.92(19) . . ?
C11 C16 C10 121.22(18) . . ?
N1 C19 C20 110.69(16) . . ?
N2 C20 C21 121.9(2) . . ?
N2 C20 C19 115.38(18) . . ?
C21 C20 C19 122.7(2) . . ?
C22 C21 C20 118.7(2) . . ?
C23 C22 C21 119.7(2) . . ?
C22 C23 C24 118.6(2) . . ?
N2 C24 C23 122.8(2) . . ?
O3 C25 C30 118.94(18) . . ?
O3 C25 C26 121.42(19) . . ?
C30 C25 C26 119.61(19) . . ?
C25 C26 C27 121.3(2) . . ?
C26 C27 C28 119.4(2) . . ?
C26 C27 C31 119.4(2) . . ?
C28 C27 C31 121.2(2) . . ?
C29 C28 C27 118.8(2) . . ?
C29 C28 C32 120.1(2) . . ?
C27 C28 C32 121.2(2) . . ?
C28 C29 C30 121.7(2) . . ?
C25 C30 C29 119.2(2) . . ?
C25 C30 C33 118.88(18) . . ?
C29 C30 C33 121.8(2) . . ?
N3 C33 C30 111.75(17) . . ?
N3 C34 C40 117.04(16) . . ?
O4 C35 C40 122.74(17) . . ?
O4 C35 C36 119.12(17) . . ?
C40 C35 C36 118.12(17) . . ?
C37 C36 C35 122.63(19) . . ?
C36 C37 C38 119.78(19) . . ?
C36 C37 C41 120.12(19) . . ?
C38 C37 C41 120.10(18) . . ?
C39 C38 C37 117.50(18) . . ?
C39 C38 C42 121.16(19) . . ?
C37 C38 C42 121.33(19) . . ?
C38 C39 C40 123.47(19) . . ?
C35 C40 C39 118.37(18) . . ?
C35 C40 C34 125.10(17) . . ?
C39 C40 C34 115.85(17) . . ?
N3 C43 C44 112.36(17) . . ?
N4 C44 C45 121.8(2) . . ?
N4 C44 C43 116.31(18) . . ?
C45 C44 C43 121.7(2) . . ?
C46 C45 C44 118.9(2) . . ?
C47 C46 C45 119.2(2) . . ?
C46 C47 C48 119.1(2) . . ?
N4 C48 C47 122.0(2) . . ?
O5 C49 C54 118.84(18) . . ?
O5 C49 C50 122.98(18) . . ?
C54 C49 C50 118.16(18) . . ?
C51 C50 C49 118.5(2) . . ?
C51 C50 C57 118.2(2) . . ?
C49 C50 C57 123.31(18) . . ?
C52 C51 C50 123.7(2) . . ?
C51 C52 C53 118.0(2) . . ?
C51 C52 C55 120.4(2) . . ?
C53 C52 C55 121.5(2) . . ?
C54 C53 C52 118.7(2) . . ?
C54 C53 C56 119.9(2) . . ?
C52 C53 C56 121.4(2) . . ?
C53 C54 C49 122.9(2) . . ?
N5 C57 C50 113.76(17) . . ?
C64 C58 N5 114.38(17) . . ?
O6 C59 C60 121.53(19) . . ?
O6 C59 C64 120.49(18) . . ?
C60 C59 C64 117.88(19) . . ?
C61 C60 C59 122.7(2) . . ?
C60 C61 C62 119.2(2) . . ?
C60 C61 C66 119.7(2) . . ?
C62 C61 C66 121.1(2) . . ?
C63 C62 C61 118.3(2) . . ?
C63 C62 C65 120.6(2) . . ?
C61 C62 C65 121.1(2) . . ?
C62 C63 C64 122.8(2) . . ?
C63 C64 C59 119.1(2) . . ?
C63 C64 C58 120.77(19) . . ?
C59 C64 C58 119.98(18) . . ?
N5 C67 C68 112.08(17) . . ?
N6 C68 C69 121.8(2) . . ?
N6 C68 C67 115.77(18) . . ?
C69 C68 C67 122.3(2) . . ?
C70 C69 C68 118.9(2) . . ?
C71 C70 C69 119.2(2) . . ?
C70 C71 C72 119.5(2) . . ?
N6 C72 C71 121.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        26.42
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.060

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
1 0.000 0.049 0.250 900.4 198.9
2 0.000 -0.049 0.750 902.4 198.6
3 0.505 0.142 0.573 21.7 -1.0
4 0.495 0.142 0.927 21.9 -0.9
5 0.500 0.451 0.750 899.9 198.8
6 0.407 0.154 0.545 7.5 -0.6
7 0.593 0.154 0.955 7.6 -0.5
8 0.004 0.364 0.071 20.9 -0.9
9 0.500 0.549 0.250 900.4 198.9
10 0.996 0.364 0.429 21.2 -0.6
11 0.093 0.346 0.455 8.2 -0.4
12 0.907 0.346 0.045 8.0 -0.5
13 0.004 0.636 0.571 20.5 -0.9
14 -0.005 0.636 0.929 20.7 -0.8
15 0.093 0.654 0.955 7.6 -0.5
16 0.907 0.654 0.545 7.5 -0.6
17 0.495 0.864 0.429 21.2 -0.6
18 0.504 0.864 0.071 20.9 -0.9
19 0.407 0.846 0.045 8.0 -0.5
20 0.593 0.846 0.455 8.2 -0.4
_platon_squeeze_details          
;
;

#===END

data_Compound3
_database_code_depnum_ccdc_archive 'CCDC 710319'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
;
bis-(m2-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine-(aqua) di-nickel(ii) acetonitrile solvate
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H58.50 N4.50 Ni2 O6.50'
_chemical_formula_weight         931.92

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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   14.083(6)
_cell_length_b                   17.120(7)
_cell_length_c                   19.394(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.000(7)
_cell_angle_gamma                90.00
_cell_volume                     4537(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    795
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      20.38

_exptl_crystal_description       Prism
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1968
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8641
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_process_details   
;
Sheldrick, G.M. SADABS: Program for absorption correction
using area detector data. University of G\"ottingen, Germany, 1996.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38942
_diffrn_reflns_av_R_equivalents  0.1172
_diffrn_reflns_av_sigmaI/netI    0.1350
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         26.48
_reflns_number_total             9334
_reflns_number_gt                4814
_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, 1997)'
_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^)+(0.0685P)^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         9334
_refine_ls_number_parameters     582
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1481
_refine_ls_wR_factor_gt          0.1266
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_restrained_S_all      0.932
_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
N1S N 0.4675(8) -0.2441(6) 0.6673(6) 0.059(3) Uiso 0.50 1 d P A 1
C1S C 0.4612(7) -0.1770(6) 0.6743(5) 0.031(2) Uiso 0.50 1 d P A 1
C2S C 0.4540(9) -0.0978(7) 0.6952(7) 0.052(3) Uiso 0.50 1 d P A 1
H1S1 H 0.4466 -0.0962 0.7442 0.078 Uiso 0.50 1 calc PR A 1
H1S2 H 0.3970 -0.0732 0.6635 0.078 Uiso 0.50 1 calc PR A 1
H1S3 H 0.5134 -0.0695 0.6923 0.078 Uiso 0.50 1 calc PR A 1
O1S O 0.4494(8) -0.2239(7) 0.6290(6) 0.090(4) Uiso 0.50 1 d P B 2
O2S O 0.4776(10) -0.0719(8) 0.6546(7) 0.130(5) Uiso 0.50 1 d P C 2
Ni1 Ni 0.45475(4) 0.09524(3) 0.88664(3) 0.01580(16) Uani 1 1 d . . .
Ni2 Ni 0.62890(4) 0.07715(3) 0.80754(3) 0.01830(16) Uani 1 1 d . . .
O1 O 0.4430(2) 0.09494(17) 0.98825(14) 0.0209(7) Uani 1 1 d . . .
O2 O 0.4805(2) 0.08505(16) 0.78688(14) 0.0186(7) Uani 1 1 d . . .
O3 O 0.6284(2) 0.02515(18) 0.71695(17) 0.0329(9) Uani 1 1 d . . .
O4 O 0.6066(2) 0.09450(16) 0.90616(14) 0.0177(7) Uani 1 1 d . . .
O5 O 0.4630(2) -0.02687(17) 0.89336(16) 0.0219(7) Uani 1 1 d D . .
O6 O 0.5963(6) -0.0556(4) 0.8137(4) 0.046(2) Uani 0.50 1 d PD . .
N1 N 0.3006(3) 0.09289(19) 0.84494(18) 0.0163(8) Uani 1 1 d . . .
N2 N 0.4274(3) 0.2156(2) 0.87779(18) 0.0189(9) Uani 1 1 d . . .
N3 N 0.7823(3) 0.06080(19) 0.84558(18) 0.0183(9) Uani 1 1 d . . .
N4 N 0.6727(3) 0.1898(2) 0.80076(18) 0.0193(9) Uani 1 1 d . . .
C1 C 0.3655(4) 0.1250(3) 1.0064(2) 0.0221(11) Uani 1 1 d . . .
C2 C 0.2705(3) 0.1132(3) 0.9656(2) 0.0206(11) Uani 1 1 d . . .
C3 C 0.1904(3) 0.1442(3) 0.9879(3) 0.0250(12) Uani 1 1 d . . .
H3 H 0.1262 0.1363 0.9592 0.030 Uiso 1 1 calc R . .
C4 C 0.2027(4) 0.1860(3) 1.0509(3) 0.0292(12) Uani 1 1 d . . .
C5 C 0.2967(4) 0.1985(3) 1.0915(2) 0.0270(12) Uani 1 1 d . . .
C6 C 0.3766(4) 0.1698(3) 1.0687(2) 0.0285(12) Uani 1 1 d . . .
H6 H 0.4408 0.1809 1.0961 0.034 Uiso 1 1 calc R . .
C7 C 0.1136(4) 0.2152(3) 1.0738(3) 0.0441(15) Uani 1 1 d . . .
H7A H 0.1071 0.1865 1.1162 0.066 Uiso 1 1 calc R . .
H7B H 0.0550 0.2068 1.0353 0.066 Uiso 1 1 calc R . .
H7C H 0.1210 0.2711 1.0848 0.066 Uiso 1 1 calc R . .
C8 C 0.3131(4) 0.2402(3) 1.1617(3) 0.0440(15) Uani 1 1 d . . .
H8A H 0.2808 0.2913 1.1547 0.066 Uiso 1 1 calc R . .
H8B H 0.3834 0.2473 1.1816 0.066 Uiso 1 1 calc R . .
H8C H 0.2856 0.2090 1.1946 0.066 Uiso 1 1 calc R . .
C9 C 0.2541(3) 0.0606(2) 0.9011(2) 0.0206(11) Uani 1 1 d . . .
H9A H 0.2818 0.0084 0.9158 0.025 Uiso 1 1 calc R . .
H9B H 0.1829 0.0544 0.8809 0.025 Uiso 1 1 calc R . .
C10 C 0.2791(3) 0.0381(2) 0.7828(2) 0.0203(10) Uani 1 1 d . . .
H10A H 0.2076 0.0291 0.7679 0.024 Uiso 1 1 calc R . .
H10B H 0.3110 -0.0127 0.7977 0.024 Uiso 1 1 calc R . .
C11 C 0.4128(3) 0.0897(2) 0.7253(2) 0.0163(10) Uani 1 1 d . . .
C12 C 0.4375(3) 0.1165(2) 0.6634(2) 0.0203(11) Uani 1 1 d . . .
H12 H 0.5033 0.1312 0.6659 0.024 Uiso 1 1 calc R . .
C13 C 0.3683(4) 0.1224(3) 0.5982(2) 0.0227(11) Uani 1 1 d . . .
C14 C 0.2711(3) 0.1029(3) 0.5936(2) 0.0235(11) Uani 1 1 d . . .
C15 C 0.2465(3) 0.0770(2) 0.6545(2) 0.0213(11) Uani 1 1 d . . .
H15 H 0.1801 0.0642 0.6517 0.026 Uiso 1 1 calc R . .
C16 C 0.3141(3) 0.0687(2) 0.7201(2) 0.0171(10) Uani 1 1 d . . .
C17 C 0.1923(4) 0.1135(3) 0.5251(2) 0.0349(13) Uani 1 1 d . . .
H17A H 0.1283 0.1004 0.5336 0.052 Uiso 1 1 calc R . .
H17B H 0.2059 0.0792 0.4883 0.052 Uiso 1 1 calc R . .
H17C H 0.1918 0.1680 0.5095 0.052 Uiso 1 1 calc R . .
C18 C 0.3998(4) 0.1514(3) 0.5334(2) 0.0327(13) Uani 1 1 d . . .
H18A H 0.3803 0.1135 0.4947 0.049 Uiso 1 1 calc R . .
H18B H 0.4710 0.1579 0.5451 0.049 Uiso 1 1 calc R . .
H18C H 0.3683 0.2018 0.5184 0.049 Uiso 1 1 calc R . .
C19 C 0.2621(3) 0.1722(2) 0.8233(2) 0.0206(11) Uani 1 1 d . . .
H19A H 0.2021 0.1808 0.8403 0.025 Uiso 1 1 calc R . .
H19B H 0.2438 0.1752 0.7708 0.025 Uiso 1 1 calc R . .
C20 C 0.3339(3) 0.2361(2) 0.8517(2) 0.0179(10) Uani 1 1 d . . .
C21 C 0.3052(4) 0.3133(3) 0.8474(2) 0.0256(12) Uani 1 1 d . . .
H21 H 0.2384 0.3267 0.8292 0.031 Uiso 1 1 calc R . .
C22 C 0.3739(4) 0.3711(3) 0.8698(2) 0.0289(12) Uani 1 1 d . . .
H22 H 0.3552 0.4245 0.8665 0.035 Uiso 1 1 calc R . .
C23 C 0.4705(4) 0.3502(3) 0.8971(2) 0.0273(12) Uani 1 1 d . . .
H23 H 0.5192 0.3889 0.9131 0.033 Uiso 1 1 calc R . .
C24 C 0.4944(3) 0.2719(2) 0.9006(2) 0.0198(10) Uani 1 1 d . . .
H24 H 0.5605 0.2571 0.9199 0.024 Uiso 1 1 calc R . .
C25 C 0.7018(4) 0.0383(3) 0.6860(3) 0.0282(12) Uani 1 1 d . . .
C26 C 0.6816(4) 0.0564(3) 0.6132(3) 0.0400(15) Uani 1 1 d . . .
H26 H 0.6153 0.0599 0.5870 0.048 Uiso 1 1 calc R . .
C27 C 0.7547(5) 0.0692(3) 0.5786(3) 0.0474(17) Uani 1 1 d . . .
C28 C 0.8537(4) 0.0625(3) 0.6160(3) 0.0390(14) Uani 1 1 d . . .
C29 C 0.8738(4) 0.0430(3) 0.6884(3) 0.0293(12) Uani 1 1 d . . .
H29 H 0.9399 0.0380 0.7144 0.035 Uiso 1 1 calc R . .
C30 C 0.7984(4) 0.0307(2) 0.7232(2) 0.0230(11) Uani 1 1 d . . .
C31 C 0.7288(5) 0.0936(4) 0.5015(3) 0.073(2) Uani 1 1 d . . .
H31A H 0.6575 0.0938 0.4836 0.110 Uiso 1 1 calc R . .
H31B H 0.7576 0.0566 0.4738 0.110 Uiso 1 1 calc R . .
H31C H 0.7546 0.1460 0.4971 0.110 Uiso 1 1 calc R . .
C32 C 0.9364(5) 0.0792(4) 0.5820(3) 0.065(2) Uani 1 1 d . . .
H32A H 0.9367 0.1350 0.5705 0.097 Uiso 1 1 calc R . .
H32B H 0.9281 0.0484 0.5384 0.097 Uiso 1 1 calc R . .
H32C H 0.9985 0.0653 0.6149 0.097 Uiso 1 1 calc R . .
C33 C 0.8194(3) 0.0044(2) 0.7994(2) 0.0223(11) Uani 1 1 d . . .
H33A H 0.7886 -0.0472 0.8017 0.027 Uiso 1 1 calc R . .
H33B H 0.8910 -0.0018 0.8178 0.027 Uiso 1 1 calc R . .
C34 C 0.7974(3) 0.0259(2) 0.9180(2) 0.0186(10) Uani 1 1 d . . .
H34A H 0.8666 0.0096 0.9343 0.022 Uiso 1 1 calc R . .
H34B H 0.7564 -0.0216 0.9147 0.022 Uiso 1 1 calc R . .
C35 C 0.6772(3) 0.1082(2) 0.9653(2) 0.0142(10) Uani 1 1 d . . .
C36 C 0.6582(3) 0.1507(2) 1.0214(2) 0.0180(10) Uani 1 1 d . . .
H36 H 0.5942 0.1711 1.0168 0.022 Uiso 1 1 calc R . .
C37 C 0.7290(3) 0.1647(2) 1.0842(2) 0.0207(11) Uani 1 1 d . . .
C38 C 0.8243(3) 0.1376(2) 1.0912(2) 0.0230(11) Uani 1 1 d . . .
C39 C 0.8441(3) 0.0954(2) 1.0347(2) 0.0199(10) Uani 1 1 d . . .
H39 H 0.9087 0.0768 1.0388 0.024 Uiso 1 1 calc R . .
C40 C 0.7733(3) 0.0793(2) 0.9724(2) 0.0178(10) Uani 1 1 d . . .
C41 C 0.7005(4) 0.2082(3) 1.1441(2) 0.0297(12) Uani 1 1 d . . .
H41A H 0.6341 0.2290 1.1273 0.045 Uiso 1 1 calc R . .
H41B H 0.7464 0.2513 1.1599 0.045 Uiso 1 1 calc R . .
H41C H 0.7025 0.1723 1.1838 0.045 Uiso 1 1 calc R . .
C42 C 0.9025(4) 0.1498(3) 1.1584(2) 0.0334(13) Uani 1 1 d . . .
H42A H 0.9636 0.1256 1.1536 0.050 Uiso 1 1 calc R . .
H42B H 0.8819 0.1259 1.1984 0.050 Uiso 1 1 calc R . .
H42C H 0.9129 0.2059 1.1672 0.050 Uiso 1 1 calc R . .
C43 C 0.8348(3) 0.1368(2) 0.8482(2) 0.0207(11) Uani 1 1 d . . .
H43A H 0.8743 0.1365 0.8124 0.025 Uiso 1 1 calc R . .
H43B H 0.8802 0.1430 0.8956 0.025 Uiso 1 1 calc R . .
C44 C 0.7652(3) 0.2052(2) 0.8343(2) 0.0184(10) Uani 1 1 d . . .
C45 C 0.7982(4) 0.2808(2) 0.8522(2) 0.0240(11) Uani 1 1 d . . .
H45 H 0.8640 0.2899 0.8775 0.029 Uiso 1 1 calc R . .
C46 C 0.7341(4) 0.3425(3) 0.8326(2) 0.0307(13) Uani 1 1 d . . .
H46 H 0.7547 0.3946 0.8448 0.037 Uiso 1 1 calc R . .
C47 C 0.6397(4) 0.3270(3) 0.7951(3) 0.0298(13) Uani 1 1 d . . .
H47 H 0.5951 0.3687 0.7794 0.036 Uiso 1 1 calc R . .
C48 C 0.6105(3) 0.2509(2) 0.7804(2) 0.0202(11) Uani 1 1 d . . .
H48 H 0.5449 0.2407 0.7554 0.024 Uiso 1 1 calc R . .
H5A H 0.496(3) -0.047(2) 0.9350(14) 0.030 Uiso 1 1 d D . .
H5B H 0.414(2) -0.053(2) 0.869(2) 0.030 Uiso 1 1 d D . .
H6A H 0.551(5) -0.086(4) 0.782(4) 0.030 Uiso 0.50 1 d PD . .
H6B H 0.550(5) -0.057(5) 0.839(4) 0.030 Uiso 0.50 1 d PD . .

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 0.0184(3) 0.0178(3) 0.0115(3) 0.0022(2) 0.0041(3) 0.0022(3)
Ni2 0.0197(3) 0.0225(3) 0.0137(3) 0.0023(3) 0.0061(3) 0.0021(3)
O1 0.0218(18) 0.0296(18) 0.0129(16) 0.0056(14) 0.0073(14) 0.0090(15)
O2 0.0199(17) 0.0250(17) 0.0112(16) -0.0010(13) 0.0040(14) -0.0013(14)
O3 0.026(2) 0.037(2) 0.035(2) -0.0195(17) 0.0055(17) -0.0015(16)
O4 0.0188(17) 0.0248(17) 0.0106(16) 0.0019(13) 0.0054(14) 0.0014(14)
O5 0.025(2) 0.0241(18) 0.0129(18) -0.0006(14) -0.0031(15) -0.0017(15)
O6 0.070(6) 0.038(5) 0.039(5) 0.003(4) 0.032(4) -0.006(4)
N1 0.020(2) 0.0171(19) 0.0124(19) 0.0040(16) 0.0054(17) 0.0009(16)
N2 0.024(2) 0.018(2) 0.014(2) 0.0041(16) 0.0033(18) 0.0022(17)
N3 0.026(2) 0.0157(19) 0.015(2) 0.0012(16) 0.0084(18) 0.0025(17)
N4 0.026(2) 0.025(2) 0.0085(19) 0.0039(16) 0.0070(18) 0.0034(18)
C1 0.030(3) 0.021(2) 0.019(3) 0.009(2) 0.014(2) 0.008(2)
C2 0.021(3) 0.025(3) 0.017(3) 0.008(2) 0.005(2) 0.001(2)
C3 0.020(3) 0.031(3) 0.026(3) 0.010(2) 0.009(2) 0.005(2)
C4 0.032(3) 0.026(3) 0.037(3) 0.009(2) 0.022(3) 0.006(2)
C5 0.038(3) 0.024(3) 0.023(3) -0.004(2) 0.016(3) 0.003(2)
C6 0.031(3) 0.034(3) 0.019(3) -0.001(2) 0.003(2) 0.005(2)
C7 0.036(3) 0.043(3) 0.060(4) -0.005(3) 0.024(3) 0.004(3)
C8 0.053(4) 0.041(3) 0.043(4) -0.015(3) 0.021(3) 0.011(3)
C9 0.022(3) 0.023(2) 0.017(2) 0.007(2) 0.006(2) -0.001(2)
C10 0.018(3) 0.021(2) 0.022(3) 0.002(2) 0.005(2) -0.006(2)
C11 0.020(3) 0.015(2) 0.012(2) 0.0007(18) -0.001(2) -0.003(2)
C12 0.023(3) 0.021(2) 0.017(3) 0.003(2) 0.006(2) -0.004(2)
C13 0.035(3) 0.020(2) 0.011(2) 0.0005(19) 0.002(2) -0.006(2)
C14 0.029(3) 0.025(3) 0.012(2) -0.002(2) -0.005(2) -0.003(2)
C15 0.020(3) 0.020(2) 0.023(3) -0.005(2) 0.003(2) -0.007(2)
C16 0.020(3) 0.017(2) 0.012(2) -0.0010(18) 0.000(2) -0.004(2)
C17 0.037(3) 0.042(3) 0.022(3) 0.011(2) 0.000(3) 0.002(3)
C18 0.042(3) 0.040(3) 0.015(3) 0.003(2) 0.005(2) -0.004(3)
C19 0.026(3) 0.016(2) 0.022(3) 0.0030(19) 0.009(2) 0.002(2)
C20 0.025(3) 0.016(2) 0.013(2) 0.0018(19) 0.006(2) 0.003(2)
C21 0.023(3) 0.027(3) 0.025(3) 0.007(2) 0.003(2) 0.016(2)
C22 0.043(4) 0.014(2) 0.026(3) -0.003(2) 0.002(3) 0.002(2)
C23 0.036(3) 0.023(3) 0.021(3) -0.003(2) 0.002(2) -0.003(2)
C24 0.022(3) 0.020(2) 0.016(2) 0.0005(19) 0.002(2) -0.001(2)
C25 0.037(3) 0.030(3) 0.020(3) -0.004(2) 0.011(3) 0.011(2)
C26 0.050(4) 0.049(3) 0.019(3) -0.010(3) 0.004(3) 0.023(3)
C27 0.084(5) 0.044(3) 0.019(3) 0.007(3) 0.020(3) 0.035(3)
C28 0.059(4) 0.038(3) 0.029(3) 0.000(3) 0.028(3) 0.007(3)
C29 0.034(3) 0.028(3) 0.029(3) -0.002(2) 0.013(3) 0.000(2)
C30 0.035(3) 0.014(2) 0.022(3) -0.001(2) 0.010(2) 0.006(2)
C31 0.109(6) 0.088(5) 0.022(3) 0.014(3) 0.016(4) 0.049(5)
C32 0.086(5) 0.075(5) 0.052(4) 0.008(3) 0.052(4) 0.007(4)
C33 0.027(3) 0.017(2) 0.027(3) 0.002(2) 0.013(2) 0.011(2)
C34 0.016(3) 0.022(2) 0.018(2) 0.006(2) 0.003(2) 0.002(2)
C35 0.023(3) 0.014(2) 0.006(2) 0.0042(17) 0.003(2) -0.0039(19)
C36 0.021(3) 0.018(2) 0.014(2) 0.0010(19) 0.001(2) -0.002(2)
C37 0.027(3) 0.022(2) 0.012(2) -0.0051(19) 0.000(2) -0.006(2)
C38 0.025(3) 0.021(2) 0.020(3) 0.005(2) -0.001(2) -0.006(2)
C39 0.021(3) 0.023(2) 0.015(2) 0.003(2) 0.004(2) 0.002(2)
C40 0.023(3) 0.021(2) 0.008(2) 0.0048(19) 0.001(2) 0.004(2)
C41 0.038(3) 0.030(3) 0.017(3) -0.001(2) 0.001(2) -0.004(2)
C42 0.031(3) 0.042(3) 0.021(3) 0.001(2) -0.006(2) -0.007(3)
C43 0.024(3) 0.019(2) 0.020(3) 0.006(2) 0.006(2) -0.003(2)
C44 0.029(3) 0.012(2) 0.015(2) 0.0019(18) 0.007(2) 0.001(2)
C45 0.028(3) 0.018(2) 0.021(3) 0.001(2) -0.003(2) -0.005(2)
C46 0.052(4) 0.018(3) 0.021(3) -0.001(2) 0.007(3) -0.002(2)
C47 0.040(3) 0.018(3) 0.028(3) 0.008(2) 0.002(3) 0.012(2)
C48 0.023(3) 0.020(2) 0.015(2) 0.007(2) 0.000(2) 0.004(2)

_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
N1S C1S 1.163(14) . ?
C1S C2S 1.426(14) . ?
Ni1 O1 2.017(3) . ?
Ni1 O2 2.060(3) . ?
Ni1 O4 2.080(3) . ?
Ni1 O5 2.096(3) . ?
Ni1 N2 2.096(4) . ?
Ni1 N1 2.126(4) . ?
Ni2 O3 1.968(3) . ?
Ni2 O4 2.034(3) . ?
Ni2 O2 2.035(3) . ?
Ni2 N4 2.039(4) . ?
Ni2 N3 2.126(4) . ?
Ni2 O6 2.328(7) . ?
O1 C1 1.329(5) . ?
O2 C11 1.338(5) . ?
O3 C25 1.335(5) . ?
O4 C35 1.345(5) . ?
N1 C19 1.485(5) . ?
N1 C10 1.499(5) . ?
N1 C9 1.505(5) . ?
N2 C20 1.338(5) . ?
N2 C24 1.346(5) . ?
N3 C43 1.492(5) . ?
N3 C34 1.493(5) . ?
N3 C33 1.495(5) . ?
N4 C44 1.333(6) . ?
N4 C48 1.361(5) . ?
C1 C2 1.394(6) . ?
C1 C6 1.408(6) . ?
C2 C3 1.406(6) . ?
C2 C9 1.513(6) . ?
C3 C4 1.391(7) . ?
C4 C5 1.383(7) . ?
C4 C7 1.514(6) . ?
C5 C6 1.394(6) . ?
C5 C8 1.506(6) . ?
C10 C16 1.512(6) . ?
C11 C12 1.405(6) . ?
C11 C16 1.416(6) . ?
C12 C13 1.401(6) . ?
C13 C14 1.391(6) . ?
C13 C18 1.514(6) . ?
C14 C15 1.382(6) . ?
C14 C17 1.521(6) . ?
C15 C16 1.400(6) . ?
C19 C20 1.500(6) . ?
C20 C21 1.379(6) . ?
C21 C22 1.378(6) . ?
C22 C23 1.381(6) . ?
C23 C24 1.381(6) . ?
C25 C30 1.383(7) . ?
C25 C26 1.406(6) . ?
C26 C27 1.375(7) . ?
C27 C28 1.411(8) . ?
C27 C31 1.510(7) . ?
C28 C29 1.403(6) . ?
C28 C32 1.499(7) . ?
C29 C30 1.405(6) . ?
C30 C33 1.504(6) . ?
C34 C40 1.496(6) . ?
C35 C36 1.387(6) . ?
C35 C40 1.416(6) . ?
C36 C37 1.396(6) . ?
C37 C38 1.397(6) . ?
C37 C41 1.512(6) . ?
C38 C39 1.395(6) . ?
C38 C42 1.504(6) . ?
C39 C40 1.394(6) . ?
C43 C44 1.509(6) . ?
C44 C45 1.390(6) . ?
C45 C46 1.382(6) . ?
C46 C47 1.378(7) . ?
C47 C48 1.376(6) . ?

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
N1S C1S C2S 170.1(13) . . ?
O1 Ni1 O2 172.72(11) . . ?
O1 Ni1 O4 98.40(11) . . ?
O2 Ni1 O4 76.32(11) . . ?
O1 Ni1 O5 87.32(12) . . ?
O2 Ni1 O5 87.37(12) . . ?
O4 Ni1 O5 86.75(12) . . ?
O1 Ni1 N2 91.47(12) . . ?
O2 Ni1 N2 94.42(12) . . ?
O4 Ni1 N2 100.46(13) . . ?
O5 Ni1 N2 172.79(14) . . ?
O1 Ni1 N1 93.10(12) . . ?
O2 Ni1 N1 92.10(12) . . ?
O4 Ni1 N1 168.41(12) . . ?
O5 Ni1 N1 92.36(13) . . ?
N2 Ni1 N1 80.61(14) . . ?
O3 Ni2 O4 159.65(13) . . ?
O3 Ni2 O2 94.15(12) . . ?
O4 Ni2 O2 77.91(11) . . ?
O3 Ni2 N4 107.83(14) . . ?
O4 Ni2 N4 92.32(13) . . ?
O2 Ni2 N4 103.71(13) . . ?
O3 Ni2 N3 91.97(13) . . ?
O4 Ni2 N3 93.90(12) . . ?
O2 Ni2 N3 170.45(12) . . ?
N4 Ni2 N3 81.31(14) . . ?
O3 Ni2 O6 69.3(2) . . ?
O4 Ni2 O6 90.9(2) . . ?
O2 Ni2 O6 82.5(2) . . ?
N4 Ni2 O6 173.5(2) . . ?
N3 Ni2 O6 92.9(2) . . ?
C1 O1 Ni1 121.7(3) . . ?
C11 O2 Ni2 130.9(3) . . ?
C11 O2 Ni1 125.7(3) . . ?
Ni2 O2 Ni1 103.09(13) . . ?
C25 O3 Ni2 119.3(3) . . ?
C35 O4 Ni2 125.3(3) . . ?
C35 O4 Ni1 132.1(3) . . ?
Ni2 O4 Ni1 102.46(12) . . ?
C19 N1 C10 110.9(3) . . ?
C19 N1 C9 110.3(3) . . ?
C10 N1 C9 108.3(3) . . ?
C19 N1 Ni1 111.1(3) . . ?
C10 N1 Ni1 107.9(3) . . ?
C9 N1 Ni1 108.3(3) . . ?
C20 N2 C24 119.0(4) . . ?
C20 N2 Ni1 115.7(3) . . ?
C24 N2 Ni1 125.2(3) . . ?
C43 N3 C34 111.1(3) . . ?
C43 N3 C33 110.0(3) . . ?
C34 N3 C33 108.3(3) . . ?
C43 N3 Ni2 110.5(3) . . ?
C34 N3 Ni2 106.3(2) . . ?
C33 N3 Ni2 110.5(3) . . ?
C44 N4 C48 118.3(4) . . ?
C44 N4 Ni2 115.5(3) . . ?
C48 N4 Ni2 124.2(3) . . ?
O1 C1 C2 122.0(4) . . ?
O1 C1 C6 120.7(4) . . ?
C2 C1 C6 117.3(4) . . ?
C1 C2 C3 120.2(4) . . ?
C1 C2 C9 119.3(4) . . ?
C3 C2 C9 120.3(4) . . ?
C4 C3 C2 121.7(5) . . ?
C5 C4 C3 118.6(4) . . ?
C5 C4 C7 122.0(5) . . ?
C3 C4 C7 119.4(5) . . ?
C4 C5 C6 120.0(4) . . ?
C4 C5 C8 120.2(4) . . ?
C6 C5 C8 119.7(5) . . ?
C5 C6 C1 122.2(5) . . ?
N1 C9 C2 112.0(3) . . ?
N1 C10 C16 112.8(3) . . ?
O2 C11 C12 120.8(4) . . ?
O2 C11 C16 121.5(4) . . ?
C12 C11 C16 117.7(4) . . ?
C13 C12 C11 122.2(4) . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 C18 120.4(4) . . ?
C12 C13 C18 119.6(4) . . ?
C15 C14 C13 117.9(4) . . ?
C15 C14 C17 120.2(4) . . ?
C13 C14 C17 121.8(4) . . ?
C14 C15 C16 123.7(4) . . ?
C15 C16 C11 118.5(4) . . ?
C15 C16 C10 119.0(4) . . ?
C11 C16 C10 122.5(4) . . ?
N1 C19 C20 113.3(4) . . ?
N2 C20 C21 121.4(4) . . ?
N2 C20 C19 117.5(4) . . ?
C21 C20 C19 121.0(4) . . ?
C22 C21 C20 119.7(4) . . ?
C21 C22 C23 119.1(4) . . ?
C22 C23 C24 118.4(4) . . ?
N2 C24 C23 122.4(4) . . ?
O3 C25 C30 121.4(4) . . ?
O3 C25 C26 119.9(5) . . ?
C30 C25 C26 118.7(5) . . ?
C27 C26 C25 122.0(5) . . ?
C26 C27 C28 120.0(5) . . ?
C26 C27 C31 119.8(6) . . ?
C28 C27 C31 120.2(6) . . ?
C29 C28 C27 117.9(5) . . ?
C29 C28 C32 119.7(5) . . ?
C27 C28 C32 122.3(5) . . ?
C28 C29 C30 121.6(5) . . ?
C25 C30 C29 119.8(4) . . ?
C25 C30 C33 118.4(4) . . ?
C29 C30 C33 121.7(4) . . ?
N3 C33 C30 112.5(3) . . ?
N3 C34 C40 114.5(3) . . ?
O4 C35 C36 121.1(4) . . ?
O4 C35 C40 120.9(4) . . ?
C36 C35 C40 117.9(4) . . ?
C35 C36 C37 122.8(4) . . ?
C36 C37 C38 119.6(4) . . ?
C36 C37 C41 119.3(4) . . ?
C38 C37 C41 121.1(4) . . ?
C39 C38 C37 117.8(4) . . ?
C39 C38 C42 120.7(4) . . ?
C37 C38 C42 121.5(4) . . ?
C40 C39 C38 123.1(4) . . ?
C39 C40 C35 118.7(4) . . ?
C39 C40 C34 119.7(4) . . ?
C35 C40 C34 121.3(4) . . ?
N3 C43 C44 112.1(4) . . ?
N4 C44 C45 122.3(4) . . ?
N4 C44 C43 116.7(4) . . ?
C45 C44 C43 120.9(4) . . ?
C46 C45 C44 119.1(5) . . ?
C47 C46 C45 118.7(4) . . ?
C48 C47 C46 119.6(4) . . ?
N4 C48 C47 121.9(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O1 0.896(19) 1.74(2) 2.629(4) 175(4) 3_657
O6 H6B O5 0.91(2) 1.86(3) 2.747(8) 163(9) .

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.48
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.105

#===END

data_Compound4
_database_code_depnum_ccdc_archive 'CCDC 710320'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            
;
bis-(m2-N,N-bis(4,5-Dimethyl-2-oxobenzyl)-N-(2-
pyridylmethyl)amine-di-copper(ii)
;
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H58 Cu2 N4 O7'
_chemical_formula_weight         930.06

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 2(1)/c'

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

_cell_length_a                   10.694(2)
_cell_length_b                   22.640(4)
_cell_length_c                   20.273(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.394(3)
_cell_angle_gamma                90.00
_cell_volume                     4886.9(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1485
_cell_measurement_theta_min      2.645
_cell_measurement_theta_max      24.94

_exptl_crystal_description       Plate
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1952
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8301
_exptl_absorpt_correction_T_max  0.9217
_exptl_absorpt_process_details   
;
Sheldrick, G.M. SADABS: Program for absorption correction
using area detector data. University of G\"ottingen, Germany, 1996.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(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  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            77473
_diffrn_reflns_av_R_equivalents  0.1015
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         26.50
_reflns_number_total             10130
_reflns_number_gt                6276
_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, 1997)'
_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^)+(0.0595P)^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         10130
_refine_ls_number_parameters     576
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1286
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.080
_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
Cu1 Cu 0.58611(4) 0.099375(18) 0.192073(19) 0.01737(12) Uani 1 1 d . . .
Cu2 Cu 0.39854(4) 0.198688(18) 0.226424(19) 0.01827(12) Uani 1 1 d . . .
O1 O 0.4872(2) 0.03217(10) 0.21582(11) 0.0223(6) Uani 1 1 d . . .
O2 O 0.5555(2) 0.16459(10) 0.26589(10) 0.0206(5) Uani 1 1 d . . .
O3 O 0.2828(2) 0.14890(10) 0.27103(11) 0.0238(6) Uani 1 1 d . . .
O4 O 0.4489(2) 0.14349(10) 0.14719(11) 0.0205(5) Uani 1 1 d . . .
N1 N 0.7489(3) 0.06833(12) 0.23866(13) 0.0161(6) Uani 1 1 d . . .
N2 N 0.7048(3) 0.13737(13) 0.13363(13) 0.0209(7) Uani 1 1 d . . .
N3 N 0.2580(3) 0.23794(12) 0.16641(13) 0.0193(7) Uani 1 1 d . . .
N4 N 0.4830(3) 0.27680(13) 0.21319(13) 0.0213(7) Uani 1 1 d . . .
C1 C 0.5385(3) -0.01903(15) 0.19874(16) 0.0203(8) Uani 1 1 d . . .
C2 C 0.6638(3) -0.03314(15) 0.22190(16) 0.0200(8) Uani 1 1 d . . .
C3 C 0.7153(3) -0.08528(15) 0.20190(16) 0.0210(8) Uani 1 1 d . . .
H3 H 0.8003 -0.0939 0.2167 0.025 Uiso 1 1 calc R . .
C4 C 0.6482(3) -0.12582(15) 0.16101(17) 0.0222(8) Uani 1 1 d . . .
C5 C 0.5232(4) -0.11247(15) 0.13954(17) 0.0248(9) Uani 1 1 d . . .
C6 C 0.4711(3) -0.05988(15) 0.15912(17) 0.0231(8) Uani 1 1 d . . .
H6 H 0.3858 -0.0516 0.1447 0.028 Uiso 1 1 calc R . .
C7 C 0.7081(4) -0.18252(16) 0.14083(18) 0.0306(9) Uani 1 1 d . . .
H7A H 0.7983 -0.1815 0.1548 0.046 Uiso 1 1 calc R . .
H7B H 0.6951 -0.1869 0.0926 0.046 Uiso 1 1 calc R . .
H7C H 0.6697 -0.2160 0.1620 0.046 Uiso 1 1 calc R . .
C8 C 0.4446(4) -0.15447(17) 0.0946(2) 0.0397(11) Uani 1 1 d . . .
H8A H 0.3589 -0.1390 0.0865 0.059 Uiso 1 1 calc R . .
H8B H 0.4424 -0.1933 0.1158 0.059 Uiso 1 1 calc R . .
H8C H 0.4816 -0.1582 0.0523 0.059 Uiso 1 1 calc R . .
C9 C 0.7337(3) 0.00920(15) 0.26942(16) 0.0210(8) Uani 1 1 d . . .
H9A H 0.6874 0.0137 0.3092 0.025 Uiso 1 1 calc R . .
H9B H 0.8176 -0.0073 0.2838 0.025 Uiso 1 1 calc R . .
C10 C 0.7982(3) 0.11280(15) 0.28964(16) 0.0203(8) Uani 1 1 d . . .
H10A H 0.8137 0.1503 0.2667 0.024 Uiso 1 1 calc R . .
H10B H 0.8799 0.0986 0.3106 0.024 Uiso 1 1 calc R . .
C11 C 0.5976(3) 0.15364(15) 0.32928(16) 0.0201(8) Uani 1 1 d . . .
C12 C 0.5303(3) 0.17108(15) 0.38174(17) 0.0199(8) Uani 1 1 d . . .
H12 H 0.4530 0.1915 0.3726 0.024 Uiso 1 1 calc R . .
C13 C 0.5740(4) 0.15924(16) 0.44703(17) 0.0257(9) Uani 1 1 d . . .
C14 C 0.6879(4) 0.13014(17) 0.46126(17) 0.0268(9) Uani 1 1 d . . .
C15 C 0.7548(3) 0.11370(16) 0.40904(16) 0.0240(8) Uani 1 1 d . . .
H15 H 0.8322 0.0935 0.4185 0.029 Uiso 1 1 calc R . .
C16 C 0.7136(3) 0.12540(14) 0.34346(16) 0.0168(7) Uani 1 1 d . . .
C17 C 0.7397(4) 0.1169(2) 0.53196(19) 0.0509(13) Uani 1 1 d . . .
H17A H 0.7436 0.1535 0.5579 0.076 Uiso 1 1 calc R . .
H17B H 0.8243 0.1002 0.5321 0.076 Uiso 1 1 calc R . .
H17C H 0.6848 0.0885 0.5516 0.076 Uiso 1 1 calc R . .
C18 C 0.4930(4) 0.17743(19) 0.50134(18) 0.0370(10) Uani 1 1 d . . .
H18A H 0.4602 0.1421 0.5216 0.055 Uiso 1 1 calc R . .
H18B H 0.4229 0.2017 0.4823 0.055 Uiso 1 1 calc R . .
H18C H 0.5438 0.2002 0.5351 0.055 Uiso 1 1 calc R . .
C19 C 0.8392(3) 0.06347(16) 0.18750(16) 0.0223(8) Uani 1 1 d . . .
H19A H 0.8283 0.0248 0.1648 0.027 Uiso 1 1 calc R . .
H19B H 0.9261 0.0655 0.2090 0.027 Uiso 1 1 calc R . .
C20 C 0.8187(3) 0.11237(15) 0.13742(16) 0.0204(8) Uani 1 1 d . . .
C21 C 0.9076(4) 0.12809(18) 0.09558(17) 0.0287(9) Uani 1 1 d . . .
H21 H 0.9875 0.1094 0.0984 0.034 Uiso 1 1 calc R . .
C22 C 0.8763(4) 0.17221(19) 0.04915(18) 0.0354(10) Uani 1 1 d . . .
H22 H 0.9353 0.1837 0.0193 0.043 Uiso 1 1 calc R . .
C23 C 0.7616(4) 0.19923(19) 0.04604(18) 0.0336(10) Uani 1 1 d . . .
H23 H 0.7408 0.2300 0.0151 0.040 Uiso 1 1 calc R . .
C24 C 0.6762(4) 0.18052(17) 0.08921(18) 0.0295(9) Uani 1 1 d . . .
H24 H 0.5958 0.1986 0.0873 0.035 Uiso 1 1 calc R . .
C25 C 0.1844(3) 0.17783(15) 0.29159(17) 0.0221(8) Uani 1 1 d . . .
C26 C 0.1559(3) 0.17234(16) 0.35738(17) 0.0225(8) Uani 1 1 d . . .
H26 H 0.2071 0.1478 0.3868 0.027 Uiso 1 1 calc R . .
C27 C 0.0543(3) 0.20200(16) 0.38087(17) 0.0245(8) Uani 1 1 d . . .
C28 C -0.0199(3) 0.23899(16) 0.33891(17) 0.0238(8) Uani 1 1 d . . .
C29 C 0.0065(3) 0.24328(16) 0.27304(17) 0.0232(8) Uani 1 1 d . . .
H29 H -0.0455 0.2675 0.2436 0.028 Uiso 1 1 calc R . .
C30 C 0.1063(3) 0.21328(15) 0.24889(17) 0.0217(8) Uani 1 1 d . . .
C31 C 0.0312(4) 0.19540(19) 0.45278(18) 0.0349(10) Uani 1 1 d . . .
H31A H 0.0508 0.2327 0.4761 0.052 Uiso 1 1 calc R . .
H31B H 0.0849 0.1640 0.4730 0.052 Uiso 1 1 calc R . .
H31C H -0.0571 0.1853 0.4560 0.052 Uiso 1 1 calc R . .
C32 C -0.1282(3) 0.27256(18) 0.36326(19) 0.0326(10) Uani 1 1 d . . .
H32A H -0.1897 0.2446 0.3781 0.049 Uiso 1 1 calc R . .
H32B H -0.1682 0.2969 0.3272 0.049 Uiso 1 1 calc R . .
H32C H -0.0973 0.2980 0.4003 0.049 Uiso 1 1 calc R . .
C33 C 0.1297(3) 0.21603(16) 0.17685(16) 0.0226(8) Uani 1 1 d . . .
H33A H 0.1184 0.1761 0.1573 0.027 Uiso 1 1 calc R . .
H33B H 0.0666 0.2424 0.1533 0.027 Uiso 1 1 calc R . .
C34 C 0.2801(3) 0.22911(15) 0.09457(16) 0.0221(8) Uani 1 1 d . . .
H34A H 0.2156 0.2518 0.0669 0.026 Uiso 1 1 calc R . .
H34B H 0.3629 0.2463 0.0874 0.026 Uiso 1 1 calc R . .
C35 C 0.3690(3) 0.12670(16) 0.09594(16) 0.0199(8) Uani 1 1 d . . .
C36 C 0.3750(3) 0.07124(16) 0.06690(16) 0.0216(8) Uani 1 1 d . . .
H36 H 0.4397 0.0447 0.0828 0.026 Uiso 1 1 calc R . .
C37 C 0.2886(3) 0.05372(16) 0.01529(17) 0.0245(8) Uani 1 1 d . . .
C38 C 0.1922(3) 0.09226(17) -0.00840(17) 0.0267(9) Uani 1 1 d . . .
C39 C 0.1915(3) 0.14851(17) 0.01841(16) 0.0250(9) Uani 1 1 d . . .
H39 H 0.1299 0.1758 0.0006 0.030 Uiso 1 1 calc R . .
C40 C 0.2773(3) 0.16676(16) 0.07036(16) 0.0203(8) Uani 1 1 d . . .
C41 C 0.3015(4) -0.00660(17) -0.01560(19) 0.0360(10) Uani 1 1 d . . .
H41A H 0.3712 -0.0280 0.0085 0.054 Uiso 1 1 calc R . .
H41B H 0.3180 -0.0020 -0.0620 0.054 Uiso 1 1 calc R . .
H41C H 0.2235 -0.0289 -0.0132 0.054 Uiso 1 1 calc R . .
C42 C 0.0930(4) 0.0745(2) -0.06265(19) 0.0385(11) Uani 1 1 d . . .
H42A H 0.0325 0.1068 -0.0710 0.058 Uiso 1 1 calc R . .
H42B H 0.0493 0.0391 -0.0490 0.058 Uiso 1 1 calc R . .
H42C H 0.1328 0.0660 -0.1032 0.058 Uiso 1 1 calc R . .
C43 C 0.2686(3) 0.30197(15) 0.18092(17) 0.0226(8) Uani 1 1 d . . .
H43A H 0.2303 0.3109 0.2224 0.027 Uiso 1 1 calc R . .
H43B H 0.2229 0.3247 0.1445 0.027 Uiso 1 1 calc R . .
C44 C 0.4041(3) 0.31972(15) 0.18803(16) 0.0210(8) Uani 1 1 d . . .
C45 C 0.4470(4) 0.37459(16) 0.17120(16) 0.0249(8) Uani 1 1 d . . .
H45 H 0.3904 0.4035 0.1520 0.030 Uiso 1 1 calc R . .
C46 C 0.5741(4) 0.38681(17) 0.18274(17) 0.0324(10) Uani 1 1 d . . .
H46 H 0.6052 0.4249 0.1733 0.039 Uiso 1 1 calc R . .
C47 C 0.6548(4) 0.34324(17) 0.20796(18) 0.0316(9) Uani 1 1 d . . .
H47 H 0.7425 0.3505 0.2153 0.038 Uiso 1 1 calc R . .
C48 C 0.6059(4) 0.28899(17) 0.22239(18) 0.0273(9) Uani 1 1 d . . .
H48 H 0.6618 0.2589 0.2396 0.033 Uiso 1 1 calc R . .
O1S O 0.3770(3) 0.04161(13) 0.32907(15) 0.0436(8) Uani 1 1 d D . .
H1SA H 0.419(4) 0.034(2) 0.2942(16) 0.065 Uiso 1 1 d D . .
H1SB H 0.348(4) 0.0769(13) 0.313(2) 0.065 Uiso 1 1 d D . .
O2S O 0.1725(3) 0.05906(18) 0.18622(19) 0.0654(10) Uani 1 1 d D . .
H2SA H 0.200(5) 0.0209(13) 0.178(3) 0.098 Uiso 1 1 d D . .
H2SB H 0.229(4) 0.079(2) 0.217(2) 0.098 Uiso 1 1 d D . .
O3S O 0.1455(5) -0.0110(2) 0.2992(3) 0.1061(16) Uani 1 1 d D . .
H3SA H 0.131(7) -0.009(4) 0.2509(11) 0.159 Uiso 1 1 d D . .
H3SB H 0.098(6) -0.015(4) 0.336(3) 0.159 Uiso 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
Cu1 0.0220(2) 0.0156(2) 0.0149(2) -0.00027(18) 0.00401(17) -0.00106(18)
Cu2 0.0233(2) 0.0165(2) 0.0154(2) -0.00071(18) 0.00358(17) 0.00074(19)
O1 0.0251(14) 0.0181(13) 0.0249(13) -0.0003(11) 0.0082(11) -0.0020(11)
O2 0.0285(14) 0.0223(13) 0.0113(11) -0.0033(10) 0.0033(10) -0.0007(11)
O3 0.0277(14) 0.0211(14) 0.0236(13) 0.0003(11) 0.0075(11) 0.0028(11)
O4 0.0246(14) 0.0206(13) 0.0161(12) -0.0042(10) 0.0009(10) 0.0026(11)
N1 0.0205(16) 0.0139(15) 0.0149(14) -0.0007(12) 0.0061(12) -0.0033(12)
N2 0.0286(18) 0.0198(16) 0.0146(14) 0.0006(13) 0.0047(13) -0.0002(14)
N3 0.0249(17) 0.0165(16) 0.0170(15) -0.0034(12) 0.0040(12) 0.0022(13)
N4 0.0310(18) 0.0199(16) 0.0136(14) -0.0023(12) 0.0048(13) -0.0011(14)
C1 0.028(2) 0.0159(19) 0.0180(18) 0.0044(15) 0.0059(15) -0.0018(16)
C2 0.031(2) 0.0152(18) 0.0147(17) 0.0045(14) 0.0059(15) -0.0027(16)
C3 0.026(2) 0.019(2) 0.0185(18) 0.0047(15) 0.0060(15) 0.0018(15)
C4 0.034(2) 0.0141(18) 0.0182(17) 0.0046(15) 0.0037(16) -0.0032(16)
C5 0.040(2) 0.0144(19) 0.0198(19) 0.0035(15) 0.0001(17) -0.0071(17)
C6 0.027(2) 0.0188(19) 0.0237(19) 0.0057(16) 0.0012(16) -0.0050(16)
C7 0.048(3) 0.019(2) 0.024(2) -0.0013(16) 0.0031(18) 0.0015(18)
C8 0.054(3) 0.024(2) 0.039(2) -0.0039(19) -0.007(2) -0.008(2)
C9 0.028(2) 0.0169(19) 0.0183(18) 0.0021(15) 0.0029(15) -0.0009(16)
C10 0.0205(19) 0.0195(19) 0.0209(18) -0.0038(15) 0.0015(15) -0.0026(15)
C11 0.034(2) 0.0141(18) 0.0122(16) 0.0008(14) 0.0003(15) -0.0044(16)
C12 0.024(2) 0.0140(18) 0.0222(18) -0.0030(15) 0.0061(15) 0.0036(15)
C13 0.043(2) 0.021(2) 0.0152(17) -0.0017(15) 0.0101(16) -0.0067(18)
C14 0.040(2) 0.027(2) 0.0138(17) 0.0005(16) 0.0032(16) 0.0025(18)
C15 0.031(2) 0.023(2) 0.0175(18) 0.0001(15) -0.0010(16) 0.0043(16)
C16 0.0232(19) 0.0115(17) 0.0161(17) -0.0018(14) 0.0040(14) -0.0050(15)
C17 0.065(3) 0.067(3) 0.020(2) 0.003(2) 0.005(2) 0.025(3)
C18 0.050(3) 0.043(3) 0.0187(19) -0.0048(18) 0.0103(18) 0.003(2)
C19 0.027(2) 0.021(2) 0.0194(18) -0.0036(15) 0.0048(15) 0.0008(16)
C20 0.025(2) 0.022(2) 0.0145(17) -0.0097(15) 0.0049(14) -0.0105(16)
C21 0.029(2) 0.038(2) 0.0203(19) -0.0084(18) 0.0071(16) -0.0078(19)
C22 0.040(3) 0.049(3) 0.0186(19) 0.0029(19) 0.0078(18) -0.018(2)
C23 0.043(3) 0.037(2) 0.021(2) 0.0055(18) 0.0038(18) -0.009(2)
C24 0.033(2) 0.032(2) 0.023(2) 0.0014(17) 0.0033(17) -0.0020(18)
C25 0.022(2) 0.0183(19) 0.0261(19) -0.0034(16) 0.0057(16) -0.0041(15)
C26 0.024(2) 0.020(2) 0.0233(19) -0.0016(16) 0.0061(16) -0.0035(16)
C27 0.026(2) 0.026(2) 0.0220(19) -0.0097(17) 0.0050(16) -0.0100(17)
C28 0.023(2) 0.024(2) 0.0253(19) -0.0127(16) 0.0051(16) -0.0049(16)
C29 0.021(2) 0.023(2) 0.0257(19) -0.0060(16) 0.0011(15) -0.0034(16)
C30 0.023(2) 0.020(2) 0.0228(18) -0.0055(15) 0.0048(15) -0.0036(15)
C31 0.037(2) 0.043(3) 0.026(2) -0.0085(19) 0.0105(18) -0.003(2)
C32 0.029(2) 0.041(3) 0.028(2) -0.0122(19) 0.0078(17) 0.0006(19)
C33 0.023(2) 0.025(2) 0.0196(18) -0.0057(16) 0.0000(15) 0.0015(16)
C34 0.029(2) 0.021(2) 0.0161(17) -0.0019(15) 0.0040(15) 0.0063(16)
C35 0.022(2) 0.023(2) 0.0159(17) -0.0031(15) 0.0052(15) -0.0035(16)
C36 0.027(2) 0.0198(19) 0.0183(17) -0.0037(15) 0.0039(15) 0.0025(16)
C37 0.031(2) 0.026(2) 0.0182(18) -0.0049(16) 0.0073(16) -0.0012(17)
C38 0.023(2) 0.039(2) 0.0184(18) -0.0115(17) 0.0023(15) 0.0000(18)
C39 0.022(2) 0.036(2) 0.0175(18) -0.0077(17) 0.0034(15) 0.0044(17)
C40 0.023(2) 0.023(2) 0.0150(17) -0.0040(15) 0.0062(15) 0.0011(16)
C41 0.045(3) 0.031(2) 0.031(2) -0.0121(19) 0.0001(19) -0.002(2)
C42 0.036(3) 0.048(3) 0.032(2) -0.016(2) 0.0000(19) -0.001(2)
C43 0.032(2) 0.0163(18) 0.0188(18) -0.0009(15) 0.0011(16) 0.0091(16)
C44 0.034(2) 0.0168(19) 0.0136(17) -0.0035(14) 0.0103(15) 0.0017(16)
C45 0.043(2) 0.0173(19) 0.0162(18) -0.0021(15) 0.0115(17) 0.0026(17)
C46 0.058(3) 0.020(2) 0.021(2) -0.0037(16) 0.0147(19) -0.011(2)
C47 0.042(3) 0.023(2) 0.030(2) -0.0039(18) 0.0044(19) -0.0062(19)
C48 0.029(2) 0.025(2) 0.027(2) -0.0041(17) 0.0012(17) -0.0070(17)
O1S 0.060(2) 0.0266(17) 0.049(2) 0.0065(15) 0.0309(16) 0.0045(15)
O2S 0.050(2) 0.087(3) 0.060(2) 0.008(2) 0.0123(18) -0.006(2)
O3S 0.107(4) 0.109(4) 0.107(4) 0.023(4) 0.034(3) -0.004(3)

_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
Cu1 O4 1.930(2) . ?
Cu1 O1 1.939(2) . ?
Cu1 N2 2.009(3) . ?
Cu1 N1 2.027(3) . ?
Cu1 O2 2.149(2) . ?
Cu2 O2 1.950(2) . ?
Cu2 O3 1.958(2) . ?
Cu2 N4 2.015(3) . ?
Cu2 N3 2.046(3) . ?
Cu2 O4 2.144(2) . ?
O1 C1 1.342(4) . ?
O2 C11 1.344(4) . ?
O3 C25 1.339(4) . ?
O4 C35 1.337(4) . ?
N1 C19 1.486(4) . ?
N1 C9 1.492(4) . ?
N1 C10 1.502(4) . ?
N2 C20 1.339(4) . ?
N2 C24 1.344(5) . ?
N3 C43 1.481(4) . ?
N3 C33 1.493(4) . ?
N3 C34 1.511(4) . ?
N4 C48 1.339(4) . ?
N4 C44 1.355(4) . ?
C1 C6 1.382(5) . ?
C1 C2 1.415(5) . ?
C2 C3 1.379(5) . ?
C2 C9 1.507(5) . ?
C3 C4 1.390(5) . ?
C4 C5 1.400(5) . ?
C4 C7 1.508(5) . ?
C5 C6 1.388(5) . ?
C5 C8 1.516(5) . ?
C10 C16 1.508(4) . ?
C11 C12 1.396(5) . ?
C11 C16 1.401(5) . ?
C12 C13 1.388(5) . ?
C13 C14 1.391(5) . ?
C13 C18 1.520(5) . ?
C14 C15 1.383(5) . ?
C14 C17 1.517(5) . ?
C15 C16 1.386(4) . ?
C19 C20 1.504(5) . ?
C20 C21 1.380(5) . ?
C21 C22 1.392(5) . ?
C22 C23 1.367(6) . ?
C23 C24 1.389(5) . ?
C25 C30 1.399(5) . ?
C25 C26 1.401(5) . ?
C26 C27 1.399(5) . ?
C27 C28 1.388(5) . ?
C27 C31 1.509(5) . ?
C28 C29 1.394(5) . ?
C28 C32 1.508(5) . ?
C29 C30 1.392(5) . ?
C30 C33 1.506(5) . ?
C34 C40 1.494(5) . ?
C35 C36 1.391(5) . ?
C35 C40 1.399(5) . ?
C36 C37 1.387(5) . ?
C37 C38 1.401(5) . ?
C37 C41 1.514(5) . ?
C38 C39 1.385(5) . ?
C38 C42 1.509(5) . ?
C39 C40 1.393(5) . ?
C43 C44 1.498(5) . ?
C44 C45 1.379(5) . ?
C45 C46 1.385(5) . ?
C46 C47 1.377(5) . ?
C47 C48 1.377(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
O4 Cu1 O1 96.61(10) . . ?
O4 Cu1 N2 89.69(11) . . ?
O1 Cu1 N2 150.66(11) . . ?
O4 Cu1 N1 168.66(10) . . ?
O1 Cu1 N1 94.39(10) . . ?
N2 Cu1 N1 82.00(11) . . ?
O4 Cu1 O2 79.29(9) . . ?
O1 Cu1 O2 104.11(9) . . ?
N2 Cu1 O2 105.21(10) . . ?
N1 Cu1 O2 95.40(10) . . ?
O2 Cu2 O3 98.04(10) . . ?
O2 Cu2 N4 91.30(11) . . ?
O3 Cu2 N4 151.38(10) . . ?
O2 Cu2 N3 166.43(10) . . ?
O3 Cu2 N3 93.65(11) . . ?
N4 Cu2 N3 81.56(12) . . ?
O2 Cu2 O4 79.00(9) . . ?
O3 Cu2 O4 103.00(9) . . ?
N4 Cu2 O4 105.33(10) . . ?
N3 Cu2 O4 91.72(10) . . ?
C1 O1 Cu1 111.61(19) . . ?
C11 O2 Cu2 131.6(2) . . ?
C11 O2 Cu1 118.7(2) . . ?
Cu2 O2 Cu1 99.66(9) . . ?
C25 O3 Cu2 114.3(2) . . ?
C35 O4 Cu1 128.4(2) . . ?
C35 O4 Cu2 124.1(2) . . ?
Cu1 O4 Cu2 100.48(9) . . ?
C19 N1 C9 109.2(3) . . ?
C19 N1 C10 108.7(3) . . ?
C9 N1 C10 111.0(2) . . ?
C19 N1 Cu1 106.6(2) . . ?
C9 N1 Cu1 112.6(2) . . ?
C10 N1 Cu1 108.6(2) . . ?
C20 N2 C24 119.6(3) . . ?
C20 N2 Cu1 114.0(2) . . ?
C24 N2 Cu1 126.1(3) . . ?
C43 N3 C33 110.6(3) . . ?
C43 N3 C34 107.8(3) . . ?
C33 N3 C34 108.8(3) . . ?
C43 N3 Cu2 105.6(2) . . ?
C33 N3 Cu2 113.9(2) . . ?
C34 N3 Cu2 110.1(2) . . ?
C48 N4 C44 118.2(3) . . ?
C48 N4 Cu2 127.5(3) . . ?
C44 N4 Cu2 114.1(2) . . ?
O1 C1 C6 121.6(3) . . ?
O1 C1 C2 120.5(3) . . ?
C6 C1 C2 117.9(3) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 C9 123.0(3) . . ?
C1 C2 C9 117.8(3) . . ?
C2 C3 C4 122.9(3) . . ?
C3 C4 C5 117.9(3) . . ?
C3 C4 C7 121.0(3) . . ?
C5 C4 C7 121.1(3) . . ?
C6 C5 C4 119.6(3) . . ?
C6 C5 C8 119.7(3) . . ?
C4 C5 C8 120.8(3) . . ?
C1 C6 C5 122.6(3) . . ?
N1 C9 C2 111.7(3) . . ?
N1 C10 C16 115.4(3) . . ?
O2 C11 C12 121.7(3) . . ?
O2 C11 C16 119.4(3) . . ?
C12 C11 C16 118.9(3) . . ?
C13 C12 C11 121.4(3) . . ?
C12 C13 C14 119.9(3) . . ?
C12 C13 C18 118.3(3) . . ?
C14 C13 C18 121.7(3) . . ?
C15 C14 C13 118.3(3) . . ?
C15 C14 C17 120.0(3) . . ?
C13 C14 C17 121.6(3) . . ?
C14 C15 C16 122.8(3) . . ?
C15 C16 C11 118.6(3) . . ?
C15 C16 C10 120.0(3) . . ?
C11 C16 C10 121.1(3) . . ?
N1 C19 C20 110.7(3) . . ?
N2 C20 C21 122.1(3) . . ?
N2 C20 C19 115.1(3) . . ?
C21 C20 C19 122.7(3) . . ?
C20 C21 C22 117.7(4) . . ?
C23 C22 C21 120.7(4) . . ?
C22 C23 C24 118.4(4) . . ?
N2 C24 C23 121.4(4) . . ?
O3 C25 C30 122.0(3) . . ?
O3 C25 C26 120.0(3) . . ?
C30 C25 C26 118.0(3) . . ?
C27 C26 C25 121.8(3) . . ?
C28 C27 C26 119.9(3) . . ?
C28 C27 C31 121.1(3) . . ?
C26 C27 C31 119.0(3) . . ?
C27 C28 C29 118.3(3) . . ?
C27 C28 C32 121.1(3) . . ?
C29 C28 C32 120.6(3) . . ?
C30 C29 C28 122.2(3) . . ?
C29 C30 C25 119.7(3) . . ?
C29 C30 C33 121.6(3) . . ?
C25 C30 C33 118.7(3) . . ?
N3 C33 C30 113.0(3) . . ?
C40 C34 N3 116.2(3) . . ?
O4 C35 C36 122.3(3) . . ?
O4 C35 C40 118.6(3) . . ?
C36 C35 C40 119.1(3) . . ?
C37 C36 C35 121.6(3) . . ?
C36 C37 C38 119.8(3) . . ?
C36 C37 C41 119.3(3) . . ?
C38 C37 C41 120.8(3) . . ?
C39 C38 C37 118.0(3) . . ?
C39 C38 C42 120.1(3) . . ?
C37 C38 C42 121.9(3) . . ?
C38 C39 C40 122.8(3) . . ?
C39 C40 C35 118.5(3) . . ?
C39 C40 C34 121.3(3) . . ?
C35 C40 C34 119.9(3) . . ?
N3 C43 C44 109.7(3) . . ?
N4 C44 C45 122.0(3) . . ?
N4 C44 C43 114.0(3) . . ?
C45 C44 C43 124.0(3) . . ?
C44 C45 C46 118.9(4) . . ?
C47 C46 C45 119.4(4) . . ?
C48 C47 C46 118.7(4) . . ?
N4 C48 C47 122.8(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1SA O1 0.889(19) 1.81(2) 2.686(4) 167(5) .
O1S H1SB O3 0.908(19) 1.94(2) 2.842(4) 175(5) .
O2S H2SB O3 0.94(2) 1.98(3) 2.847(5) 152(5) .
O3S H3SA O2S 0.98(2) 2.10(7) 2.823(6) 129(7) .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.092

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
1 0.004 0.500 0.000 355.3 62.4
2 -0.039 1.000 0.500 355.3 62.2
_platon_squeeze_details          
;
;