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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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#  data retrieval see:
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data_1
_database_code_depnum_ccdc_archive 'CCDC 268278'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H32 Cl Mn N12 Ni2 O11'
_chemical_formula_weight         1016.55

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'
Cl Cl 0.1484 0.1585 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   13.7375(4)
_cell_length_b                   13.7375(4)
_cell_length_c                   21.5674(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3524.87(18)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15658
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      28.28

_exptl_crystal_description       'opaque block'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1554
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '783 images at 1 deg. in\ w and 60 sec.'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20351
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.55
_diffrn_reflns_theta_max         28.31
_reflns_number_total             1941
_reflns_number_gt                1787
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius Collect Software'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+6.8151P] 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         1941
_refine_ls_number_parameters     127
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0970
_refine_ls_wR_factor_gt          0.0944
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.0000 0.334463(16) 0.01954(13) Uani 1 d S . .
Mn1 Mn 0.0000 0.0000 0.5000 0.01714(16) Uani 1 d S . .
N1 N -0.14715(13) -0.06149(13) 0.28067(7) 0.0227(3) Uani 1 d . . .
C2 C -0.17025(17) -0.11167(17) 0.22492(9) 0.0287(4) Uani 1 d . . .
H2 H -0.1197 -0.1329 0.2080 0.034 Uiso 1 calc R . .
C3 C -0.26534(18) -0.13386(17) 0.19093(9) 0.0330(4) Uani 1 d . . .
H3 H -0.2788 -0.1688 0.1514 0.040 Uiso 1 calc R . .
C4 C -0.33958(17) -0.10431(18) 0.21547(10) 0.0343(5) Uani 1 d . . .
H4 H -0.4052 -0.1191 0.1932 0.041 Uiso 1 calc R . .
C5 C -0.31727(17) -0.05253(18) 0.27322(10) 0.0312(4) Uani 1 d . . .
H5 H -0.3672 -0.0312 0.2910 0.037 Uiso 1 calc R . .
C6 C -0.22023(15) -0.03253(15) 0.30456(8) 0.0234(3) Uani 1 d . . .
C7 C -0.19347(16) 0.01646(16) 0.36685(8) 0.0258(4) Uani 1 d . . .
H7 H -0.2417 0.0355 0.3886 0.031 Uiso 1 calc R . .
N8 N -0.10055(13) 0.03208(12) 0.39024(6) 0.0218(3) Uani 1 d . . .
O9 O -0.07726(12) 0.06627(11) 0.44945(5) 0.0255(3) Uani 1 d . . .
Cl20 Cl -0.3884(3) 0.1483(4) 0.3752(2) 0.0591(10) Uani 0.17 d PD . .
O21 O -0.2736(9) 0.2135(10) 0.3676(6) 0.087(4) Uani 0.17 d PD . .
O22 O -0.4145(10) 0.0484(10) 0.4019(6) 0.099(6) Uani 0.17 d PD . .
O23 O -0.4254(11) 0.2041(12) 0.4130(5) 0.091(5) Uani 0.17 d PD . .
O24 O -0.4385(11) 0.1312(13) 0.3180(5) 0.087(4) Uani 0.17 d PD . .
O30 O -0.5000 0.0000 0.5000 0.126(5) Uiso 0.33 d SP . .

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 0.02312(16) 0.02312(16) 0.01239(19) 0.000 0.000 0.01156(8)
Mn1 0.0203(2) 0.0203(2) 0.0108(3) 0.000 0.000 0.01015(10)
N1 0.0236(7) 0.0239(7) 0.0180(7) -0.0001(5) -0.0016(5) 0.0098(6)
C2 0.0308(10) 0.0312(10) 0.0224(9) -0.0048(7) -0.0034(7) 0.0143(8)
C3 0.0329(10) 0.0320(10) 0.0251(9) -0.0048(7) -0.0093(8) 0.0095(8)
C4 0.0246(9) 0.0352(10) 0.0332(10) 0.0034(8) -0.0084(8) 0.0075(8)
C5 0.0249(9) 0.0363(10) 0.0314(10) 0.0042(8) -0.0007(7) 0.0147(8)
C6 0.0223(8) 0.0243(8) 0.0203(8) 0.0026(6) 0.0003(6) 0.0090(7)
C7 0.0265(9) 0.0301(9) 0.0217(8) 0.0000(7) 0.0031(7) 0.0149(7)
N8 0.0260(7) 0.0220(7) 0.0149(6) -0.0012(5) 0.0011(5) 0.0101(6)
O9 0.0316(7) 0.0295(7) 0.0152(6) -0.0038(5) 0.0014(5) 0.0153(6)
Cl20 0.049(2) 0.080(3) 0.051(2) -0.005(2) -0.0040(17) 0.034(2)
O21 0.105(10) 0.083(7) 0.067(9) -0.012(7) -0.008(7) 0.043(8)
O22 0.058(9) 0.171(19) 0.088(11) 0.033(12) 0.011(8) 0.072(11)
O23 0.105(12) 0.136(16) 0.052(8) 0.012(9) 0.028(8) 0.075(12)
O24 0.105(10) 0.083(7) 0.067(9) -0.012(7) -0.008(7) 0.043(8)

_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 N8 2.0392(15) 3 ?
Ni1 N8 2.0392(15) . ?
Ni1 N8 2.0392(15) 2 ?
Ni1 N1 2.1067(15) . ?
Ni1 N1 2.1067(15) 3 ?
Ni1 N1 2.1067(15) 2 ?
Mn1 O9 2.0273(14) 11_556 ?
Mn1 O9 2.0273(14) 12_556 ?
Mn1 O9 2.0273(14) 10_556 ?
Mn1 O9 2.0273(14) . ?
Mn1 O9 2.0273(14) 3 ?
Mn1 O9 2.0273(14) 2 ?
N1 C2 1.343(2) . ?
N1 C6 1.353(2) . ?
C2 C3 1.392(3) . ?
C3 C4 1.378(3) . ?
C4 C5 1.390(3) . ?
C5 C6 1.394(3) . ?
C6 C7 1.465(2) . ?
C7 N8 1.287(2) . ?
N8 O9 1.3429(18) . ?
Cl20 O22 1.361(10) . ?
Cl20 O24 1.373(11) . ?
Cl20 O23 1.379(10) . ?
Cl20 O21 1.380(11) . ?
Cl20 O21 1.887(15) 17_445 ?
Cl20 O24 1.897(14) 18 ?
O21 O24 0.61(2) 18 ?
O21 Cl20 1.887(15) 18 ?
O24 O21 0.61(2) 17_445 ?
O24 Cl20 1.897(14) 17_445 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Ni1 N8 88.74(6) 3 . ?
N8 Ni1 N8 88.74(6) 3 2 ?
N8 Ni1 N8 88.74(6) . 2 ?
N8 Ni1 N1 161.75(6) 3 . ?
N8 Ni1 N1 78.09(6) . . ?
N8 Ni1 N1 103.37(6) 2 . ?
N8 Ni1 N1 78.09(6) 3 3 ?
N8 Ni1 N1 103.37(6) . 3 ?
N8 Ni1 N1 161.75(6) 2 3 ?
N1 Ni1 N1 92.59(6) . 3 ?
N8 Ni1 N1 103.37(6) 3 2 ?
N8 Ni1 N1 161.75(6) . 2 ?
N8 Ni1 N1 78.09(6) 2 2 ?
N1 Ni1 N1 92.59(6) . 2 ?
N1 Ni1 N1 92.59(6) 3 2 ?
O9 Mn1 O9 93.80(5) 11_556 12_556 ?
O9 Mn1 O9 93.80(5) 11_556 10_556 ?
O9 Mn1 O9 93.80(5) 12_556 10_556 ?
O9 Mn1 O9 86.20(5) 11_556 . ?
O9 Mn1 O9 86.20(5) 12_556 . ?
O9 Mn1 O9 180.0 10_556 . ?
O9 Mn1 O9 86.20(5) 11_556 3 ?
O9 Mn1 O9 180.0 12_556 3 ?
O9 Mn1 O9 86.20(5) 10_556 3 ?
O9 Mn1 O9 93.80(5) . 3 ?
O9 Mn1 O9 180.0 11_556 2 ?
O9 Mn1 O9 86.20(5) 12_556 2 ?
O9 Mn1 O9 86.20(5) 10_556 2 ?
O9 Mn1 O9 93.80(5) . 2 ?
O9 Mn1 O9 93.80(5) 3 2 ?
C2 N1 C6 118.19(16) . . ?
C2 N1 Ni1 129.20(13) . . ?
C6 N1 Ni1 112.13(11) . . ?
N1 C2 C3 122.61(19) . . ?
C4 C3 C2 118.99(18) . . ?
C3 C4 C5 119.24(18) . . ?
C4 C5 C6 118.66(19) . . ?
N1 C6 C5 122.30(17) . . ?
N1 C6 C7 115.57(16) . . ?
C5 C6 C7 122.06(18) . . ?
N8 C7 C6 115.87(16) . . ?
C7 N8 O9 118.30(15) . . ?
C7 N8 Ni1 117.09(12) . . ?
O9 N8 Ni1 124.60(11) . . ?
N8 O9 Mn1 116.17(10) . . ?
O22 Cl20 O24 110.6(6) . . ?
O22 Cl20 O23 109.0(5) . . ?
O24 Cl20 O23 109.5(5) . . ?
O22 Cl20 O21 110.1(6) . . ?
O24 Cl20 O21 108.6(6) . . ?
O23 Cl20 O21 109.1(6) . . ?
O22 Cl20 O21 121.2(9) . 17_445 ?
O24 Cl20 O21 11.4(8) . 17_445 ?
O23 Cl20 O21 100.5(7) . 17_445 ?
O21 Cl20 O21 106.3(7) . 17_445 ?
O22 Cl20 O24 111.7(8) . 18 ?
O24 Cl20 O24 98.1(6) . 18 ?
O23 Cl20 O24 117.5(7) . 18 ?
O21 Cl20 O24 11.2(6) . 18 ?
O21 Cl20 O24 96.8(5) 17_445 18 ?
O24 O21 Cl20 142.7(17) 18 . ?
O24 O21 Cl20 26.7(19) 18 18 ?
Cl20 O21 Cl20 123.9(8) . 18 ?
O21 O24 Cl20 142(3) 17_445 . ?
O21 O24 Cl20 26.2(12) 17_445 17_445 ?
Cl20 O24 Cl20 123.6(8) . 17_445 ?

_diffrn_measured_fraction_theta_max 0.330
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.330
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.065


data_2
_database_code_depnum_ccdc_archive 'CCDC 268279'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         '[C36 H30 Cr N12 Ni2 O6]+, (Cl O4)-'
_chemical_formula_sum            'C36 H30 Cl Cr N12 Ni2 O10'
_chemical_formula_weight         995.59

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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           Trigonal
_symmetry_space_group_name_H-M   R-3 #No.148

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   13.6398(3)
_cell_length_b                   13.6398(3)
_cell_length_c                   21.5949(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3479.35(13)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1521
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.8654
_exptl_absorpt_correction_T_max  0.9172

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '959 images at 1.0 deg. in \w, 20 sec./frame'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29998
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         4.12
_diffrn_reflns_theta_max         31.04
_reflns_number_total             2467
_reflns_number_gt                2246
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Nonius Collect Software'
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      
'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+7.1441P] 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         2467
_refine_ls_number_parameters     132
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1088
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.008
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.0000 0.0000 0.0000 0.01514(13) Uani 1 d S . .
Ni1 Ni 0.0000 0.0000 0.164490(14) 0.01630(11) Uani 1 d S . .
N1 N 0.14801(12) 0.06154(12) 0.21845(6) 0.0202(3) Uani 1 d . . .
C2 C 0.17084(15) 0.11131(16) 0.27430(8) 0.0259(3) Uani 1 d . . .
H2 H 0.1201 0.1329 0.2912 0.031 Uiso 1 calc R . .
C3 C 0.26622(16) 0.13252(17) 0.30844(8) 0.0301(4) Uani 1 d . . .
H3 H 0.2799 0.1676 0.3479 0.036 Uiso 1 calc R . .
C4 C 0.34049(16) 0.10183(17) 0.28402(9) 0.0302(4) Uani 1 d . . .
H4 H 0.4061 0.1156 0.3065 0.036 Uiso 1 calc R . .
C5 C 0.31804(15) 0.05048(17) 0.22611(8) 0.0277(3) Uani 1 d . . .
H5 H 0.3679 0.0286 0.2084 0.033 Uiso 1 calc R . .
C6 C 0.22096(13) 0.03177(14) 0.19459(7) 0.0209(3) Uani 1 d . . .
C7 C 0.19489(14) -0.01610(15) 0.13203(7) 0.0214(3) Uani 1 d . . .
H7 H 0.2433 -0.0356 0.1103 0.026 Uiso 1 calc R . .
N8 N 0.10222(11) -0.02995(11) 0.10845(6) 0.0174(2) Uani 1 d . . .
O9 O 0.07974(10) -0.06274(10) 0.04919(5) 0.0195(2) Uani 1 d . . .
Cl10 Cl 0.8464(5) 0.4584(4) -0.1241(2) 0.0598(11) Uani 0.17 d PD . .
O11 O 0.7820(12) 0.5137(13) -0.1324(8) 0.42(7) Uani 0.17 d PD . .
O12 O 0.9531(8) 0.5355(9) -0.0995(6) 0.095(6) Uani 0.17 d PD . .
O13 O 0.7869(12) 0.3660(9) -0.0831(5) 0.113(8) Uani 0.17 d PD . .
O14 O 0.8588(13) 0.4183(11) -0.1826(4) 0.095(7) Uani 0.17 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
Cr1 0.01822(18) 0.01822(18) 0.0090(2) 0.000 0.000 0.00911(9)
Ni1 0.01924(13) 0.01924(13) 0.01042(16) 0.000 0.000 0.00962(7)
N1 0.0215(6) 0.0226(6) 0.0144(5) -0.0005(4) -0.0019(4) 0.0093(5)
C2 0.0278(8) 0.0301(8) 0.0188(7) -0.0053(6) -0.0044(6) 0.0138(7)
C3 0.0298(9) 0.0326(9) 0.0215(7) -0.0065(6) -0.0095(6) 0.0108(7)
C4 0.0240(8) 0.0352(9) 0.0242(8) -0.0002(7) -0.0084(6) 0.0095(7)
C5 0.0223(7) 0.0377(9) 0.0223(7) 0.0011(6) -0.0034(6) 0.0143(7)
C6 0.0209(7) 0.0249(7) 0.0153(6) 0.0021(5) -0.0017(5) 0.0103(6)
C7 0.0223(7) 0.0291(8) 0.0156(6) 0.0005(5) -0.0007(5) 0.0148(6)
N8 0.0219(6) 0.0200(6) 0.0110(5) 0.0006(4) -0.0004(4) 0.0108(5)
O9 0.0259(5) 0.0258(5) 0.0104(4) -0.0010(4) -0.0014(4) 0.0157(5)
Cl10 0.080(3) 0.062(3) 0.054(2) -0.0039(19) 0.001(2) 0.048(2)
O11 0.81(15) 0.046(14) 0.085(18) -0.001(14) 0.02(5) -0.04(3)
O12 0.149(18) 0.095(13) 0.095(12) -0.013(10) -0.029(12) 0.101(14)
O13 0.17(2) 0.072(11) 0.069(10) 0.007(9) -0.045(12) 0.039(12)
O14 0.090(14) 0.111(14) 0.120(16) 0.058(12) 0.050(12) 0.078(13)

_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
Cr1 O9 1.9936(11) 2 ?
Cr1 O9 1.9936(11) 10 ?
Cr1 O9 1.9936(11) 3 ?
Cr1 O9 1.9936(11) 12 ?
Cr1 O9 1.9937(11) 11 ?
Cr1 O9 1.9937(11) . ?
Ni1 N8 2.0359(13) 2 ?
Ni1 N8 2.0359(13) 3 ?
Ni1 N8 2.0359(13) . ?
Ni1 N1 2.1080(13) 2 ?
Ni1 N1 2.1080(13) . ?
Ni1 N1 2.1081(13) 3 ?
N1 C2 1.342(2) . ?
N1 C6 1.351(2) . ?
C2 C3 1.394(2) . ?
C3 C4 1.380(3) . ?
C4 C5 1.391(3) . ?
C5 C6 1.394(2) . ?
C6 C7 1.465(2) . ?
C7 N8 1.286(2) . ?
N8 O9 1.3396(15) . ?
Cl10 O12 1.406(5) . ?
Cl10 O13 1.417(5) . ?
Cl10 O14 1.422(5) . ?
Cl10 O11 1.425(5) . ?
Cl10 O14 1.746(13) 18_544 ?
Cl10 O11 1.853(16) 17_554 ?
O11 O14 0.460(16) 18_544 ?
O11 Cl10 1.852(16) 18_544 ?
O14 O11 0.460(16) 17_554 ?
O14 Cl10 1.746(13) 17_554 ?

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
O9 Cr1 O9 85.75(4) 2 10 ?
O9 Cr1 O9 94.25(4) 2 3 ?
O9 Cr1 O9 85.75(4) 10 3 ?
O9 Cr1 O9 85.75(4) 2 12 ?
O9 Cr1 O9 94.25(4) 10 12 ?
O9 Cr1 O9 180.0 3 12 ?
O9 Cr1 O9 180.0 2 11 ?
O9 Cr1 O9 94.25(4) 10 11 ?
O9 Cr1 O9 85.75(4) 3 11 ?
O9 Cr1 O9 94.25(4) 12 11 ?
O9 Cr1 O9 94.25(4) 2 . ?
O9 Cr1 O9 180.0 10 . ?
O9 Cr1 O9 94.25(4) 3 . ?
O9 Cr1 O9 85.75(4) 12 . ?
O9 Cr1 O9 85.75(4) 11 . ?
N8 Ni1 N8 88.28(5) 2 3 ?
N8 Ni1 N8 88.28(5) 2 . ?
N8 Ni1 N8 88.28(5) 3 . ?
N8 Ni1 N1 78.05(5) 2 2 ?
N8 Ni1 N1 104.35(5) 3 2 ?
N8 Ni1 N1 160.92(5) . 2 ?
N8 Ni1 N1 104.35(5) 2 . ?
N8 Ni1 N1 160.93(5) 3 . ?
N8 Ni1 N1 78.05(5) . . ?
N1 Ni1 N1 92.38(5) 2 . ?
N8 Ni1 N1 160.92(5) 2 3 ?
N8 Ni1 N1 78.05(5) 3 3 ?
N8 Ni1 N1 104.35(5) . 3 ?
N1 Ni1 N1 92.39(5) 2 3 ?
N1 Ni1 N1 92.39(5) . 3 ?
C2 N1 C6 118.38(14) . . ?
C2 N1 Ni1 129.20(12) . . ?
C6 N1 Ni1 111.85(10) . . ?
N1 C2 C3 122.45(17) . . ?
C4 C3 C2 119.05(16) . . ?
C3 C4 C5 119.11(16) . . ?
C4 C5 C6 118.74(17) . . ?
N1 C6 C5 122.26(15) . . ?
N1 C6 C7 115.76(13) . . ?
C5 C6 C7 121.90(15) . . ?
N8 C7 C6 115.62(14) . . ?
C7 N8 O9 118.12(13) . . ?
C7 N8 Ni1 117.17(10) . . ?
O9 N8 Ni1 124.71(10) . . ?
N8 O9 Cr1 116.65(9) . . ?
O12 Cl10 O13 110.4(5) . . ?
O12 Cl10 O14 110.2(5) . . ?
O13 Cl10 O14 109.7(5) . . ?
O12 Cl10 O11 109.5(5) . . ?
O13 Cl10 O11 108.7(5) . . ?
O14 Cl10 O11 108.4(5) . . ?
O12 Cl10 O14 112.3(8) . 18_544 ?
O13 Cl10 O14 116.7(8) . 18_544 ?
O14 Cl10 O14 96.7(5) . 18_544 ?
O11 Cl10 O14 12.0(6) . 18_544 ?
O12 Cl10 O11 115.9(9) . 17_554 ?
O13 Cl10 O11 107.0(6) . 17_554 ?
O14 Cl10 O11 5.7(9) . 17_554 ?
O11 Cl10 O11 105.2(7) . 17_554 ?
O14 Cl10 O11 93.8(6) 18_544 17_554 ?
O14 O11 Cl10 128(2) 18_544 . ?
O14 O11 Cl10 18(3) 18_544 18_544 ?
Cl10 O11 Cl10 120.2(9) . 18_544 ?
O11 O14 Cl10 156(4) 17_554 . ?
O11 O14 Cl10 40.1(16) 17_554 17_554 ?
Cl10 O14 Cl10 127.9(9) . 17_554 ?

_diffrn_measured_fraction_theta_max 0.331
_diffrn_reflns_theta_full        31.04
_diffrn_measured_fraction_theta_full 0.331
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.092


data_3
_database_code_depnum_ccdc_archive 'CCDC 268280'

_audit_creation_method           SHELXL
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     '[C36 H31 N12 Ni3 O6], ClO4, CH3CN'
_chemical_formula_sum            'C38 H34 Cl N13 Ni3 O10'
_chemical_formula_weight         1044.36
_chemical_melting_point          ?
_chemical_compound_source        ?

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'
Cl Cl 0.1484 0.1585 '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                   11.1498(3)
_cell_length_b                   15.8194(3)
_cell_length_c                   23.9548(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.13(1)
_cell_angle_gamma                90.00
_cell_volume                     4130.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    142301
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      31.00

_exptl_crystal_description       'opaque block'
_exptl_crystal_colour            red-orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2136
_exptl_absorpt_coefficient_mu    1.494
_exptl_absorpt_correction_type   None
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Nonius Kappa-CCD'
_diffrn_measurement_method       '\w-scan, 1071 images at 1 deg. and 30 sec.'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            106567
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         31.03
_reflns_number_total             13148
_reflns_number_observed          11275
_reflns_observed_criterion       >2sigma(I)

_computing_data_collection       'Nonius Collect Software'
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for 16 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+4.6892P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13132
_refine_ls_number_parameters     593
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_obs          0.0355
_refine_ls_wR_factor_all         0.0821
_refine_ls_wR_factor_obs         0.0726
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.087
_refine_ls_restrained_S_all      1.134
_refine_ls_restrained_S_obs      1.087
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni1 Ni 0.30602(2) 0.661138(13) 0.169383(9) 0.01208(5) Uani 1 d . .
Ni2 Ni 0.41995(2) 0.745564(13) 0.068749(9) 0.01275(5) Uani 1 d . .
Ni3 Ni 0.07885(2) 0.765044(13) 0.089683(9) 0.01251(5) Uani 1 d . .
N1 N 0.34559(13) 0.67571(9) 0.25926(6) 0.0151(3) Uani 1 d . .
C2 C 0.2784(2) 0.65284(12) 0.29697(8) 0.0193(3) Uani 1 d . .
H2 H 0.1961(2) 0.63509(12) 0.28300(8) 0.023 Uiso 1 calc R .
C3 C 0.3235(2) 0.65391(13) 0.35552(8) 0.0235(4) Uani 1 d . .
H3 H 0.2739(2) 0.63572(13) 0.38098(8) 0.028 Uiso 1 calc R .
C4 C 0.4426(2) 0.68210(13) 0.37625(8) 0.0225(4) Uani 1 d . .
H4 H 0.4752(2) 0.68448(13) 0.41619(8) 0.027 Uiso 1 calc R .
C5 C 0.5131(2) 0.70666(12) 0.33791(8) 0.0196(3) Uani 1 d . .
H5 H 0.5943(2) 0.72703(12) 0.35110(8) 0.024 Uiso 1 calc R .
C6 C 0.4628(2) 0.70098(11) 0.27947(7) 0.0161(3) Uani 1 d . .
C7 C 0.5337(2) 0.71963(11) 0.23646(7) 0.0171(3) Uani 1 d . .
H7 H 0.6135(2) 0.74365(11) 0.24616(7) 0.020 Uiso 1 calc R .
N8 N 0.48202(13) 0.70168(9) 0.18425(6) 0.0147(3) Uani 1 d . .
O9 O 0.54184(11) 0.71926(8) 0.14303(5) 0.0173(2) Uani 1 d . .
N11 N 0.32932(13) 0.53120(9) 0.18706(6) 0.0142(3) Uani 1 d . .
C12 C 0.4327(2) 0.48609(11) 0.19919(7) 0.0164(3) Uani 1 d . .
H12 H 0.5060(2) 0.51035(11) 0.19202(7) 0.020 Uiso 1 calc R .
C13 C 0.4375(2) 0.40482(11) 0.22196(8) 0.0199(3) Uani 1 d . .
H13 H 0.5117(2) 0.37339(11) 0.22867(8) 0.024 Uiso 1 calc R .
C14 C 0.3317(2) 0.37061(11) 0.23467(8) 0.0208(4) Uani 1 d . .
H14 H 0.3336(2) 0.31667(11) 0.25226(8) 0.025 Uiso 1 calc R .
C15 C 0.2229(2) 0.41629(11) 0.22133(7) 0.0184(3) Uani 1 d . .
H15 H 0.1490(2) 0.39355(11) 0.22889(7) 0.022 Uiso 1 calc R .
C16 C 0.2240(2) 0.49628(11) 0.19660(7) 0.0152(3) Uani 1 d . .
C17 C 0.1136(2) 0.54721(11) 0.17863(8) 0.0169(3) Uani 1 d . .
H17 H 0.0342(2) 0.52611(11) 0.17951(8) 0.020 Uiso 1 calc R .
N18 N 0.13058(13) 0.62313(9) 0.16138(6) 0.0145(3) Uani 1 d . .
O19 O 0.03429(11) 0.67262(8) 0.14183(5) 0.0172(2) Uani 1 d . .
N21 N 0.50328(13) 0.86266(9) 0.06584(6) 0.0151(3) Uani 1 d . .
C22 C 0.5874(2) 0.88572(12) 0.03618(8) 0.0192(3) Uani 1 d . .
H22 H 0.6141(2) 0.84496(12) 0.01230(8) 0.023 Uiso 1 calc R .
C23 C 0.6375(2) 0.96644(13) 0.03874(8) 0.0230(4) Uani 1 d . .
H23 H 0.6978(2) 0.98027(13) 0.01748(8) 0.028 Uiso 1 calc R .
C24 C 0.5978(2) 1.02610(13) 0.07287(8) 0.0242(4) Uani 1 d . .
H24 H 0.6302(2) 1.08184(13) 0.07538(8) 0.029 Uiso 1 calc R .
C25 C 0.5097(2) 1.00351(12) 0.10350(8) 0.0215(4) Uani 1 d . .
H25 H 0.4808(2) 1.04366(12) 0.12708(8) 0.026 Uiso 1 calc R .
C26 C 0.4645(2) 0.92139(11) 0.09913(7) 0.0157(3) Uani 1 d . .
C27 C 0.3713(2) 0.89269(11) 0.13007(7) 0.0162(3) Uani 1 d . .
H27 H 0.3441(2) 0.92764(11) 0.15718(7) 0.019 Uiso 1 calc R .
N28 N 0.32877(13) 0.81809(9) 0.11856(6) 0.0132(3) Uani 1 d . .
O29 O 0.24574(11) 0.78775(7) 0.14857(5) 0.0134(2) Uani 1 d . .
N31 N 0.52023(14) 0.66520(9) 0.02785(7) 0.0178(3) Uani 1 d . .
C32 C 0.6149(2) 0.61648(12) 0.05320(8) 0.0214(4) Uani 1 d . .
H32 H 0.6504(2) 0.62572(12) 0.09237(8) 0.026 Uiso 1 calc R .
C33 C 0.6626(2) 0.55309(13) 0.02410(9) 0.0268(4) Uani 1 d . .
H33 H 0.7294(2) 0.51948(13) 0.04313(9) 0.032 Uiso 1 calc R .
C34 C 0.6115(2) 0.53964(12) -0.03288(10) 0.0283(4) Uani 1 d . .
H34 H 0.6423(2) 0.49631(12) -0.05348(10) 0.034 Uiso 1 calc R .
C35 C 0.5141(2) 0.59045(12) -0.05985(9) 0.0244(4) Uani 1 d . .
H35 H 0.4784(2) 0.58285(12) -0.09917(9) 0.029 Uiso 1 calc R .
C36 C 0.4703(2) 0.65254(11) -0.02802(8) 0.0194(3) Uani 1 d . .
C37 C 0.3661(2) 0.70655(11) -0.05219(8) 0.0187(3) Uani 1 d . .
H37 H 0.3296(2) 0.70506(11) -0.09176(8) 0.022 Uiso 1 calc R .
N38 N 0.32558(14) 0.75645(9) -0.01767(6) 0.0163(3) Uani 1 d . .
O39 O 0.22807(12) 0.80469(9) -0.04258(6) 0.0204(3) Uani 1 d D .
H39 H 0.2153(47) 0.8430(31) -0.0168(19) 0.026 Uiso 0.50 d PD .
N41 N -0.04676(13) 0.72176(10) 0.01909(6) 0.0160(3) Uani 1 d . .
C42 C -0.1612(2) 0.74955(12) -0.00018(8) 0.0193(3) Uani 1 d . .
H42 H -0.1912(2) 0.79374(12) 0.02001(8) 0.023 Uiso 1 calc R .
C43 C -0.2380(2) 0.71656(13) -0.04846(8) 0.0225(4) Uani 1 d . .
H43 H -0.3189(2) 0.73771(13) -0.06105(8) 0.027 Uiso 1 calc R .
C44 C -0.1942(2) 0.65209(14) -0.07793(8) 0.0240(4) Uani 1 d . .
H44 H -0.2451(2) 0.62811(14) -0.11092(8) 0.029 Uiso 1 calc R .
C45 C -0.0753(2) 0.62288(13) -0.05885(8) 0.0230(4) Uani 1 d . .
H45 H -0.0434(2) 0.57899(13) -0.07856(8) 0.028 Uiso 1 calc R .
C46 C -0.0036(2) 0.65951(12) -0.00998(7) 0.0177(3) Uani 1 d . .
C47 C 0.1229(2) 0.63314(11) 0.01356(7) 0.0178(3) Uani 1 d . .
H47 H 0.1598(2) 0.58731(11) -0.00219(7) 0.021 Uiso 1 calc R .
N48 N 0.18114(13) 0.67524(9) 0.05656(6) 0.0139(3) Uani 1 d . .
O49 O 0.29746(11) 0.64935(7) 0.08117(5) 0.0138(2) Uani 1 d . .
N51 N -0.04484(13) 0.84016(9) 0.12057(6) 0.0166(3) Uani 1 d . .
C52 C -0.1308(2) 0.81294(12) 0.14787(8) 0.0192(3) Uani 1 d . .
H52 H -0.1429(2) 0.75378(12) 0.15074(8) 0.023 Uiso 1 calc R .
C53 C -0.2032(2) 0.86755(13) 0.17218(8) 0.0217(4) Uani 1 d . .
H53 H -0.2651(2) 0.84636(13) 0.19030(8) 0.026 Uiso 1 calc R .
C54 C -0.1827(2) 0.95367(13) 0.16928(8) 0.0224(4) Uani 1 d . .
H54 H -0.2264(2) 0.99237(13) 0.18793(8) 0.027 Uiso 1 calc R .
C55 C -0.0981(2) 0.98294(12) 0.13896(8) 0.0222(4) Uani 1 d . .
H55 H -0.0850(2) 1.04188(12) 0.13546(8) 0.027 Uiso 1 calc R .
C56 C -0.0323(2) 0.92448(11) 0.11367(7) 0.0181(3) Uani 1 d . .
C57 C 0.0485(2) 0.94849(12) 0.07605(8) 0.0208(3) Uani 1 d . .
H57 H 0.0628(2) 1.00616(12) 0.06847(8) 0.025 Uiso 1 calc R .
N58 N 0.10066(14) 0.88777(10) 0.05313(7) 0.0199(3) Uani 1 d . .
O59 O 0.16924(13) 0.91396(9) 0.01673(6) 0.0249(3) Uani 1 d D .
H59 H 0.1823(49) 0.8645(29) 0.0000(22) 0.032 Uiso 0.50 d PD .
N60 N 0.4874(2) 0.21015(13) 0.14779(10) 0.0375(4) Uani 1 d . .
C61 C 0.5431(2) 0.18660(12) 0.19021(10) 0.0259(4) Uani 1 d . .
C62 C 0.6115(2) 0.1540(2) 0.24403(10) 0.0383(5) Uani 1 d . .
H62A H 0.5645(8) 0.1629(11) 0.2738(2) 0.057 Uiso 1 calc R .
H62B H 0.6903(8) 0.1836(8) 0.2545(4) 0.057 Uiso 1 calc R .
H62C H 0.6262(15) 0.0933(3) 0.2402(2) 0.057 Uiso 1 calc R .
Cl70 Cl 0.80327(4) 0.42428(3) 0.18700(2) 0.02144(9) Uani 1 d . .
O71 O 0.72356(15) 0.49670(11) 0.18191(8) 0.0373(4) Uani 1 d . .
O72 O 0.89967(14) 0.43324(10) 0.23726(7) 0.0333(3) Uani 1 d . .
O73 O 0.8558(2) 0.41885(11) 0.13705(7) 0.0372(4) Uani 1 d . .
O74 O 0.73368(14) 0.34818(10) 0.19147(6) 0.0294(3) Uani 1 d . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01219(9) 0.01152(9) 0.01332(9) 0.00069(7) 0.00446(7) -0.00072(7)
Ni2 0.01298(9) 0.01213(10) 0.01445(10) 0.00083(7) 0.00586(7) 0.00026(7)
Ni3 0.01185(9) 0.01328(10) 0.01301(9) -0.00043(7) 0.00398(7) -0.00013(7)
N1 0.0165(7) 0.0135(6) 0.0158(6) 0.0003(5) 0.0046(5) 0.0016(5)
C2 0.0186(8) 0.0212(8) 0.0193(8) -0.0010(6) 0.0070(7) 0.0018(6)
C3 0.0267(10) 0.0276(10) 0.0188(8) 0.0005(7) 0.0104(7) 0.0035(8)
C4 0.0263(9) 0.0269(9) 0.0138(8) -0.0024(7) 0.0030(7) 0.0037(7)
C5 0.0190(8) 0.0204(8) 0.0179(8) -0.0018(6) 0.0003(6) 0.0022(7)
C6 0.0172(8) 0.0136(7) 0.0178(8) 0.0005(6) 0.0041(6) 0.0021(6)
C7 0.0149(8) 0.0167(8) 0.0196(8) 0.0010(6) 0.0033(6) -0.0015(6)
N8 0.0140(6) 0.0134(6) 0.0175(7) 0.0024(5) 0.0050(5) 0.0011(5)
O9 0.0143(6) 0.0215(6) 0.0176(6) 0.0048(5) 0.0067(5) 0.0006(5)
N11 0.0157(6) 0.0139(6) 0.0138(6) 0.0000(5) 0.0049(5) -0.0001(5)
C12 0.0171(8) 0.0169(8) 0.0147(7) -0.0008(6) 0.0024(6) 0.0003(6)
C13 0.0221(9) 0.0177(8) 0.0174(8) 0.0001(6) -0.0015(7) 0.0029(6)
C14 0.0309(10) 0.0142(8) 0.0164(8) 0.0017(6) 0.0031(7) -0.0010(7)
C15 0.0252(9) 0.0148(8) 0.0166(8) -0.0003(6) 0.0075(7) -0.0038(6)
C16 0.0181(8) 0.0140(7) 0.0153(7) -0.0006(6) 0.0073(6) -0.0019(6)
C17 0.0160(8) 0.0156(8) 0.0213(8) 0.0000(6) 0.0088(6) -0.0027(6)
N18 0.0138(6) 0.0153(6) 0.0156(6) -0.0001(5) 0.0060(5) 0.0003(5)
O19 0.0137(6) 0.0173(6) 0.0218(6) 0.0033(5) 0.0065(5) 0.0021(4)
N21 0.0125(6) 0.0164(7) 0.0165(7) 0.0030(5) 0.0032(5) -0.0013(5)
C22 0.0148(8) 0.0235(9) 0.0195(8) 0.0066(7) 0.0043(6) 0.0001(6)
C23 0.0165(8) 0.0289(10) 0.0229(9) 0.0100(7) 0.0021(7) -0.0049(7)
C24 0.0221(9) 0.0217(9) 0.0263(9) 0.0070(7) -0.0005(7) -0.0084(7)
C25 0.0221(9) 0.0174(8) 0.0237(9) 0.0012(7) 0.0016(7) -0.0043(7)
C26 0.0144(7) 0.0155(7) 0.0166(7) 0.0017(6) 0.0018(6) -0.0027(6)
C27 0.0184(8) 0.0153(7) 0.0159(7) -0.0007(6) 0.0054(6) -0.0007(6)
N28 0.0119(6) 0.0140(6) 0.0144(6) 0.0024(5) 0.0046(5) -0.0002(5)
O29 0.0133(5) 0.0145(5) 0.0137(5) 0.0002(4) 0.0058(4) -0.0017(4)
N31 0.0202(7) 0.0149(7) 0.0217(7) 0.0009(5) 0.0120(6) -0.0004(5)
C32 0.0215(9) 0.0189(8) 0.0269(9) 0.0041(7) 0.0122(7) 0.0021(7)
C33 0.0279(10) 0.0201(9) 0.0369(11) 0.0045(8) 0.0170(9) 0.0065(7)
C34 0.0344(11) 0.0162(8) 0.0419(12) -0.0019(8) 0.0253(9) 0.0012(8)
C35 0.0290(10) 0.0201(9) 0.0289(10) -0.0051(7) 0.0169(8) -0.0035(7)
C36 0.0226(9) 0.0156(8) 0.0236(9) -0.0017(6) 0.0133(7) -0.0046(6)
C37 0.0216(8) 0.0195(8) 0.0167(8) -0.0017(6) 0.0082(7) -0.0043(7)
N38 0.0169(7) 0.0154(7) 0.0176(7) 0.0015(5) 0.0062(5) -0.0016(5)
O39 0.0194(6) 0.0230(7) 0.0182(6) 0.0010(5) 0.0028(5) 0.0028(5)
N41 0.0141(7) 0.0201(7) 0.0143(6) -0.0001(5) 0.0036(5) -0.0018(5)
C42 0.0149(8) 0.0260(9) 0.0175(8) 0.0007(7) 0.0049(6) -0.0006(7)
C43 0.0155(8) 0.0349(10) 0.0168(8) 0.0034(7) 0.0032(6) -0.0039(7)
C44 0.0194(9) 0.0376(11) 0.0144(8) -0.0040(7) 0.0026(7) -0.0087(8)
C45 0.0212(9) 0.0300(10) 0.0185(8) -0.0069(7) 0.0056(7) -0.0062(7)
C46 0.0173(8) 0.0219(8) 0.0150(8) -0.0018(6) 0.0056(6) -0.0032(6)
C47 0.0172(8) 0.0187(8) 0.0187(8) -0.0037(6) 0.0063(6) -0.0008(6)
N48 0.0128(6) 0.0151(6) 0.0146(6) 0.0009(5) 0.0049(5) -0.0004(5)
O49 0.0120(5) 0.0145(5) 0.0157(5) 0.0008(4) 0.0043(4) 0.0009(4)
N51 0.0162(7) 0.0169(7) 0.0161(7) -0.0007(5) 0.0016(5) 0.0020(5)
C52 0.0178(8) 0.0198(8) 0.0201(8) 0.0012(7) 0.0040(6) 0.0020(6)
C53 0.0180(8) 0.0274(9) 0.0205(8) 0.0012(7) 0.0059(7) 0.0036(7)
C54 0.0206(9) 0.0262(9) 0.0202(8) -0.0036(7) 0.0042(7) 0.0081(7)
C55 0.0246(9) 0.0186(8) 0.0241(9) -0.0043(7) 0.0067(7) 0.0028(7)
C56 0.0181(8) 0.0180(8) 0.0174(8) -0.0015(6) 0.0018(6) 0.0019(6)
C57 0.0237(9) 0.0162(8) 0.0239(9) 0.0014(7) 0.0084(7) 0.0021(7)
N58 0.0155(7) 0.0256(8) 0.0185(7) 0.0026(6) 0.0034(6) 0.0000(6)
O59 0.0268(7) 0.0225(7) 0.0284(7) 0.0040(6) 0.0126(6) 0.0002(6)
N60 0.0331(10) 0.0310(10) 0.0489(12) 0.0062(9) 0.0097(9) 0.0007(8)
C61 0.0261(10) 0.0186(9) 0.0366(11) -0.0058(8) 0.0145(9) -0.0036(7)
C62 0.0362(12) 0.0492(14) 0.0308(11) -0.0044(10) 0.0101(10) -0.0048(11)
Cl70 0.0171(2) 0.0226(2) 0.0258(2) -0.0010(2) 0.0070(2) -0.0032(2)
O71 0.0282(8) 0.0324(8) 0.0506(10) -0.0015(7) 0.0065(7) 0.0078(7)
O72 0.0260(8) 0.0347(8) 0.0352(8) 0.0021(7) -0.0026(6) -0.0084(6)
O73 0.0378(9) 0.0425(9) 0.0384(9) -0.0078(7) 0.0240(7) -0.0124(7)
O74 0.0280(7) 0.0313(8) 0.0294(7) 0.0003(6) 0.0069(6) -0.0141(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N18 2.0167(14) . ?
Ni1 N8 2.0238(14) . ?
Ni1 O49 2.1035(12) . ?
Ni1 N11 2.1037(14) . ?
Ni1 N1 2.1174(14) . ?
Ni1 O29 2.1381(12) . ?
Ni2 O9 2.0420(13) . ?
Ni2 N28 2.0696(14) . ?
Ni2 N31 2.0704(15) . ?
Ni2 N21 2.0801(14) . ?
Ni2 O49 2.1074(12) . ?
Ni2 N38 2.123(2) . ?
Ni3 O19 2.0508(12) . ?
Ni3 N51 2.0714(15) . ?
Ni3 N41 2.0724(15) . ?
Ni3 N48 2.0806(14) . ?
Ni3 O29 2.1162(12) . ?
Ni3 N58 2.164(2) . ?
N1 C2 1.339(2) . ?
N1 C6 1.355(2) . ?
C2 C3 1.387(3) . ?
C3 C4 1.390(3) . ?
C4 C5 1.384(3) . ?
C5 C6 1.397(2) . ?
C6 C7 1.455(2) . ?
C7 N8 1.294(2) . ?
N8 O9 1.332(2) . ?
N11 C12 1.335(2) . ?
N11 C16 1.360(2) . ?
C12 C13 1.393(2) . ?
C13 C14 1.388(3) . ?
C14 C15 1.390(3) . ?
C15 C16 1.398(2) . ?
C16 C17 1.458(2) . ?
C17 N18 1.297(2) . ?
N18 O19 1.332(2) . ?
N21 C22 1.341(2) . ?
N21 C26 1.353(2) . ?
C22 C23 1.390(3) . ?
C23 C24 1.381(3) . ?
C24 C25 1.391(3) . ?
C25 C26 1.389(2) . ?
C26 C27 1.469(2) . ?
C27 N28 1.280(2) . ?
N28 O29 1.373(2) . ?
N31 C32 1.344(2) . ?
N31 C36 1.352(2) . ?
C32 C33 1.389(3) . ?
C33 C34 1.380(3) . ?
C34 C35 1.396(3) . ?
C35 C36 1.394(2) . ?
C36 C37 1.460(3) . ?
C37 N38 1.292(2) . ?
N38 O39 1.359(2) . ?
N41 C42 1.337(2) . ?
N41 C46 1.351(2) . ?
C42 C43 1.388(3) . ?
C43 C44 1.387(3) . ?
C44 C45 1.387(3) . ?
C45 C46 1.397(2) . ?
C46 C47 1.466(2) . ?
C47 N48 1.283(2) . ?
N48 O49 1.370(2) . ?
N51 C52 1.340(2) . ?
N51 C56 1.355(2) . ?
C52 C53 1.391(3) . ?
C53 C54 1.386(3) . ?
C54 C55 1.386(3) . ?
C55 C56 1.395(2) . ?
C56 C57 1.453(3) . ?
C57 N58 1.302(2) . ?
N58 O59 1.341(2) . ?
N60 C61 1.137(3) . ?
C61 C62 1.448(3) . ?
Cl70 O71 1.439(2) . ?
Cl70 O73 1.441(2) . ?
Cl70 O72 1.443(2) . ?
Cl70 O74 1.4484(14) . ?

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
N18 Ni1 N8 175.24(6) . . ?
N18 Ni1 O49 92.28(5) . . ?
N8 Ni1 O49 92.43(5) . . ?
N18 Ni1 N11 78.70(6) . . ?
N8 Ni1 N11 101.54(6) . . ?
O49 Ni1 N11 95.35(5) . . ?
N18 Ni1 N1 96.88(6) . . ?
N8 Ni1 N1 78.43(6) . . ?
O49 Ni1 N1 170.70(5) . . ?
N11 Ni1 N1 84.90(5) . . ?
N18 Ni1 O29 90.35(5) . . ?
N8 Ni1 O29 89.42(5) . . ?
O49 Ni1 O29 84.44(4) . . ?
N11 Ni1 O29 169.04(5) . . ?
N1 Ni1 O29 97.08(5) . . ?
O9 Ni2 N28 85.88(5) . . ?
O9 Ni2 N31 87.74(6) . . ?
N28 Ni2 N31 173.10(6) . . ?
O9 Ni2 N21 89.46(5) . . ?
N28 Ni2 N21 78.62(6) . . ?
N31 Ni2 N21 103.98(6) . . ?
O9 Ni2 O49 93.56(5) . . ?
N28 Ni2 O49 84.70(5) . . ?
N31 Ni2 O49 93.08(5) . . ?
N21 Ni2 O49 162.79(5) . . ?
O9 Ni2 N38 165.69(5) . . ?
N28 Ni2 N38 108.32(6) . . ?
N31 Ni2 N38 78.15(6) . . ?
N21 Ni2 N38 91.63(6) . . ?
O49 Ni2 N38 89.61(5) . . ?
O19 Ni3 N51 85.80(5) . . ?
O19 Ni3 N41 93.02(5) . . ?
N51 Ni3 N41 95.42(6) . . ?
O19 Ni3 N48 88.16(5) . . ?
N51 Ni3 N48 170.91(6) . . ?
N41 Ni3 N48 78.10(6) . . ?
O19 Ni3 O29 90.38(5) . . ?
N51 Ni3 O29 102.87(5) . . ?
N41 Ni3 O29 161.59(5) . . ?
N48 Ni3 O29 83.94(5) . . ?
O19 Ni3 N58 161.46(5) . . ?
N51 Ni3 N58 76.69(6) . . ?
N41 Ni3 N58 94.61(6) . . ?
N48 Ni3 N58 109.94(6) . . ?
O29 Ni3 N58 87.69(5) . . ?
C2 N1 C6 118.2(2) . . ?
C2 N1 Ni1 129.04(12) . . ?
C6 N1 Ni1 112.01(11) . . ?
N1 C2 C3 122.9(2) . . ?
C2 C3 C4 118.8(2) . . ?
C5 C4 C3 119.1(2) . . ?
C4 C5 C6 118.8(2) . . ?
N1 C6 C5 122.1(2) . . ?
N1 C6 C7 115.69(15) . . ?
C5 C6 C7 122.2(2) . . ?
N8 C7 C6 116.3(2) . . ?
C7 N8 O9 118.70(14) . . ?
C7 N8 Ni1 117.25(12) . . ?
O9 N8 Ni1 123.63(11) . . ?
N8 O9 Ni2 110.08(10) . . ?
C12 N11 C16 118.89(15) . . ?
C12 N11 Ni1 129.09(12) . . ?
C16 N11 Ni1 110.87(11) . . ?
N11 C12 C13 122.6(2) . . ?
C14 C13 C12 118.8(2) . . ?
C13 C14 C15 119.2(2) . . ?
C14 C15 C16 118.9(2) . . ?
N11 C16 C15 121.6(2) . . ?
N11 C16 C17 115.54(15) . . ?
C15 C16 C17 122.9(2) . . ?
N18 C17 C16 115.77(15) . . ?
C17 N18 O19 119.70(14) . . ?
C17 N18 Ni1 116.72(12) . . ?
O19 N18 Ni1 123.52(10) . . ?
N18 O19 Ni3 110.66(9) . . ?
C22 N21 C26 118.1(2) . . ?
C22 N21 Ni2 128.84(13) . . ?
C26 N21 Ni2 113.03(11) . . ?
N21 C22 C23 123.1(2) . . ?
C24 C23 C22 118.6(2) . . ?
C23 C24 C25 119.1(2) . . ?
C26 C25 C24 119.1(2) . . ?
N21 C26 C25 122.0(2) . . ?
N21 C26 C27 115.64(15) . . ?
C25 C26 C27 122.3(2) . . ?
N28 C27 C26 116.5(2) . . ?
C27 N28 O29 118.01(14) . . ?
C27 N28 Ni2 115.50(11) . . ?
O29 N28 Ni2 125.12(10) . . ?
N28 O29 Ni3 107.80(9) . . ?
N28 O29 Ni1 103.66(9) . . ?
Ni3 O29 Ni1 100.70(5) . . ?
C32 N31 C36 118.9(2) . . ?
C32 N31 Ni2 126.09(13) . . ?
C36 N31 Ni2 114.09(12) . . ?
N31 C32 C33 122.3(2) . . ?
C34 C33 C32 119.1(2) . . ?
C33 C34 C35 119.2(2) . . ?
C36 C35 C34 118.7(2) . . ?
N31 C36 C35 121.8(2) . . ?
N31 C36 C37 115.7(2) . . ?
C35 C36 C37 122.5(2) . . ?
N38 C37 C36 117.4(2) . . ?
C37 N38 O39 114.65(15) . . ?
C37 N38 Ni2 113.98(12) . . ?
O39 N38 Ni2 131.33(11) . . ?
C42 N41 C46 118.6(2) . . ?
C42 N41 Ni3 127.26(12) . . ?
C46 N41 Ni3 114.11(12) . . ?
N41 C42 C43 122.8(2) . . ?
C44 C43 C42 118.6(2) . . ?
C43 C44 C45 119.5(2) . . ?
C44 C45 C46 118.5(2) . . ?
N41 C46 C45 122.1(2) . . ?
N41 C46 C47 115.29(15) . . ?
C45 C46 C47 122.6(2) . . ?
N48 C47 C46 116.4(2) . . ?
C47 N48 O49 117.65(14) . . ?
C47 N48 Ni3 115.81(12) . . ?
O49 N48 Ni3 125.83(10) . . ?
N48 O49 Ni1 104.17(9) . . ?
N48 O49 Ni2 107.84(9) . . ?
Ni1 O49 Ni2 100.60(5) . . ?
C52 N51 C56 118.6(2) . . ?
C52 N51 Ni3 126.04(12) . . ?
C56 N51 Ni3 115.33(12) . . ?
N51 C52 C53 122.8(2) . . ?
C54 C53 C52 118.3(2) . . ?
C53 C54 C55 119.5(2) . . ?
C54 C55 C56 118.9(2) . . ?
N51 C56 C55 121.5(2) . . ?
N51 C56 C57 115.2(2) . . ?
C55 C56 C57 123.2(2) . . ?
N58 C57 C56 117.3(2) . . ?
C57 N58 O59 114.3(2) . . ?
C57 N58 Ni3 113.15(12) . . ?
O59 N58 Ni3 131.94(12) . . ?
N60 C61 C62 178.0(2) . . ?
O71 Cl70 O73 109.19(11) . . ?
O71 Cl70 O72 109.33(10) . . ?
O73 Cl70 O72 109.70(10) . . ?
O71 Cl70 O74 109.69(10) . . ?
O73 Cl70 O74 109.24(9) . . ?
O72 Cl70 O74 109.68(9) . . ?

_refine_diff_density_max         1.405
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.074


#===END