# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


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#
#                 Cambridge Crystallographic Data Centre
#                                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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#  except for the purpose of generating routine backup copies 
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data_Co
_database_code_depnum_ccdc_archive 'CCDC 916432'
#TrackingRef 'web_deposit_cif_file_0_Xiao-ZengLi_1355888311.Co.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H28 Co N4 Ni O10'
_chemical_formula_weight         698.18
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'
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   P21/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                   16.091(12)
_cell_length_b                   8.987(6)
_cell_length_c                   24.710(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.62(3)
_cell_angle_gamma                90.00
_cell_volume                     2792(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6901
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      29.99
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1436
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7487
_exptl_absorpt_correction_T_max  0.8248
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11500
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_av_sigmaI/netI    0.0993
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4912
_reflns_number_gt                3568
_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, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.1160P)^2^+1.0193P] 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         4912
_refine_ls_number_parameters     401
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1763
_refine_ls_wR_factor_gt          0.1686
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.081
_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
Ni1 Ni 0.19284(4) 0.44888(6) 0.88790(2) 0.0290(2) Uani 1 1 d . . .
Co1 Co 0.24774(5) 0.52892(8) 0.70514(3) 0.0359(2) Uani 1 1 d . . .
O1 O 0.2071(2) 0.3438(4) 0.74175(14) 0.0384(8) Uani 1 1 d . . .
O2 O 0.3243(2) 0.5881(4) 0.80915(14) 0.0388(8) Uani 1 1 d . . .
O3 O 0.2576(3) 0.8949(5) 1.03992(19) 0.0567(10) Uani 1 1 d . . .
O4 O 0.2941(3) 0.6728(5) 1.09206(17) 0.0598(11) Uani 1 1 d . . .
O5 O 0.0177(3) 0.0929(4) 0.93426(15) 0.0435(8) Uani 1 1 d . . .
O6 O -0.1096(2) 0.1164(4) 0.81846(14) 0.0368(7) Uani 1 1 d . . .
O7 O 0.3038(3) 0.7298(5) 0.69721(18) 0.0683(11) Uani 1 1 d DU . .
H7' H 0.3142 0.7377 0.6676 0.103 Uiso 1 1 d R . .
O8 O 0.3710(4) 0.4039(6) 0.7228(2) 0.0813(14) Uani 1 1 d DU . .
H8' H 0.3910 0.4191 0.6986 0.122 Uiso 1 1 d R . .
O9 O 0.1685(3) 0.4921(4) 0.59942(16) 0.0440(8) Uani 1 1 d . . .
H9A H 0.1051 0.5214 0.5793 0.066 Uiso 1 1 d R . .
H9B H 0.1973 0.5183 0.5815 0.066 Uiso 1 1 d R . .
N1 N 0.1880(3) 0.3134(4) 0.82805(16) 0.0304(8) Uani 1 1 d . . .
N2 N 0.2969(3) 0.5491(4) 0.89071(17) 0.0299(8) Uani 1 1 d . . .
N3 N 0.1925(3) 0.5916(4) 0.94377(17) 0.0316(8) Uani 1 1 d . . .
N4 N 0.0865(3) 0.3494(4) 0.88429(17) 0.0324(9) Uani 1 1 d . . .
C1 C 0.2192(3) 0.3812(5) 0.7949(2) 0.0316(10) Uani 1 1 d . . .
C2 C 0.2850(3) 0.5213(5) 0.8334(2) 0.0311(10) Uani 1 1 d . . .
C3 C 0.3747(3) 0.6488(5) 0.9431(2) 0.0334(10) Uani 1 1 d . . .
C4 C 0.3643(3) 0.7031(5) 0.9926(2) 0.0333(10) Uani 1 1 d . . .
C5 C 0.4473(4) 0.7914(6) 1.0472(2) 0.0461(12) Uani 1 1 d . . .
H5 H 0.4420 0.8272 1.0803 0.055 Uiso 1 1 calc R . .
C6 C 0.5362(4) 0.8263(7) 1.0532(2) 0.0534(14) Uani 1 1 d . . .
H6 H 0.5890 0.8868 1.0891 0.064 Uiso 1 1 calc R . .
C7 C 0.5460(4) 0.7707(7) 1.0055(3) 0.0564(15) Uani 1 1 d . . .
H7 H 0.6065 0.7924 1.0100 0.068 Uiso 1 1 calc R . .
C8 C 0.4672(4) 0.6829(6) 0.9511(2) 0.0459(12) Uani 1 1 d . . .
H8 H 0.4753 0.6461 0.9194 0.055 Uiso 1 1 calc R . .
C9 C 0.2708(3) 0.6794(5) 0.9888(2) 0.0331(10) Uani 1 1 d . . .
C10 C 0.2742(4) 0.7562(7) 1.0458(2) 0.0444(12) Uani 1 1 d . . .
C11 C 0.0959(3) 0.5816(5) 0.9351(2) 0.0338(10) Uani 1 1 d . . .
C12 C 0.0388(3) 0.4483(5) 0.9040(2) 0.0315(10) Uani 1 1 d . . .
C13 C -0.0594(4) 0.4319(6) 0.8901(2) 0.0400(11) Uani 1 1 d . . .
H13 H -0.0989 0.3456 0.8686 0.048 Uiso 1 1 calc R . .
C14 C -0.0980(4) 0.5407(6) 0.9076(3) 0.0444(12) Uani 1 1 d . . .
H14 H -0.1617 0.5259 0.9001 0.053 Uiso 1 1 calc R . .
C15 C -0.0436(4) 0.6715(6) 0.9362(2) 0.0436(12) Uani 1 1 d . . .
H15 H -0.0708 0.7452 0.9477 0.052 Uiso 1 1 calc R . .
C16 C 0.0524(4) 0.6947(6) 0.9483(2) 0.0385(11) Uani 1 1 d . . .
H16 H 0.0870 0.7858 0.9651 0.046 Uiso 1 1 calc R . .
C17 C 0.0604(3) 0.2086(5) 0.86829(19) 0.0305(9) Uani 1 1 d . . .
C18 C -0.0179(3) 0.1328(5) 0.8753(2) 0.0330(10) Uani 1 1 d . . .
C19 C 0.1008(3) 0.1132(5) 0.8418(2) 0.0317(10) Uani 1 1 d . . .
C20 C 0.1558(3) 0.1652(5) 0.81739(19) 0.0314(10) Uani 1 1 d . . .
C21 C 0.1811(4) 0.0625(5) 0.7868(2) 0.0416(12) Uani 1 1 d . . .
H21 H 0.2131 0.0964 0.7682 0.050 Uiso 1 1 calc R . .
C22 C 0.1597(4) -0.0871(6) 0.7835(2) 0.0444(12) Uani 1 1 d . . .
H22 H 0.1800 -0.1532 0.7647 0.053 Uiso 1 1 calc R . .
C23 C 0.1078(4) -0.1394(6) 0.8084(2) 0.0434(11) Uani 1 1 d . . .
H23 H 0.0929 -0.2403 0.8060 0.052 Uiso 1 1 calc R . .
C24 C 0.0786(4) -0.0413(6) 0.8365(2) 0.0408(11) Uani 1 1 d . . .
H24 H 0.0433 -0.0772 0.8526 0.049 Uiso 1 1 calc R . .
C25 C 0.3712(8) 0.8423(11) 0.7480(4) 0.141(3) Uani 1 1 d DU . .
C26 C 0.4198(7) 0.9039(11) 0.8153(4) 0.117(3) Uani 1 1 d DU . .
H26A H 0.3921 0.8549 0.8356 0.175 Uiso 1 1 calc R . .
H26B H 0.4044 1.0084 0.8111 0.175 Uiso 1 1 calc R . .
H26C H 0.4954 0.8895 0.8443 0.175 Uiso 1 1 calc R . .
C27 C 0.4342(8) 0.2883(12) 0.7726(5) 0.141(4) Uani 1 1 d DU . .
H27A H 0.4450 0.3099 0.8147 0.212 Uiso 1 1 calc R . .
H27B H 0.5018 0.2830 0.7821 0.212 Uiso 1 1 calc R . .
H27C H 0.3980 0.1947 0.7544 0.212 Uiso 1 1 calc R . .
O10 O 0.6347(4) 0.6458(7) 0.3907(3) 0.0881(15) Uani 1 1 d D . .
C28 C 0.6955(8) 0.7817(11) 0.4297(5) 0.119(3) Uani 1 1 d DU . .
H28A H 0.7204 0.7741 0.4764 0.178 Uiso 1 1 calc R . .
H28B H 0.6503 0.8673 0.4078 0.178 Uiso 1 1 calc R . .
H28C H 0.7552 0.7916 0.4300 0.178 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 0.0407(4) 0.0285(4) 0.0350(3) -0.0032(2) 0.0321(3) -0.0014(3)
Co1 0.0455(4) 0.0436(5) 0.0378(4) 0.0035(3) 0.0353(3) 0.0026(3)
O1 0.0581(18) 0.037(2) 0.0383(15) -0.0018(14) 0.0391(15) 0.0043(16)
O2 0.0473(17) 0.049(2) 0.0378(15) -0.0023(14) 0.0351(14) -0.0118(17)
O3 0.068(2) 0.049(3) 0.072(2) -0.023(2) 0.053(2) -0.010(2)
O4 0.077(2) 0.077(3) 0.0435(18) -0.0041(19) 0.0462(18) 0.008(2)
O5 0.0505(18) 0.051(2) 0.0419(16) 0.0053(15) 0.0350(15) 0.0004(18)
O6 0.0454(17) 0.040(2) 0.0396(15) -0.0016(14) 0.0335(14) -0.0053(16)
O7 0.094(3) 0.080(3) 0.0587(19) 0.0124(17) 0.061(2) -0.013(2)
O8 0.086(3) 0.116(4) 0.080(3) 0.023(3) 0.070(3) 0.035(3)
O9 0.059(2) 0.048(2) 0.0487(17) -0.0036(15) 0.0450(17) -0.0035(18)
N1 0.0434(19) 0.027(2) 0.0370(17) -0.0052(15) 0.0332(16) -0.0057(18)
N2 0.0386(19) 0.029(2) 0.0348(17) -0.0019(15) 0.0292(15) -0.0036(17)
N3 0.042(2) 0.030(2) 0.0383(18) -0.0001(16) 0.0330(16) -0.0003(18)
N4 0.044(2) 0.032(2) 0.0399(18) -0.0032(16) 0.0357(17) -0.0007(19)
C1 0.043(2) 0.030(3) 0.038(2) 0.0010(19) 0.0326(19) 0.004(2)
C2 0.036(2) 0.033(3) 0.035(2) 0.0019(18) 0.0269(18) 0.004(2)
C3 0.040(2) 0.037(3) 0.034(2) 0.0003(19) 0.0285(18) -0.002(2)
C4 0.040(2) 0.033(3) 0.035(2) -0.0014(18) 0.0271(18) -0.002(2)
C5 0.052(3) 0.049(3) 0.046(2) -0.014(2) 0.035(2) -0.008(3)
C6 0.047(3) 0.065(4) 0.047(3) -0.017(3) 0.028(2) -0.014(3)
C7 0.042(3) 0.076(4) 0.062(3) -0.009(3) 0.037(2) -0.016(3)
C8 0.046(3) 0.054(3) 0.050(2) -0.012(2) 0.036(2) -0.007(3)
C9 0.044(2) 0.032(3) 0.036(2) -0.0030(18) 0.0311(19) 0.000(2)
C10 0.050(3) 0.049(4) 0.049(3) -0.016(2) 0.038(2) -0.009(3)
C11 0.045(2) 0.034(3) 0.037(2) 0.0023(19) 0.033(2) 0.002(2)
C12 0.045(2) 0.029(3) 0.036(2) -0.0009(18) 0.033(2) 0.004(2)
C13 0.046(3) 0.035(3) 0.055(3) -0.004(2) 0.039(2) -0.004(2)
C14 0.046(3) 0.047(3) 0.060(3) -0.003(2) 0.043(2) 0.002(3)
C15 0.057(3) 0.037(3) 0.058(3) -0.001(2) 0.047(2) 0.003(3)
C16 0.052(3) 0.029(3) 0.050(2) -0.006(2) 0.039(2) 0.001(2)
C17 0.037(2) 0.031(3) 0.0332(19) 0.0032(18) 0.0269(18) 0.001(2)
C18 0.047(2) 0.025(3) 0.047(2) 0.0000(19) 0.039(2) 0.003(2)
C19 0.039(2) 0.030(3) 0.0334(19) -0.0003(18) 0.0261(18) 0.002(2)
C20 0.037(2) 0.034(3) 0.0323(19) -0.0040(18) 0.0261(17) -0.002(2)
C21 0.058(3) 0.038(3) 0.048(2) -0.006(2) 0.043(2) 0.000(3)
C22 0.063(3) 0.033(3) 0.053(3) -0.005(2) 0.043(2) 0.007(3)
C23 0.057(3) 0.027(3) 0.054(3) -0.003(2) 0.039(2) -0.002(2)
C24 0.054(3) 0.035(3) 0.048(3) 0.002(2) 0.039(2) 0.000(2)
C25 0.155(5) 0.129(4) 0.117(4) -0.040(3) 0.073(3) -0.030(4)
C26 0.118(6) 0.105(6) 0.121(5) -0.040(4) 0.071(4) -0.021(5)
C27 0.144(7) 0.170(8) 0.124(6) 0.066(5) 0.090(5) 0.080(6)
O10 0.092(3) 0.103(4) 0.089(3) 0.006(3) 0.066(3) 0.009(3)
C28 0.132(6) 0.128(7) 0.135(6) -0.039(5) 0.102(5) -0.039(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 N2 1.863(4) . ?
Ni1 N1 1.879(3) . ?
Ni1 N4 1.882(4) . ?
Ni1 N3 1.887(4) . ?
Co1 O6 2.070(3) 2_556 ?
Co1 O8 2.074(4) . ?
Co1 O7 2.081(4) . ?
Co1 O9 2.098(3) . ?
Co1 O2 2.111(3) . ?
Co1 O1 2.180(3) . ?
O1 C1 1.247(4) . ?
O2 C2 1.262(5) . ?
O3 C10 1.264(7) . ?
O4 C10 1.231(6) . ?
O5 C18 1.240(5) . ?
O6 C18 1.258(5) . ?
O6 Co1 2.070(3) 2_546 ?
O7 C25 1.440(7) . ?
O7 H7' 0.8500 . ?
O8 C27 1.437(7) . ?
O8 H8' 0.8501 . ?
O9 H9A 0.8500 . ?
O9 H9B 0.8500 . ?
N1 C1 1.345(5) . ?
N1 C20 1.394(6) . ?
N2 C2 1.329(5) . ?
N2 C3 1.423(6) . ?
N3 C9 1.303(6) . ?
N3 C11 1.434(5) . ?
N4 C17 1.314(6) . ?
N4 C12 1.444(5) . ?
C1 C2 1.534(6) . ?
C3 C8 1.408(6) . ?
C3 C4 1.419(5) . ?
C4 C5 1.409(6) . ?
C4 C9 1.464(6) . ?
C5 C6 1.380(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.377(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.382(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.537(5) . ?
C11 C16 1.384(6) . ?
C11 C12 1.410(6) . ?
C12 C13 1.399(6) . ?
C13 C14 1.367(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.369(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.394(6) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 C19 1.454(6) . ?
C17 C18 1.535(5) . ?
C19 C24 1.419(7) . ?
C19 C20 1.426(5) . ?
C20 C21 1.406(6) . ?
C21 C22 1.377(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.393(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.373(6) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.437(8) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
O10 C28 1.483(7) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
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
N2 Ni1 N1 86.41(15) . . ?
N2 Ni1 N4 179.32(17) . . ?
N1 Ni1 N4 93.71(15) . . ?
N2 Ni1 N3 93.27(16) . . ?
N1 Ni1 N3 176.88(15) . . ?
N4 Ni1 N3 86.58(16) . . ?
O6 Co1 O8 169.31(18) 2_556 . ?
O6 Co1 O7 95.55(16) 2_556 . ?
O8 Co1 O7 94.36(19) . . ?
O6 Co1 O9 89.87(13) 2_556 . ?
O8 Co1 O9 86.30(16) . . ?
O7 Co1 O9 88.97(14) . . ?
O6 Co1 O2 87.41(12) 2_556 . ?
O8 Co1 O2 97.21(15) . . ?
O7 Co1 O2 86.46(14) . . ?
O9 Co1 O2 174.44(14) . . ?
O6 Co1 O1 81.89(13) 2_556 . ?
O8 Co1 O1 89.67(16) . . ?
O7 Co1 O1 163.93(12) . . ?
O9 Co1 O1 106.84(13) . . ?
O2 Co1 O1 77.59(12) . . ?
C1 O1 Co1 109.9(3) . . ?
C2 O2 Co1 112.0(3) . . ?
C18 O6 Co1 131.6(3) . 2_546 ?
C25 O7 Co1 131.5(5) . . ?
C25 O7 H7' 104.2 . . ?
Co1 O7 H7' 118.9 . . ?
C27 O8 Co1 130.1(5) . . ?
C27 O8 H8' 110.0 . . ?
Co1 O8 H8' 119.8 . . ?
Co1 O9 H9A 104.8 . . ?
Co1 O9 H9B 119.9 . . ?
H9A O9 H9B 117.1 . . ?
C1 N1 C20 123.7(3) . . ?
C1 N1 Ni1 109.7(3) . . ?
C20 N1 Ni1 126.6(2) . . ?
C2 N2 C3 123.2(4) . . ?
C2 N2 Ni1 109.9(3) . . ?
C3 N2 Ni1 126.7(3) . . ?
C9 N3 C11 123.0(3) . . ?
C9 N3 Ni1 126.5(3) . . ?
C11 N3 Ni1 110.2(3) . . ?
C17 N4 C12 123.9(4) . . ?
C17 N4 Ni1 125.6(3) . . ?
C12 N4 Ni1 110.5(3) . . ?
O1 C1 N1 130.3(4) . . ?
O1 C1 C2 117.9(4) . . ?
N1 C1 C2 111.7(3) . . ?
O2 C2 N2 129.4(4) . . ?
O2 C2 C1 116.9(3) . . ?
N2 C2 C1 113.6(4) . . ?
C8 C3 C4 119.2(4) . . ?
C8 C3 N2 121.1(4) . . ?
C4 C3 N2 119.4(4) . . ?
C5 C4 C3 117.9(4) . . ?
C5 C4 C9 117.7(4) . . ?
C3 C4 C9 124.4(4) . . ?
C6 C5 C4 122.0(4) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C7 C6 C5 119.4(5) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 120.9(5) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 C3 120.5(4) . . ?
C7 C8 H8 119.7 . . ?
C3 C8 H8 119.7 . . ?
N3 C9 C4 123.3(4) . . ?
N3 C9 C10 121.2(4) . . ?
C4 C9 C10 115.4(4) . . ?
O4 C10 O3 128.4(4) . . ?
O4 C10 C9 114.6(5) . . ?
O3 C10 C9 117.0(4) . . ?
C16 C11 C12 120.0(4) . . ?
C16 C11 N3 125.4(4) . . ?
C12 C11 N3 114.3(4) . . ?
C13 C12 C11 118.4(4) . . ?
C13 C12 N4 127.5(4) . . ?
C11 C12 N4 113.9(4) . . ?
C14 C13 C12 120.9(5) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 120.5(4) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C16 120.3(4) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C11 C16 C15 119.7(5) . . ?
C11 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
N4 C17 C19 123.7(4) . . ?
N4 C17 C18 121.6(4) . . ?
C19 C17 C18 114.7(4) . . ?
O5 C18 O6 129.6(4) . . ?
O5 C18 C17 116.8(4) . . ?
O6 C18 C17 113.5(3) . . ?
C24 C19 C20 117.9(4) . . ?
C24 C19 C17 117.5(4) . . ?
C20 C19 C17 124.5(4) . . ?
N1 C20 C21 122.0(4) . . ?
N1 C20 C19 119.3(4) . . ?
C21 C20 C19 118.6(4) . . ?
C22 C21 C20 121.7(4) . . ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
C21 C22 C23 120.1(4) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 119.7(5) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C19 122.0(4) . . ?
C23 C24 H24 119.0 . . ?
C19 C24 H24 119.0 . . ?
C26 C25 O7 148.1(9) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O8 C27 H27A 109.5 . . ?
O8 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O8 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O10 C28 H28A 109.5 . . ?
O10 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O10 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Co1 O1 C1 -69.7(3) 2_556 . . . ?
O8 Co1 O1 C1 116.9(3) . . . . ?
O7 Co1 O1 C1 12.2(6) . . . . ?
O9 Co1 O1 C1 -157.1(3) . . . . ?
O2 Co1 O1 C1 19.4(3) . . . . ?
O6 Co1 O2 C2 61.9(3) 2_556 . . . ?
O8 Co1 O2 C2 -108.4(3) . . . . ?
O7 Co1 O2 C2 157.6(3) . . . . ?
O9 Co1 O2 C2 122.7(12) . . . . ?
O1 Co1 O2 C2 -20.4(3) . . . . ?
O6 Co1 O7 C25 90.5(7) 2_556 . . . ?
O8 Co1 O7 C25 -93.5(7) . . . . ?
O9 Co1 O7 C25 -179.7(7) . . . . ?
O2 Co1 O7 C25 3.5(7) . . . . ?
O1 Co1 O7 C25 10.6(10) . . . . ?
O6 Co1 O8 C27 -66.8(11) 2_556 . . . ?
O7 Co1 O8 C27 135.3(8) . . . . ?
O9 Co1 O8 C27 -136.0(8) . . . . ?
O2 Co1 O8 C27 48.3(8) . . . . ?
O1 Co1 O8 C27 -29.1(8) . . . . ?
N2 Ni1 N1 C1 -26.1(3) . . . . ?
N4 Ni1 N1 C1 153.2(3) . . . . ?
N3 Ni1 N1 C1 58(3) . . . . ?
N2 Ni1 N1 C20 154.9(4) . . . . ?
N4 Ni1 N1 C20 -25.8(4) . . . . ?
N3 Ni1 N1 C20 -121(3) . . . . ?
N1 Ni1 N2 C2 25.5(3) . . . . ?
N4 Ni1 N2 C2 -75(13) . . . . ?
N3 Ni1 N2 C2 -151.4(3) . . . . ?
N1 Ni1 N2 C3 -158.2(4) . . . . ?
N4 Ni1 N2 C3 102(13) . . . . ?
N3 Ni1 N2 C3 24.9(4) . . . . ?
N2 Ni1 N3 C9 -25.5(4) . . . . ?
N1 Ni1 N3 C9 -109(3) . . . . ?
N4 Ni1 N3 C9 155.2(4) . . . . ?
N2 Ni1 N3 C11 160.2(3) . . . . ?
N1 Ni1 N3 C11 76(3) . . . . ?
N4 Ni1 N3 C11 -19.2(3) . . . . ?
N2 Ni1 N4 C17 123(13) . . . . ?
N1 Ni1 N4 C17 23.0(4) . . . . ?
N3 Ni1 N4 C17 -160.1(4) . . . . ?
N2 Ni1 N4 C12 -59(13) . . . . ?
N1 Ni1 N4 C12 -158.9(3) . . . . ?
N3 Ni1 N4 C12 18.0(3) . . . . ?
Co1 O1 C1 N1 167.9(4) . . . . ?
Co1 O1 C1 C2 -16.1(4) . . . . ?
C20 N1 C1 O1 15.9(7) . . . . ?
Ni1 N1 C1 O1 -163.1(4) . . . . ?
C20 N1 C1 C2 -160.3(4) . . . . ?
Ni1 N1 C1 C2 20.7(4) . . . . ?
Co1 O2 C2 N2 -165.6(4) . . . . ?
Co1 O2 C2 C1 18.7(5) . . . . ?
C3 N2 C2 O2 -11.8(7) . . . . ?
Ni1 N2 C2 O2 164.6(4) . . . . ?
C3 N2 C2 C1 164.0(4) . . . . ?
Ni1 N2 C2 C1 -19.6(4) . . . . ?
O1 C1 C2 O2 -1.2(6) . . . . ?
N1 C1 C2 O2 175.5(4) . . . . ?
O1 C1 C2 N2 -177.6(4) . . . . ?
N1 C1 C2 N2 -0.9(5) . . . . ?
C2 N2 C3 C8 -23.4(7) . . . . ?
Ni1 N2 C3 C8 160.8(4) . . . . ?
C2 N2 C3 C4 163.1(4) . . . . ?
Ni1 N2 C3 C4 -12.8(6) . . . . ?
C8 C3 C4 C5 1.0(7) . . . . ?
N2 C3 C4 C5 174.7(4) . . . . ?
C8 C3 C4 C9 177.9(5) . . . . ?
N2 C3 C4 C9 -8.4(7) . . . . ?
C3 C4 C5 C6 0.5(8) . . . . ?
C9 C4 C5 C6 -176.7(5) . . . . ?
C4 C5 C6 C7 -1.6(9) . . . . ?
C5 C6 C7 C8 1.3(9) . . . . ?
C6 C7 C8 C3 0.2(9) . . . . ?
C4 C3 C8 C7 -1.3(8) . . . . ?
N2 C3 C8 C7 -174.9(5) . . . . ?
C11 N3 C9 C4 -172.7(4) . . . . ?
Ni1 N3 C9 C4 13.6(6) . . . . ?
C11 N3 C9 C10 12.2(7) . . . . ?
Ni1 N3 C9 C10 -161.5(4) . . . . ?
C5 C4 C9 N3 -175.0(4) . . . . ?
C3 C4 C9 N3 8.1(8) . . . . ?
C5 C4 C9 C10 0.5(6) . . . . ?
C3 C4 C9 C10 -176.5(4) . . . . ?
N3 C9 C10 O4 72.2(6) . . . . ?
C4 C9 C10 O4 -103.4(5) . . . . ?
N3 C9 C10 O3 -108.5(5) . . . . ?
C4 C9 C10 O3 76.0(6) . . . . ?
C9 N3 C11 C16 28.3(6) . . . . ?
Ni1 N3 C11 C16 -157.1(4) . . . . ?
C9 N3 C11 C12 -158.2(4) . . . . ?
Ni1 N3 C11 C12 16.4(4) . . . . ?
C16 C11 C12 C13 -2.8(6) . . . . ?
N3 C11 C12 C13 -176.7(4) . . . . ?
C16 C11 C12 N4 171.6(4) . . . . ?
N3 C11 C12 N4 -2.3(5) . . . . ?
C17 N4 C12 C13 -21.0(7) . . . . ?
Ni1 N4 C12 C13 160.8(4) . . . . ?
C17 N4 C12 C11 165.1(4) . . . . ?
Ni1 N4 C12 C11 -13.0(4) . . . . ?
C11 C12 C13 C14 -1.5(6) . . . . ?
N4 C12 C13 C14 -175.1(4) . . . . ?
C12 C13 C14 C15 3.1(7) . . . . ?
C13 C14 C15 C16 -0.4(7) . . . . ?
C12 C11 C16 C15 5.5(6) . . . . ?
N3 C11 C16 C15 178.7(4) . . . . ?
C14 C15 C16 C11 -3.9(7) . . . . ?
C12 N4 C17 C19 173.6(4) . . . . ?
Ni1 N4 C17 C19 -8.6(6) . . . . ?
C12 N4 C17 C18 -5.4(6) . . . . ?
Ni1 N4 C17 C18 172.5(3) . . . . ?
Co1 O6 C18 O5 4.4(8) 2_546 . . . ?
Co1 O6 C18 C17 -178.1(3) 2_546 . . . ?
N4 C17 C18 O5 -79.5(5) . . . . ?
C19 C17 C18 O5 101.4(4) . . . . ?
N4 C17 C18 O6 102.7(5) . . . . ?
C19 C17 C18 O6 -76.3(5) . . . . ?
N4 C17 C19 C24 170.8(4) . . . . ?
C18 C17 C19 C24 -10.2(5) . . . . ?
N4 C17 C19 C20 -12.8(6) . . . . ?
C18 C17 C19 C20 166.2(4) . . . . ?
C1 N1 C20 C21 18.5(6) . . . . ?
Ni1 N1 C20 C21 -162.6(3) . . . . ?
C1 N1 C20 C19 -165.2(4) . . . . ?
Ni1 N1 C20 C19 13.7(6) . . . . ?
C24 C19 C20 N1 -173.7(4) . . . . ?
C17 C19 C20 N1 9.9(6) . . . . ?
C24 C19 C20 C21 2.7(6) . . . . ?
C17 C19 C20 C21 -173.7(4) . . . . ?
N1 C20 C21 C22 172.5(4) . . . . ?
C19 C20 C21 C22 -3.8(7) . . . . ?
C20 C21 C22 C23 2.7(8) . . . . ?
C21 C22 C23 C24 -0.4(7) . . . . ?
C22 C23 C24 C19 -0.7(7) . . . . ?
C20 C19 C24 C23 -0.5(7) . . . . ?
C17 C19 C24 C23 176.1(4) . . . . ?
Co1 O7 C25 C26 -15(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.809
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.108


data_Cu
_database_code_depnum_ccdc_archive 'CCDC 916436'
#TrackingRef 'web_deposit_cif_file_0_Xiao-ZengLi_1355888777.Cu.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H24 Cu N4 Ni O12'
_chemical_formula_weight         682.72
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                   15.674(3)
_cell_length_b                   8.6916(17)
_cell_length_c                   19.060(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.30(3)
_cell_angle_gamma                90.00
_cell_volume                     2595.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    8130
_cell_measurement_theta_min      1.7013
_cell_measurement_theta_max      27.8585
_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1396
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7592
_exptl_absorpt_correction_T_max  0.8548
_exptl_absorpt_process_details   crystalclear
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  confocal
_diffrn_measurement_device_type  'rigaku saturn CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            22476
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         27.83
_reflns_number_total             6141
_reflns_number_gt                5167
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'crystalclear(Rigaku/MSC Inc., 2005)'
_computing_cell_refinement       crystalclear
_computing_data_reduction        crystalclear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.0586P)^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     SHELXL
_refine_ls_extinction_coef       0.0147(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6141
_refine_ls_number_parameters     380
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0945
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_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
Cu1 Cu 1.051044(15) -0.01758(3) 0.295074(13) 0.01332(9) Uani 1 1 d . . .
Ni1 Ni 0.806115(15) 0.07648(3) 0.109865(13) 0.01091(9) Uani 1 1 d . . .
O1 O 1.01841(9) -0.06055(17) 0.19506(8) 0.0146(3) Uani 1 1 d . . .
O2 O 0.97113(9) 0.20915(18) 0.25240(7) 0.0169(3) Uani 1 1 d . . .
O3 O 0.72839(10) -0.38672(18) -0.04452(8) 0.0207(3) Uani 1 1 d . . .
O4 O 0.71237(10) -0.1580(2) -0.09773(8) 0.0255(4) Uani 1 1 d . . .
O5 O 0.56883(9) 0.42530(18) 0.06291(8) 0.0180(3) Uani 1 1 d . . .
O6 O 0.56199(9) 0.40863(17) 0.18097(8) 0.0150(3) Uani 1 1 d . . .
O7 O 1.08589(10) 0.01364(18) 0.39412(8) 0.0174(3) Uani 1 1 d D . .
H7A H 1.0412 -0.0053 0.4167 0.021 Uiso 1 1 d RD . .
H7B H 1.1320 -0.0269 0.4088 0.021 Uiso 1 1 d RD . .
O8 O 1.15838(9) 0.07399(19) 0.26430(8) 0.0198(3) Uani 1 1 d D . .
H8A H 1.1795 0.0237 0.2291 0.024 Uiso 1 1 d RD . .
H8B H 1.1962 0.0833 0.2980 0.024 Uiso 1 1 d RD . .
O9 O 1.11126(11) -0.25717(19) 0.29159(9) 0.0266(4) Uani 1 1 d D . .
H9A H 1.1454 -0.2662 0.3272 0.032 Uiso 1 1 d RD . .
H9B H 1.1019 -0.3411 0.2696 0.032 Uiso 1 1 d RD . .
N1 N 0.91109(11) -0.0267(2) 0.11053(9) 0.0128(4) Uani 1 1 d . . .
N2 N 0.75230(11) -0.0707(2) 0.05246(9) 0.0133(4) Uani 1 1 d . . .
N3 N 0.69895(10) 0.1732(2) 0.11316(9) 0.0128(3) Uani 1 1 d . . .
N4 N 0.85921(10) 0.2203(2) 0.16925(9) 0.0126(3) Uani 1 1 d . . .
C1 C 0.95551(13) 0.0082(2) 0.16863(11) 0.0130(4) Uani 1 1 d . . .
C2 C 0.92744(12) 0.1584(2) 0.20264(10) 0.0134(4) Uani 1 1 d . . .
C3 C 0.93906(13) -0.1334(2) 0.06066(11) 0.0136(4) Uani 1 1 d . . .
C4 C 1.02424(13) -0.1822(3) 0.05890(12) 0.0191(5) Uani 1 1 d . . .
H4 H 1.0631 -0.1511 0.0951 0.023 Uiso 1 1 calc R . .
C5 C 1.05265(14) -0.2749(3) 0.00535(12) 0.0213(5) Uani 1 1 d . . .
H5 H 1.1106 -0.3068 0.0054 0.026 Uiso 1 1 calc R . .
C6 C 0.99793(14) -0.3220(3) -0.04833(12) 0.0211(5) Uani 1 1 d . . .
H6 H 1.0181 -0.3844 -0.0854 0.025 Uiso 1 1 calc R . .
C7 C 0.91375(14) -0.2768(3) -0.04732(11) 0.0187(5) Uani 1 1 d . . .
H7 H 0.8763 -0.3079 -0.0845 0.022 Uiso 1 1 calc R . .
C8 C 0.88146(13) -0.1857(2) 0.00738(10) 0.0138(4) Uani 1 1 d . . .
C9 C 0.78964(13) -0.1604(2) 0.00817(11) 0.0135(4) Uani 1 1 d . . .
C10 C 0.73807(13) -0.2439(3) -0.04994(11) 0.0174(4) Uani 1 1 d . . .
C11 C 0.66148(13) -0.0664(2) 0.06092(11) 0.0134(4) Uani 1 1 d . . .
C12 C 0.60512(13) -0.1846(3) 0.04456(11) 0.0155(4) Uani 1 1 d . . .
H12 H 0.6251 -0.2759 0.0229 0.019 Uiso 1 1 calc R . .
C13 C 0.51930(13) -0.1691(3) 0.05991(11) 0.0177(4) Uani 1 1 d . . .
H13 H 0.4801 -0.2482 0.0471 0.021 Uiso 1 1 calc R . .
C14 C 0.49087(14) -0.0389(3) 0.09374(12) 0.0180(4) Uani 1 1 d . . .
H14 H 0.4322 -0.0292 0.1042 0.022 Uiso 1 1 calc R . .
C15 C 0.54714(13) 0.0776(3) 0.11251(11) 0.0165(4) Uani 1 1 d . . .
H15 H 0.5275 0.1649 0.1375 0.020 Uiso 1 1 calc R . .
C16 C 0.63280(13) 0.0663(2) 0.09464(10) 0.0134(4) Uani 1 1 d . . .
C17 C 0.68560(12) 0.3167(3) 0.12847(10) 0.0132(4) Uani 1 1 d . . .
C18 C 0.59653(13) 0.3898(2) 0.12148(11) 0.0141(4) Uani 1 1 d . . .
C19 C 0.75141(13) 0.4209(2) 0.15485(10) 0.0130(4) Uani 1 1 d . . .
C20 C 0.72929(14) 0.5780(2) 0.16138(11) 0.0162(4) Uani 1 1 d . . .
H20 H 0.6739 0.6105 0.1464 0.019 Uiso 1 1 calc R . .
C21 C 0.78535(14) 0.6850(3) 0.18863(11) 0.0172(4) Uani 1 1 d . . .
H21 H 0.7696 0.7903 0.1914 0.021 Uiso 1 1 calc R . .
C22 C 0.86529(14) 0.6367(3) 0.21206(12) 0.0192(5) Uani 1 1 d . . .
H22 H 0.9045 0.7097 0.2312 0.023 Uiso 1 1 calc R . .
C23 C 0.88873(14) 0.4843(3) 0.20804(12) 0.0184(5) Uani 1 1 d . . .
H23 H 0.9434 0.4538 0.2254 0.022 Uiso 1 1 calc R . .
C24 C 0.83341(12) 0.3729(2) 0.17876(10) 0.0126(4) Uani 1 1 d . . .
O10 O 0.75529(11) 0.0932(2) 0.82964(9) 0.0267(4) Uani 1 1 d D . .
H10A H 0.7664 0.1849 0.8445 0.032 Uiso 1 1 d RD . .
H10B H 0.7463 0.0287 0.8626 0.032 Uiso 1 1 d RD . .
O11 O 0.29274(10) 0.1002(2) 0.36124(9) 0.0263(4) Uani 1 1 d D . .
H11A H 0.3379 0.0614 0.3429 0.032 Uiso 1 1 d RD . .
H11B H 0.2771 0.0513 0.3983 0.032 Uiso 1 1 d RD . .
O12 O 0.11442(11) 0.4299(2) 0.23483(9) 0.0283(4) Uani 1 1 d D . .
H12A H 0.1600 0.4050 0.2575 0.034 Uiso 1 1 d RD . .
H12B H 0.0753 0.3621 0.2330 0.034 Uiso 1 1 d RD . .
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 0.01055(14) 0.01593(16) 0.01335(14) 0.00051(10) -0.00291(9) -0.00139(10)
Ni1 0.00887(14) 0.01099(15) 0.01274(14) -0.00247(10) -0.00288(9) -0.00002(10)
O1 0.0120(7) 0.0184(8) 0.0133(7) 0.0003(6) -0.0036(5) 0.0024(6)
O2 0.0163(7) 0.0188(8) 0.0152(7) -0.0038(6) -0.0067(6) -0.0008(6)
O3 0.0185(8) 0.0175(8) 0.0261(9) -0.0076(7) 0.0010(6) -0.0041(7)
O4 0.0285(9) 0.0292(10) 0.0183(8) 0.0015(7) -0.0081(6) -0.0073(8)
O5 0.0154(7) 0.0221(9) 0.0165(8) 0.0003(6) -0.0026(6) 0.0013(6)
O6 0.0127(7) 0.0166(8) 0.0156(7) -0.0014(6) -0.0011(5) 0.0025(6)
O7 0.0131(7) 0.0224(9) 0.0164(8) -0.0006(6) -0.0032(6) 0.0011(6)
O8 0.0151(8) 0.0235(9) 0.0208(8) -0.0010(7) -0.0022(6) -0.0028(6)
O9 0.0316(9) 0.0214(9) 0.0262(9) -0.0032(7) -0.0128(7) 0.0078(7)
N1 0.0118(8) 0.0126(9) 0.0138(9) -0.0021(7) -0.0019(6) 0.0001(7)
N2 0.0111(8) 0.0133(9) 0.0153(9) 0.0000(7) -0.0017(6) -0.0005(7)
N3 0.0116(8) 0.0132(9) 0.0135(8) -0.0011(7) -0.0017(6) -0.0002(7)
N4 0.0112(8) 0.0132(9) 0.0134(8) -0.0015(7) -0.0021(6) -0.0003(7)
C1 0.0111(9) 0.0143(11) 0.0136(10) 0.0017(8) 0.0003(7) -0.0025(8)
C2 0.0105(9) 0.0148(11) 0.0149(10) -0.0004(8) 0.0008(7) -0.0020(8)
C3 0.0145(10) 0.0124(10) 0.0140(10) 0.0008(8) 0.0004(7) -0.0009(8)
C4 0.0161(10) 0.0232(12) 0.0182(11) -0.0026(9) -0.0002(8) 0.0026(9)
C5 0.0148(10) 0.0254(13) 0.0239(12) -0.0009(10) 0.0032(8) 0.0047(9)
C6 0.0222(11) 0.0199(12) 0.0215(11) -0.0045(9) 0.0078(9) -0.0005(9)
C7 0.0179(11) 0.0202(12) 0.0179(11) -0.0046(9) -0.0003(8) -0.0042(9)
C8 0.0159(10) 0.0125(10) 0.0129(10) -0.0015(8) 0.0007(7) -0.0011(8)
C9 0.0161(10) 0.0114(10) 0.0129(10) 0.0011(8) -0.0035(7) -0.0020(8)
C10 0.0129(10) 0.0213(12) 0.0181(11) -0.0039(9) 0.0011(8) -0.0016(9)
C11 0.0126(10) 0.0148(11) 0.0127(10) 0.0012(8) -0.0022(7) 0.0000(8)
C12 0.0178(10) 0.0117(10) 0.0169(10) -0.0027(8) -0.0016(8) -0.0012(8)
C13 0.0150(10) 0.0180(11) 0.0200(11) 0.0008(9) -0.0036(8) -0.0048(9)
C14 0.0117(10) 0.0214(12) 0.0208(11) 0.0005(9) -0.0012(8) -0.0022(9)
C15 0.0134(10) 0.0170(11) 0.0190(11) -0.0011(9) -0.0006(8) 0.0018(8)
C16 0.0132(10) 0.0137(10) 0.0131(10) -0.0001(8) -0.0030(7) -0.0018(8)
C17 0.0122(9) 0.0156(10) 0.0117(9) -0.0003(8) 0.0002(7) -0.0003(8)
C18 0.0135(10) 0.0098(10) 0.0189(11) -0.0020(8) -0.0021(8) -0.0019(8)
C19 0.0143(10) 0.0130(10) 0.0117(9) 0.0002(8) 0.0000(7) -0.0013(8)
C20 0.0168(10) 0.0157(11) 0.0161(10) -0.0003(8) -0.0011(8) 0.0006(8)
C21 0.0239(11) 0.0096(10) 0.0183(10) -0.0006(8) 0.0015(8) 0.0005(8)
C22 0.0197(11) 0.0173(11) 0.0203(11) -0.0043(9) -0.0025(8) -0.0058(9)
C23 0.0141(10) 0.0189(12) 0.0221(11) -0.0026(9) -0.0044(8) -0.0021(8)
C24 0.0140(9) 0.0124(10) 0.0114(9) -0.0016(8) 0.0009(7) -0.0009(8)
O10 0.0294(9) 0.0236(9) 0.0270(9) 0.0006(7) 0.0010(7) -0.0016(7)
O11 0.0234(9) 0.0262(10) 0.0294(9) 0.0061(7) 0.0012(7) 0.0003(7)
O12 0.0222(9) 0.0241(10) 0.0383(11) 0.0014(8) -0.0036(7) -0.0034(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
Cu1 O6 1.9482(14) 2_645 ?
Cu1 O8 1.9629(16) . ?
Cu1 O7 1.9720(16) . ?
Cu1 O1 1.9976(15) . ?
Cu1 O9 2.2879(17) . ?
Ni1 N4 1.8691(17) . ?
Ni1 N2 1.8719(18) . ?
Ni1 N1 1.8737(18) . ?
Ni1 N3 1.8807(17) . ?
O1 C1 1.249(3) . ?
O2 C2 1.238(2) . ?
O3 C10 1.255(3) . ?
O4 C10 1.238(3) . ?
O5 C18 1.228(3) . ?
O6 C18 1.278(3) . ?
O6 Cu1 1.9481(14) 2_655 ?
O7 H7A 0.8463 . ?
O7 H7B 0.8464 . ?
O8 H8A 0.8724 . ?
O8 H8B 0.8688 . ?
O9 H9A 0.8582 . ?
O9 H9B 0.8526 . ?
N1 C1 1.329(3) . ?
N1 C3 1.405(3) . ?
N2 C9 1.298(3) . ?
N2 C11 1.437(3) . ?
N3 C17 1.298(3) . ?
N3 C16 1.430(3) . ?
N4 C2 1.344(3) . ?
N4 C24 1.399(3) . ?
C1 C2 1.527(3) . ?
C3 C4 1.402(3) . ?
C3 C8 1.418(3) . ?
C4 C5 1.382(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.412(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.456(3) . ?
C9 C10 1.538(3) . ?
C11 C12 1.386(3) . ?
C11 C16 1.400(3) . ?
C12 C13 1.390(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(3) . ?
C15 H15 0.9500 . ?
C17 C19 1.454(3) . ?
C17 C18 1.537(3) . ?
C19 C20 1.415(3) . ?
C19 C24 1.417(3) . ?
C20 C21 1.373(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.386(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.376(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.407(3) . ?
C23 H23 0.9500 . ?
O10 H10A 0.8620 . ?
O10 H10B 0.8559 . ?
O11 H11A 0.8655 . ?
O11 H11B 0.8645 . ?
O12 H12A 0.8542 . ?
O12 H12B 0.8512 . ?
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
O6 Cu1 O8 173.58(6) 2_645 . ?
O6 Cu1 O7 93.12(7) 2_645 . ?
O8 Cu1 O7 90.56(7) . . ?
O6 Cu1 O1 87.00(7) 2_645 . ?
O8 Cu1 O1 89.61(7) . . ?
O7 Cu1 O1 176.92(6) . . ?
O6 Cu1 O9 94.88(6) 2_645 . ?
O8 Cu1 O9 90.20(7) . . ?
O7 Cu1 O9 92.73(6) . . ?
O1 Cu1 O9 84.20(6) . . ?
N4 Ni1 N2 178.49(8) . . ?
N4 Ni1 N1 86.40(8) . . ?
N2 Ni1 N1 93.48(8) . . ?
N4 Ni1 N3 93.81(8) . . ?
N2 Ni1 N3 86.23(8) . . ?
N1 Ni1 N3 176.94(8) . . ?
C1 O1 Cu1 118.57(14) . . ?
C18 O6 Cu1 130.99(14) . 2_655 ?
Cu1 O7 H7A 104.3 . . ?
Cu1 O7 H7B 118.3 . . ?
H7A O7 H7B 117.5 . . ?
Cu1 O8 H8A 111.7 . . ?
Cu1 O8 H8B 113.1 . . ?
H8A O8 H8B 110.6 . . ?
Cu1 O9 H9A 108.1 . . ?
Cu1 O9 H9B 136.6 . . ?
H9A O9 H9B 114.1 . . ?
C1 N1 C3 123.25(18) . . ?
C1 N1 Ni1 109.86(14) . . ?
C3 N1 Ni1 126.78(14) . . ?
C9 N2 C11 123.44(18) . . ?
C9 N2 Ni1 125.93(14) . . ?
C11 N2 Ni1 110.56(13) . . ?
C17 N3 C16 124.02(17) . . ?
C17 N3 Ni1 125.84(14) . . ?
C16 N3 Ni1 110.13(13) . . ?
C2 N4 C24 123.15(17) . . ?
C2 N4 Ni1 110.95(14) . . ?
C24 N4 Ni1 125.90(14) . . ?
O1 C1 N1 128.4(2) . . ?
O1 C1 C2 118.04(18) . . ?
N1 C1 C2 113.45(18) . . ?
O2 C2 N4 129.8(2) . . ?
O2 C2 C1 118.03(18) . . ?
N4 C2 C1 112.02(17) . . ?
C4 C3 N1 121.86(19) . . ?
C4 C3 C8 118.48(19) . . ?
N1 C3 C8 119.51(18) . . ?
C5 C4 C3 121.1(2) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C6 C5 C4 121.0(2) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C7 C6 C5 118.9(2) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C6 C7 C8 122.0(2) . . ?
C6 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
C7 C8 C3 118.38(19) . . ?
C7 C8 C9 117.59(19) . . ?
C3 C8 C9 123.88(18) . . ?
N2 C9 C8 123.89(18) . . ?
N2 C9 C10 120.96(18) . . ?
C8 C9 C10 115.12(17) . . ?
O4 C10 O3 128.3(2) . . ?
O4 C10 C9 113.70(19) . . ?
O3 C10 C9 118.04(19) . . ?
C12 C11 C16 120.31(19) . . ?
C12 C11 N2 125.71(19) . . ?
C16 C11 N2 113.72(18) . . ?
C11 C12 C13 119.7(2) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C14 C13 C12 120.1(2) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.6(2) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C16 119.7(2) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C11 119.38(19) . . ?
C15 C16 N3 126.14(19) . . ?
C11 C16 N3 114.22(17) . . ?
N3 C17 C19 123.99(18) . . ?
N3 C17 C18 121.89(18) . . ?
C19 C17 C18 114.11(18) . . ?
O5 C18 O6 128.76(19) . . ?
O5 C18 C17 118.98(18) . . ?
O6 C18 C17 112.23(17) . . ?
C20 C19 C24 118.55(19) . . ?
C20 C19 C17 117.28(18) . . ?
C24 C19 C17 124.02(19) . . ?
C21 C20 C19 122.1(2) . . ?
C21 C20 H20 119.0 . . ?
C19 C20 H20 119.0 . . ?
C20 C21 C22 118.8(2) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C23 C22 C21 120.9(2) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 121.4(2) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 H23 119.3 . . ?
N4 C24 C23 121.77(19) . . ?
N4 C24 C19 119.99(18) . . ?
C23 C24 C19 118.14(19) . . ?
H10A O10 H10B 113.6 . . ?
H11A O11 H11B 112.8 . . ?
H12A O12 H12B 116.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Cu1 O1 C1 60.14(15) 2_645 . . . ?
O8 Cu1 O1 C1 -114.41(15) . . . . ?
O7 Cu1 O1 C1 152.5(11) . . . . ?
O9 Cu1 O1 C1 155.35(16) . . . . ?
N4 Ni1 N1 C1 24.68(15) . . . . ?
N2 Ni1 N1 C1 -153.81(15) . . . . ?
N3 Ni1 N1 C1 -69.3(15) . . . . ?
N4 Ni1 N1 C3 -159.17(18) . . . . ?
N2 Ni1 N1 C3 22.34(18) . . . . ?
N3 Ni1 N1 C3 106.9(14) . . . . ?
N4 Ni1 N2 C9 -111(3) . . . . ?
N1 Ni1 N2 C9 -25.86(19) . . . . ?
N3 Ni1 N2 C9 157.19(19) . . . . ?
N4 Ni1 N2 C11 72(3) . . . . ?
N1 Ni1 N2 C11 157.35(14) . . . . ?
N3 Ni1 N2 C11 -19.59(14) . . . . ?
N4 Ni1 N3 C17 22.86(18) . . . . ?
N2 Ni1 N3 C17 -158.65(18) . . . . ?
N1 Ni1 N3 C17 116.6(14) . . . . ?
N4 Ni1 N3 C16 -158.43(14) . . . . ?
N2 Ni1 N3 C16 20.06(14) . . . . ?
N1 Ni1 N3 C16 -64.6(15) . . . . ?
N2 Ni1 N4 C2 63(3) . . . . ?
N1 Ni1 N4 C2 -22.47(14) . . . . ?
N3 Ni1 N4 C2 154.47(14) . . . . ?
N2 Ni1 N4 C24 -117(3) . . . . ?
N1 Ni1 N4 C24 157.29(17) . . . . ?
N3 Ni1 N4 C24 -25.77(17) . . . . ?
Cu1 O1 C1 N1 -162.98(17) . . . . ?
Cu1 O1 C1 C2 21.8(2) . . . . ?
C3 N1 C1 O1 -13.2(3) . . . . ?
Ni1 N1 C1 O1 163.14(18) . . . . ?
C3 N1 C1 C2 162.22(18) . . . . ?
Ni1 N1 C1 C2 -21.5(2) . . . . ?
C24 N4 C2 O2 11.4(3) . . . . ?
Ni1 N4 C2 O2 -168.87(18) . . . . ?
C24 N4 C2 C1 -164.32(17) . . . . ?
Ni1 N4 C2 C1 15.4(2) . . . . ?
O1 C1 C2 O2 3.8(3) . . . . ?
N1 C1 C2 O2 -172.08(18) . . . . ?
O1 C1 C2 N4 -179.93(18) . . . . ?
N1 C1 C2 N4 4.2(2) . . . . ?
C1 N1 C3 C4 -16.4(3) . . . . ?
Ni1 N1 C3 C4 167.92(16) . . . . ?
C1 N1 C3 C8 168.1(2) . . . . ?
Ni1 N1 C3 C8 -7.6(3) . . . . ?
N1 C3 C4 C5 -173.4(2) . . . . ?
C8 C3 C4 C5 2.2(3) . . . . ?
C3 C4 C5 C6 0.2(4) . . . . ?
C4 C5 C6 C7 -0.9(4) . . . . ?
C5 C6 C7 C8 -0.8(4) . . . . ?
C6 C7 C8 C3 3.2(3) . . . . ?
C6 C7 C8 C9 -172.5(2) . . . . ?
C4 C3 C8 C7 -3.8(3) . . . . ?
N1 C3 C8 C7 171.84(19) . . . . ?
C4 C3 C8 C9 171.6(2) . . . . ?
N1 C3 C8 C9 -12.8(3) . . . . ?
C11 N2 C9 C8 -168.90(19) . . . . ?
Ni1 N2 C9 C8 14.7(3) . . . . ?
C11 N2 C9 C10 13.4(3) . . . . ?
Ni1 N2 C9 C10 -162.99(15) . . . . ?
C7 C8 C9 N2 -175.1(2) . . . . ?
C3 C8 C9 N2 9.4(3) . . . . ?
C7 C8 C9 C10 2.7(3) . . . . ?
C3 C8 C9 C10 -172.7(2) . . . . ?
N2 C9 C10 O4 72.7(3) . . . . ?
C8 C9 C10 O4 -105.2(2) . . . . ?
N2 C9 C10 O3 -108.6(2) . . . . ?
C8 C9 C10 O3 73.5(3) . . . . ?
C9 N2 C11 C12 24.1(3) . . . . ?
Ni1 N2 C11 C12 -159.00(18) . . . . ?
C9 N2 C11 C16 -161.9(2) . . . . ?
Ni1 N2 C11 C16 15.0(2) . . . . ?
C16 C11 C12 C13 1.9(3) . . . . ?
N2 C11 C12 C13 175.55(19) . . . . ?
C11 C12 C13 C14 -2.5(3) . . . . ?
C12 C13 C14 C15 0.2(3) . . . . ?
C13 C14 C15 C16 2.6(3) . . . . ?
C14 C15 C16 C11 -3.1(3) . . . . ?
C14 C15 C16 N3 -176.9(2) . . . . ?
C12 C11 C16 C15 0.9(3) . . . . ?
N2 C11 C16 C15 -173.50(18) . . . . ?
C12 C11 C16 N3 175.37(18) . . . . ?
N2 C11 C16 N3 1.0(3) . . . . ?
C17 N3 C16 C15 -23.6(3) . . . . ?
Ni1 N3 C16 C15 157.64(18) . . . . ?
C17 N3 C16 C11 162.32(19) . . . . ?
Ni1 N3 C16 C11 -16.4(2) . . . . ?
C16 N3 C17 C19 172.79(18) . . . . ?
Ni1 N3 C17 C19 -8.7(3) . . . . ?
C16 N3 C17 C18 -5.8(3) . . . . ?
Ni1 N3 C17 C18 172.77(14) . . . . ?
Cu1 O6 C18 O5 6.3(3) 2_655 . . . ?
Cu1 O6 C18 C17 -175.69(13) 2_655 . . . ?
N3 C17 C18 O5 -77.3(3) . . . . ?
C19 C17 C18 O5 104.0(2) . . . . ?
N3 C17 C18 O6 104.5(2) . . . . ?
C19 C17 C18 O6 -74.2(2) . . . . ?
N3 C17 C19 C20 172.83(19) . . . . ?
C18 C17 C19 C20 -8.5(3) . . . . ?
N3 C17 C19 C24 -11.8(3) . . . . ?
C18 C17 C19 C24 166.86(19) . . . . ?
C24 C19 C20 C21 1.4(3) . . . . ?
C17 C19 C20 C21 177.1(2) . . . . ?
C19 C20 C21 C22 -1.7(3) . . . . ?
C20 C21 C22 C23 0.2(3) . . . . ?
C21 C22 C23 C24 1.4(3) . . . . ?
C2 N4 C24 C23 18.0(3) . . . . ?
Ni1 N4 C24 C23 -161.69(16) . . . . ?
C2 N4 C24 C19 -165.78(19) . . . . ?
Ni1 N4 C24 C19 14.5(3) . . . . ?
C22 C23 C24 N4 174.7(2) . . . . ?
C22 C23 C24 C19 -1.6(3) . . . . ?
C20 C19 C24 N4 -176.15(18) . . . . ?
C17 C19 C24 N4 8.5(3) . . . . ?
C20 C19 C24 C23 0.2(3) . . . . ?
C17 C19 C24 C23 -175.14(19) . . . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.83
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.112


data_Mn
_database_code_depnum_ccdc_archive 'CCDC 916437'
#TrackingRef 'web_deposit_cif_file_1_Xiao-ZengLi_1355888777.Mn.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H24 N4 Mn Ni O12'
_chemical_formula_weight         674.10
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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   15.90(2)
_cell_length_b                   8.875(11)
_cell_length_c                   24.97(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.93(5)
_cell_angle_gamma                90.00
_cell_volume                     2741(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       Prism
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1356
_exptl_absorpt_coefficient_mu    1.218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7927
_exptl_absorpt_correction_T_max  0.7927
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22349
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_av_sigmaI/netI    0.0705
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4830
_reflns_number_gt                3049
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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^)+(0.1561P)^2^+5.6518P] 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     SHELXL
_refine_ls_extinction_coef       0.0030(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4830
_refine_ls_number_parameters     426
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.0894
_refine_ls_wR_factor_ref         0.2940
_refine_ls_wR_factor_gt          0.2367
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.91520(7) 0.44230(11) 0.10807(5) 0.0600(4) Uani 1 1 d . A .
Mn1 Mn 1.34021(11) 0.5094(2) 0.28831(8) 0.0902(6) Uani 1 1 d . . .
C1 C 0.9924(6) 0.6437(9) 0.0538(4) 0.066(2) Uani 1 1 d . A .
C2 C 1.0731(7) 0.6917(11) 0.0503(4) 0.075(2) Uani 1 1 d . . .
H2 H 1.1441 0.6611 0.0843 0.090 Uiso 1 1 calc R . .
C3 C 1.0494(9) 0.7834(12) -0.0025(5) 0.090(3) Uani 1 1 d . . .
H3 H 1.1040 0.8155 -0.0035 0.109 Uiso 1 1 calc R . .
C4 C 0.9428(10) 0.8268(13) -0.0540(6) 0.097(3) Uani 1 1 d . . .
H4 H 0.9265 0.8898 -0.0892 0.116 Uiso 1 1 calc R . .
C5 C 0.8629(9) 0.7784(12) -0.0534(5) 0.091(3) Uani 1 1 d . . .
H5 H 0.7920 0.8059 -0.0894 0.109 Uiso 1 1 calc R . .
C6 C 0.8834(7) 0.6874(10) 0.0003(5) 0.079(2) Uani 1 1 d . . .
C7 C 0.7945(7) 0.6552(11) 0.0004(6) 0.089(3) Uani 1 1 d . A .
C8 C 0.6826(13) 0.719(2) -0.0612(9) 0.140(5) Uani 1 1 d U . .
C9 C 0.7225(6) 0.5717(9) 0.0575(5) 0.080(3) Uani 1 1 d . A .
C10 C 0.6482(7) 0.6866(12) 0.0383(6) 0.100(3) Uani 1 1 d U . .
H10 H 0.6447 0.7719 0.0153 0.119 Uiso 1 1 calc R . .
C11 C 0.5798(8) 0.6696(14) 0.0546(7) 0.110(4) Uani 1 1 d U . .
H11 H 0.5265 0.7412 0.0397 0.132 Uiso 1 1 calc R . .
C12 C 0.5898(8) 0.5483(11) 0.0924(7) 0.096(3) Uani 1 1 d . . .
H12 H 0.5456 0.5416 0.1047 0.115 Uiso 1 1 calc R . .
C13 C 0.6639(6) 0.4372(11) 0.1122(5) 0.080(3) Uani 1 1 d . . .
H13 H 0.6707 0.3556 0.1380 0.096 Uiso 1 1 calc R . .
C14 C 0.7289(6) 0.4488(9) 0.0930(5) 0.070(2) Uani 1 1 d . A .
C15 C 0.8189(6) 0.2043(9) 0.1305(4) 0.0621(19) Uani 1 1 d . A .
C16 C 0.7248(6) 0.1286(10) 0.1231(5) 0.070(2) Uani 1 1 d . . .
C17 C 0.9110(6) 0.1070(9) 0.1566(4) 0.0612(18) Uani 1 1 d . . .
C18 C 0.8972(7) -0.0506(10) 0.1619(5) 0.071(2) Uani 1 1 d . . .
H18 H 0.8300 -0.0853 0.1463 0.085 Uiso 1 1 calc R . .
C19 C 0.9795(7) -0.1504(10) 0.1890(4) 0.072(2) Uani 1 1 d . . .
H19 H 0.9678 -0.2528 0.1898 0.086 Uiso 1 1 calc R . .
C20 C 1.0811(7) -0.0981(11) 0.2154(5) 0.078(2) Uani 1 1 d . . .
H20 H 1.1384 -0.1656 0.2354 0.094 Uiso 1 1 calc R . .
C21 C 1.0982(7) 0.0526(9) 0.2125(4) 0.065(2) Uani 1 1 d . . .
H21 H 1.1674 0.0854 0.2316 0.078 Uiso 1 1 calc R . .
C22 C 1.0147(6) 0.1571(9) 0.1819(4) 0.0586(17) Uani 1 1 d . . .
C23 C 1.1216(6) 0.3732(9) 0.1990(4) 0.0597(18) Uani 1 1 d . . .
C24 C 1.1150(6) 0.5140(9) 0.1611(4) 0.0640(19) Uani 1 1 d . A .
N1 N 1.0159(5) 0.5429(7) 0.1054(3) 0.0607(16) Uani 1 1 d . . .
N2 N 1.0266(4) 0.3080(7) 0.1689(3) 0.0567(14) Uani 1 1 d . A .
N3 N 0.8154(4) 0.3450(7) 0.1133(3) 0.0597(15) Uani 1 1 d . . .
N4 N 0.8032(5) 0.5765(7) 0.0481(4) 0.0728(19) Uani 1 1 d . . .
O1 O 1.2135(4) 0.3320(7) 0.2509(3) 0.0777(16) Uani 1 1 d . A .
O2 O 1.2021(4) 0.5774(7) 0.1846(3) 0.0783(17) Uani 1 1 d . A .
O3 O 0.677(2) 0.879(3) -0.0393(12) 0.080(6) Uani 0.354(18) 1 d P A 1
O4 O 0.6071(12) 0.643(2) -0.0918(9) 0.067(5) Uani 0.354(18) 1 d P A 1
O7 O 1.4118(13) 0.749(2) 0.2965(10) 0.071(6) Uani 0.354(18) 1 d PD A 1
H7A H 1.3697 0.8205 0.2710 0.086 Uiso 0.354(18) 1 d PRD A 1
H7B H 1.4797 0.7632 0.3247 0.086 Uiso 0.354(18) 1 d PRD A 1
O13 O 0.373(4) 1.043(14) 0.234(3) 0.49(10) Uani 0.354(18) 1 d P A 1
O12 O 0.384(2) 0.800(3) 0.1845(14) 0.127(10) Uani 0.354(18) 1 d PU A 1
O3' O 0.6541(13) 0.831(3) -0.0822(12) 0.148(9) Uani 0.646(18) 1 d P A 2
O4' O 0.6418(13) 0.586(3) -0.1145(8) 0.144(8) Uani 0.646(18) 1 d P A 2
O7' O 1.4298(16) 0.672(3) 0.2919(11) 0.153(8) Uani 0.646(18) 1 d PDU A 2
H7C H 1.4184 0.7638 0.2951 0.184 Uiso 0.646(18) 1 d PRD A 2
H7D H 1.4803 0.6486 0.2906 0.184 Uiso 0.646(18) 1 d PRD A 2
O13' O 0.314(3) 0.951(5) 0.196(2) 0.33(2) Uani 0.646(18) 1 d P A 2
O12' O 0.370(2) 0.699(4) 0.118(2) 0.30(2) Uani 0.646(18) 1 d P A 2
O5 O 0.6459(5) 0.0891(7) 0.0643(3) 0.0806(17) Uani 1 1 d . . .
O6 O 0.7426(4) 0.1157(7) 0.1793(3) 0.0770(16) Uani 1 1 d . . .
O8 O 1.4719(6) 0.4795(12) 0.3965(4) 0.126(3) Uani 1 1 d D A .
O9 O 1.4138(8) 0.384(2) 0.2553(7) 0.219(7) Uani 1 1 d D A .
H9A H 1.4549 0.4274 0.2491 0.263 Uiso 1 1 d RD . .
H9B H 1.4018 0.2903 0.2480 0.263 Uiso 1 1 d RD . .
O14 O 0.6915(14) 0.116(2) 0.9693(10) 0.250(7) Uani 1 1 d U . .
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 0.0414(6) 0.0572(6) 0.0651(7) 0.0011(4) 0.0256(5) 0.0065(4)
Mn1 0.0413(8) 0.1372(15) 0.0834(10) 0.0052(9) 0.0350(7) 0.0048(7)
C1 0.062(5) 0.066(5) 0.064(4) 0.005(4) 0.036(4) 0.004(4)
C2 0.076(5) 0.082(6) 0.065(5) 0.007(4) 0.044(4) 0.007(4)
C3 0.105(8) 0.092(7) 0.085(6) 0.003(5) 0.065(6) 0.005(6)
C4 0.124(9) 0.087(7) 0.087(7) 0.011(6) 0.070(7) 0.024(7)
C5 0.091(7) 0.080(6) 0.076(6) 0.010(5) 0.040(6) 0.009(5)
C6 0.066(5) 0.067(5) 0.082(6) 0.008(4) 0.036(5) 0.010(4)
C7 0.046(4) 0.072(6) 0.103(7) 0.021(5) 0.024(5) 0.011(4)
C8 0.114(8) 0.126(8) 0.144(9) 0.056(7) 0.064(6) 0.004(7)
C9 0.038(4) 0.058(5) 0.106(7) -0.003(4) 0.026(4) -0.002(3)
C10 0.060(5) 0.072(5) 0.140(7) 0.012(5) 0.050(5) 0.009(4)
C11 0.059(5) 0.092(6) 0.153(8) -0.007(6) 0.055(5) 0.013(4)
C12 0.060(5) 0.072(6) 0.153(10) -0.016(6) 0.066(7) 0.001(4)
C13 0.049(5) 0.079(6) 0.103(7) -0.018(5) 0.043(5) 0.004(4)
C14 0.046(4) 0.054(4) 0.082(5) -0.008(4) 0.027(4) 0.007(3)
C15 0.050(4) 0.060(5) 0.072(5) -0.005(4) 0.036(4) 0.005(3)
C16 0.056(5) 0.066(5) 0.082(6) -0.007(4) 0.041(5) 0.002(4)
C17 0.056(4) 0.063(4) 0.058(4) -0.007(3) 0.033(4) 0.005(3)
C18 0.068(5) 0.069(5) 0.075(5) -0.003(4) 0.045(5) -0.002(4)
C19 0.079(6) 0.061(5) 0.069(5) 0.001(4) 0.043(5) 0.008(4)
C20 0.070(5) 0.079(6) 0.067(5) 0.014(4) 0.034(4) 0.029(5)
C21 0.053(4) 0.066(5) 0.066(5) 0.010(4) 0.032(4) 0.014(3)
C22 0.055(4) 0.060(4) 0.060(4) 0.000(3) 0.036(4) 0.004(3)
C23 0.048(4) 0.067(5) 0.064(4) -0.004(4) 0.035(4) 0.004(3)
C24 0.046(4) 0.073(5) 0.073(5) 0.002(4) 0.037(4) 0.005(3)
N1 0.042(3) 0.063(4) 0.061(4) 0.004(3) 0.024(3) 0.003(3)
N2 0.050(3) 0.055(3) 0.068(4) 0.006(3) 0.039(3) 0.011(3)
N3 0.041(3) 0.061(4) 0.068(4) -0.002(3) 0.030(3) 0.010(3)
N4 0.049(4) 0.056(4) 0.087(5) 0.008(3) 0.029(4) 0.006(3)
O1 0.046(3) 0.086(4) 0.079(4) 0.005(3) 0.029(3) 0.017(3)
O2 0.052(3) 0.107(5) 0.070(3) 0.014(3) 0.035(3) 0.001(3)
O3 0.094(14) 0.075(12) 0.081(13) 0.007(11) 0.060(12) 0.010(10)
O4 0.039(8) 0.080(11) 0.064(10) -0.010(8) 0.023(7) -0.001(7)
O7 0.029(7) 0.067(11) 0.074(11) 0.023(9) 0.012(7) -0.007(7)
O13 0.12(3) 1.2(3) 0.16(4) -0.22(8) 0.10(3) -0.09(7)
O12 0.105(12) 0.128(13) 0.141(13) 0.016(8) 0.073(9) -0.014(8)
O3' 0.097(10) 0.168(17) 0.187(19) 0.133(16) 0.094(13) 0.084(12)
O4' 0.094(10) 0.211(19) 0.093(9) 0.030(11) 0.042(8) -0.006(11)
O7' 0.125(10) 0.168(12) 0.164(11) 0.009(8) 0.090(8) -0.032(8)
O13' 0.20(3) 0.40(5) 0.27(4) 0.17(4) 0.09(3) 0.19(3)
O12' 0.23(3) 0.26(3) 0.51(6) -0.01(4) 0.28(4) -0.03(2)
O5 0.057(3) 0.083(4) 0.082(4) -0.021(3) 0.034(3) -0.009(3)
O6 0.057(3) 0.085(4) 0.081(4) -0.002(3) 0.040(3) -0.003(3)
O8 0.066(5) 0.193(9) 0.104(6) 0.063(6) 0.047(4) 0.037(5)
O9 0.083(6) 0.36(2) 0.203(12) -0.078(13) 0.085(8) 0.018(9)
O14 0.240(11) 0.264(12) 0.234(11) -0.022(8) 0.142(8) 0.016(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 N4 1.865(7) . ?
Ni1 N2 1.866(6) . ?
Ni1 N1 1.871(7) . ?
Ni1 N3 1.882(6) . ?
Mn1 O7' 1.989(19) . ?
Mn1 O9 2.120(11) . ?
Mn1 O6 2.149(6) 2_755 ?
Mn1 O8 2.155(8) . ?
Mn1 O2 2.178(6) . ?
Mn1 O1 2.246(7) . ?
Mn1 O7 2.358(19) . ?
C1 C2 1.405(11) . ?
C1 N1 1.412(10) . ?
C1 C6 1.425(11) . ?
C2 C3 1.385(13) . ?
C2 H2 0.9300 . ?
C3 C4 1.391(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.351(14) . ?
C4 H4 0.9300 . ?
C5 C6 1.417(14) . ?
C5 H5 0.9300 . ?
C6 C7 1.442(13) . ?
C7 N4 1.313(12) . ?
C7 C8 1.553(17) . ?
C8 O3' 1.083(19) . ?
C8 O4 1.15(2) . ?
C8 O3 1.54(3) . ?
C8 O4' 1.58(3) . ?
C9 C14 1.369(13) . ?
C9 C10 1.398(12) . ?
C9 N4 1.442(12) . ?
C10 C11 1.389(14) . ?
C10 H10 0.9300 . ?
C11 C12 1.373(17) . ?
C11 H11 0.9300 . ?
C12 C13 1.368(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.389(12) . ?
C13 H13 0.9300 . ?
C14 N3 1.456(9) . ?
C15 N3 1.310(10) . ?
C15 C17 1.454(10) . ?
C15 C16 1.543(11) . ?
C16 O5 1.239(10) . ?
C16 O6 1.249(10) . ?
C17 C22 1.417(10) . ?
C17 C18 1.435(12) . ?
C18 C19 1.357(12) . ?
C18 H18 0.9300 . ?
C19 C20 1.387(12) . ?
C19 H19 0.9300 . ?
C20 C21 1.376(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.390(10) . ?
C21 H21 0.9300 . ?
C22 N2 1.418(10) . ?
C23 O1 1.253(9) . ?
C23 N2 1.325(9) . ?
C23 C24 1.532(12) . ?
C24 O2 1.247(9) . ?
C24 N1 1.315(10) . ?
O7 H7A 0.8500 . ?
O7 H7B 0.8499 . ?
O7 H7C 0.1859 . ?
O7' H7B 1.0675 . ?
O7' H7C 0.8500 . ?
O7' H7D 0.8501 . ?
O6 Mn1 2.149(6) 2_745 ?
O9 H9A 0.8500 . ?
O9 H9B 0.8501 . ?
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 Ni1 N2 179.1(3) . . ?
N4 Ni1 N1 94.2(3) . . ?
N2 Ni1 N1 86.5(3) . . ?
N4 Ni1 N3 85.8(3) . . ?
N2 Ni1 N3 93.5(3) . . ?
N1 Ni1 N3 178.1(3) . . ?
O7' Mn1 O9 80.9(9) . . ?
O7' Mn1 O6 104.8(8) . 2_755 ?
O9 Mn1 O6 174.2(5) . 2_755 ?
O7' Mn1 O8 85.9(7) . . ?
O9 Mn1 O8 94.9(4) . . ?
O6 Mn1 O8 85.7(3) 2_755 . ?
O7' Mn1 O2 90.6(7) . . ?
O9 Mn1 O2 94.2(4) . . ?
O6 Mn1 O2 85.8(3) 2_755 . ?
O8 Mn1 O2 169.7(3) . . ?
O7' Mn1 O1 163.1(7) . . ?
O9 Mn1 O1 92.4(5) . . ?
O6 Mn1 O1 82.1(2) 2_755 . ?
O8 Mn1 O1 110.2(3) . . ?
O2 Mn1 O1 74.3(2) . . ?
O7' Mn1 O7 18.1(9) . . ?
O9 Mn1 O7 98.7(8) . . ?
O6 Mn1 O7 87.1(6) 2_755 . ?
O8 Mn1 O7 88.1(5) . . ?
O2 Mn1 O7 85.7(4) . . ?
O1 Mn1 O7 157.8(4) . . ?
C2 C1 N1 121.3(7) . . ?
C2 C1 C6 118.7(8) . . ?
N1 C1 C6 119.8(7) . . ?
C3 C2 C1 121.6(9) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 119.2(10) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 120.6(10) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 122.2(10) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 117.6(9) . . ?
C5 C6 C7 118.1(9) . . ?
C1 C6 C7 124.1(9) . . ?
N4 C7 C6 124.2(8) . . ?
N4 C7 C8 119.6(9) . . ?
C6 C7 C8 116.2(10) . . ?
O3' C8 O4 106(2) . . ?
O3' C8 O3 39.4(15) . . ?
O4 C8 O3 120.4(19) . . ?
O3' C8 C7 133(2) . . ?
O4 C8 C7 120.9(15) . . ?
O3 C8 C7 105.6(16) . . ?
O3' C8 O4' 117(2) . . ?
O4 C8 O4' 45.6(11) . . ?
O3 C8 O4' 154.2(16) . . ?
C7 C8 O4' 99.8(13) . . ?
C14 C9 C10 120.4(9) . . ?
C14 C9 N4 114.7(7) . . ?
C10 C9 N4 124.7(9) . . ?
C11 C10 C9 117.9(10) . . ?
C11 C10 H10 121.0 . . ?
C9 C10 H10 121.0 . . ?
C12 C11 C10 120.8(9) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C13 C12 C11 121.0(10) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 118.6(10) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
C9 C14 C13 121.0(8) . . ?
C9 C14 N3 113.5(8) . . ?
C13 C14 N3 125.3(8) . . ?
N3 C15 C17 122.5(7) . . ?
N3 C15 C16 122.5(6) . . ?
C17 C15 C16 115.0(7) . . ?
O5 C16 O6 130.6(8) . . ?
O5 C16 C15 116.6(8) . . ?
O6 C16 C15 112.8(7) . . ?
C22 C17 C18 117.9(7) . . ?
C22 C17 C15 125.1(7) . . ?
C18 C17 C15 116.8(7) . . ?
C19 C18 C17 121.8(8) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C18 C19 C20 119.3(8) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
C21 C20 C19 120.6(8) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 121.8(8) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 H21 119.1 . . ?
C21 C22 C17 118.5(7) . . ?
C21 C22 N2 122.6(7) . . ?
C17 C22 N2 118.6(6) . . ?
O1 C23 N2 129.3(8) . . ?
O1 C23 C24 117.4(7) . . ?
N2 C23 C24 113.3(6) . . ?
O2 C24 N1 130.4(8) . . ?
O2 C24 C23 116.9(7) . . ?
N1 C24 C23 112.6(7) . . ?
C24 N1 C1 122.9(7) . . ?
C24 N1 Ni1 110.6(5) . . ?
C1 N1 Ni1 126.4(5) . . ?
C23 N2 C22 123.4(6) . . ?
C23 N2 Ni1 110.1(5) . . ?
C22 N2 Ni1 126.5(5) . . ?
C15 N3 C14 123.6(7) . . ?
C15 N3 Ni1 126.5(5) . . ?
C14 N3 Ni1 109.8(5) . . ?
C7 N4 C9 124.5(7) . . ?
C7 N4 Ni1 124.8(6) . . ?
C9 N4 Ni1 110.4(6) . . ?
C23 O1 Mn1 112.6(5) . . ?
C24 O2 Mn1 115.3(5) . . ?
Mn1 O7 H7A 120.0 . . ?
Mn1 O7 H7B 120.0 . . ?
H7A O7 H7B 120.0 . . ?
Mn1 O7 H7C 158.1 . . ?
H7A O7 H7C 66.1 . . ?
H7B O7 H7C 58.3 . . ?
Mn1 O7' H7B 138.7 . . ?
Mn1 O7' H7C 120.7 . . ?
H7B O7' H7C 45.5 . . ?
Mn1 O7' H7D 119.2 . . ?
H7B O7' H7D 87.0 . . ?
H7C O7' H7D 120.0 . . ?
C16 O6 Mn1 134.6(6) . 2_745 ?
Mn1 O9 H9A 120.6 . . ?
Mn1 O9 H9B 119.4 . . ?
H9A O9 H9B 120.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 176.1(8) . . . . ?
C6 C1 C2 C3 2.0(14) . . . . ?
C1 C2 C3 C4 -1.2(15) . . . . ?
C2 C3 C4 C5 -1.1(16) . . . . ?
C3 C4 C5 C6 2.6(17) . . . . ?
C4 C5 C6 C1 -1.7(15) . . . . ?
C4 C5 C6 C7 173.3(10) . . . . ?
C2 C1 C6 C5 -0.6(13) . . . . ?
N1 C1 C6 C5 -174.7(8) . . . . ?
C2 C1 C6 C7 -175.2(9) . . . . ?
N1 C1 C6 C7 10.6(14) . . . . ?
C5 C6 C7 N4 -177.8(9) . . . . ?
C1 C6 C7 N4 -3.1(16) . . . . ?
C5 C6 C7 C8 2.6(16) . . . . ?
C1 C6 C7 C8 177.2(11) . . . . ?
N4 C7 C8 O3' 125(3) . . . . ?
C6 C7 C8 O3' -55(3) . . . . ?
N4 C7 C8 O4 -49(3) . . . . ?
C6 C7 C8 O4 130.6(19) . . . . ?
N4 C7 C8 O3 92.2(15) . . . . ?
C6 C7 C8 O3 -88.2(16) . . . . ?
N4 C7 C8 O4' -92.6(14) . . . . ?
C6 C7 C8 O4' 87.1(13) . . . . ?
C14 C9 C10 C11 -1.8(15) . . . . ?
N4 C9 C10 C11 -176.0(10) . . . . ?
C9 C10 C11 C12 4.2(17) . . . . ?
C10 C11 C12 C13 -3.2(18) . . . . ?
C11 C12 C13 C14 -0.4(16) . . . . ?
C10 C9 C14 C13 -1.6(14) . . . . ?
N4 C9 C14 C13 173.0(8) . . . . ?
C10 C9 C14 N3 -175.8(8) . . . . ?
N4 C9 C14 N3 -1.1(11) . . . . ?
C12 C13 C14 C9 2.8(14) . . . . ?
C12 C13 C14 N3 176.2(9) . . . . ?
N3 C15 C16 O5 77.6(10) . . . . ?
C17 C15 C16 O5 -101.2(9) . . . . ?
N3 C15 C16 O6 -103.4(9) . . . . ?
C17 C15 C16 O6 77.8(9) . . . . ?
N3 C15 C17 C22 15.9(13) . . . . ?
C16 C15 C17 C22 -165.3(7) . . . . ?
N3 C15 C17 C18 -169.2(7) . . . . ?
C16 C15 C17 C18 9.6(10) . . . . ?
C22 C17 C18 C19 -1.1(12) . . . . ?
C15 C17 C18 C19 -176.4(8) . . . . ?
C17 C18 C19 C20 3.2(13) . . . . ?
C18 C19 C20 C21 -1.9(13) . . . . ?
C19 C20 C21 C22 -1.5(13) . . . . ?
C20 C21 C22 C17 3.5(12) . . . . ?
C20 C21 C22 N2 -170.1(8) . . . . ?
C18 C17 C22 C21 -2.2(11) . . . . ?
C15 C17 C22 C21 172.7(8) . . . . ?
C18 C17 C22 N2 171.7(7) . . . . ?
C15 C17 C22 N2 -13.5(11) . . . . ?
O1 C23 C24 O2 0.2(11) . . . . ?
N2 C23 C24 O2 -176.7(7) . . . . ?
O1 C23 C24 N1 176.5(7) . . . . ?
N2 C23 C24 N1 -0.4(9) . . . . ?
O2 C24 N1 C1 10.8(14) . . . . ?
C23 C24 N1 C1 -165.0(7) . . . . ?
O2 C24 N1 Ni1 -165.8(8) . . . . ?
C23 C24 N1 Ni1 18.4(8) . . . . ?
C2 C1 N1 C24 15.6(12) . . . . ?
C6 C1 N1 C24 -170.4(8) . . . . ?
C2 C1 N1 Ni1 -168.3(6) . . . . ?
C6 C1 N1 Ni1 5.7(11) . . . . ?
N4 Ni1 N1 C24 156.0(6) . . . . ?
N2 Ni1 N1 C24 -23.4(6) . . . . ?
N3 Ni1 N1 C24 65(8) . . . . ?
N4 Ni1 N1 C1 -20.5(7) . . . . ?
N2 Ni1 N1 C1 160.2(7) . . . . ?
N3 Ni1 N1 C1 -112(8) . . . . ?
O1 C23 N2 C22 -15.0(12) . . . . ?
C24 C23 N2 C22 161.5(6) . . . . ?
O1 C23 N2 Ni1 165.7(7) . . . . ?
C24 C23 N2 Ni1 -17.8(7) . . . . ?
C21 C22 N2 C23 -17.4(11) . . . . ?
C17 C22 N2 C23 169.0(7) . . . . ?
C21 C22 N2 Ni1 161.8(6) . . . . ?
C17 C22 N2 Ni1 -11.8(10) . . . . ?
N4 Ni1 N2 C23 -114(19) . . . . ?
N1 Ni1 N2 C23 22.9(5) . . . . ?
N3 Ni1 N2 C23 -155.2(5) . . . . ?
N4 Ni1 N2 C22 67(19) . . . . ?
N1 Ni1 N2 C22 -156.4(6) . . . . ?
N3 Ni1 N2 C22 25.5(6) . . . . ?
C17 C15 N3 C14 -174.2(7) . . . . ?
C16 C15 N3 C14 7.0(12) . . . . ?
C17 C15 N3 Ni1 7.9(11) . . . . ?
C16 C15 N3 Ni1 -170.9(6) . . . . ?
C9 C14 N3 C15 -160.8(8) . . . . ?
C13 C14 N3 C15 25.3(12) . . . . ?
C9 C14 N3 Ni1 17.4(9) . . . . ?
C13 C14 N3 Ni1 -156.5(7) . . . . ?
N4 Ni1 N3 C15 157.0(7) . . . . ?
N2 Ni1 N3 C15 -23.6(7) . . . . ?
N1 Ni1 N3 C15 -112(8) . . . . ?
N4 Ni1 N3 C14 -21.2(5) . . . . ?
N2 Ni1 N3 C14 158.2(5) . . . . ?
N1 Ni1 N3 C14 70(8) . . . . ?
C6 C7 N4 C9 165.4(9) . . . . ?
C8 C7 N4 C9 -14.9(16) . . . . ?
C6 C7 N4 Ni1 -20.5(14) . . . . ?
C8 C7 N4 Ni1 159.2(10) . . . . ?
C14 C9 N4 C7 159.0(9) . . . . ?
C10 C9 N4 C7 -26.6(15) . . . . ?
C14 C9 N4 Ni1 -15.8(10) . . . . ?
C10 C9 N4 Ni1 158.6(9) . . . . ?
N2 Ni1 N4 C7 165(18) . . . . ?
N1 Ni1 N4 C7 27.7(8) . . . . ?
N3 Ni1 N4 C7 -154.2(8) . . . . ?
N2 Ni1 N4 C9 -20(19) . . . . ?
N1 Ni1 N4 C9 -157.5(6) . . . . ?
N3 Ni1 N4 C9 20.6(6) . . . . ?
N2 C23 O1 Mn1 -170.0(6) . . . . ?
C24 C23 O1 Mn1 13.7(8) . . . . ?
O7' Mn1 O1 C23 -43(3) . . . . ?
O9 Mn1 O1 C23 -109.3(7) . . . . ?
O6 Mn1 O1 C23 72.3(5) 2_755 . . . ?
O8 Mn1 O1 C23 154.6(5) . . . . ?
O2 Mn1 O1 C23 -15.6(5) . . . . ?
O7 Mn1 O1 C23 10.8(18) . . . . ?
N1 C24 O2 Mn1 169.8(7) . . . . ?
C23 C24 O2 Mn1 -14.6(9) . . . . ?
O7' Mn1 O2 C24 -171.7(9) . . . . ?
O9 Mn1 O2 C24 107.4(7) . . . . ?
O6 Mn1 O2 C24 -66.9(6) 2_755 . . . ?
O8 Mn1 O2 C24 -101.2(16) . . . . ?
O1 Mn1 O2 C24 16.1(6) . . . . ?
O7 Mn1 O2 C24 -154.2(8) . . . . ?
O5 C16 O6 Mn1 4.9(15) . . . 2_745 ?
C15 C16 O6 Mn1 -174.0(5) . . . 2_745 ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.108