# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/1763

###############################################################################
#
#   Exchange Coupling ia a Bis[heterodinuclear) [Cu(II)Ni(II)]2 and 
#   a Linear Heterotrinuclear Complex Co(III)Cu(II)Ni(II).
#   Synthesis, Structures, and Properties
#   
#   C. N. Verani, E. Rentschler, T. Weyhermuller, E. Bill, P. Chaudhuri
#
#   Max-Planck-Institut f. Strahlenchemie
#   Stiftstr. 34-36, D-45470 Muelheim, Germany
#
#   email: chaudh@mpi-muelheim.mpg.de
#
#
#   contains 2 crystal structures
#
#
###############################################################################



data_2
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      '[C42 H42 Cu2 N14 Ni2], 2 CH3OH' 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C44 H50 Cu2 N14 Ni2 O10' 
_chemical_formula_weight          1179.48 
_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' 
 'Ni'  'Ni'   0.3393   1.1124 
 '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    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                    8.726(1) 
_cell_length_b                    15.024(3) 
_cell_length_c                    17.649(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  100.18(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2277.3(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     8192 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        'non-transparent block' 
_exptl_crystal_colour             'almost black' 
_exptl_crystal_size_max           0.53
_exptl_crystal_size_mid           0.46 
_exptl_crystal_size_min           0.35 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.720 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1212 
_exptl_absorpt_coefficient_mu     1.812 
_exptl_absorpt_correction_type    'SADABS, G. Sheldrick 1994' 
_exptl_absorpt_correction_T_min   0.411
_exptl_absorpt_correction_T_max   0.634 
 
_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        'Siemens SMART CCD Detector'
_diffrn_measurement_method        '\w-scans, 0.3 deg./frame' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             24243 
_diffrn_reflns_av_R_equivalents   0.0204 
_diffrn_reflns_av_sigmaI/netI     0.0252 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -19 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          1.79 
_diffrn_reflns_theta_max          32.50 
_reflns_number_total              7860 
_reflns_number_observed           6836 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 191 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^)+(0.0308P)^2^+1.4429P] 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      SHELXL 
_refine_ls_extinction_coef        0.0049(2) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          7669 
_refine_ls_number_parameters      335 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0357 
_refine_ls_R_factor_obs           0.0275 
_refine_ls_wR_factor_all          0.0698 
_refine_ls_wR_factor_obs          0.0657 
_refine_ls_goodness_of_fit_all    1.034 
_refine_ls_goodness_of_fit_obs    1.057 
_refine_ls_restrained_S_all       1.044 
_refine_ls_restrained_S_obs       1.057 
_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 
Cu Cu 0.96181(2) 0.562988(10) 0.073320(9) 0.01089(4) Uani 1 d . . 
Ni Ni 1.24483(2) 0.452142(11) 0.149888(10) 0.01146(4) Uani 1 d . . 
O1 O 0.79354(12) 0.72329(7) 0.01872(7) 0.0186(2) Uani 1 d . . 
H1 H 0.7485(25) 0.6762(15) -0.0029(12) 0.028 Uiso 1 d . . 
O2 O 1.31525(11) 0.41953(6) 0.04058(5) 0.0133(2) Uani 1 d . . 
O3 O 1.01821(11) 0.43893(6) 0.09788(6) 0.0125(2) Uani 1 d . . 
O4 O 1.18278(11) 0.57846(6) 0.11530(5) 0.0122(2) Uani 1 d . . 
N1 N 0.93835(13) 0.68993(7) 0.05113(7) 0.0129(2) Uani 1 d . . 
N2 N 1.46219(13) 0.49006(8) 0.19392(6) 0.0141(2) Uani 1 d . . 
N3 N 1.25852(13) 0.32321(8) 0.17932(7) 0.0147(2) Uani 1 d . . 
N4 N 0.76117(13) 0.52556(7) 0.01659(6) 0.0118(2) Uani 1 d . . 
N5 N 1.16028(15) 0.49038(9) 0.25603(7) 0.0202(2) Uani 1 d . . 
N6 N 1.04125(14) 0.53061(9) 0.23827(7) 0.0173(2) Uani 1 d . . 
N7 N 0.9244(2) 0.56932(9) 0.21733(8) 0.0228(3) Uani 1 d . . 
C1 C 1.0442(2) 0.75015(9) 0.06510(8) 0.0137(2) Uani 1 d . . 
H1 H 1.0134(2) 0.80972(9) 0.05237(8) 0.016 Uiso 1 calc R . 
C2 C 1.20631(15) 0.73553(8) 0.09848(7) 0.0126(2) Uani 1 d . . 
C3 C 1.26974(15) 0.65130(9) 0.12297(7) 0.0119(2) Uani 1 d . . 
C4 C 1.4315(2) 0.64741(9) 0.15367(8) 0.0141(2) Uani 1 d . . 
C5 C 1.5233(2) 0.72451(10) 0.15406(8) 0.0173(3) Uani 1 d . . 
H5 H 1.6319(2) 0.72029(10) 0.17313(8) 0.021 Uiso 1 calc R . 
C6 C 1.4622(2) 0.80637(9) 0.12782(9) 0.0178(3) Uani 1 d . . 
C7 C 1.3029(2) 0.81082(9) 0.10209(8) 0.0160(2) Uani 1 d . . 
H7 H 1.2573(2) 0.86676(9) 0.08632(8) 0.019 Uiso 1 calc R . 
C8 C 1.5652(2) 0.88705(10) 0.12785(11) 0.0267(3) Uani 1 d . . 
H8A H 1.6571(8) 0.8712(3) 0.1059(8) 0.040 Uiso 1 calc R . 
H8B H 1.5980(14) 0.9081(6) 0.18079(14) 0.040 Uiso 1 calc R . 
H8C H 1.5072(6) 0.9343(3) 0.0969(7) 0.040 Uiso 1 calc R . 
C9 C 1.5154(2) 0.56895(9) 0.18762(8) 0.0152(2) Uani 1 d . . 
H9 H 1.6228(2) 0.57725(9) 0.20759(8) 0.018 Uiso 1 calc R . 
C10 C 1.5777(2) 0.42587(10) 0.23400(9) 0.0186(3) Uani 1 d . . 
H10A H 1.6514(2) 0.45791(10) 0.27384(9) 0.022 Uiso 1 calc R . 
H10B H 1.6379(2) 0.40083(10) 0.19645(9) 0.022 Uiso 1 calc R . 
C11 C 1.5040(2) 0.34995(10) 0.27186(8) 0.0185(3) Uani 1 d . . 
H11A H 1.4351(2) 0.37534(10) 0.30525(8) 0.022 Uiso 1 calc R . 
H11B H 1.5874(2) 0.31631(10) 0.30522(8) 0.022 Uiso 1 calc R . 
C12 C 1.4099(2) 0.28561(10) 0.21523(9) 0.0185(3) Uani 1 d . . 
H12A H 1.4703(2) 0.27037(10) 0.17453(9) 0.022 Uiso 1 calc R . 
H12B H 1.3922(2) 0.23002(10) 0.24256(9) 0.022 Uiso 1 calc R . 
C13 C 1.1416(2) 0.27035(9) 0.17172(8) 0.0162(2) Uani 1 d . . 
H13 H 1.1622(2) 0.21220(9) 0.19214(8) 0.019 Uiso 1 calc R . 
C14 C 0.9810(2) 0.28810(9) 0.13573(8) 0.0143(2) Uani 1 d . . 
C15 C 0.92378(15) 0.37002(8) 0.10146(7) 0.0119(2) Uani 1 d . . 
C16 C 0.76442(15) 0.37428(8) 0.06743(7) 0.0122(2) Uani 1 d . . 
C17 C 0.6693(2) 0.29850(9) 0.06609(8) 0.0151(2) Uani 1 d . . 
H17 H 0.5629(2) 0.30278(9) 0.04252(8) 0.018 Uiso 1 calc R . 
C18 C 0.7248(2) 0.21780(9) 0.09785(8) 0.0161(2) Uani 1 d . . 
C19 C 0.8805(2) 0.21446(9) 0.13276(8) 0.0169(2) Uani 1 d . . 
H19 H 0.9208(2) 0.16012(9) 0.15560(8) 0.020 Uiso 1 calc R . 
C20 C 0.6230(2) 0.13586(10) 0.09273(10) 0.0233(3) Uani 1 d . . 
H20A H 0.6065(13) 0.1192(5) 0.14438(13) 0.035 Uiso 1 calc R . 
H20B H 0.6741(7) 0.0867(3) 0.0704(7) 0.035 Uiso 1 calc R . 
H20C H 0.5224(6) 0.1485(3) 0.0601(6) 0.035 Uiso 1 calc R . 
C21 C 0.69412(15) 0.44999(9) 0.02326(8) 0.0126(2) Uani 1 d . . 
H21 H 0.58990(15) 0.44339(9) -0.00298(8) 0.015 Uiso 1 calc R . 
O30 O 1.3951(2) 0.51787(10) 0.38787(9) 0.0372(3) Uani 1 d . . 
H30 H 1.3329(33) 0.5160(19) 0.3489(17) 0.056 Uiso 1 d . . 
C30 C 1.3219(2) 0.55815(12) 0.44415(12) 0.0352(4) Uani 1 d . . 
H30A H 1.2184(8) 0.5320(8) 0.4422(6) 0.053 Uiso 1 calc R . 
H30B H 1.3116(17) 0.6222(2) 0.4342(6) 0.053 Uiso 1 calc R . 
H30C H 1.3847(10) 0.5482(9) 0.49523(15) 0.053 Uiso 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 
Cu 0.00832(7) 0.01065(7) 0.01306(8) 0.00109(5) 0.00012(5) -0.00037(5) 
Ni 0.00925(8) 0.01270(8) 0.01186(8) 0.00241(6) 0.00028(5) 0.00049(5) 
O1 0.0106(4) 0.0144(4) 0.0282(6) 0.0003(4) -0.0037(4) 0.0025(3) 
O2 0.0114(4) 0.0150(4) 0.0124(4) 0.0028(3) -0.0006(3) 0.0017(3) 
O3 0.0101(4) 0.0114(4) 0.0156(4) 0.0028(3) 0.0013(3) -0.0005(3) 
O4 0.0096(4) 0.0122(4) 0.0142(4) 0.0012(3) 0.0004(3) -0.0011(3) 
N1 0.0098(5) 0.0135(5) 0.0150(5) 0.0002(4) 0.0010(4) 0.0010(4) 
N2 0.0112(5) 0.0185(5) 0.0122(5) 0.0020(4) 0.0007(4) 0.0016(4) 
N3 0.0143(5) 0.0157(5) 0.0140(5) 0.0036(4) 0.0026(4) 0.0027(4) 
N4 0.0098(5) 0.0146(5) 0.0107(5) 0.0016(4) 0.0010(4) 0.0008(4) 
N5 0.0176(6) 0.0286(6) 0.0141(5) 0.0028(5) 0.0019(4) 0.0033(5) 
N6 0.0178(6) 0.0219(6) 0.0127(5) -0.0012(4) 0.0043(4) -0.0021(4) 
N7 0.0178(6) 0.0289(7) 0.0225(6) -0.0010(5) 0.0055(5) 0.0032(5) 
C1 0.0145(6) 0.0124(5) 0.0139(6) -0.0004(4) 0.0021(4) 0.0001(4) 
C2 0.0121(5) 0.0120(5) 0.0136(6) -0.0015(4) 0.0019(4) -0.0010(4) 
C3 0.0112(5) 0.0137(5) 0.0109(5) -0.0013(4) 0.0019(4) -0.0010(4) 
C4 0.0120(6) 0.0158(6) 0.0139(6) -0.0014(5) 0.0010(4) -0.0014(4) 
C5 0.0115(6) 0.0191(6) 0.0205(6) -0.0030(5) 0.0005(5) -0.0031(5) 
C6 0.0152(6) 0.0156(6) 0.0221(7) -0.0037(5) 0.0022(5) -0.0044(5) 
C7 0.0155(6) 0.0127(5) 0.0194(6) -0.0018(5) 0.0022(5) -0.0017(4) 
C8 0.0171(7) 0.0176(6) 0.0441(10) -0.0030(6) 0.0019(6) -0.0067(5) 
C9 0.0108(6) 0.0197(6) 0.0146(6) -0.0013(5) 0.0004(4) 0.0001(4) 
C10 0.0115(6) 0.0217(6) 0.0215(7) 0.0052(5) -0.0004(5) 0.0030(5) 
C11 0.0157(6) 0.0228(7) 0.0163(6) 0.0060(5) 0.0012(5) 0.0045(5) 
C12 0.0152(6) 0.0179(6) 0.0223(7) 0.0057(5) 0.0029(5) 0.0053(5) 
C13 0.0178(6) 0.0142(6) 0.0167(6) 0.0049(5) 0.0037(5) 0.0017(4) 
C14 0.0157(6) 0.0133(5) 0.0139(6) 0.0015(4) 0.0027(4) -0.0004(4) 
C15 0.0131(6) 0.0126(5) 0.0108(5) -0.0008(4) 0.0042(4) -0.0010(4) 
C16 0.0123(6) 0.0125(5) 0.0125(5) -0.0009(4) 0.0037(4) -0.0011(4) 
C17 0.0137(6) 0.0166(6) 0.0154(6) -0.0003(5) 0.0039(5) -0.0038(4) 
C18 0.0193(6) 0.0138(6) 0.0159(6) 0.0001(5) 0.0055(5) -0.0046(5) 
C19 0.0212(7) 0.0135(6) 0.0164(6) 0.0023(5) 0.0047(5) -0.0021(5) 
C20 0.0252(8) 0.0179(6) 0.0272(8) 0.0006(6) 0.0060(6) -0.0089(5) 
C21 0.0097(5) 0.0149(5) 0.0134(5) -0.0014(4) 0.0029(4) -0.0010(4) 
O30 0.0260(7) 0.0418(8) 0.0387(8) -0.0156(6) -0.0077(5) 0.0035(5) 
C30 0.0357(10) 0.0271(8) 0.0389(10) -0.0116(7) -0.0039(8) 0.0016(7) 
 
_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 
Cu N4 1.9402(12) . ? 
Cu N1 1.9504(12) . ? 
Cu O4 1.9534(10) . ? 
Cu O3 1.9566(10) . ? 
Ni N2 2.0012(12) . ? 
Ni N3 2.0036(12) . ? 
Ni O4 2.0373(10) . ? 
Ni O3 2.0374(11) . ? 
Ni O2 2.1814(11) . ? 
Ni N5 2.2072(13) . ? 
O1 N1 1.3856(15) . ? 
O2 N4 1.3803(14) 3_765 ? 
O3 C15 1.332(2) . ? 
O4 C3 1.325(2) . ? 
N1 C1 1.286(2) . ? 
N2 C9 1.285(2) . ? 
N2 C10 1.481(2) . ? 
N3 C13 1.281(2) . ? 
N3 C12 1.473(2) . ? 
N4 C21 1.292(2) . ? 
N4 O2 1.3803(14) 3_765 ? 
N5 N6 1.195(2) . ? 
N6 N7 1.175(2) . ? 
C1 C2 1.449(2) . ? 
C2 C7 1.405(2) . ? 
C2 C3 1.418(2) . ? 
C3 C4 1.421(2) . ? 
C4 C5 1.408(2) . ? 
C4 C9 1.459(2) . ? 
C5 C6 1.387(2) . ? 
C6 C7 1.386(2) . ? 
C6 C8 1.509(2) . ? 
C10 C11 1.521(2) . ? 
C11 C12 1.523(2) . ? 
C13 C14 1.457(2) . ? 
C14 C19 1.407(2) . ? 
C14 C15 1.422(2) . ? 
C15 C16 1.415(2) . ? 
C16 C17 1.407(2) . ? 
C16 C21 1.452(2) . ? 
C17 C18 1.387(2) . ? 
C18 C19 1.391(2) . ? 
C18 C20 1.511(2) . ? 
O30 C30 1.409(2) . ? 
 
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 
N4 Cu N1 97.28(5) . . ? 
N4 Cu O4 166.03(4) . . ? 
N1 Cu O4 91.22(4) . . ? 
N4 Cu O3 90.40(4) . . ? 
N1 Cu O3 171.60(4) . . ? 
O4 Cu O3 80.59(4) . . ? 
N2 Ni N3 99.53(5) . . ? 
N2 Ni O4 91.98(4) . . ? 
N3 Ni O4 168.18(4) . . ? 
N2 Ni O3 168.67(4) . . ? 
N3 Ni O3 91.79(4) . . ? 
O4 Ni O3 76.72(4) . . ? 
N2 Ni O2 90.67(5) . . ? 
N3 Ni O2 89.94(4) . . ? 
O4 Ni O2 92.62(4) . . ? 
O3 Ni O2 88.99(4) . . ? 
N2 Ni N5 91.85(5) . . ? 
N3 Ni N5 92.59(5) . . ? 
O4 Ni N5 84.31(4) . . ? 
O3 Ni N5 87.95(5) . . ? 
O2 Ni N5 176.09(4) . . ? 
N4 O2 Ni 109.68(7) 3_765 . ? 
C15 O3 Cu 128.14(8) . . ? 
C15 O3 Ni 127.87(8) . . ? 
Cu O3 Ni 101.14(4) . . ? 
C3 O4 Cu 130.25(8) . . ? 
C3 O4 Ni 128.44(8) . . ? 
Cu O4 Ni 101.25(4) . . ? 
C1 N1 O1 113.38(11) . . ? 
C1 N1 Cu 127.11(9) . . ? 
O1 N1 Cu 119.49(8) . . ? 
C9 N2 C10 114.60(12) . . ? 
C9 N2 Ni 124.12(9) . . ? 
C10 N2 Ni 121.22(9) . . ? 
C13 N3 C12 116.38(12) . . ? 
C13 N3 Ni 124.21(10) . . ? 
C12 N3 Ni 119.36(9) . . ? 
C21 N4 O2 115.07(11) . 3_765 ? 
C21 N4 Cu 126.12(9) . . ? 
O2 N4 Cu 118.64(8) 3_765 . ? 
N6 N5 Ni 108.33(10) . . ? 
N7 N6 N5 176.93(15) . . ? 
N1 C1 C2 126.01(12) . . ? 
C7 C2 C3 120.40(12) . . ? 
C7 C2 C1 115.51(12) . . ? 
C3 C2 C1 124.02(12) . . ? 
O4 C3 C2 121.36(11) . . ? 
O4 C3 C4 121.16(11) . . ? 
C2 C3 C4 117.45(12) . . ? 
C5 C4 C3 119.61(12) . . ? 
C5 C4 C9 114.78(12) . . ? 
C3 C4 C9 125.60(12) . . ? 
C6 C5 C4 122.90(13) . . ? 
C7 C6 C5 117.15(13) . . ? 
C7 C6 C8 121.61(13) . . ? 
C5 C6 C8 121.24(13) . . ? 
C6 C7 C2 122.33(13) . . ? 
N2 C9 C4 128.19(12) . . ? 
N2 C10 C11 113.17(11) . . ? 
C10 C11 C12 114.13(12) . . ? 
N3 C12 C11 112.20(12) . . ? 
N3 C13 C14 128.23(12) . . ? 
C19 C14 C15 119.67(12) . . ? 
C19 C14 C13 114.66(12) . . ? 
C15 C14 C13 125.60(12) . . ? 
O3 C15 C16 120.96(11) . . ? 
O3 C15 C14 121.28(12) . . ? 
C16 C15 C14 117.67(12) . . ? 
C17 C16 C15 120.21(12) . . ? 
C17 C16 C21 115.65(12) . . ? 
C15 C16 C21 123.60(12) . . ? 
C18 C17 C16 122.54(13) . . ? 
C17 C18 C19 117.06(12) . . ? 
C17 C18 C20 121.90(13) . . ? 
C19 C18 C20 121.01(13) . . ? 
C18 C19 C14 122.83(13) . . ? 
N4 C21 C16 125.60(12) . . ? 
 
_refine_diff_density_max    0.602 
_refine_diff_density_min   -0.500 
_refine_diff_density_rms    0.075 


#===END


data_3 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      
'[C30 H46 Co Cu N7 Ni O7]2+, 2 (ClO4)-, solv.'  
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C30.75 H52.5 Cl2 Co Cu N7 Ni O17.5' 
_chemical_formula_weight          1052.38 
_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' 
 'Co'  'Co'   0.3494   0.9721 
 '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' 
 'Cu'  'Cu'   0.3201   1.2651 
 '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                    7.4430(10) 
_cell_length_b                    14.281(2) 
_cell_length_c                    21.582(3) 
_cell_angle_alpha                 104.04(2) 
_cell_angle_beta                  96.90(2) 
_cell_angle_gamma                 104.31(2) 
_cell_volume                      2116.5(5) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     8192 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        'transparent block'
_exptl_crystal_colour             'dark red' 
_exptl_crystal_size_max           0.70 
_exptl_crystal_size_mid           0.25 
_exptl_crystal_size_min           0.14 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.651 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1088 
_exptl_absorpt_coefficient_mu     1.532 
_exptl_absorpt_correction_type    'SADABS, G.M. Sheldrick 1994' 
_exptl_absorpt_correction_T_min   0.622 
_exptl_absorpt_correction_T_max   0.850 
 
_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        'Siemens SMART CCD-Detector' 
_diffrn_measurement_method        '\w-scan, 0.3 deg./frame' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             14817 
_diffrn_reflns_av_R_equivalents   0.0349 
_diffrn_reflns_av_sigmaI/netI     0.0549 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -33 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          1.53 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              7050 
_reflns_number_observed           5591 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_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 345 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^)+(0.0652P)^2^+10.7954P] 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          6705 
_refine_ls_number_parameters      560 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0835 
_refine_ls_R_factor_obs           0.0623 
_refine_ls_wR_factor_all          0.1635 
_refine_ls_wR_factor_obs          0.1495 
_refine_ls_goodness_of_fit_all    1.076 
_refine_ls_goodness_of_fit_obs    1.125 
_refine_ls_restrained_S_all       1.086 
_refine_ls_restrained_S_obs       1.125 
_refine_ls_shift/esd_max          0.000 
_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 0.83950(11) 0.34599(6) 0.17276(3) 0.0249(2) Uani 1 d . . 
Cu1 Cu 0.71044(10) 0.18277(5) 0.24171(3) 0.0197(2) Uani 1 d . . 
Co1 Co 0.40885(11) 0.03688(6) 0.30316(4) 0.0202(2) Uani 1 d . . 
O1 O 0.3890(5) 0.1382(3) 0.2609(2) 0.0230(9) Uani 1 d . . 
O2 O 0.5371(6) -0.0236(3) 0.2420(2) 0.0265(9) Uani 1 d . . 
O3 O 0.7106(6) 0.1958(3) 0.1531(2) 0.0231(9) Uani 1 d . . 
O4 O 0.8501(6) 0.3254(3) 0.2620(2) 0.0266(9) Uani 1 d . . 
O5 O 0.6422(6) 0.1176(3) 0.3558(2) 0.0283(10) Uani 1 d . . 
O6 O 0.5849(7) 0.3839(4) 0.1802(2) 0.0507(14) Uani 1 d . . 
O7 O 1.0928(6) 0.3057(3) 0.1661(2) 0.0347(11) Uani 1 d . . 
N1 N 0.4257(7) -0.0673(4) 0.3489(2) 0.0280(12) Uani 1 d . . 
N2 N 0.1574(7) -0.0565(4) 0.2539(2) 0.0306(12) Uani 1 d . . 
N3 N 0.2705(8) 0.0890(4) 0.3710(2) 0.0314(12) Uani 1 d . . 
N4 N 0.6181(7) 0.0353(3) 0.2056(2) 0.0215(10) Uani 1 d . . 
N5 N 0.8032(7) 0.3375(4) 0.0781(2) 0.0294(12) Uani 1 d . . 
N6 N 0.9810(9) 0.4925(4) 0.2072(3) 0.0407(15) Uani 1 d . . 
N7 N 0.7429(7) 0.1932(4) 0.3344(2) 0.0237(11) Uani 1 d . . 
C1 C 0.2671(25) -0.1626(12) 0.3163(8) 0.037(5) Uiso 0.50 d P 1 
H1A H 0.3162(25) -0.2202(12) 0.3129(8) 0.044 Uiso 0.50 calc PR 1 
H1B H 0.1717(25) -0.1683(12) 0.3432(8) 0.044 Uiso 0.50 calc PR 1 
C2 C 0.1808(20) -0.1649(10) 0.2523(6) 0.032(3) Uiso 0.50 d P 1 
H2A H 0.0581(20) -0.2149(10) 0.2389(6) 0.038 Uiso 0.50 calc PR 1 
H2B H 0.2590(20) -0.1832(10) 0.2213(6) 0.038 Uiso 0.50 calc PR 1 
C3 C 0.0094(21) -0.0449(12) 0.2820(7) 0.039(3) Uiso 0.50 d P 1 
H3A H -0.0240(21) -0.0950(12) 0.3052(7) 0.047 Uiso 0.50 calc PR 1 
H3B H -0.0990(21) -0.0540(12) 0.2490(7) 0.047 Uiso 0.50 calc PR 1 
C4 C 0.0616(21) 0.0593(12) 0.3287(9) 0.041(4) Uiso 0.50 d P 1 
H4A H -0.0284(21) 0.0620(12) 0.3577(9) 0.049 Uiso 0.50 calc PR 1 
H4B H 0.0550(21) 0.1078(12) 0.3045(9) 0.049 Uiso 0.50 calc PR 1 
C5 C 0.2622(23) 0.0229(12) 0.4167(7) 0.043(4) Uiso 0.50 d P 1 
H5A H 0.2714(23) 0.0636(12) 0.4607(7) 0.051 Uiso 0.50 calc PR 1 
H5B H 0.1414(23) -0.0286(12) 0.4044(7) 0.051 Uiso 0.50 calc PR 1 
C6 C 0.4104(27) -0.0241(14) 0.4155(8) 0.041(5) Uiso 0.50 d P 1 
H6A H 0.3849(27) -0.0767(14) 0.4372(8) 0.050 Uiso 0.50 calc PR 1 
H6B H 0.5289(27) 0.0252(14) 0.4386(8) 0.050 Uiso 0.50 calc PR 1 
C1X C 0.3057(23) -0.1619(11) 0.3015(8) 0.030(4) Uiso 0.50 d P 2 
H1X1 H 0.2857(23) -0.2161(11) 0.3220(8) 0.036 Uiso 0.50 calc PR 2 
H1X2 H 0.3671(23) -0.1799(11) 0.2650(8) 0.036 Uiso 0.50 calc PR 2 
C2X C 0.1158(17) -0.1461(9) 0.2777(6) 0.022(2) Uiso 0.50 d P 2 
H2X1 H 0.0394(17) -0.2046(9) 0.2430(6) 0.027 Uiso 0.50 calc PR 2 
H2X2 H 0.0471(17) -0.1361(9) 0.3130(6) 0.027 Uiso 0.50 calc PR 2 
C3X C 0.0198(17) 0.0074(10) 0.2791(6) 0.023(3) Uiso 0.50 d P 2 
H3X1 H 0.0334(17) 0.0639(10) 0.2609(6) 0.028 Uiso 0.50 calc PR 2 
H3X2 H -0.1103(17) -0.0344(10) 0.2654(6) 0.028 Uiso 0.50 calc PR 2 
C4X C 0.0701(17) 0.0462(9) 0.3546(6) 0.023(3) Uiso 0.50 d P 2 
H4X1 H 0.0073(17) 0.0967(9) 0.3705(6) 0.027 Uiso 0.50 calc PR 2 
H4X2 H 0.0315(17) -0.0088(9) 0.3735(6) 0.027 Uiso 0.50 calc PR 2 
C5X C 0.3561(17) 0.0678(9) 0.4321(5) 0.018(2) Uiso 0.50 d P 2 
H5X1 H 0.2852(17) 0.0818(9) 0.4665(5) 0.022 Uiso 0.50 calc PR 2 
H5X2 H 0.4866(17) 0.1084(9) 0.4477(5) 0.022 Uiso 0.50 calc PR 2 
C6X C 0.3424(23) -0.0446(10) 0.4102(6) 0.023(3) Uiso 0.50 d P 2 
H6X1 H 0.4108(23) -0.0625(10) 0.4445(6) 0.027 Uiso 0.50 calc PR 2 
H6X2 H 0.2112(23) -0.0843(10) 0.4014(6) 0.027 Uiso 0.50 calc PR 2 
C7 C 0.6121(11) -0.0822(7) 0.3603(5) 0.062(3) Uani 1 d . . 
H7A H 0.6078(11) -0.1333(7) 0.3824(5) 0.092 Uiso 1 calc R . 
H7B H 0.7013(11) -0.0202(7) 0.3866(5) 0.092 Uiso 1 calc R . 
H7C H 0.6503(11) -0.1028(7) 0.3194(5) 0.092 Uiso 1 calc R . 
C8 C 0.1236(10) -0.0719(5) 0.1831(3) 0.039(2) Uani 1 d . . 
H8A H 0.0002(10) -0.1175(5) 0.1640(3) 0.059 Uiso 1 calc R . 
H8B H 0.2171(10) -0.0997(5) 0.1650(3) 0.059 Uiso 1 calc R . 
H8C H 0.1316(10) -0.0085(5) 0.1742(3) 0.059 Uiso 1 calc R . 
C9 C 0.3233(12) 0.2000(6) 0.3942(4) 0.053(2) Uani 1 d . . 
H9A H 0.2519(12) 0.2201(6) 0.4266(4) 0.079 Uiso 1 calc R . 
H9B H 0.2966(12) 0.2264(6) 0.3583(4) 0.079 Uiso 1 calc R . 
H9C H 0.4557(12) 0.2258(6) 0.4127(4) 0.079 Uiso 1 calc R . 
C10 C 0.6306(8) -0.0157(4) 0.1490(3) 0.0215(12) Uani 1 d . . 
H10 H 0.5925(8) -0.0855(4) 0.1397(3) 0.026 Uiso 1 calc R . 
C11 C 0.6986(8) 0.0262(4) 0.0985(3) 0.0221(12) Uani 1 d . . 
C12 C 0.7272(8) 0.1283(5) 0.1008(3) 0.0243(13) Uani 1 d . . 
C13 C 0.7662(9) 0.1567(5) 0.0438(3) 0.0278(14) Uani 1 d . . 
C14 C 0.7778(9) 0.0825(5) -0.0108(3) 0.0291(14) Uani 1 d . . 
H14 H 0.8032(9) 0.1018(5) -0.0478(3) 0.035 Uiso 1 calc R . 
C15 C 0.7539(8) -0.0166(5) -0.0128(3) 0.0267(14) Uani 1 d . . 
C16 C 0.7130(8) -0.0436(5) 0.0425(3) 0.0288(14) Uani 1 d . . 
H16 H 0.6944(8) -0.1105(5) 0.0425(3) 0.035 Uiso 1 calc R . 
C17 C 0.7644(10) -0.0955(5) -0.0728(3) 0.036(2) Uani 1 d . . 
H17A H 0.7438(10) -0.1596(5) -0.0640(3) 0.053 Uiso 1 calc R . 
H17B H 0.8868(10) -0.0765(5) -0.0838(3) 0.053 Uiso 1 calc R . 
H17C H 0.6692(10) -0.1001(5) -0.1085(3) 0.053 Uiso 1 calc R . 
C18 C 0.7863(9) 0.2559(5) 0.0346(3) 0.033(2) Uani 1 d . . 
H18 H 0.7869(9) 0.2604(5) -0.0077(3) 0.039 Uiso 1 calc R . 
C19 C 0.8174(11) 0.4303(5) 0.0584(3) 0.043(2) Uani 1 d . . 
H19A H 0.7062(11) 0.4523(5) 0.0653(3) 0.051 Uiso 1 calc R . 
H19B H 0.8205(11) 0.4162(5) 0.0123(3) 0.051 Uiso 1 calc R . 
C20 C 0.9916(13) 0.5140(6) 0.0961(4) 0.053(2) Uani 1 d . . 
H20A H 1.0994(13) 0.4872(6) 0.0960(4) 0.064 Uiso 1 calc R . 
H20B H 1.0129(13) 0.5657(6) 0.0736(4) 0.064 Uiso 1 calc R . 
C21 C 0.9836(15) 0.5622(6) 0.1652(4) 0.062(3) Uani 1 d . . 
H21A H 1.0924(15) 0.6209(6) 0.1833(4) 0.075 Uiso 1 calc R . 
H21B H 0.8712(15) 0.5849(6) 0.1659(4) 0.075 Uiso 1 calc R . 
C22 C 1.0738(12) 0.5308(5) 0.2652(4) 0.047(2) Uani 1 d . . 
H22 H 1.1481(12) 0.5972(5) 0.2751(4) 0.056 Uiso 1 calc R . 
C23 C 1.0790(9) 0.4843(5) 0.3180(3) 0.0316(15) Uani 1 d . . 
C24 C 0.9671(8) 0.3871(4) 0.3167(3) 0.0240(13) Uani 1 d . . 
C25 C 0.9795(8) 0.3581(4) 0.3745(3) 0.0227(13) Uani 1 d . . 
C26 C 1.1021(8) 0.4234(5) 0.4314(3) 0.0258(13) Uani 1 d . . 
H26 H 1.1067(8) 0.4031(5) 0.4693(3) 0.031 Uiso 1 calc R . 
C27 C 1.2164(9) 0.5168(5) 0.4332(3) 0.0307(15) Uani 1 d . . 
C28 C 1.2003(10) 0.5455(5) 0.3767(3) 0.036(2) Uani 1 d . . 
H28 H 1.2735(10) 0.6090(5) 0.3774(3) 0.043 Uiso 1 calc R . 
C29 C 1.3488(10) 0.5870(5) 0.4944(3) 0.040(2) Uani 1 d . . 
H29A H 1.3422(10) 0.5550(5) 0.5288(3) 0.061 Uiso 1 calc R . 
H29B H 1.3126(10) 0.6479(5) 0.5068(3) 0.061 Uiso 1 calc R . 
H29C H 1.4756(10) 0.6027(5) 0.4867(3) 0.061 Uiso 1 calc R . 
C30 C 0.8598(8) 0.2656(4) 0.3812(3) 0.0230(13) Uani 1 d . . 
H30 H 0.8674(8) 0.2575(4) 0.4228(3) 0.028 Uiso 1 calc R . 
O11 O 0.5053(10) 0.5862(4) 0.1020(4) 0.087(2) Uani 1 d . . 
O12 O 0.3933(10) 0.7276(4) 0.1132(4) 0.081(2) Uani 1 d . . 
O13 O 0.6853(8) 0.7405(4) 0.1742(3) 0.067(2) Uani 1 d . . 
Cl1 Cl 0.5629(4) 0.6895(2) 0.11463(14) 0.0492(7) Uani 0.75 d P . 
O10 O 0.6703(21) 0.7192(9) 0.0685(5) 0.131(5) Uani 0.75 d P . 
Cl1X Cl 0.4947(13) 0.6794(7) 0.1457(5) 0.057(2) Uiso 0.25 d P . 
O10X O 0.4225(51) 0.6462(26) 0.2009(17) 0.107(11) Uiso 0.25 d P . 
Cl2 Cl 0.9190(4) 0.7537(2) 0.43016(10) 0.0611(6) Uani 1 d . . 
O20 O 0.9272(14) 0.8564(7) 0.4514(6) 0.143(4) Uani 1 d . . 
O21 O 1.1070(14) 0.7547(7) 0.4590(4) 0.110(3) Uani 1 d . . 
O22 O 0.9072(12) 0.7359(8) 0.3635(3) 0.135(4) Uani 1 d . . 
O23 O 0.7825(18) 0.6959(9) 0.4479(5) 0.173(5) Uani 1 d . . 
O40 O 0.3112(8) 0.3603(6) 0.0718(3) 0.073(2) Uani 1 d . . 
O50 O 0.3767(9) 0.3239(4) 0.2664(2) 0.0326(14) Uani 0.75 d P . 
O51 O 0.4815(21) 0.3989(11) 0.3255(7) 0.020(3) Uiso 0.25 d P . 
C51 C 0.6250(31) 0.4866(16) 0.3602(10) 0.019(5) Uiso 0.25 d P . 
O60 O 0.6236(17) 0.5885(7) 0.2525(5) 0.051(3) Uani 0.50 d P . 
C60 C 0.5478(36) 0.6488(18) 0.2865(14) 0.100(8) Uani 0.50 d P . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Ni1 0.0291(4) 0.0237(4) 0.0196(4) 0.0074(3) 0.0062(3) 0.0019(3) 
Cu1 0.0217(4) 0.0202(4) 0.0145(3) 0.0042(3) 0.0034(3) 0.0020(3) 
Co1 0.0187(4) 0.0235(4) 0.0177(4) 0.0090(3) 0.0031(3) 0.0019(3) 
O1 0.022(2) 0.023(2) 0.022(2) 0.009(2) 0.003(2) 0.002(2) 
O2 0.036(2) 0.021(2) 0.027(2) 0.012(2) 0.016(2) 0.007(2) 
O3 0.027(2) 0.022(2) 0.016(2) 0.004(2) 0.004(2) 0.000(2) 
O4 0.033(2) 0.024(2) 0.017(2) 0.002(2) 0.003(2) 0.001(2) 
O5 0.025(2) 0.032(2) 0.023(2) 0.015(2) 0.001(2) -0.006(2) 
O6 0.044(3) 0.080(4) 0.038(3) 0.027(3) 0.014(2) 0.024(3) 
O7 0.030(2) 0.039(3) 0.033(2) 0.010(2) 0.011(2) 0.005(2) 
N1 0.023(3) 0.034(3) 0.027(3) 0.016(2) 0.003(2) 0.002(2) 
N2 0.020(3) 0.039(3) 0.030(3) 0.019(2) 0.001(2) -0.004(2) 
N3 0.035(3) 0.036(3) 0.026(3) 0.012(2) 0.015(2) 0.010(2) 
N4 0.023(3) 0.023(3) 0.020(2) 0.011(2) 0.007(2) 0.004(2) 
N5 0.032(3) 0.033(3) 0.023(3) 0.014(2) 0.006(2) 0.003(2) 
N6 0.061(4) 0.027(3) 0.034(3) 0.012(3) 0.013(3) 0.008(3) 
N7 0.020(3) 0.028(3) 0.021(2) 0.010(2) 0.005(2) 0.000(2) 
C7 0.035(4) 0.086(6) 0.096(7) 0.073(6) 0.021(4) 0.026(4) 
C8 0.040(4) 0.040(4) 0.025(3) 0.005(3) 0.000(3) -0.005(3) 
C9 0.063(5) 0.042(4) 0.035(4) -0.012(3) 0.025(4) -0.003(4) 
C10 0.022(3) 0.018(3) 0.024(3) 0.005(2) 0.003(2) 0.006(2) 
C11 0.019(3) 0.028(3) 0.016(3) 0.003(2) 0.002(2) 0.005(2) 
C12 0.016(3) 0.031(3) 0.019(3) 0.005(3) -0.001(2) -0.002(2) 
C13 0.026(3) 0.038(4) 0.014(3) 0.007(3) 0.002(2) 0.001(3) 
C14 0.028(3) 0.043(4) 0.015(3) 0.011(3) 0.004(2) 0.004(3) 
C15 0.022(3) 0.040(4) 0.015(3) 0.002(3) 0.002(2) 0.008(3) 
C16 0.021(3) 0.035(4) 0.023(3) 0.004(3) 0.001(2) 0.002(3) 
C17 0.033(4) 0.050(4) 0.017(3) -0.001(3) 0.001(3) 0.013(3) 
C18 0.037(4) 0.036(4) 0.021(3) 0.010(3) 0.009(3) 0.001(3) 
C19 0.057(5) 0.041(4) 0.037(4) 0.023(3) 0.016(3) 0.009(4) 
C20 0.071(6) 0.039(4) 0.044(4) 0.025(4) 0.006(4) -0.007(4) 
C21 0.100(7) 0.031(4) 0.050(5) 0.016(4) 0.007(5) 0.007(4) 
C22 0.069(5) 0.022(3) 0.038(4) 0.007(3) 0.004(4) -0.004(3) 
C23 0.037(4) 0.021(3) 0.031(3) 0.001(3) 0.007(3) 0.003(3) 
C24 0.020(3) 0.026(3) 0.022(3) -0.002(3) 0.005(2) 0.007(2) 
C25 0.020(3) 0.027(3) 0.020(3) 0.003(3) 0.004(2) 0.009(2) 
C26 0.022(3) 0.029(3) 0.023(3) -0.001(3) 0.003(2) 0.008(3) 
C27 0.028(3) 0.029(3) 0.029(3) -0.005(3) 0.004(3) 0.010(3) 
C28 0.039(4) 0.021(3) 0.039(4) 0.003(3) 0.006(3) -0.001(3) 
C29 0.035(4) 0.031(4) 0.040(4) -0.008(3) -0.002(3) 0.004(3) 
C30 0.022(3) 0.031(3) 0.015(3) 0.004(3) 0.007(2) 0.007(3) 
O11 0.076(5) 0.029(3) 0.131(6) 0.011(4) -0.016(4) 0.001(3) 
O12 0.077(5) 0.044(3) 0.101(5) 0.013(3) -0.047(4) 0.016(3) 
O13 0.050(4) 0.052(4) 0.076(4) 0.009(3) -0.022(3) -0.001(3) 
Cl1 0.058(2) 0.0263(12) 0.051(2) 0.0160(11) -0.0193(13) -0.0018(11) 
O10 0.197(14) 0.095(8) 0.059(6) 0.024(6) 0.005(7) -0.025(8) 
Cl2 0.091(2) 0.0747(15) 0.0588(12) 0.0521(12) 0.0489(12) 0.0491(13) 
O20 0.109(7) 0.089(6) 0.267(14) 0.066(8) 0.078(8) 0.058(6) 
O21 0.143(8) 0.123(7) 0.078(5) 0.016(5) -0.007(5) 0.087(6) 
O22 0.103(6) 0.211(10) 0.048(4) 0.065(5) 0.010(4) -0.054(6) 
O23 0.204(12) 0.174(10) 0.132(8) 0.081(8) 0.095(8) -0.030(9) 
O40 0.050(4) 0.131(6) 0.053(4) 0.039(4) 0.022(3) 0.038(4) 
O50 0.057(4) 0.022(3) 0.018(3) 0.006(2) -0.003(3) 0.015(3) 
O60 0.084(8) 0.024(5) 0.040(6) 0.002(5) 0.014(6) 0.013(5) 
C60 0.088(17) 0.069(15) 0.130(22) 0.028(15) 0.025(16) -0.002(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 
Ni1 N5 1.997(5) . ? 
Ni1 N6 2.002(6) . ? 
Ni1 O4 2.012(4) . ? 
Ni1 O3 2.035(4) . ? 
Ni1 O6 2.109(5) . ? 
Ni1 O7 2.113(5) . ? 
Cu1 N7 1.951(5) . ? 
Cu1 O4 1.958(4) . ? 
Cu1 O3 1.967(4) . ? 
Cu1 N4 1.969(5) . ? 
Cu1 O1 2.432(4) . ? 
Co1 O5 1.880(4) . ? 
Co1 O2 1.886(4) . ? 
Co1 O1 1.913(4) . ? 
Co1 N3 1.992(5) . ? 
Co1 N1 1.994(5) . ? 
Co1 N2 2.003(5) . ? 
O2 N4 1.367(6) . ? 
O3 C12 1.335(7) . ? 
O4 C24 1.341(7) . ? 
O5 N7 1.366(6) . ? 
N1 C6 1.45(2) . ? 
N1 C7 1.457(9) . ? 
N1 C1X 1.48(2) . ? 
N1 C1 1.51(2) . ? 
N1 C6X 1.527(14) . ? 
N2 C3 1.35(2) . ? 
N2 C8 1.470(8) . ? 
N2 C2X 1.471(12) . ? 
N2 C3X 1.591(14) . ? 
N2 C2 1.594(14) . ? 
N3 C4X 1.429(13) . ? 
N3 C9 1.476(9) . ? 
N3 C5 1.52(2) . ? 
N3 C5X 1.525(12) . ? 
N3 C4 1.60(2) . ? 
N4 C10 1.288(7) . ? 
N5 C18 1.274(8) . ? 
N5 C19 1.472(8) . ? 
N6 C22 1.273(9) . ? 
N6 C21 1.497(9) . ? 
N7 C30 1.297(7) . ? 
C1 C2 1.44(2) . ? 
C3 C4 1.51(2) . ? 
C5 C6 1.43(2) . ? 
C1X C2X 1.53(2) . ? 
C3X C4X 1.55(2) . ? 
C5X C6X 1.53(2) . ? 
C10 C11 1.449(8) . ? 
C11 C16 1.402(8) . ? 
C11 C12 1.408(8) . ? 
C12 C13 1.425(8) . ? 
C13 C14 1.409(9) . ? 
C13 C18 1.451(9) . ? 
C14 C15 1.370(9) . ? 
C15 C16 1.385(8) . ? 
C15 C17 1.521(8) . ? 
C19 C20 1.510(10) . ? 
C20 C21 1.499(11) . ? 
C22 C23 1.452(10) . ? 
C23 C28 1.408(9) . ? 
C23 C24 1.422(8) . ? 
C24 C25 1.407(8) . ? 
C25 C26 1.401(8) . ? 
C25 C30 1.449(8) . ? 
C26 C27 1.382(9) . ? 
C27 C28 1.379(9) . ? 
C27 C29 1.510(9) . ? 
O11 Cl1 1.378(6) . ? 
O11 Cl1X 1.459(11) . ? 
O12 Cl1X 1.377(11) . ? 
O12 Cl1 1.493(7) . ? 
O13 Cl1 1.397(6) . ? 
O13 Cl1X 1.439(11) . ? 
Cl1 Cl1X 0.906(10) . ? 
Cl1 O10 1.427(12) . ? 
Cl1X O10X 1.49(4) . ? 
Cl2 O23 1.302(8) . ? 
Cl2 O22 1.387(7) . ? 
Cl2 O20 1.410(9) . ? 
Cl2 O21 1.457(9) . ? 
O50 O51 1.44(2) . ? 
O51 C51 1.40(3) . ? 
O60 C60 1.28(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 
N5 Ni1 N6 97.8(2) . . ? 
N5 Ni1 O4 168.8(2) . . ? 
N6 Ni1 O4 93.4(2) . . ? 
N5 Ni1 O3 91.5(2) . . ? 
N6 Ni1 O3 170.4(2) . . ? 
O4 Ni1 O3 77.2(2) . . ? 
N5 Ni1 O6 91.3(2) . . ? 
N6 Ni1 O6 89.1(2) . . ? 
O4 Ni1 O6 89.3(2) . . ? 
O3 Ni1 O6 93.0(2) . . ? 
N5 Ni1 O7 89.5(2) . . ? 
N6 Ni1 O7 91.7(2) . . ? 
O4 Ni1 O7 89.8(2) . . ? 
O3 Ni1 O7 86.1(2) . . ? 
O6 Ni1 O7 178.9(2) . . ? 
N7 Cu1 O4 90.0(2) . . ? 
N7 Cu1 O3 169.9(2) . . ? 
O4 Cu1 O3 80.1(2) . . ? 
N7 Cu1 N4 99.7(2) . . ? 
O4 Cu1 N4 164.7(2) . . ? 
O3 Cu1 N4 89.6(2) . . ? 
N7 Cu1 O1 76.1(2) . . ? 
O4 Cu1 O1 118.9(2) . . ? 
O3 Cu1 O1 110.41(15) . . ? 
N4 Cu1 O1 75.3(2) . . ? 
O5 Co1 O2 89.8(2) . . ? 
O5 Co1 O1 92.2(2) . . ? 
O2 Co1 O1 93.2(2) . . ? 
O5 Co1 N3 91.1(2) . . ? 
O2 Co1 N3 174.4(2) . . ? 
O1 Co1 N3 92.2(2) . . ? 
O5 Co1 N1 87.9(2) . . ? 
O2 Co1 N1 88.2(2) . . ? 
O1 Co1 N1 178.5(2) . . ? 
N3 Co1 N1 86.3(2) . . ? 
O5 Co1 N2 174.3(2) . . ? 
O2 Co1 N2 92.1(2) . . ? 
O1 Co1 N2 93.1(2) . . ? 
N3 Co1 N2 86.5(2) . . ? 
N1 Co1 N2 86.8(2) . . ? 
Co1 O1 Cu1 98.1(2) . . ? 
N4 O2 Co1 115.4(3) . . ? 
C12 O3 Cu1 127.7(4) . . ? 
C12 O3 Ni1 122.4(3) . . ? 
Cu1 O3 Ni1 100.6(2) . . ? 
C24 O4 Cu1 129.8(4) . . ? 
C24 O4 Ni1 126.1(4) . . ? 
Cu1 O4 Ni1 101.8(2) . . ? 
N7 O5 Co1 117.1(3) . . ? 
C6 N1 C7 99.6(9) . . ? 
C7 N1 C1X 105.2(8) . . ? 
C6 N1 C1 111.4(11) . . ? 
C7 N1 C1 114.7(9) . . ? 
C7 N1 C6X 113.9(7) . . ? 
C1X N1 C6X 110.6(10) . . ? 
C6 N1 Co1 105.8(7) . . ? 
C7 N1 Co1 114.9(4) . . ? 
C1X N1 Co1 103.4(7) . . ? 
C1 N1 Co1 109.7(7) . . ? 
C6X N1 Co1 108.4(6) . . ? 
C3 N2 C8 114.7(8) . . ? 
C8 N2 C2X 117.9(7) . . ? 
C8 N2 C3X 104.3(6) . . ? 
C2X N2 C3X 107.0(8) . . ? 
C3 N2 C2 108.6(9) . . ? 
C8 N2 C2 96.9(6) . . ? 
C3 N2 Co1 115.1(7) . . ? 
C8 N2 Co1 115.7(4) . . ? 
C2X N2 Co1 109.0(5) . . ? 
C3X N2 Co1 101.0(5) . . ? 
C2 N2 Co1 103.0(5) . . ? 
C4X N3 C9 111.4(7) . . ? 
C9 N3 C5 122.9(8) . . ? 
C4X N3 C5X 111.9(8) . . ? 
C9 N3 C5X 99.2(6) . . ? 
C9 N3 C4 103.4(7) . . ? 
C5 N3 C4 106.7(10) . . ? 
C4X N3 Co1 114.5(6) . . ? 
C9 N3 Co1 113.7(4) . . ? 
C5 N3 Co1 106.7(7) . . ? 
C5X N3 Co1 104.8(5) . . ? 
C4 N3 Co1 101.0(6) . . ? 
C10 N4 O2 113.4(4) . . ? 
C10 N4 Cu1 126.0(4) . . ? 
O2 N4 Cu1 120.5(3) . . ? 
C18 N5 C19 118.6(5) . . ? 
C18 N5 Ni1 121.9(4) . . ? 
C19 N5 Ni1 119.1(4) . . ? 
C22 N6 C21 116.8(6) . . ? 
C22 N6 Ni1 121.9(5) . . ? 
C21 N6 Ni1 121.2(5) . . ? 
C30 N7 O5 112.9(4) . . ? 
C30 N7 Cu1 126.7(4) . . ? 
O5 N7 Cu1 120.3(3) . . ? 
C2 C1 N1 112.6(12) . . ? 
C1 C2 N2 109.1(11) . . ? 
N2 C3 C4 109.1(12) . . ? 
C3 C4 N3 111.2(11) . . ? 
C6 C5 N3 111.9(12) . . ? 
C5 C6 N1 110.3(13) . . ? 
N1 C1X C2X 108.5(11) . . ? 
N2 C2X C1X 107.2(10) . . ? 
C4X C3X N2 109.1(9) . . ? 
N3 C4X C3X 106.1(9) . . ? 
N3 C5X C6X 104.1(9) . . ? 
N1 C6X C5X 109.7(9) . . ? 
N4 C10 C11 125.8(5) . . ? 
C16 C11 C12 120.7(5) . . ? 
C16 C11 C10 115.7(5) . . ? 
C12 C11 C10 123.1(5) . . ? 
O3 C12 C11 121.7(5) . . ? 
O3 C12 C13 120.7(5) . . ? 
C11 C12 C13 117.5(5) . . ? 
C14 C13 C12 118.7(6) . . ? 
C14 C13 C18 115.2(5) . . ? 
C12 C13 C18 126.0(6) . . ? 
C15 C14 C13 123.9(5) . . ? 
C14 C15 C16 116.8(6) . . ? 
C14 C15 C17 122.8(6) . . ? 
C16 C15 C17 120.4(6) . . ? 
C15 C16 C11 122.3(6) . . ? 
N5 C18 C13 127.1(6) . . ? 
N5 C19 C20 112.1(6) . . ? 
C21 C20 C19 115.1(7) . . ? 
N6 C21 C20 113.0(6) . . ? 
N6 C22 C23 128.4(6) . . ? 
C28 C23 C24 118.3(6) . . ? 
C28 C23 C22 115.1(6) . . ? 
C24 C23 C22 126.5(6) . . ? 
O4 C24 C25 120.8(5) . . ? 
O4 C24 C23 120.8(5) . . ? 
C25 C24 C23 118.4(5) . . ? 
C26 C25 C24 120.2(5) . . ? 
C26 C25 C30 115.9(5) . . ? 
C24 C25 C30 123.6(5) . . ? 
C27 C26 C25 122.3(6) . . ? 
C28 C27 C26 117.1(6) . . ? 
C28 C27 C29 120.6(6) . . ? 
C26 C27 C29 122.3(6) . . ? 
C27 C28 C23 123.7(6) . . ? 
N7 C30 C25 126.0(5) . . ? 
Cl1 O11 Cl1X 37.1(4) . . ? 
Cl1X O12 Cl1 36.5(4) . . ? 
Cl1 O13 Cl1X 37.2(4) . . ? 
Cl1X Cl1 O11 76.3(7) . . ? 
Cl1X Cl1 O13 73.9(7) . . ? 
O11 Cl1 O13 114.6(4) . . ? 
Cl1X Cl1 O10 172.3(9) . . ? 
O11 Cl1 O10 111.2(7) . . ? 
O13 Cl1 O10 103.1(6) . . ? 
Cl1X Cl1 O12 64.8(7) . . ? 
O11 Cl1 O12 109.1(4) . . ? 
O13 Cl1 O12 108.3(4) . . ? 
O10 Cl1 O12 110.3(7) . . ? 
Cl1 Cl1X O12 78.7(8) . . ? 
Cl1 Cl1X O13 68.8(7) . . ? 
O12 Cl1X O13 112.5(8) . . ? 
Cl1 Cl1X O11 66.6(7) . . ? 
O12 Cl1X O11 111.1(8) . . ? 
O13 Cl1X O11 107.4(7) . . ? 
Cl1 Cl1X O10X 163.2(17) . . ? 
O12 Cl1X O10X 118.1(16) . . ? 
O13 Cl1X O10X 103.6(15) . . ? 
O11 Cl1X O10X 103.2(15) . . ? 
O23 Cl2 O22 115.3(6) . . ? 
O23 Cl2 O20 112.7(7) . . ? 
O22 Cl2 O20 103.2(7) . . ? 
O23 Cl2 O21 114.0(8) . . ? 
O22 Cl2 O21 108.5(6) . . ? 
O20 Cl2 O21 101.8(6) . . ? 
C51 O51 O50 152.6(15) . . ? 
 
_refine_diff_density_max    1.244 
_refine_diff_density_min   -0.768 
_refine_diff_density_rms    0.115 

#===END