# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#\#CIF_1.1

#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2013-11-28 at 15:16:10
#  Using CIFtbx version 3.0.4  1 Sep 2006

#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.4.3
#  Request file    : c:\wingx\files\archive.reqdat
#  CIF files read  : agrb52_0m project

#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------#

data_global

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date             2013-11-28
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?

#------------------ AUTHOR DETAILS -------------------------------------------#

# Name and address of author for correspondence

_publ_contact_author_name        "Barceló-Oliver, Miquel"
_publ_contact_author_address     
;
Universitat de les Illes Balears; Department of Chemistry
campus UIB; ctra. Valldemossa km 7.5; Ed. Mateu Orfila i Rotger
E-07122 Palma de Mallorca; Spain
;
_publ_contact_author_email       miquel.barcelo@uib.es
_publ_contact_author_fax         '(+34) 971.173.426'
_publ_contact_author_phone       '(+34) 971.173.199'


# Insert blank lines between references

_publ_section_references         
;
Blessing, R. H. (1995) Acta Cryst., A51, 33-38.
 
Blessing, R. H. (1987) Cryst. Rev. 1, 3-58.
 
Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397.
 
Bruker (2012) APEX2 (Version 2012.10-0), SAINT (version 8.27B), SADABS
(version 2012/1), BrukerAXS Inc, Madison, Wisconsin, USA.
 
ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
 
CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS).
Enraf-Nonius, Delft, The Netherlands.
 
Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388.
 
CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON.
Chemical Crystallography Laboratory, Oxford, England.
 
CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006).
Program name(s). Oxford Diffraction Ltd, Abingdon, England.
 
CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. &
Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487.
 
COLLECT: Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.
 
DENZO/SCALEPACK:  Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology,
Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr
& R. M. Sweet, pp. 307-326. New York: Academic Press.
 
DIAMOND: Brandenburg, K.(2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
 
DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt,
Germany.
 
DIFABS: Walker, N. &  Stuart, D. (1983). Acta Cryst., A39, 158 - 166.
 
DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96.
 
DIRDIF-2008: Beurskens, P.T., Beurskens, G., de Gelder, R., Garciía-Granda,
S., Gould, R.O. & Smits, J.M.M. (2008) The DIRDIF-2008 program
system, Crystallography Laboratory, Radboud University  Nijmegen,
The Netherlands.
 
EDMA: Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012) J. Appl. Cryst.
45, 575-580.
 
enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler,
M. (2004). J. Appl. Cryst. 37, 335-338.
 
EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs,
A. M. M. (2003). J. Appl. Cryst. 36, 220-229.
 
JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics,
Czech Academy of Sciences, Prague, Czech Republic.
 
MERCURY: Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington,
P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R.,
van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.
 
MOGUL: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell,
W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris,
S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144.
 
ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge
National Laboratory, Tennessee, USA.
 
ORTEPIII:  Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII.
Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.
 
ORTEP-3: Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
 
PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659.
 
PLATON: Spek, A. L. (2009). Acta. Cryst. D65, 148-155.
 
PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan.
 
PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.
 
PublCIF: Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.
 
SCHAKAL: Keller, E. (1999) University of Freiburg, Germany.
 
SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
 
SHELXD: Schneider, T. R. & Sheldrick, G. M. (2002) Acta Cryst. D58, 1772-1779.
 
SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla,
M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
 
SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L.,
Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. &
Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.
 
SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L.,
Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103.
 
SIR2004: Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R.
(2005). J. Appl. Cryst. 38, 381-388.
 
SIR2008 & IL MILIONE: Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D.,
& Spagna, R. (2007). J. Appl. Cryst. 40, 609-613.
 
SIR2011: Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., Giacovazzo, C., Mallamo, M., Mazzone, A., Polidori, G.
& Spagna, R. (2012). J. Appl. Cryst. 45, 357-361.
 
SUPERFLIP: Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790.
 
TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC,
The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.
 
WinGX: Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
 
X-AREA, X-RED, X-RED32, X-SHAPE:  Stoe & Cie (2002). Program name(s).
Stoe & Cie GmbH, Darmstadt, Germany.
 
XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.
 
XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc.,
Madison, Wisconsin, USA.
 
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_1

_audit_creation_date             2013-11-28T15:16:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category         FM

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C46 H48 N6 Ni2 O11'
_chemical_formula_sum            'C46 H48 N6 Ni2 O11'
_chemical_formula_weight         978.28

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.194(5)
_cell_length_b                   12.681(5)
_cell_length_c                   14.833(5)
_cell_angle_alpha                99.696(5)
_cell_angle_beta                 97.420(5)
_cell_angle_gamma                91.907(5)
_cell_volume                     2238.4(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15344
_cell_measurement_theta_min      1.406
_cell_measurement_theta_max      24.893
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.909
_exptl_absorpt_correction_type   empirical
_shelx_estimated_absorpt_T_min   0.898
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_T_min  0.8983
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_process_details   
;
"SADABS v.2.10 (Bruker,2003) was used for absorption correction."
;

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_number            15344
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.406
_diffrn_reflns_theta_max         24.893
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.94
_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.94
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.94
_diffrn_reflns_point_group_measured_fraction_max 0.978
_reflns_number_total             7613
_reflns_number_gt                6206
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0364P)²+0.6041P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7613
_refine_ls_number_parameters     792
_refine_ls_number_restraints     39
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0816
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.045

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.27496(2) 0.17457(2) 0.35699(2) 0.03313(9) Uani 1 d . .
Ni1 Ni 0.30115(2) 0.15756(2) 0.16424(2) 0.03163(9) Uani 1 d . .
O2 O 0.38367(12) 0.09333(11) 0.28417(10) 0.0365(4) Uani 1 d . .
O3 O 0.30733(16) 0.28486(12) 0.27368(11) 0.0344(4) Uani 1 d . .
O1 O 0.16902(12) 0.11287(11) 0.22192(10) 0.0359(4) Uani 1 d . .
N2 N 0.28050(16) 0.02224(15) 0.07256(13) 0.0388(5) Uani 1 d . .
N1 N 0.22805(16) 0.24029(16) 0.05966(13) 0.0424(5) Uani 1 d . .
N4 N 0.25505(16) 0.05110(15) 0.42165(14) 0.0412(5) Uani 1 d . .
N3 N 0.38622(18) 0.25109(17) 0.47588(14) 0.0491(5) Uani 1 d . .
C15 C 0.04489(19) -0.0032(2) 0.27136(17) 0.0411(6) Uani 1 d . .
H15 H 0.0258 0.0543 0.313 0.049 Uiso 1 calc . .
C7 C 0.15040(18) -0.07228(18) 0.14801(16) 0.0353(5) Uani 1 d . .
C24 C 0.3545(2) -0.19557(19) 0.29386(18) 0.0449(6) Uani 1 d . .
C14 C -0.0036(2) -0.1011(2) 0.26853(18) 0.0482(6) Uani 1 d . .
H14 H -0.0566 -0.1091 0.307 0.058 Uiso 1 calc . .
C8 C 0.10449(19) -0.17847(19) 0.14886(16) 0.0402(6) Uani 1 d . .
C23 C 0.34387(19) -0.08101(18) 0.31871(17) 0.0390(6) Uani 1 d . .
C31 C 0.4671(2) -0.0535(2) 0.20763(19) 0.0483(6) Uani 1 d . .
H31 H 0.5034 -0.0069 0.1776 0.058 Uiso 1 calc . .
C13 C 0.0249(2) -0.1921(2) 0.20797(17) 0.0454(6) Uani 1 d . .
C32 C 0.39596(18) -0.01134(18) 0.27189(17) 0.0388(6) Uani 1 d . .
O4 O 0.45858(14) 0.19894(15) 0.14074(13) 0.0408(4) Uani 0.5 d A 1
C40 C 0.5304(17) 0.2553(17) 0.1865(16) 0.044(5) Uani 0.5 d A 1
O7 O 0.5093(18) 0.339(2) 0.2448(11) 0.039(2) Uani 0.5 d A 1
C41 C 0.642(3) 0.256(2) 0.192(3) 0.036(5) Uani 0.5 d A 1
C42 C 0.692(2) 0.178(2) 0.2350(16) 0.077(8) Uani 0.5 d A 1
H42 H 0.6488 0.1365 0.2649 0.092 Uiso 0.5 calc A 1
C43 C 0.800(2) 0.158(2) 0.2355(19) 0.090(9) Uani 0.5 d A 1
H43 H 0.8311 0.1044 0.264 0.108 Uiso 0.5 calc A 1
C44 C 0.8584(18) 0.217(2) 0.196(2) 0.081(9) Uani 0.5 d A 1
H44 H 0.933 0.2031 0.1975 0.098 Uiso 0.5 calc A 1
C45 C 0.825(2) 0.296(2) 0.1517(19) 0.088(9) Uani 0.5 d A 1
H45 H 0.8755 0.3391 0.1301 0.105 Uiso 0.5 calc A 1
C46 C 0.715(2) 0.3098(19) 0.1398(14) 0.043(5) Uani 0.5 d A 1
N6 N 0.6837(13) 0.3874(10) 0.1008(8) 0.051(3) Uani 0.5 d A 1
O10 O 0.7425(12) 0.4445(13) 0.0752(13) 0.115(5) Uani 0.5 d A 1
O11 O 0.5742(17) 0.4078(17) 0.0915(14) 0.131(8) Uani 0.5 d A 1
O4' O 0.45858(14) 0.19894(15) 0.14074(13) 0.0408(4) Uani 0.5 d A 2
C40' C 0.5226(10) 0.2727(15) 0.2011(14) 0.024(3) Uani 0.5 d A 2
O7' O 0.5018(19) 0.335(2) 0.2693(12) 0.045(3) Uani 0.5 d A 2
C41' C 0.653(3) 0.238(2) 0.188(3) 0.037(5) Uani 0.5 d A 2
C42' C 0.6931(15) 0.1623(17) 0.2367(11) 0.035(3) Uani 0.5 d A 2
H42' H 0.6453 0.1242 0.2651 0.042 Uiso 0.5 calc A 2
C43' C 0.8051(12) 0.1411(17) 0.2441(13) 0.038(2) Uani 0.5 d A 2
H43' H 0.8322 0.0903 0.2785 0.046 Uiso 0.5 calc A 2
C44' C 0.8794(15) 0.1989(17) 0.1978(17) 0.040(3) Uani 0.5 d A 2
H44' H 0.9538 0.1843 0.1992 0.048 Uiso 0.5 calc A 2
C45' C 0.8338(19) 0.2772(19) 0.1513(14) 0.042(3) Uani 0.5 d A 2
H45' H 0.875 0.3145 0.117 0.05 Uiso 0.5 calc A 2
C46' C 0.721(2) 0.297(2) 0.1590(14) 0.041(4) Uani 0.5 d A 2
N6' N 0.666(2) 0.3870(17) 0.1006(14) 0.115(8) Uani 0.5 d A 2
O10' O 0.7398(15) 0.4666(15) 0.1050(15) 0.162(7) Uani 0.5 d A 2
O11' O 0.5818(12) 0.3796(14) 0.0698(11) 0.090(4) Uani 0.5 d A 2
C16 C 0.12476(18) 0.01471(18) 0.21226(16) 0.0346(5) Uani 1 d . .
C6 C 0.21733(19) -0.05903(19) 0.07676(17) 0.0400(6) Uani 1 d . .
H6 H 0.2142 -0.1163 0.0281 0.048 Uiso 1 calc . .
C22 C 0.2872(2) -0.04372(19) 0.39650(17) 0.0424(6) Uani 1 d . .
H22 H 0.2721 -0.0941 0.4328 0.051 Uiso 1 calc . .
O6 O 0.14118(14) 0.25749(14) 0.39991(11) 0.0398(4) Uani 0.5 d B 3
C33 C 0.117(3) 0.336(2) 0.3755(17) 0.044(6) Uani 0.5 d B 3
O5 O 0.1659(19) 0.4020(16) 0.3393(16) 0.051(3) Uani 0.5 d B 3
C34 C 0.005(2) 0.369(2) 0.4015(19) 0.033(4) Uani 0.5 d B 3
C36 C -0.175(3) 0.345(2) 0.463(2) 0.064(7) Uani 0.5 d B 3
H36 H -0.2176 0.3126 0.4995 0.077 Uiso 0.5 calc B 3
C37 C -0.217(3) 0.424(3) 0.413(3) 0.079(11) Uani 0.5 d B 3
H37 H -0.2892 0.4424 0.4204 0.095 Uiso 0.5 calc B 3
C38 C -0.1720(16) 0.4700(15) 0.3630(18) 0.055(4) Uani 0.5 d B 3
H38 H -0.2083 0.5191 0.3315 0.066 Uiso 0.5 calc B 3
C39 C -0.055(3) 0.445(3) 0.3528(18) 0.066(9) Uani 0.5 d B 3
H39 H -0.0189 0.48 0.3138 0.08 Uiso 0.5 calc B 3
C35 C -0.0662(17) 0.3185(12) 0.4554(12) 0.028(3) Uani 0.5 d B 3
N5 N -0.030(3) 0.241(3) 0.509(3) 0.065(7) Uani 0.5 d B 3
O8 O -0.060(3) 0.1490(18) 0.4689(19) 0.106(6) Uani 0.5 d B 3
O9 O 0.048(3) 0.2729(19) 0.571(2) 0.074(5) Uani 0.5 d B 3
O6' O 0.14118(14) 0.25749(14) 0.39991(11) 0.0398(4) Uani 0.5 d B 4
C33' C 0.098(2) 0.3455(17) 0.3732(16) 0.031(4) Uani 0.5 d B 4
O5' O 0.1435(19) 0.3910(18) 0.3158(16) 0.056(4) Uani 0.5 d B 4
C34' C -0.0147(19) 0.3835(19) 0.3893(16) 0.026(3) Uani 0.5 d B 4
C36' C -0.184(2) 0.358(3) 0.445(2) 0.060(6) Uani 0.5 d B 4
H36' H -0.2238 0.3209 0.4806 0.072 Uiso 0.5 calc B 4
C37' C -0.233(3) 0.433(3) 0.401(3) 0.067(6) Uani 0.5 d B 4
H37' H -0.3077 0.4464 0.399 0.08 Uiso 0.5 calc B 4
C38' C -0.1500(18) 0.4929(18) 0.3554(19) 0.054(3) Uani 0.5 d B 4
H38' H -0.1726 0.5515 0.3291 0.065 Uiso 0.5 calc B 4
C39' C -0.050(2) 0.464(3) 0.3525(13) 0.038(3) Uani 0.5 d B 4
H39' H -0.0024 0.5017 0.3236 0.046 Uiso 0.5 calc B 4
C35' C -0.077(2) 0.3390(15) 0.4379(14) 0.039(3) Uani 0.5 d B 4
N5' N -0.029(2) 0.253(3) 0.494(2) 0.056(6) Uani 0.5 d B 4
O8' O -0.074(3) 0.1626(18) 0.4845(19) 0.117(7) Uani 0.5 d B 4
O9' O 0.035(4) 0.278(2) 0.564(3) 0.094(8) Uani 0.5 d B 4
C29 C 0.4275(2) -0.2336(2) 0.2309(2) 0.0540(7) Uani 1 d . .
C5 C 0.3289(2) 0.0225(2) -0.01292(18) 0.0524(7) Uani 1 d . .
H5A H 0.3261 -0.0499 -0.0473 0.063 Uiso 1 calc . .
H5B H 0.4059 0.0487 0.0018 0.063 Uiso 1 calc . .
C9 C 0.1392(2) -0.2722(2) 0.09647(18) 0.0511(7) Uani 1 d . .
H9 H 0.1953 -0.2664 0.0603 0.061 Uiso 1 calc . .
C25 C 0.2913(3) -0.2720(2) 0.3267(2) 0.0591(8) Uani 1 d . .
H25 H 0.2374 -0.2494 0.3635 0.071 Uiso 1 calc . .
C30 C 0.4833(2) -0.1594(2) 0.1889(2) 0.0579(7) Uani 1 d . .
H30 H 0.532 -0.1839 0.1478 0.069 Uiso 1 calc . .
C12 C -0.0230(3) -0.2956(2) 0.2075(2) 0.0639(8) Uani 1 d . .
H12 H -0.0771 -0.3039 0.2449 0.077 Uiso 1 calc . .
C3 C 0.2750(2) 0.2109(2) -0.02903(18) 0.0542(7) Uani 1 d . .
H3A H 0.3528 0.2347 -0.0184 0.065 Uiso 1 calc . .
H3B H 0.2381 0.2503 -0.0738 0.065 Uiso 1 calc . .
C21 C 0.2167(2) 0.0743(2) 0.51219(18) 0.0565(7) Uani 1 d . .
H21A H 0.1989 0.0077 0.5324 0.068 Uiso 1 calc . .
H21B H 0.1501 0.1139 0.5075 0.068 Uiso 1 calc . .
C1 C 0.1075(2) 0.2161(3) 0.0452(2) 0.0701(9) Uani 1 d . .
H1A H 0.0923 0.1403 0.0268 0.105 Uiso 1 calc . .
H1B H 0.0736 0.2523 -0.0022 0.105 Uiso 1 calc . .
H1C H 0.0779 0.2401 0.1016 0.105 Uiso 1 calc . .
C19 C 0.3367(3) 0.2492(2) 0.56217(19) 0.0634(8) Uani 1 d . .
H19A H 0.2706 0.2897 0.5594 0.076 Uiso 1 calc . .
H19B H 0.3887 0.2861 0.6137 0.076 Uiso 1 calc . .
C10 C 0.0919(3) -0.3714(2) 0.0979(2) 0.0675(9) Uani 1 d . .
H10 H 0.1152 -0.4315 0.0619 0.081 Uiso 1 calc . .
C20 C 0.3057(3) 0.1394(3) 0.58213(19) 0.0696(9) Uani 1 d . .
H20A H 0.3717 0.0989 0.5855 0.084 Uiso 1 calc . .
H20B H 0.2806 0.1485 0.6423 0.084 Uiso 1 calc . .
C4 C 0.2655(3) 0.0933(2) -0.07094(19) 0.0591(7) Uani 1 d . .
H4A H 0.1879 0.0691 -0.0815 0.071 Uiso 1 calc . .
H4B H 0.292 0.0848 -0.1305 0.071 Uiso 1 calc . .
C26 C 0.3077(3) -0.3791(2) 0.3057(3) 0.0792(11) Uani 1 d . .
H26 H 0.2661 -0.4281 0.3294 0.095 Uiso 1 calc . .
C28 C 0.4428(3) -0.3452(2) 0.2105(2) 0.0747(10) Uani 1 d . .
H28 H 0.4923 -0.3705 0.1703 0.09 Uiso 1 calc . .
C11 C 0.0097(3) -0.3831(2) 0.1525(2) 0.0765(10) Uani 1 d . .
H11 H -0.0232 -0.4505 0.1517 0.092 Uiso 1 calc . .
C18 C 0.4117(3) 0.3651(2) 0.4727(2) 0.0691(9) Uani 1 d . .
H18A H 0.3447 0.4028 0.4722 0.104 Uiso 1 calc . .
H18B H 0.4439 0.3704 0.4178 0.104 Uiso 1 calc . .
H18C H 0.463 0.3961 0.5259 0.104 Uiso 1 calc . .
C17 C 0.4914(2) 0.1962(3) 0.4770(2) 0.0709(9) Uani 1 d . .
H17A H 0.4773 0.1219 0.4798 0.106 Uiso 1 calc . .
H17B H 0.5421 0.2289 0.5301 0.106 Uiso 1 calc . .
H17C H 0.523 0.202 0.422 0.106 Uiso 1 calc . .
C2 C 0.2503(3) 0.3574(2) 0.0874(2) 0.0668(8) Uani 1 d . .
H2A H 0.3288 0.3739 0.0966 0.1 Uiso 1 calc . .
H2B H 0.2208 0.3814 0.1438 0.1 Uiso 1 calc . .
H2C H 0.2158 0.3929 0.0397 0.1 Uiso 1 calc . .
C27 C 0.3858(4) -0.4151(2) 0.2494(3) 0.0854(12) Uani 1 d . .
H27 H 0.3992 -0.4875 0.2382 0.102 Uiso 1 calc . .
H3WB H 0.371(3) 0.310(2) 0.273(2) 0.068(10) Uiso 1 d . .
H3WA H 0.259(3) 0.330(2) 0.289(2) 0.067(9) Uiso 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Ni2 N4 1.993(2) . ?
Ni2 O2 2.0177(16) . ?
Ni2 O3 2.0761(17) . ?
Ni2 O6 2.0806(19) . ?
Ni2 N3 2.147(2) . ?
Ni2 O1 2.2431(16) . ?
Ni2 Ni1 2.8906(10) . ?
Ni1 N2 1.988(2) . ?
Ni1 O1 2.0267(16) . ?
Ni1 O4 2.0615(18) . ?
Ni1 O3 2.0796(17) . ?
Ni1 N1 2.134(2) . ?
Ni1 O2 2.2183(16) . ?
O2 C32 1.325(3) . ?
O1 C16 1.318(3) . ?
N2 C6 1.281(3) . ?
N2 C5 1.466(3) . ?
N1 C1 1.472(3) . ?
N1 C2 1.479(3) . ?
N1 C3 1.497(3) . ?
N4 C22 1.287(3) . ?
N4 C21 1.465(3) . ?
N3 C18 1.478(3) . ?
N3 C17 1.479(3) . ?
N3 C19 1.488(3) . ?
C15 C14 1.348(3) . ?
C15 C16 1.429(3) . ?
C7 C16 1.403(3) . ?
C7 C8 1.444(3) . ?
C7 C6 1.444(3) . ?
C24 C25 1.406(4) . ?
C24 C29 1.411(4) . ?
C24 C23 1.452(3) . ?
C14 C13 1.421(4) . ?
C8 C13 1.415(3) . ?
C8 C9 1.416(3) . ?
C23 C32 1.396(3) . ?
C23 C22 1.441(3) . ?
C31 C30 1.351(3) . ?
C31 C32 1.421(3) . ?
C13 C12 1.416(4) . ?
O4 C40 1.17(2) . ?
C40 O7 1.31(3) . ?
C40 C41 1.36(5) . ?
C41 C42 1.38(4) . ?
C41 C46 1.47(5) . ?
C42 C43 1.35(3) . ?
C43 C44 1.28(3) . ?
C44 C45 1.32(4) . ?
C45 C46 1.36(4) . ?
C46 N6 1.27(3) . ?
N6 O10 1.15(2) . ?
N6 O11 1.36(2) . ?
C40' O7' 1.23(3) . ?
C40' C41' 1.69(4) . ?
C41' C46' 1.26(5) . ?
C41' C42' 1.37(4) . ?
C42' C43' 1.39(2) . ?
C43' C44' 1.46(2) . ?
C44' C45' 1.39(3) . ?
C45' C46' 1.43(3) . ?
C46' N6' 1.65(3) . ?
N6' O11' 1.07(2) . ?
N6' O10' 1.32(3) . ?
O6 C33 1.15(3) . ?
C33 O5 1.25(3) . ?
C33 C34 1.52(4) . ?
C34 C35 1.46(4) . ?
C34 C39 1.47(3) . ?
C36 C35 1.39(4) . ?
C36 C37 1.41(6) . ?
C37 C38 1.20(5) . ?
C38 C39 1.49(4) . ?
C35 N5 1.41(4) . ?
N5 O8 1.24(4) . ?
N5 O9 1.24(5) . ?
C33' O5' 1.28(3) . ?
C33' C34' 1.50(4) . ?
C34' C35' 1.29(4) . ?
C34' C39' 1.30(3) . ?
C36' C37' 1.35(6) . ?
C36' C35' 1.36(4) . ?
C37' C38' 1.54(5) . ?
C38' C39' 1.29(4) . ?
C35' N5' 1.56(4) . ?
N5' O9' 1.21(5) . ?
N5' O8' 1.23(4) . ?
C29 C30 1.415(4) . ?
C29 C28 1.420(4) . ?
C5 C4 1.510(4) . ?
C9 C10 1.370(4) . ?
C25 C26 1.369(4) . ?
C12 C11 1.365(4) . ?
C3 C4 1.511(4) . ?
C21 C20 1.515(4) . ?
C19 C20 1.517(4) . ?
C10 C11 1.387(5) . ?
C26 C27 1.385(5) . ?
C28 C27 1.354(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ni2 O2 90.01(7) . . ?
N4 Ni2 O3 170.33(8) . . ?
O2 Ni2 O3 80.72(7) . . ?
N4 Ni2 O6 96.87(8) . . ?
O2 Ni2 O6 165.83(6) . . ?
O3 Ni2 O6 91.61(7) . . ?
N4 Ni2 N3 88.44(8) . . ?
O2 Ni2 N3 99.74(8) . . ?
O3 Ni2 N3 95.79(8) . . ?
O6 Ni2 N3 92.84(8) . . ?
N4 Ni2 O1 99.81(7) . . ?
O2 Ni2 O1 78.26(6) . . ?
O3 Ni2 O1 75.74(6) . . ?
O6 Ni2 O1 88.34(6) . . ?
N3 Ni2 O1 171.48(7) . . ?
N4 Ni2 Ni1 125.14(6) . . ?
O2 Ni2 Ni1 49.95(4) . . ?
O3 Ni2 Ni1 45.98(5) . . ?
O6 Ni2 Ni1 116.57(5) . . ?
N3 Ni2 Ni1 128.45(6) . . ?
O1 Ni2 Ni1 44.31(4) . . ?
N2 Ni1 O1 90.28(7) . . ?
N2 Ni1 O4 96.31(8) . . ?
O1 Ni1 O4 164.08(7) . . ?
N2 Ni1 O3 170.13(7) . . ?
O1 Ni1 O3 80.54(7) . . ?
O4 Ni1 O3 91.69(8) . . ?
N2 Ni1 N1 88.97(8) . . ?
O1 Ni1 N1 102.95(7) . . ?
O4 Ni1 N1 91.67(7) . . ?
O3 Ni1 N1 96.59(8) . . ?
N2 Ni1 O2 98.63(7) . . ?
O1 Ni1 O2 78.66(6) . . ?
O4 Ni1 O2 86.01(6) . . ?
O3 Ni1 O2 76.11(6) . . ?
N1 Ni1 O2 172.25(7) . . ?
N2 Ni1 Ni2 124.81(6) . . ?
O1 Ni1 Ni2 50.63(4) . . ?
O4 Ni1 Ni2 114.46(5) . . ?
O3 Ni1 Ni2 45.88(5) . . ?
N1 Ni1 Ni2 131.53(6) . . ?
O2 Ni1 Ni2 44.13(4) . . ?
C32 O2 Ni2 126.90(14) . . ?
C32 O2 Ni1 116.65(14) . . ?
Ni2 O2 Ni1 85.92(6) . . ?
Ni2 O3 Ni1 88.15(7) . . ?
C16 O1 Ni1 126.03(14) . . ?
C16 O1 Ni2 115.84(13) . . ?
Ni1 O1 Ni2 85.06(6) . . ?
C6 N2 C5 117.5(2) . . ?
C6 N2 Ni1 125.36(17) . . ?
C5 N2 Ni1 116.49(16) . . ?
C1 N1 C2 108.9(2) . . ?
C1 N1 C3 110.6(2) . . ?
C2 N1 C3 105.5(2) . . ?
C1 N1 Ni1 108.61(16) . . ?
C2 N1 Ni1 110.99(16) . . ?
C3 N1 Ni1 112.20(15) . . ?
C22 N4 C21 117.2(2) . . ?
C22 N4 Ni2 125.12(17) . . ?
C21 N4 Ni2 117.01(16) . . ?
C18 N3 C17 107.8(2) . . ?
C18 N3 C19 106.4(2) . . ?
C17 N3 C19 111.6(2) . . ?
C18 N3 Ni2 111.83(16) . . ?
C17 N3 Ni2 108.23(16) . . ?
C19 N3 Ni2 111.04(17) . . ?
C14 C15 C16 121.9(2) . . ?
C16 C7 C8 119.9(2) . . ?
C16 C7 C6 122.2(2) . . ?
C8 C7 C6 117.9(2) . . ?
C25 C24 C29 117.6(2) . . ?
C25 C24 C23 123.0(3) . . ?
C29 C24 C23 119.4(2) . . ?
C15 C14 C13 121.3(2) . . ?
C13 C8 C9 117.2(2) . . ?
C13 C8 C7 119.5(2) . . ?
C9 C8 C7 123.2(2) . . ?
C32 C23 C22 122.6(2) . . ?
C32 C23 C24 119.3(2) . . ?
C22 C23 C24 117.9(2) . . ?
C30 C31 C32 121.8(3) . . ?
C8 C13 C12 119.9(3) . . ?
C8 C13 C14 118.8(2) . . ?
C12 C13 C14 121.3(3) . . ?
O2 C32 C23 123.7(2) . . ?
O2 C32 C31 117.3(2) . . ?
C23 C32 C31 119.0(2) . . ?
C40 O4 Ni1 131.7(11) . . ?
O4 C40 O7 121(2) . . ?
O4 C40 C41 133(2) . . ?
O7 C40 C41 106(2) . . ?
C40 C41 C42 115(3) . . ?
C40 C41 C46 129(3) . . ?
C42 C41 C46 114(3) . . ?
C43 C42 C41 123(3) . . ?
C44 C43 C42 118(3) . . ?
C43 C44 C45 128(2) . . ?
C44 C45 C46 117(2) . . ?
N6 C46 C45 117(2) . . ?
N6 C46 C41 122(2) . . ?
C45 C46 C41 119(2) . . ?
O10 N6 C46 123.9(19) . . ?
O10 N6 O11 117.2(15) . . ?
C46 N6 O11 119(2) . . ?
O7' C40' C41' 121.9(19) . . ?
C46' C41' C42' 118(3) . . ?
C46' C41' C40' 123(3) . . ?
C42' C41' C40' 116(3) . . ?
C41' C42' C43' 121(3) . . ?
C42' C43' C44' 120(2) . . ?
C45' C44' C43' 116.8(17) . . ?
C44' C45' C46' 116.5(15) . . ?
C41' C46' C45' 126(3) . . ?
C41' C46' N6' 116(3) . . ?
C45' C46' N6' 116(2) . . ?
O11' N6' O10' 128(2) . . ?
O11' N6' C46' 122(2) . . ?
O10' N6' C46' 110(2) . . ?
O1 C16 C7 124.5(2) . . ?
O1 C16 C15 117.2(2) . . ?
C7 C16 C15 118.3(2) . . ?
N2 C6 C7 127.7(2) . . ?
N4 C22 C23 127.6(2) . . ?
C33 O6 Ni2 122.1(16) . . ?
O6 C33 O5 134(3) . . ?
O6 C33 C34 112(2) . . ?
O5 C33 C34 114(3) . . ?
C35 C34 C39 111(2) . . ?
C35 C34 C33 128.5(19) . . ?
C39 C34 C33 119(3) . . ?
C35 C36 C37 117(3) . . ?
C38 C37 C36 128(4) . . ?
C37 C38 C39 117(3) . . ?
C34 C39 C38 123(3) . . ?
C36 C35 N5 113(2) . . ?
C36 C35 C34 123.7(19) . . ?
N5 C35 C34 123(2) . . ?
O8 N5 O9 130(4) . . ?
O8 N5 C35 112(3) . . ?
O9 N5 C35 115(4) . . ?
O5' C33' C34' 114(2) . . ?
C35' C34' C39' 119(3) . . ?
C35' C34' C33' 122.4(18) . . ?
C39' C34' C33' 118(2) . . ?
C37' C36' C35' 119(3) . . ?
C36' C37' C38' 112(3) . . ?
C39' C38' C37' 122(3) . . ?
C38' C39' C34' 121(3) . . ?
C34' C35' C36' 126(2) . . ?
C34' C35' N5' 120(2) . . ?
C36' C35' N5' 114(3) . . ?
O9' N5' O8' 114(4) . . ?
O9' N5' C35' 121(3) . . ?
O8' N5' C35' 123(3) . . ?
C24 C29 C30 119.0(2) . . ?
C24 C29 C28 119.5(3) . . ?
C30 C29 C28 121.5(3) . . ?
N2 C5 C4 109.9(2) . . ?
C10 C9 C8 121.3(3) . . ?
C26 C25 C24 121.3(3) . . ?
C31 C30 C29 121.2(3) . . ?
C11 C12 C13 120.6(3) . . ?
N1 C3 C4 116.0(2) . . ?
N4 C21 C20 110.2(2) . . ?
N3 C19 C20 116.3(2) . . ?
C9 C10 C11 120.8(3) . . ?
C21 C20 C19 115.3(2) . . ?
C5 C4 C3 114.5(2) . . ?
C25 C26 C27 120.4(3) . . ?
C27 C28 C29 120.4(3) . . ?
C12 C11 C10 120.0(3) . . ?
C28 C27 C26 120.4(3) . . ?

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
C16 C15 C14 C13 1.7(4) . . . . ?
C16 C7 C8 C13 6.7(3) . . . . ?
C6 C7 C8 C13 -170.1(2) . . . . ?
C16 C7 C8 C9 -169.9(2) . . . . ?
C6 C7 C8 C9 13.2(3) . . . . ?
C25 C24 C23 C32 -169.7(2) . . . . ?
C29 C24 C23 C32 7.5(3) . . . . ?
C25 C24 C23 C22 15.4(3) . . . . ?
C29 C24 C23 C22 -167.4(2) . . . . ?
C9 C8 C13 C12 -4.9(3) . . . . ?
C7 C8 C13 C12 178.3(2) . . . . ?
C9 C8 C13 C14 173.6(2) . . . . ?
C7 C8 C13 C14 -3.2(3) . . . . ?
C15 C14 C13 C8 -1.0(4) . . . . ?
C15 C14 C13 C12 177.6(2) . . . . ?
Ni2 O2 C32 C23 -8.9(3) . . . . ?
Ni1 O2 C32 C23 -115.0(2) . . . . ?
Ni2 O2 C32 C31 171.55(16) . . . . ?
Ni1 O2 C32 C31 65.4(2) . . . . ?
C22 C23 C32 O2 -11.2(3) . . . . ?
C24 C23 C32 O2 174.2(2) . . . . ?
C22 C23 C32 C31 168.3(2) . . . . ?
C24 C23 C32 C31 -6.3(3) . . . . ?
C30 C31 C32 O2 -178.7(2) . . . . ?
C30 C31 C32 C23 1.7(4) . . . . ?
Ni1 O4 C40 O7 -31(3) . . . . ?
Ni1 O4 C40 C41 151(3) . . . . ?
O4 C40 C41 C42 -74(4) . . . . ?
O7 C40 C41 C42 108(3) . . . . ?
O4 C40 C41 C46 89(4) . . . . ?
O7 C40 C41 C46 -88(3) . . . . ?
C40 C41 C42 C43 171(3) . . . . ?
C46 C41 C42 C43 5(4) . . . . ?
C41 C42 C43 C44 1(5) . . . . ?
C42 C43 C44 C45 -1(5) . . . . ?
C43 C44 C45 C46 -7(5) . . . . ?
C44 C45 C46 N6 177(2) . . . . ?
C44 C45 C46 C41 13(4) . . . . ?
C40 C41 C46 N6 20(4) . . . . ?
C42 C41 C46 N6 -176(2) . . . . ?
C40 C41 C46 C45 -176(3) . . . . ?
C42 C41 C46 C45 -13(4) . . . . ?
C45 C46 N6 O10 0(3) . . . . ?
C41 C46 N6 O10 164(2) . . . . ?
C45 C46 N6 O11 -177(2) . . . . ?
C41 C46 N6 O11 -13(3) . . . . ?
O7' C40' C41' C46' -81(4) . . . . ?
O7' C40' C41' C42' 79(3) . . . . ?
C46' C41' C42' C43' -8(4) . . . . ?
C40' C41' C42' C43' -168.8(19) . . . . ?
C41' C42' C43' C44' -1(3) . . . . ?
C42' C43' C44' C45' 3(3) . . . . ?
C43' C44' C45' C46' 4(3) . . . . ?
C42' C41' C46' C45' 16(5) . . . . ?
C40' C41' C46' C45' 176(2) . . . . ?
C42' C41' C46' N6' 180(2) . . . . ?
C40' C41' C46' N6' -21(4) . . . . ?
C44' C45' C46' C41' -14(4) . . . . ?
C44' C45' C46' N6' -177.9(18) . . . . ?
C41' C46' N6' O11' -20(3) . . . . ?
C45' C46' N6' O11' 145(2) . . . . ?
C41' C46' N6' O10' 156(3) . . . . ?
C45' C46' N6' O10' -39(2) . . . . ?
Ni1 O1 C16 C7 -11.2(3) . . . . ?
Ni2 O1 C16 C7 -114.7(2) . . . . ?
Ni1 O1 C16 C15 169.12(15) . . . . ?
Ni2 O1 C16 C15 65.6(2) . . . . ?
C8 C7 C16 O1 174.4(2) . . . . ?
C6 C7 C16 O1 -8.9(3) . . . . ?
C8 C7 C16 C15 -5.9(3) . . . . ?
C6 C7 C16 C15 170.8(2) . . . . ?
C14 C15 C16 O1 -178.5(2) . . . . ?
C14 C15 C16 C7 1.8(3) . . . . ?
C5 N2 C6 C7 -172.1(2) . . . . ?
Ni1 N2 C6 C7 -1.7(4) . . . . ?
C16 C7 C6 N2 16.4(4) . . . . ?
C8 C7 C6 N2 -166.9(2) . . . . ?
C21 N4 C22 C23 -169.5(2) . . . . ?
Ni2 N4 C22 C23 0.5(4) . . . . ?
C32 C23 C22 N4 16.2(4) . . . . ?
C24 C23 C22 N4 -169.1(2) . . . . ?
Ni2 O6 C33 O5 -18(4) . . . . ?
Ni2 O6 C33 C34 169.2(13) . . . . ?
O6 C33 C34 C35 4(4) . . . . ?
O5 C33 C34 C35 -171(2) . . . . ?
O6 C33 C34 C39 -161(2) . . . . ?
O5 C33 C34 C39 24(4) . . . . ?
C35 C36 C37 C38 2(5) . . . . ?
C36 C37 C38 C39 -2(5) . . . . ?
C35 C34 C39 C38 3(4) . . . . ?
C33 C34 C39 C38 170(2) . . . . ?
C37 C38 C39 C34 0(4) . . . . ?
C37 C36 C35 N5 179(3) . . . . ?
C37 C36 C35 C34 2(4) . . . . ?
C39 C34 C35 C36 -4(3) . . . . ?
C33 C34 C35 C36 -169(2) . . . . ?
C39 C34 C35 N5 180(3) . . . . ?
C33 C34 C35 N5 14(4) . . . . ?
C36 C35 N5 O8 82(3) . . . . ?
C34 C35 N5 O8 -101(3) . . . . ?
C36 C35 N5 O9 -116(3) . . . . ?
C34 C35 N5 O9 61(4) . . . . ?
O5' C33' C34' C35' 173(2) . . . . ?
O5' C33' C34' C39' -7(3) . . . . ?
C35' C36' C37' C38' -6(4) . . . . ?
C36' C37' C38' C39' 7(5) . . . . ?
C37' C38' C39' C34' -1(4) . . . . ?
C35' C34' C39' C38' -8(4) . . . . ?
C33' C34' C39' C38' 172(2) . . . . ?
C39' C34' C35' C36' 9(4) . . . . ?
C33' C34' C35' C36' -170(2) . . . . ?
C39' C34' C35' N5' -172(2) . . . . ?
C33' C34' C35' N5' 8(4) . . . . ?
C37' C36' C35' C34' -2(4) . . . . ?
C37' C36' C35' N5' 179(3) . . . . ?
C34' C35' N5' O9' 75(4) . . . . ?
C36' C35' N5' O9' -106(4) . . . . ?
C34' C35' N5' O8' -125(3) . . . . ?
C36' C35' N5' O8' 54(4) . . . . ?
C25 C24 C29 C30 173.3(2) . . . . ?
C23 C24 C29 C30 -4.0(4) . . . . ?
C25 C24 C29 C28 -6.3(4) . . . . ?
C23 C24 C29 C28 176.4(2) . . . . ?
C6 N2 C5 C4 101.5(3) . . . . ?
Ni1 N2 C5 C4 -69.8(2) . . . . ?
C13 C8 C9 C10 4.6(4) . . . . ?
C7 C8 C9 C10 -178.7(2) . . . . ?
C29 C24 C25 C26 6.2(4) . . . . ?
C23 C24 C25 C26 -176.5(3) . . . . ?
C32 C31 C30 C29 1.8(4) . . . . ?
C24 C29 C30 C31 -0.5(4) . . . . ?
C28 C29 C30 C31 179.0(3) . . . . ?
C8 C13 C12 C11 2.1(4) . . . . ?
C14 C13 C12 C11 -176.4(3) . . . . ?
C1 N1 C3 C4 -64.0(3) . . . . ?
C2 N1 C3 C4 178.4(2) . . . . ?
Ni1 N1 C3 C4 57.4(3) . . . . ?
C22 N4 C21 C20 102.5(3) . . . . ?
Ni2 N4 C21 C20 -68.3(3) . . . . ?
C18 N3 C19 C20 -178.6(3) . . . . ?
C17 N3 C19 C20 -61.4(3) . . . . ?
Ni2 N3 C19 C20 59.5(3) . . . . ?
C8 C9 C10 C11 -1.3(4) . . . . ?
N4 C21 C20 C19 62.9(3) . . . . ?
N3 C19 C20 C21 -63.2(4) . . . . ?
N2 C5 C4 C3 66.1(3) . . . . ?
N1 C3 C4 C5 -63.8(3) . . . . ?
C24 C25 C26 C27 -1.4(5) . . . . ?
C24 C29 C28 C27 1.6(4) . . . . ?
C30 C29 C28 C27 -177.9(3) . . . . ?
C13 C12 C11 C10 1.3(5) . . . . ?
C9 C10 C11 C12 -1.7(5) . . . . ?
C29 C28 C27 C26 3.4(5) . . . . ?
C25 C26 C27 C28 -3.5(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C5 H5B O4 0.97 2.56 3.133(3) 118 .
C3 H3A O4 0.97 2.66 3.173(3) 113.7 .
C21 H21A O8 0.97 2.56 3.44(2) 149.5 2_556
C21 H21A O8' 0.97 2.56 3.43(2) 149.9 2_556
C21 H21B O6 0.97 2.61 3.173(3) 117 .
C21 H21B O8 0.97 2.62 3.54(3) 158.7 .
C21 H21B O9 0.97 2.51 3.37(3) 147.8 .
C21 H21B O9' 0.97 2.63 3.51(4) 151.3 .
C19 H19A O6 0.97 2.63 3.179(4) 116.1 .
C18 H18B O7 0.96 2.75 3.694(14) 166.3 .
C2 H2B O3 0.96 2.59 3.061(3) 110.8 .
O3 H3WB O4 0.83(3) 2.58(3) 2.971(3) 110(2) .
O3 H3WB O7 0.83(3) 1.83(4) 2.643(19) 165(3) .
O3 H3WA O5 0.86(3) 1.65(4) 2.50(3) 166(3) .
O3 H3WA O5' 0.86(3) 1.69(4) 2.53(3) 165(3) .


# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 963144'
#\#CIF_1.1

#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2014-01-28 at 11:54:00
#  Using CIFtbx version 3.0.4  1 Sep 2006

#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.4.3
#  Request file    : c:\wingx\files\archive.reqdat
#  CIF files read  : agrb57_0m project

#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------#

data_global

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date             2014-01-28
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?

#------------------ AUTHOR DETAILS -------------------------------------------#

# Name and address of author for correspondence

_publ_contact_author_name        "Barceló-Oliver, Miquel"
_publ_contact_author_address     
;
Universitat de les Illes Balears; Department of Chemistry
campus UIB; ctra. Valldemossa km 7.5; Ed. Mateu Orfila i Rotger
E-07122 Palma de Mallorca; Spain
;
_publ_contact_author_email       miquel.barcelo@uib.es
_publ_contact_author_fax         '(+34) 971.173.426'
_publ_contact_author_phone       '(+34) 971.173.199'


# Insert blank lines between references

_publ_section_references         
;
Blessing, R. H. (1995) Acta Cryst., A51, 33-38.
 
Blessing, R. H. (1987) Cryst. Rev. 1, 3-58.
 
Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397.
 
Bruker (2012) APEX2 (Version 2012.10-0), SAINT (version 8.27B), SADABS
(version 2012/1), BrukerAXS Inc, Madison, Wisconsin, USA.
 
ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
 
CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS).
Enraf-Nonius, Delft, The Netherlands.
 
Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388.
 
CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON.
Chemical Crystallography Laboratory, Oxford, England.
 
CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006).
Program name(s). Oxford Diffraction Ltd, Abingdon, England.
 
CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. &
Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487.
 
COLLECT: Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.
 
DENZO/SCALEPACK:  Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology,
Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr
& R. M. Sweet, pp. 307-326. New York: Academic Press.
 
DIAMOND: Brandenburg, K.(2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
 
DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt,
Germany.
 
DIFABS: Walker, N. &  Stuart, D. (1983). Acta Cryst., A39, 158 - 166.
 
DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96.
 
DIRDIF-2008: Beurskens, P.T., Beurskens, G., de Gelder, R., Garciía-Granda,
S., Gould, R.O. & Smits, J.M.M. (2008) The DIRDIF-2008 program
system, Crystallography Laboratory, Radboud University  Nijmegen,
The Netherlands.
 
EDMA: Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012) J. Appl. Cryst.
45, 575-580.
 
enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler,
M. (2004). J. Appl. Cryst. 37, 335-338.
 
EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs,
A. M. M. (2003). J. Appl. Cryst. 36, 220-229.
 
JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics,
Czech Academy of Sciences, Prague, Czech Republic.
 
MERCURY: Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington,
P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R.,
van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.
 
MOGUL: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell,
W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris,
S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144.
 
ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge
National Laboratory, Tennessee, USA.
 
ORTEPIII:  Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII.
Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.
 
ORTEP-3: Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
 
PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659.
 
PLATON: Spek, A. L. (2009). Acta. Cryst. D65, 148-155.
 
PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan.
 
PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.
 
PublCIF: Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.
 
SCHAKAL: Keller, E. (1999) University of Freiburg, Germany.
 
SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
 
SHELXD: Schneider, T. R. & Sheldrick, G. M. (2002) Acta Cryst. D58, 1772-1779.
 
SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla,
M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
 
SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L.,
Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. &
Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.
 
SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L.,
Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103.
 
SIR2004: Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R.
(2005). J. Appl. Cryst. 38, 381-388.
 
SIR2008 & IL MILIONE: Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D.,
& Spagna, R. (2007). J. Appl. Cryst. 40, 609-613.
 
SIR2011: Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., Giacovazzo, C., Mallamo, M., Mazzone, A., Polidori, G.
& Spagna, R. (2012). J. Appl. Cryst. 45, 357-361.
 
SUPERFLIP: Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790.
 
TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC,
The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.
 
WinGX: Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
 
X-AREA, X-RED, X-RED32, X-SHAPE:  Stoe & Cie (2002). Program name(s).
Stoe & Cie GmbH, Darmstadt, Germany.
 
XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.
 
XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc.,
Madison, Wisconsin, USA.
 
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_2

_audit_creation_date             2014-01-28T11:54:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category         FM

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C46  H48  N6  Ni2 O11), C H4 O'
_chemical_formula_sum            'C93 H100 N12 Ni4 O23'
_chemical_formula_weight         1988.61

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
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                   9.691(5)
_cell_length_b                   30.326(5)
_cell_length_c                   16.498(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.900(5)
_cell_angle_gamma                90
_cell_volume                     4823(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9088
_cell_measurement_theta_min      1.34
_cell_measurement_theta_max      26.00
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2076
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_type   empirical
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_T_min  0.3281
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   
;
"SADABS v.2.10 (Bruker,2003) was used for absorption correction."
;
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '/p and /o scans'
_diffrn_reflns_av_R_equivalents  0.1261
_diffrn_reflns_number            32872
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.343
_diffrn_reflns_theta_max         26.005
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.958
_reflns_number_total             9088
_reflns_number_gt                4324
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1361P)²+14.1038P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9088
_refine_ls_number_parameters     709
_refine_ls_number_restraints     96
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.1973
_refine_ls_R_factor_gt           0.1067
_refine_ls_wR_factor_ref         0.3132
_refine_ls_wR_factor_gt          0.2534
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.02
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.989
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.107

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.31966(12) 0.13161(4) 0.28119(7) 0.0560(4) Uani 1 d . .
O4 O 0.1986(7) 0.0879(2) 0.2125(4) 0.0683(18) Uani 0.5 d A 1
C40 C 0.077(7) 0.098(2) 0.178(2) 0.13(2) Uani 0.5 d A 1
O7 O 0.014(4) 0.1284(15) 0.169(2) 0.112(16) Uani 0.5 d A 1
C41 C -0.004(4) 0.0591(11) 0.134(2) 0.065(13) Uani 0.5 d A 1
C42 C -0.132(4) 0.0584(11) 0.104(2) 0.063(9) Uani 0.5 d A 1
H42 H -0.1824 0.0842 0.1086 0.076 Uiso 0.5 calc A 1
C43 C -0.203(3) 0.0241(9) 0.0649(17) 0.067(8) Uani 0.5 d A 1
H43 H -0.2911 0.0273 0.0372 0.081 Uiso 0.5 calc A 1
C44 C -0.134(5) -0.0148(17) 0.070(3) 0.076(17) Uani 0.5 d A 1
C45 C -0.008(5) -0.0224(18) 0.103(2) 0.078(16) Uani 0.5 d A 1
H45 H 0.0303 -0.0504 0.1009 0.094 Uiso 0.5 calc A 1
C46 C 0.083(7) 0.019(2) 0.147(3) 0.074(17) Uani 0.5 d A 1
H46 H 0.1708 0.0175 0.175 0.089 Uiso 0.5 calc A 1
N6 N -0.205(3) -0.0546(9) 0.0335(16) 0.090(9) Uani 0.5 d A 1
O11 O -0.320(2) -0.0489(8) 0.0002(15) 0.111(8) Uani 0.5 d A 1
O10 O -0.145(4) -0.0898(13) 0.034(3) 0.16(2) Uani 0.5 d A 1
O4' O 0.1986(7) 0.0879(2) 0.2125(4) 0.0683(18) Uani 0.5 d A 2
C40' C 0.083(2) 0.0923(8) 0.1731(8) 0.023(5) Uani 0.5 d A 2
O7' O 0.016(4) 0.1295(10) 0.1594(16) 0.065(10) Uani 0.5 d A 2
C41' C 0.018(3) 0.0484(12) 0.1432(17) 0.038(7) Uani 0.5 d A 2
C42' C -0.111(4) 0.0456(10) 0.101(2) 0.065(10) Uani 0.5 d A 2
H42' H -0.1608 0.0717 0.0931 0.078 Uiso 0.5 calc A 2
C43' C -0.174(3) 0.0079(11) 0.0707(18) 0.061(7) Uani 0.5 d A 2
H43' H -0.265 0.0074 0.0468 0.073 Uiso 0.5 calc A 2
C44' C -0.094(4) -0.0283(14) 0.077(2) 0.055(9) Uani 0.5 d A 2
C45' C 0.039(4) -0.0271(17) 0.125(2) 0.057(10) Uani 0.5 d A 2
H45' H 0.0927 -0.0521 0.1376 0.069 Uiso 0.5 calc A 2
C46' C 0.072(7) 0.007(2) 0.144(4) 0.08(2) Uani 0.5 d A 2
H46' H 0.1636 0.0075 0.168 0.092 Uiso 0.5 calc A 2
N6' N -0.154(3) -0.0700(10) 0.0469(19) 0.077(10) Uani 0.5 d A 2
O11' O -0.259(3) -0.0665(9) 0.0015(17) 0.100(8) Uani 0.5 d A 2
O10' O -0.088(4) -0.1029(9) 0.061(3) 0.126(12) Uani 0.5 d A 2
Ni2 Ni 0.18233(12) 0.19743(4) 0.36653(6) 0.0542(4) Uani 1 d . .
O6 O 0.2421(7) 0.26112(19) 0.3488(4) 0.0656(17) Uani 1 d . .
C33 C 0.2956(9) 0.2748(3) 0.2861(5) 0.055(2) Uani 1 d . .
O5 O 0.2856(9) 0.2585(2) 0.2186(4) 0.089(2) Uani 1 d . .
C34 C 0.3785(9) 0.3167(3) 0.3002(6) 0.056(2) Uani 1 d . .
C35 C 0.4553(12) 0.3312(3) 0.2383(7) 0.080(3) Uani 1 d . .
H35 H 0.4569 0.3145 0.1911 0.095 Uiso 1 calc . .
C36 C 0.5283(11) 0.3700(4) 0.2469(8) 0.084(3) Uani 1 d . .
H36 H 0.582 0.3795 0.2067 0.1 Uiso 1 calc . .
C37 C 0.5205(12) 0.3943(3) 0.3161(8) 0.080(3) Uani 1 d . .
C38 C 0.4474(13) 0.3812(4) 0.3785(7) 0.087(3) Uani 1 d . .
H38 H 0.4457 0.3982 0.4253 0.104 Uiso 1 calc . .
C39 C 0.3760(11) 0.3418(3) 0.3694(6) 0.068(3) Uani 1 d . .
H39 H 0.3253 0.332 0.4109 0.082 Uiso 1 calc . .
N5 N 0.5995(15) 0.4364(4) 0.3239(11) 0.124(4) Uani 1 d . .
O8 O 0.6607(15) 0.4483(4) 0.2678(10) 0.179(6) Uani 1 d . .
O9 O 0.5934(16) 0.4572(4) 0.3837(9) 0.178(6) Uani 1 d . .
O3 O 0.1865(6) 0.18298(19) 0.2424(3) 0.0565(15) Uani 1 d . .
H3A H 0.0981 0.1735 0.215 0.068 Uiso 1 calc . .
H3B H 0.2286 0.2057 0.2117 0.068 Uiso 1 calc . .
O1 O 0.3957(6) 0.1793(2) 0.3573(3) 0.0592(15) Uani 1 d . .
C16 C 0.4842(9) 0.1763(3) 0.4223(5) 0.056(2) Uani 1 d . .
C15 C 0.5119(11) 0.2154(4) 0.4675(6) 0.074(3) Uani 1 d . .
H15 H 0.4639 0.2411 0.4514 0.089 Uiso 1 calc . .
C14 C 0.6063(11) 0.2164(4) 0.5333(6) 0.074(3) Uani 1 d . .
H14 H 0.6254 0.2431 0.56 0.089 Uiso 1 calc . .
C13 C 0.6755(11) 0.1789(4) 0.5622(6) 0.073(3) Uani 1 d . .
C12 C 0.7814(12) 0.1798(5) 0.6290(7) 0.088(3) Uani 1 d . .
H12 H 0.8027 0.2066 0.6547 0.105 Uiso 1 calc . .
C11 C 0.8522(13) 0.1435(5) 0.6567(8) 0.098(4) Uani 1 d . .
H11 H 0.9193 0.1451 0.7011 0.118 Uiso 1 calc . .
C10 C 0.8229(13) 0.1045(6) 0.6178(7) 0.110(5) Uani 1 d . .
H10 H 0.8724 0.0794 0.6355 0.131 Uiso 1 calc . .
C9 C 0.7205(12) 0.1011(4) 0.5520(7) 0.086(3) Uani 1 d . .
H9 H 0.6998 0.0736 0.5289 0.103 Uiso 1 calc . .
C8 C 0.6498(10) 0.1377(4) 0.5207(6) 0.065(3) Uani 1 d . .
C7 C 0.5500(9) 0.1376(3) 0.4490(5) 0.056(2) Uani 1 d . .
C6 C 0.5358(11) 0.0978(3) 0.4012(6) 0.070(3) Uani 1 d . .
H6 H 0.5957 0.075 0.4187 0.084 Uiso 1 calc . .
N2 N 0.4515(8) 0.0895(2) 0.3375(5) 0.061(2) Uani 1 d . .
C5 C 0.4790(12) 0.0497(3) 0.2921(7) 0.077(3) Uani 1 d . .
H5A H 0.3921 0.036 0.2711 0.092 Uiso 1 calc . .
H5B H 0.5306 0.0288 0.328 0.092 Uiso 1 calc . .
C4 C 0.5620(13) 0.0614(4) 0.2221(7) 0.092(4) Uani 1 d . .
H4A H 0.6488 0.0746 0.2446 0.11 Uiso 1 calc . .
H4B H 0.5847 0.0343 0.1952 0.11 Uiso 1 calc . .
C3 C 0.4944(12) 0.0920(4) 0.1590(7) 0.087(4) Uani 1 d . .
H3C H 0.5562 0.0957 0.1169 0.105 Uiso 1 calc . .
H3D H 0.4106 0.078 0.134 0.105 Uiso 1 calc . .
N1 N 0.4572(8) 0.1362(3) 0.1876(4) 0.063(2) Uani 1 d . .
C1 C 0.5821(12) 0.1609(4) 0.2198(7) 0.094(4) Uani 1 d . .
H1A H 0.6337 0.1439 0.2616 0.141 Uiso 1 calc . .
H1B H 0.555 0.1884 0.2423 0.141 Uiso 1 calc . .
H1C H 0.6388 0.1665 0.1766 0.141 Uiso 1 calc . .
C2 C 0.3917(13) 0.1598(4) 0.1154(6) 0.091(4) Uani 1 d . .
H2A H 0.3768 0.19 0.1292 0.136 Uiso 1 calc . .
H2B H 0.3044 0.1462 0.0974 0.136 Uiso 1 calc . .
H2C H 0.4514 0.1584 0.0725 0.136 Uiso 1 calc . .
O2 O 0.1684(6) 0.13193(18) 0.3679(3) 0.0553(15) Uani 1 d . .
C32 C 0.1744(9) 0.1057(3) 0.4301(6) 0.054(2) Uani 1 d . .
C31 C 0.1631(12) 0.0598(3) 0.4109(7) 0.079(3) Uani 1 d . .
H31 H 0.1568 0.0508 0.3567 0.095 Uiso 1 calc . .
C30 C 0.1615(12) 0.0288(3) 0.4717(8) 0.080(3) Uani 1 d . .
H30 H 0.1537 -0.0009 0.458 0.096 Uiso 1 calc . .
C29 C 0.1714(11) 0.0410(4) 0.5530(7) 0.076(3) Uani 1 d . .
C28 C 0.1678(11) 0.0088(4) 0.6166(9) 0.092(4) Uani 1 d . .
H28 H 0.1621 -0.0209 0.6031 0.11 Uiso 1 calc . .
C27 C 0.1725(13) 0.0207(5) 0.6949(9) 0.102(4) Uani 1 d . .
H27 H 0.1665 -0.0006 0.7349 0.123 Uiso 1 calc . .
C26 C 0.1864(14) 0.0648(5) 0.7166(7) 0.103(4) Uani 1 d . .
H26 H 0.1912 0.0727 0.7713 0.124 Uiso 1 calc . .
C25 C 0.1931(11) 0.0964(4) 0.6597(6) 0.078(3) Uani 1 d . .
H25 H 0.2032 0.1257 0.6758 0.094 Uiso 1 calc . .
C24 C 0.1851(10) 0.0858(4) 0.5759(6) 0.068(3) Uani 1 d . .
C23 C 0.1831(10) 0.1186(3) 0.5115(5) 0.061(2) Uani 1 d . .
C22 C 0.1838(10) 0.1644(3) 0.5341(6) 0.064(3) Uani 1 d . .
H22 H 0.1815 0.1703 0.5892 0.077 Uiso 1 calc . .
N4 N 0.1872(8) 0.1981(2) 0.4870(4) 0.0572(19) Uani 1 d . .
C21 C 0.1595(13) 0.2407(3) 0.5222(6) 0.079(3) Uani 1 d . .
H21A H 0.2169 0.2631 0.5005 0.095 Uiso 1 calc . .
H21B H 0.182 0.2397 0.5809 0.095 Uiso 1 calc . .
C20 C 0.0079(15) 0.2522(4) 0.5023(7) 0.095(4) Uani 1 d . .
H20A H -0.0466 0.23 0.5269 0.114 Uiso 1 calc . .
H20B H -0.0088 0.2801 0.5283 0.114 Uiso 1 calc . .
C19 C -0.0462(12) 0.2559(4) 0.4139(7) 0.089(3) Uani 1 d . .
H19A H -0.1441 0.2631 0.4109 0.106 Uiso 1 calc . .
H19B H 0.0001 0.2806 0.3909 0.106 Uiso 1 calc . .
N3 N -0.0303(8) 0.2167(3) 0.3614(5) 0.067(2) Uani 1 d . .
C17 C -0.1151(12) 0.1799(4) 0.3868(7) 0.089(3) Uani 1 d . .
H17A H -0.2096 0.1894 0.3868 0.133 Uiso 1 calc . .
H17B H -0.0802 0.1705 0.4406 0.133 Uiso 1 calc . .
H17C H -0.1108 0.1558 0.3495 0.133 Uiso 1 calc . .
C18 C -0.0836(11) 0.2304(4) 0.2778(7) 0.089(4) Uani 1 d . .
H18A H -0.0798 0.2059 0.2414 0.133 Uiso 1 calc . .
H18B H -0.0276 0.254 0.2605 0.133 Uiso 1 calc . .
H18C H -0.1778 0.2402 0.2775 0.133 Uiso 1 calc . .
O1S O 0.8036(15) 0.1656(5) 1.0600(10) 0.081(4) Uani 0.5 d . .
H1S H 0.8203 0.1451 1.0921 0.122 Uiso 0.5 calc . .
C2S C 0.783(3) 0.1507(9) 0.989(2) 0.119(10) Uani 0.5 d . .
H2S1 H 0.7328 0.172 0.9547 0.178 Uiso 0.5 calc . .
H2S2 H 0.7307 0.1239 0.9894 0.178 Uiso 0.5 calc . .
H2S3 H 0.8709 0.1449 0.9688 0.178 Uiso 0.5 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 1.971(8) . ?
Ni1 O1 2.005(6) . ?
Ni1 O4 2.036(7) . ?
Ni1 O3 2.081(6) . ?
Ni1 N1 2.145(8) . ?
Ni1 O2 2.150(6) . ?
Ni1 Ni2 2.8500(17) . ?
O4 C40 1.29(7) . ?
C40 O7 1.11(8) . ?
C40 C41 1.55(7) . ?
C41 C42 1.29(5) . ?
C41 C46 1.48(8) . ?
C42 C43 1.37(4) . ?
C43 C44 1.35(5) . ?
C44 C45 1.30(6) . ?
C44 N6 1.48(6) . ?
C45 C46 1.66(8) . ?
N6 O11 1.206(14) . ?
N6 O10 1.21(4) . ?
C40' O7' 1.31(5) . ?
C40' C41' 1.53(4) . ?
C41' C46' 1.35(8) . ?
C41' C42' 1.37(5) . ?
C42' C43' 1.37(4) . ?
C43' C44' 1.34(6) . ?
C44' C45' 1.44(5) . ?
C44' N6' 1.46(4) . ?
C45' C46' 1.13(8) . ?
N6' O10' 1.193(19) . ?
N6' O11' 1.205(19) . ?
Ni2 N4 1.983(7) . ?
Ni2 O2 1.991(6) . ?
Ni2 O6 2.046(6) . ?
Ni2 O3 2.099(5) . ?
Ni2 N3 2.135(8) . ?
Ni2 O1 2.161(6) . ?
O6 C33 1.274(10) . ?
C33 O5 1.212(10) . ?
C33 C34 1.508(12) . ?
C34 C39 1.374(12) . ?
C34 C35 1.394(13) . ?
C35 C36 1.373(14) . ?
C36 C37 1.369(15) . ?
C37 C38 1.366(16) . ?
C37 N5 1.486(14) . ?
C38 C39 1.383(13) . ?
N5 O9 1.180(15) . ?
N5 O8 1.204(16) . ?
O1 C16 1.305(10) . ?
C16 C7 1.385(12) . ?
C16 C15 1.412(13) . ?
C15 C14 1.346(14) . ?
C14 C13 1.381(15) . ?
C13 C12 1.427(14) . ?
C13 C8 1.434(14) . ?
C12 C11 1.351(17) . ?
C11 C10 1.362(18) . ?
C10 C9 1.397(15) . ?
C9 C8 1.378(14) . ?
C8 C7 1.449(13) . ?
C7 C6 1.441(13) . ?
C6 N2 1.288(12) . ?
N2 C5 1.459(11) . ?
C5 C4 1.516(16) . ?
C4 C3 1.494(15) . ?
C3 N1 1.478(12) . ?
N1 C2 1.476(13) . ?
N1 C1 1.476(12) . ?
O2 C32 1.296(10) . ?
C32 C23 1.393(12) . ?
C32 C31 1.429(13) . ?
C31 C30 1.377(14) . ?
C30 C29 1.385(15) . ?
C29 C24 1.411(14) . ?
C29 C28 1.437(15) . ?
C28 C27 1.337(17) . ?
C27 C26 1.387(18) . ?
C26 C25 1.348(15) . ?
C25 C24 1.413(14) . ?
C24 C23 1.455(13) . ?
C23 C22 1.437(13) . ?
C22 N4 1.286(11) . ?
N4 C21 1.455(12) . ?
C21 C20 1.513(16) . ?
C20 C19 1.502(15) . ?
C19 N3 1.489(13) . ?
N3 C17 1.471(12) . ?
N3 C18 1.482(12) . ?
O1S C2S 1.25(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
N2 Ni1 O1 89.6(3) . . ?
N2 Ni1 O4 98.5(3) . . ?
O1 Ni1 O4 166.4(3) . . ?
N2 Ni1 O3 169.0(3) . . ?
O1 Ni1 O3 80.2(2) . . ?
O4 Ni1 O3 90.7(3) . . ?
N2 Ni1 N1 87.7(3) . . ?
O1 Ni1 N1 100.9(3) . . ?
O4 Ni1 N1 90.4(3) . . ?
O3 Ni1 N1 98.1(3) . . ?
N2 Ni1 O2 98.2(3) . . ?
O1 Ni1 O2 79.2(2) . . ?
O4 Ni1 O2 88.9(2) . . ?
O3 Ni1 O2 76.0(2) . . ?
N1 Ni1 O2 174.1(3) . . ?
N2 Ni1 Ni2 122.3(2) . . ?
O1 Ni1 Ni2 49.16(18) . . ?
O4 Ni1 Ni2 117.4(2) . . ?
O3 Ni1 Ni2 47.27(15) . . ?
N1 Ni1 Ni2 131.8(2) . . ?
O2 Ni1 Ni2 44.24(15) . . ?
C40 O4 Ni1 123(3) . . ?
O7 C40 O4 136(6) . . ?
O7 C40 C41 109(6) . . ?
O4 C40 C41 115(5) . . ?
C42 C41 C46 123(4) . . ?
C42 C41 C40 128(4) . . ?
C46 C41 C40 108(5) . . ?
C41 C42 C43 128(3) . . ?
C44 C43 C42 114(3) . . ?
C45 C44 C43 128(5) . . ?
C45 C44 N6 113(4) . . ?
C43 C44 N6 119(4) . . ?
C44 C45 C46 119(5) . . ?
C41 C46 C45 107(5) . . ?
O11 N6 O10 123(3) . . ?
O11 N6 C44 116(3) . . ?
O10 N6 C44 121(3) . . ?
O7' C40' C41' 121(2) . . ?
C46' C41' C42' 106(4) . . ?
C46' C41' C40' 130(4) . . ?
C42' C41' C40' 123(3) . . ?
C41' C42' C43' 126(3) . . ?
C44' C43' C42' 115(3) . . ?
C43' C44' C45' 120(3) . . ?
C43' C44' N6' 118(3) . . ?
C45' C44' N6' 121(5) . . ?
C46' C45' C44' 113(6) . . ?
C45' C46' C41' 139(6) . . ?
O10' N6' O11' 126(3) . . ?
O10' N6' C44' 118(3) . . ?
O11' N6' C44' 115(3) . . ?
N4 Ni2 O2 89.6(3) . . ?
N4 Ni2 O6 99.0(3) . . ?
O2 Ni2 O6 164.5(3) . . ?
N4 Ni2 O3 168.3(3) . . ?
O2 Ni2 O3 79.1(2) . . ?
O6 Ni2 O3 91.3(2) . . ?
N4 Ni2 N3 87.7(3) . . ?
O2 Ni2 N3 102.0(3) . . ?
O6 Ni2 N3 91.3(3) . . ?
O3 Ni2 N3 97.7(3) . . ?
N4 Ni2 O1 98.5(3) . . ?
O2 Ni2 O1 79.2(2) . . ?
O6 Ni2 O1 86.8(3) . . ?
O3 Ni2 O1 76.3(2) . . ?
N3 Ni2 O1 173.7(3) . . ?
N4 Ni2 Ni1 122.5(2) . . ?
O2 Ni2 Ni1 48.88(17) . . ?
O6 Ni2 Ni1 115.91(19) . . ?
O3 Ni2 Ni1 46.76(16) . . ?
N3 Ni2 Ni1 132.1(2) . . ?
O1 Ni2 Ni1 44.59(16) . . ?
C33 O6 Ni2 124.7(6) . . ?
O5 C33 O6 127.7(9) . . ?
O5 C33 C34 118.5(8) . . ?
O6 C33 C34 113.9(8) . . ?
C39 C34 C35 119.4(9) . . ?
C39 C34 C33 122.6(8) . . ?
C35 C34 C33 117.9(9) . . ?
C36 C35 C34 120.2(10) . . ?
C37 C36 C35 118.5(10) . . ?
C38 C37 C36 123.2(10) . . ?
C38 C37 N5 119.2(12) . . ?
C36 C37 N5 117.6(12) . . ?
C37 C38 C39 117.6(10) . . ?
C34 C39 C38 121.1(10) . . ?
O9 N5 O8 123.5(14) . . ?
O9 N5 C37 117.6(14) . . ?
O8 N5 C37 118.8(14) . . ?
Ni1 O3 Ni2 86.0(2) . . ?
C16 O1 Ni1 129.3(6) . . ?
C16 O1 Ni2 120.8(5) . . ?
Ni1 O1 Ni2 86.3(2) . . ?
O1 C16 C7 124.1(8) . . ?
O1 C16 C15 116.7(9) . . ?
C7 C16 C15 119.2(9) . . ?
C14 C15 C16 121.4(11) . . ?
C15 C14 C13 121.7(10) . . ?
C14 C13 C12 122.4(11) . . ?
C14 C13 C8 119.9(9) . . ?
C12 C13 C8 117.5(11) . . ?
C11 C12 C13 123.1(12) . . ?
C12 C11 C10 118.3(12) . . ?
C11 C10 C9 121.9(14) . . ?
C8 C9 C10 121.1(12) . . ?
C9 C8 C13 117.9(10) . . ?
C9 C8 C7 124.7(10) . . ?
C13 C8 C7 117.4(9) . . ?
C16 C7 C6 121.4(8) . . ?
C16 C7 C8 120.3(8) . . ?
C6 C7 C8 117.8(9) . . ?
N2 C6 C7 128.9(10) . . ?
C6 N2 C5 116.5(9) . . ?
C6 N2 Ni1 125.7(7) . . ?
C5 N2 Ni1 116.0(6) . . ?
N2 C5 C4 109.6(9) . . ?
C3 C4 C5 116.5(10) . . ?
N1 C3 C4 116.4(8) . . ?
C2 N1 C1 108.2(9) . . ?
C2 N1 C3 106.3(8) . . ?
C1 N1 C3 111.0(8) . . ?
C2 N1 Ni1 111.4(7) . . ?
C1 N1 Ni1 108.7(6) . . ?
C3 N1 Ni1 111.2(7) . . ?
C32 O2 Ni2 128.6(5) . . ?
C32 O2 Ni1 123.1(5) . . ?
Ni2 O2 Ni1 86.9(2) . . ?
O2 C32 C23 125.8(8) . . ?
O2 C32 C31 115.2(8) . . ?
C23 C32 C31 118.9(9) . . ?
C30 C31 C32 120.7(10) . . ?
C31 C30 C29 121.1(10) . . ?
C30 C29 C24 120.9(10) . . ?
C30 C29 C28 121.4(11) . . ?
C24 C29 C28 117.8(11) . . ?
C27 C28 C29 121.5(13) . . ?
C28 C27 C26 120.1(12) . . ?
C25 C26 C27 121.0(13) . . ?
C26 C25 C24 121.2(12) . . ?
C29 C24 C25 118.4(10) . . ?
C29 C24 C23 117.9(9) . . ?
C25 C24 C23 123.6(10) . . ?
C32 C23 C22 121.3(8) . . ?
C32 C23 C24 120.4(9) . . ?
C22 C23 C24 118.2(8) . . ?
N4 C22 C23 127.7(9) . . ?
C22 N4 C21 116.6(8) . . ?
C22 N4 Ni2 126.7(6) . . ?
C21 N4 Ni2 115.1(6) . . ?
N4 C21 C20 109.4(9) . . ?
C19 C20 C21 117.6(10) . . ?
N3 C19 C20 117.3(10) . . ?
C17 N3 C18 109.0(8) . . ?
C17 N3 C19 110.3(8) . . ?
C18 N3 C19 105.6(9) . . ?
C17 N3 Ni2 110.3(7) . . ?
C18 N3 Ni2 110.9(6) . . ?
C19 N3 Ni2 110.7(6) . . ?

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
Ni1 O4 C40 O7 7.3(7) . . . . ?
Ni1 O4 C40 C41 -175.4(16) . . . . ?
O7 C40 C41 C42 -12(4) . . . . ?
O4 C40 C41 C42 170(3) . . . . ?
O7 C40 C41 C46 -180(3) . . . . ?
O4 C40 C41 C46 2(3) . . . . ?
C46 C41 C42 C43 -14(6) . . . . ?
C40 C41 C42 C43 -180(3) . . . . ?
C41 C42 C43 C44 10(5) . . . . ?
C42 C43 C44 C45 -5(6) . . . . ?
C42 C43 C44 N6 178(3) . . . . ?
C43 C44 C45 C46 3(7) . . . . ?
N6 C44 C45 C46 -179(3) . . . . ?
C42 C41 C46 C45 9(6) . . . . ?
C40 C41 C46 C45 178(3) . . . . ?
C44 C45 C46 C41 -4(6) . . . . ?
C45 C44 N6 O11 -177(4) . . . . ?
C43 C44 N6 O11 0(5) . . . . ?
C45 C44 N6 O10 -1(6) . . . . ?
C43 C44 N6 O10 177(4) . . . . ?
O7' C40' C41' C46' 174(3) . . . . ?
O7' C40' C41' C42' 0(3) . . . . ?
C46' C41' C42' C43' 3(5) . . . . ?
C40' C41' C42' C43' 178(3) . . . . ?
C41' C42' C43' C44' -6(5) . . . . ?
C42' C43' C44' C45' 9(4) . . . . ?
C42' C43' C44' N6' 179(3) . . . . ?
C43' C44' C45' C46' -9(5) . . . . ?
N6' C44' C45' C46' -180(4) . . . . ?
C44' C45' C46' C41' 8(8) . . . . ?
C42' C41' C46' C45' -5(8) . . . . ?
C40' C41' C46' C45' -179(5) . . . . ?
C43' C44' N6' O10' -172(4) . . . . ?
C45' C44' N6' O10' -1(5) . . . . ?
C43' C44' N6' O11' 16(4) . . . . ?
C45' C44' N6' O11' -173(3) . . . . ?
Ni2 O6 C33 O5 23.1(14) . . . . ?
Ni2 O6 C33 C34 -157.9(6) . . . . ?
O5 C33 C34 C39 168.2(10) . . . . ?
O6 C33 C34 C39 -10.9(13) . . . . ?
O5 C33 C34 C35 -8.8(14) . . . . ?
O6 C33 C34 C35 172.1(9) . . . . ?
C39 C34 C35 C36 0.5(16) . . . . ?
C33 C34 C35 C36 177.6(9) . . . . ?
C34 C35 C36 C37 -1.9(17) . . . . ?
C35 C36 C37 C38 2.4(19) . . . . ?
C35 C36 C37 N5 -179.5(11) . . . . ?
C36 C37 C38 C39 -1.5(19) . . . . ?
N5 C37 C38 C39 -179.5(11) . . . . ?
C35 C34 C39 C38 0.5(16) . . . . ?
C33 C34 C39 C38 -176.5(10) . . . . ?
C37 C38 C39 C34 0.0(17) . . . . ?
C38 C37 N5 O9 -1(2) . . . . ?
C36 C37 N5 O9 -179.5(15) . . . . ?
C38 C37 N5 O8 -178.1(15) . . . . ?
C36 C37 N5 O8 4(2) . . . . ?
Ni1 O1 C16 C7 3.7(13) . . . . ?
Ni2 O1 C16 C7 116.7(8) . . . . ?
Ni1 O1 C16 C15 -175.8(6) . . . . ?
Ni2 O1 C16 C15 -62.9(10) . . . . ?
O1 C16 C15 C14 -176.9(9) . . . . ?
C7 C16 C15 C14 3.6(15) . . . . ?
C16 C15 C14 C13 -3.3(16) . . . . ?
C15 C14 C13 C12 176.4(10) . . . . ?
C15 C14 C13 C8 1.5(16) . . . . ?
C14 C13 C12 C11 -178.4(11) . . . . ?
C8 C13 C12 C11 -3.4(17) . . . . ?
C13 C12 C11 C10 1.4(19) . . . . ?
C12 C11 C10 C9 -1(2) . . . . ?
C11 C10 C9 C8 4(2) . . . . ?
C10 C9 C8 C13 -5.5(16) . . . . ?
C10 C9 C8 C7 175.1(10) . . . . ?
C14 C13 C8 C9 -179.6(10) . . . . ?
C12 C13 C8 C9 5.3(14) . . . . ?
C14 C13 C8 C7 -0.1(14) . . . . ?
C12 C13 C8 C7 -175.2(9) . . . . ?
O1 C16 C7 C6 6.5(14) . . . . ?
C15 C16 C7 C6 -174.0(9) . . . . ?
O1 C16 C7 C8 178.3(8) . . . . ?
C15 C16 C7 C8 -2.2(13) . . . . ?
C9 C8 C7 C16 180.0(9) . . . . ?
C13 C8 C7 C16 0.5(13) . . . . ?
C9 C8 C7 C6 -7.9(14) . . . . ?
C13 C8 C7 C6 172.6(9) . . . . ?
C16 C7 C6 N2 -10.8(16) . . . . ?
C8 C7 C6 N2 177.2(10) . . . . ?
C7 C6 N2 C5 168.0(10) . . . . ?
C7 C6 N2 Ni1 3.8(15) . . . . ?
C6 N2 C5 C4 -95.7(11) . . . . ?
Ni1 N2 C5 C4 70.0(10) . . . . ?
N2 C5 C4 C3 -61.9(13) . . . . ?
C5 C4 C3 N1 60.5(15) . . . . ?
C4 C3 N1 C2 -179.5(10) . . . . ?
C4 C3 N1 C1 63.0(13) . . . . ?
C4 C3 N1 Ni1 -58.1(11) . . . . ?
Ni2 O2 C32 C23 4.6(13) . . . . ?
Ni1 O2 C32 C23 120.5(8) . . . . ?
Ni2 O2 C32 C31 -179.1(7) . . . . ?
Ni1 O2 C32 C31 -63.1(10) . . . . ?
O2 C32 C31 C30 -176.9(9) . . . . ?
C23 C32 C31 C30 -0.3(15) . . . . ?
C32 C31 C30 C29 -0.3(17) . . . . ?
C31 C30 C29 C24 -0.8(17) . . . . ?
C31 C30 C29 C28 179.1(11) . . . . ?
C30 C29 C28 C27 -177.7(11) . . . . ?
C24 C29 C28 C27 2.2(17) . . . . ?
C29 C28 C27 C26 -2.5(19) . . . . ?
C28 C27 C26 C25 1(2) . . . . ?
C27 C26 C25 C24 0.5(19) . . . . ?
C30 C29 C24 C25 179.3(10) . . . . ?
C28 C29 C24 C25 -0.6(15) . . . . ?
C30 C29 C24 C23 2.4(15) . . . . ?
C28 C29 C24 C23 -177.6(9) . . . . ?
C26 C25 C24 C29 -0.7(16) . . . . ?
C26 C25 C24 C23 176.1(11) . . . . ?
O2 C32 C23 C22 1.1(15) . . . . ?
C31 C32 C23 C22 -175.1(10) . . . . ?
O2 C32 C23 C24 178.2(8) . . . . ?
C31 C32 C23 C24 2.0(14) . . . . ?
C29 C24 C23 C32 -3.0(14) . . . . ?
C25 C24 C23 C32 -179.7(9) . . . . ?
C29 C24 C23 C22 174.2(9) . . . . ?
C25 C24 C23 C22 -2.5(15) . . . . ?
C32 C23 C22 N4 -5.5(16) . . . . ?
C24 C23 C22 N4 177.4(9) . . . . ?
C23 C22 N4 C21 168.2(10) . . . . ?
C23 C22 N4 Ni2 3.6(15) . . . . ?
C22 N4 C21 C20 -95.5(11) . . . . ?
Ni2 N4 C21 C20 70.9(10) . . . . ?
N4 C21 C20 C19 -60.2(14) . . . . ?
C21 C20 C19 N3 57.3(15) . . . . ?
C20 C19 N3 C17 65.8(13) . . . . ?
C20 C19 N3 C18 -176.5(10) . . . . ?
C20 C19 N3 Ni2 -56.4(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S O7 0.82 2.21 2.81(4) 130 1_656
O1S H1S O7' 0.82 2.15 2.72(4) 127.3 1_656
C2S H2S3 O10' 0.96 2.55 3.46(5) 159.4 3_656
C38 H38 O11 0.93 2.42 3.25(3) 147.2 2
C38 H38 O11' 0.93 2.52 3.24(3) 135.2 2
O3 H3A O7 0.97 1.73 2.57(4) 142.5 .
O3 H3A O7' 0.97 1.76 2.60(3) 142.9 .
O3 H3B O5 0.97 1.69 2.530(9) 142.1 .
C5 H5A O4 0.97 2.56 3.117(13) 116.6 .
C3 H3D O4 0.97 2.56 3.087(14) 114.5 .
C3 H3D O11 0.97 2.46 3.25(2) 138.2 3
C3 H3D O11' 0.97 2.57 3.40(3) 143.9 3
C1 H1B O1 0.96 2.58 3.092(13) 113.5 .
C1 H1C O1S 0.96 2.62 3.570(19) 169 1_554
C21 H21A O6 0.97 2.54 3.112(12) 117.7 .
C21 H21B O5 0.97 2.39 3.343(13) 167.8 4_566
C20 H20B O1S 0.97 2.55 3.38(2) 144.2 4_465
C19 H19B O6 0.97 2.58 3.099(14) 113.5 .
O1S H1S O7 0.82 2.21 2.81(4) 130 1_656
O1S H1S O7' 0.82 2.15 2.72(4) 127.3 1_656
C2S H2S3 O10' 0.96 2.55 3.46(5) 159.4 3_656


# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 963145'
#\#CIF_1.1

#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2014-01-29 at 13:34:12
#  Using CIFtbx version 3.0.4  1 Sep 2006

#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.4.3
#  Request file    : c:\wingx\files\archive.reqdat
#  CIF files read  : agrb56_0m project

#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------#

data_global

#------------------ AUDIT DETAILS -------------------------------------------#

_audit_creation_date             2014-01-29
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record             ?

#------------------ AUTHOR DETAILS -------------------------------------------#

# Name and address of author for correspondence

_publ_contact_author_name        "Barceló-Oliver, Miquel"
_publ_contact_author_address     
;
Universitat de les Illes Balears; Department of Chemistry
campus UIB; ctra. Valldemossa km 7.5; Ed. Mateu Orfila i Rotger
E-07122 Palma de Mallorca; Spain
;
_publ_contact_author_email       miquel.barcelo@uib.es
_publ_contact_author_fax         '(+34) 971.173.426'
_publ_contact_author_phone       '(+34) 971.173.199'


# Insert blank lines between references

_publ_section_references         
;
Blessing, R. H. (1995) Acta Cryst., A51, 33-38.
 
Blessing, R. H. (1987) Cryst. Rev. 1, 3-58.
 
Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397.
 
Bruker (2012) APEX2 (Version 2012.10-0), SAINT (version 8.27B), SADABS
(version 2012/1), BrukerAXS Inc, Madison, Wisconsin, USA.
 
ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan.
 
CAD-4 Software: Enraf-Nonius (1989). CAD-4 Software (or CAD-4 EXPRESS).
Enraf-Nonius, Delft, The Netherlands.
 
Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388.
 
CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON.
Chemical Crystallography Laboratory, Oxford, England.
 
CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006).
Program name(s). Oxford Diffraction Ltd, Abingdon, England.
 
CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. &
Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487.
 
COLLECT: Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands.
 
DENZO/SCALEPACK:  Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology,
Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr
& R. M. Sweet, pp. 307-326. New York: Academic Press.
 
DIAMOND: Brandenburg, K.(2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
 
DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt,
Germany.
 
DIFABS: Walker, N. &  Stuart, D. (1983). Acta Cryst., A39, 158 - 166.
 
DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96.
 
DIRDIF-2008: Beurskens, P.T., Beurskens, G., de Gelder, R., Garciía-Granda,
S., Gould, R.O. & Smits, J.M.M. (2008) The DIRDIF-2008 program
system, Crystallography Laboratory, Radboud University  Nijmegen,
The Netherlands.
 
EDMA: Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012) J. Appl. Cryst.
45, 575-580.
 
enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler,
M. (2004). J. Appl. Cryst. 37, 335-338.
 
EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs,
A. M. M. (2003). J. Appl. Cryst. 36, 220-229.
 
JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics,
Czech Academy of Sciences, Prague, Czech Republic.
 
MERCURY: Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington,
P. R., McCabe, P., Pidcock, E., Rodriguez-Monge, L., Taylor, R.,
van de Streek, J. & Wood, P. A. (2008). J. Appl. Cryst. 41, 466-470.
 
MOGUL: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell,
W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris,
S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144.
 
ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge
National Laboratory, Tennessee, USA.
 
ORTEPIII:  Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII.
Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA.
 
ORTEP-3: Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
 
PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659.
 
PLATON: Spek, A. L. (2009). Acta. Cryst. D65, 148-155.
 
PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan.
 
PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan.
 
PublCIF: Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.
 
SCHAKAL: Keller, E. (1999) University of Freiburg, Germany.
 
SHELX: Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
 
SHELXD: Schneider, T. R. & Sheldrick, G. M. (2002) Acta Cryst. D58, 1772-1779.
 
SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla,
M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
 
SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L.,
Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. &
Spagna, R. (1999). J. Appl. Cryst. 32, 115-119.
 
SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L.,
Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103.
 
SIR2004: Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G. & Spagna, R.
(2005). J. Appl. Cryst. 38, 381-388.
 
SIR2008 & IL MILIONE: Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D.,
& Spagna, R. (2007). J. Appl. Cryst. 40, 609-613.
 
SIR2011: Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B.,
Cascarano, G. L., Giacovazzo, C., Mallamo, M., Mazzone, A., Polidori, G.
& Spagna, R. (2012). J. Appl. Cryst. 45, 357-361.
 
SUPERFLIP: Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790.
 
TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC,
The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan.
 
WinGX: Farrugia, L. J. (2012). J. Appl. Cryst. 45, 849-854.
 
X-AREA, X-RED, X-RED32, X-SHAPE:  Stoe & Cie (2002). Program name(s).
Stoe & Cie GmbH, Darmstadt, Germany.
 
XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany.
 
XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc.,
Madison, Wisconsin, USA.
 
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_3

_audit_creation_date             2014-01-29T13:34:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category         FM

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C60 H54 N8 Ni3 O18, C2 H6 O'
_chemical_formula_sum            'C62 H60 N8 Ni3 O19'
_chemical_formula_weight         1397.31

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
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                   12.597(5)
_cell_length_b                   20.605(5)
_cell_length_c                   14.151(5)
_cell_angle_alpha                90
_cell_angle_beta                 108.141(5)
_cell_angle_gamma                90
_cell_volume                     3490(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14920
_cell_measurement_theta_min      1.701
_cell_measurement_theta_max      25.04
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.9021
_exptl_absorpt_correction_T_max  0.9493
_exptl_absorpt_process_details   
;
"SADABS v.2.10 (Bruker,2003) was used for absorption correction."
;

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_number            14920
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.701
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.944
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.944
_reflns_number_total             5823
_reflns_number_gt                4285
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0783P)²+20.7700P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5823
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.101
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.2255
_refine_ls_wR_factor_gt          0.2009
_refine_ls_goodness_of_fit_ref   1.1
_refine_ls_restrained_S_all      1.1
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.1
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.12

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.5 0 0.5 0.0342(3) Uani 1 d . .
Ni1 Ni 0.55927(7) 0.11594(4) 0.64052(6) 0.0350(3) Uani 1 d . .
N1 N 0.3097(9) 0.1988(4) 0.0470(6) 0.075(2) Uani 1 d . .
O5 O 0.6481(4) -0.0234(2) 0.6012(3) 0.0415(11) Uani 1 d . .
O7 O 0.5509(4) 0.0969(2) 0.4894(3) 0.0393(11) Uani 1 d . .
O8 O 0.4388(4) 0.1697(2) 0.5214(4) 0.0482(12) Uani 1 d . .
N2 N 1.0399(8) -0.1537(5) 0.9486(9) 0.094(3) Uani 1 d . .
O9 O 0.4494(4) 0.0409(2) 0.6111(3) 0.0377(11) Uani 1 d . .
O6 O 0.6824(4) 0.0555(2) 0.7159(4) 0.0451(12) Uani 1 d . .
O1 O 0.3640(8) 0.1780(3) -0.0053(5) 0.097(3) Uani 1 d . .
N4 N 0.5166(5) 0.1358(3) 0.7610(4) 0.0390(13) Uani 1 d . .
C26 C 0.4331(6) 0.1567(3) 0.3532(5) 0.0428(17) Uani 1 d . .
N3 N 0.6806(5) 0.1913(3) 0.6589(5) 0.0449(14) Uani 1 d . .
C7 C 0.4216(6) 0.1194(3) 0.7689(5) 0.0429(16) Uani 1 d . .
H7 H 0.408 0.1327 0.8269 0.052 Uiso 1 calc . .
C9 C 0.3532(6) 0.0419(3) 0.6292(5) 0.0376(15) Uani 1 d . .
C8 C 0.3333(6) 0.0833(3) 0.7008(5) 0.0387(15) Uani 1 d . .
C25 C 0.4738(6) 0.1403(3) 0.4599(5) 0.0388(16) Uani 1 d . .
C14 C 0.1940(7) 0.1247(4) 0.7822(6) 0.057(2) Uani 1 d . .
H14 H 0.244 0.1567 0.815 0.068 Uiso 1 calc . .
C18 C 0.6992(5) 0.0003(3) 0.6847(5) 0.0352(15) Uani 1 d . .
C27 C 0.4712(7) 0.1223(4) 0.2854(5) 0.0480(18) Uani 1 d . .
H27 H 0.5242 0.0897 0.3078 0.058 Uiso 1 calc . .
O2 O 0.2260(8) 0.2290(5) 0.0168(6) 0.109(3) Uani 1 d . .
C10 C 0.2688(7) -0.0031(4) 0.5787(6) 0.053(2) Uani 1 d . .
H10 H 0.2827 -0.0315 0.5329 0.063 Uiso 1 calc . .
C4 C 0.6618(7) 0.2187(4) 0.8252(6) 0.057(2) Uani 1 d . .
H4A H 0.7063 0.2383 0.8873 0.068 Uiso 1 calc . .
H4B H 0.6086 0.2511 0.7891 0.068 Uiso 1 calc . .
C23 C 0.8380(7) -0.0902(4) 0.7166(6) 0.055(2) Uani 1 d . .
H23 H 0.8145 -0.0994 0.6489 0.067 Uiso 1 calc . .
C13 C 0.2239(6) 0.0817(4) 0.7158(6) 0.0482(18) Uani 1 d . .
O4 O 1.0705(8) -0.1391(6) 1.0364(8) 0.134(4) Uani 1 d . .
C12 C 0.1432(6) 0.0371(4) 0.6645(6) 0.056(2) Uani 1 d . .
C19 C 0.7895(6) -0.0395(3) 0.7535(6) 0.0420(16) Uani 1 d . .
C31 C 0.3569(7) 0.2057(4) 0.3187(6) 0.055(2) Uani 1 d . .
H31 H 0.3335 0.2298 0.3642 0.066 Uiso 1 calc . .
C22 C 0.9523(7) -0.1138(4) 0.8804(7) 0.063(2) Uani 1 d . .
C24 C 0.9224(7) -0.1272(4) 0.7819(8) 0.067(2) Uani 1 d . .
H24 H 0.9574 -0.1603 0.7582 0.081 Uiso 1 calc . .
C3 C 0.7386(7) 0.2019(4) 0.7646(6) 0.054(2) Uani 1 d . .
H3A H 0.7921 0.2368 0.7712 0.065 Uiso 1 calc . .
H3B H 0.78 0.1629 0.792 0.065 Uiso 1 calc . .
C21 C 0.9064(7) -0.0645(4) 0.9191(7) 0.063(2) Uani 1 d . .
H21 H 0.9295 -0.0562 0.9871 0.076 Uiso 1 calc . .
C20 C 0.8250(7) -0.0273(4) 0.8542(6) 0.055(2) Uani 1 d . .
H20 H 0.7931 0.0068 0.879 0.067 Uiso 1 calc . .
C11 C 0.1697(7) -0.0056(4) 0.5952(7) 0.061(2) Uani 1 d . .
H11 H 0.1169 -0.0358 0.5608 0.073 Uiso 1 calc . .
C5 C 0.5987(7) 0.1629(4) 0.8485(5) 0.053(2) Uani 1 d . .
H5A H 0.6512 0.1291 0.8806 0.063 Uiso 1 calc . .
H5B H 0.561 0.1771 0.895 0.063 Uiso 1 calc . .
C30 C 0.3138(8) 0.2205(4) 0.2184(6) 0.060(2) Uani 1 d . .
H30 H 0.2606 0.2529 0.1956 0.072 Uiso 1 calc . .
C28 C 0.4309(8) 0.1360(4) 0.1863(6) 0.061(2) Uani 1 d . .
H28 H 0.4554 0.1127 0.1408 0.073 Uiso 1 calc . .
C29 C 0.3531(7) 0.1851(4) 0.1546(6) 0.055(2) Uani 1 d . .
C1 C 0.7652(8) 0.1699(5) 0.6120(7) 0.071(3) Uani 1 d . .
H1A H 0.7319 0.1689 0.5411 0.106 Uiso 1 calc . .
H1B H 0.7915 0.1273 0.6355 0.106 Uiso 1 calc . .
H1C H 0.8268 0.1997 0.6291 0.106 Uiso 1 calc . .
C17 C 0.0392(7) 0.0339(5) 0.6824(7) 0.071(3) Uani 1 d . .
H17 H -0.0139 0.0039 0.6478 0.085 Uiso 1 calc . .
O3 O 1.0760(10) -0.1986(6) 0.9159(8) 0.166(5) Uani 1 d . .
C2 C 0.6350(8) 0.2525(4) 0.6117(8) 0.071(3) Uani 1 d . .
H2A H 0.5762 0.2666 0.6367 0.106 Uiso 1 calc . .
H2B H 0.6058 0.2464 0.5411 0.106 Uiso 1 calc . .
H2C H 0.6929 0.2846 0.6264 0.106 Uiso 1 calc . .
C16 C 0.0158(8) 0.0737(5) 0.7490(8) 0.075(3) Uani 1 d . .
H16 H -0.0522 0.0704 0.7615 0.09 Uiso 1 calc . .
C15 C 0.0934(8) 0.1194(5) 0.7984(8) 0.074(3) Uani 1 d . .
H15 H 0.0765 0.1471 0.8435 0.089 Uiso 1 calc . .
O11 O 0.7495(12) 0.0476(8) 1.0882(11) 0.086(4) Uani 0.5 d . .
H11A H 0.7815 0.0711 1.1351 0.129 Uiso 0.5 calc . .
C41 C 0.628(2) 0.0446(10) 1.0781(16) 0.094(8) Uani 0.5 d . .
H41A H 0.6227 0.0323 1.1425 0.113 Uiso 0.5 calc . .
H41B H 0.5994 0.0885 1.065 0.113 Uiso 0.5 calc . .
C43 C 0.5607(18) 0.0068(9) 1.0118(15) 0.071(5) Uani 0.5 d . .
H43A H 0.5552 0.022 0.9463 0.107 Uiso 0.5 calc . .
H43B H 0.4881 0.0075 1.0205 0.107 Uiso 0.5 calc . .
H43C H 0.5892 -0.0367 1.02 0.107 Uiso 0.5 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Ni2 O5 2.025(5) 3_656 ?
Ni2 O5 2.025(5) . ?
Ni2 O9 2.052(4) . ?
Ni2 O9 2.052(4) 3_656 ?
Ni2 O7 2.116(4) . ?
Ni2 O7 2.116(4) 3_656 ?
Ni1 N4 1.984(6) . ?
Ni1 O6 2.016(5) . ?
Ni1 O9 2.029(4) . ?
Ni1 N3 2.137(6) . ?
Ni1 O7 2.144(5) . ?
Ni1 O8 2.186(5) . ?
Ni1 C25 2.496(7) . ?
N1 O2 1.184(11) . ?
N1 O1 1.230(11) . ?
N1 C29 1.475(11) . ?
O5 C18 1.255(8) . ?
O7 C25 1.291(8) . ?
O8 C25 1.248(8) . ?
N2 O3 1.187(13) . ?
N2 O4 1.218(12) . ?
N2 C22 1.471(12) . ?
O9 C9 1.315(8) . ?
O6 C18 1.261(8) . ?
N4 C7 1.282(9) . ?
N4 C5 1.455(9) . ?
C26 C31 1.373(11) . ?
C26 C27 1.393(10) . ?
C26 C25 1.475(10) . ?
N3 C2 1.458(10) . ?
N3 C3 1.461(10) . ?
N3 C1 1.486(10) . ?
C7 C8 1.432(10) . ?
C9 C8 1.405(9) . ?
C9 C10 1.424(10) . ?
C8 C13 1.459(10) . ?
C14 C15 1.361(12) . ?
C14 C13 1.424(11) . ?
C18 C19 1.492(9) . ?
C27 C28 1.364(11) . ?
C10 C11 1.340(11) . ?
C4 C5 1.492(11) . ?
C4 C3 1.519(11) . ?
C23 C19 1.392(10) . ?
C23 C24 1.397(12) . ?
C13 C12 1.395(11) . ?
C12 C17 1.411(11) . ?
C12 C11 1.431(12) . ?
C19 C20 1.377(11) . ?
C31 C30 1.387(11) . ?
C22 C24 1.354(13) . ?
C22 C21 1.365(12) . ?
C21 C20 1.377(11) . ?
C30 C29 1.368(12) . ?
C28 C29 1.382(12) . ?
C17 C16 1.350(13) . ?
C16 C15 1.380(14) . ?
O11 C41 1.49(3) . ?
C41 C43 1.31(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
O5 Ni2 O5 180.0(2) 3_656 . ?
O5 Ni2 O9 90.38(19) 3_656 . ?
O5 Ni2 O9 89.62(19) . . ?
O5 Ni2 O9 89.62(19) 3_656 3_656 ?
O5 Ni2 O9 90.38(19) . 3_656 ?
O9 Ni2 O9 180 . 3_656 ?
O5 Ni2 O7 87.62(19) 3_656 . ?
O5 Ni2 O7 92.38(19) . . ?
O9 Ni2 O7 80.77(17) . . ?
O9 Ni2 O7 99.23(17) 3_656 . ?
O5 Ni2 O7 92.38(19) 3_656 3_656 ?
O5 Ni2 O7 87.62(19) . 3_656 ?
O9 Ni2 O7 99.23(17) . 3_656 ?
O9 Ni2 O7 80.77(17) 3_656 3_656 ?
O7 Ni2 O7 180 . 3_656 ?
N4 Ni1 O6 92.4(2) . . ?
N4 Ni1 O9 89.1(2) . . ?
O6 Ni1 O9 90.06(19) . . ?
N4 Ni1 N3 96.9(2) . . ?
O6 Ni1 N3 88.9(2) . . ?
O9 Ni1 N3 174.0(2) . . ?
N4 Ni1 O7 162.3(2) . . ?
O6 Ni1 O7 101.85(19) . . ?
O9 Ni1 O7 80.61(17) . . ?
N3 Ni1 O7 93.8(2) . . ?
N4 Ni1 O8 104.4(2) . . ?
O6 Ni1 O8 162.96(19) . . ?
O9 Ni1 O8 87.82(19) . . ?
N3 Ni1 O8 91.4(2) . . ?
O7 Ni1 O8 61.13(17) . . ?
N4 Ni1 C25 133.9(2) . . ?
O6 Ni1 C25 133.0(2) . . ?
O9 Ni1 C25 83.9(2) . . ?
N3 Ni1 C25 92.4(2) . . ?
O7 Ni1 C25 31.1(2) . . ?
O8 Ni1 C25 30.0(2) . . ?
O2 N1 O1 124.4(9) . . ?
O2 N1 C29 118.4(10) . . ?
O1 N1 C29 117.2(10) . . ?
C18 O5 Ni2 131.5(4) . . ?
C25 O7 Ni2 117.6(4) . . ?
C25 O7 Ni1 89.6(4) . . ?
Ni2 O7 Ni1 91.40(17) . . ?
C25 O8 Ni1 88.9(4) . . ?
O3 N2 O4 123.5(10) . . ?
O3 N2 C22 118.8(11) . . ?
O4 N2 C22 117.7(10) . . ?
C9 O9 Ni1 124.0(4) . . ?
C9 O9 Ni2 132.9(4) . . ?
Ni1 O9 Ni2 96.65(18) . . ?
C18 O6 Ni1 123.8(4) . . ?
C7 N4 C5 117.6(6) . . ?
C7 N4 Ni1 122.0(5) . . ?
C5 N4 Ni1 119.9(5) . . ?
C31 C26 C27 118.8(7) . . ?
C31 C26 C25 120.9(7) . . ?
C27 C26 C25 120.2(7) . . ?
C2 N3 C3 109.9(6) . . ?
C2 N3 C1 106.7(7) . . ?
C3 N3 C1 107.6(6) . . ?
C2 N3 Ni1 114.0(5) . . ?
C3 N3 Ni1 110.1(5) . . ?
C1 N3 Ni1 108.4(5) . . ?
N4 C7 C8 129.0(6) . . ?
O9 C9 C8 122.2(6) . . ?
O9 C9 C10 118.8(6) . . ?
C8 C9 C10 118.9(6) . . ?
C9 C8 C7 121.7(6) . . ?
C9 C8 C13 118.7(6) . . ?
C7 C8 C13 119.0(6) . . ?
O8 C25 O7 120.3(6) . . ?
O8 C25 C26 121.1(6) . . ?
O7 C25 C26 118.5(6) . . ?
O8 C25 Ni1 61.1(4) . . ?
O7 C25 Ni1 59.2(3) . . ?
C26 C25 Ni1 175.0(5) . . ?
C15 C14 C13 120.8(9) . . ?
O5 C18 O6 126.0(6) . . ?
O5 C18 C19 117.7(6) . . ?
O6 C18 C19 116.4(6) . . ?
C28 C27 C26 120.3(8) . . ?
C11 C10 C9 121.9(7) . . ?
C5 C4 C3 115.1(7) . . ?
C19 C23 C24 119.5(8) . . ?
C12 C13 C14 117.0(7) . . ?
C12 C13 C8 120.5(7) . . ?
C14 C13 C8 122.5(7) . . ?
C13 C12 C17 120.3(8) . . ?
C13 C12 C11 118.3(7) . . ?
C17 C12 C11 121.5(8) . . ?
C20 C19 C23 119.1(7) . . ?
C20 C19 C18 120.7(6) . . ?
C23 C19 C18 120.2(7) . . ?
C26 C31 C30 122.2(8) . . ?
C24 C22 C21 123.2(8) . . ?
C24 C22 N2 118.2(9) . . ?
C21 C22 N2 118.6(9) . . ?
C22 C24 C23 118.7(8) . . ?
N3 C3 C4 114.1(7) . . ?
C22 C21 C20 117.9(8) . . ?
C21 C20 C19 121.5(8) . . ?
C10 C11 C12 121.6(8) . . ?
N4 C5 C4 113.3(6) . . ?
C29 C30 C31 116.9(8) . . ?
C27 C28 C29 119.0(8) . . ?
C30 C29 C28 122.7(8) . . ?
C30 C29 N1 119.0(9) . . ?
C28 C29 N1 118.2(8) . . ?
C16 C17 C12 120.9(9) . . ?
C17 C16 C15 119.6(8) . . ?
C14 C15 C16 121.3(9) . . ?
C43 C41 O11 120.9(18) . . ?

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
C5 N4 C7 C8 -169.7(7) . . . . ?
Ni1 N4 C7 C8 3.0(11) . . . . ?
Ni1 O9 C9 C8 -23.3(9) . . . . ?
Ni2 O9 C9 C8 -168.2(5) . . . . ?
Ni1 O9 C9 C10 160.4(5) . . . . ?
Ni2 O9 C9 C10 15.5(9) . . . . ?
O9 C9 C8 C7 -9.9(11) . . . . ?
C10 C9 C8 C7 166.4(7) . . . . ?
O9 C9 C8 C13 179.5(6) . . . . ?
C10 C9 C8 C13 -4.2(10) . . . . ?
N4 C7 C8 C9 21.9(12) . . . . ?
N4 C7 C8 C13 -167.5(7) . . . . ?
Ni1 O8 C25 O7 1.9(6) . . . . ?
Ni1 O8 C25 C26 -174.8(6) . . . . ?
Ni2 O7 C25 O8 89.5(7) . . . . ?
Ni1 O7 C25 O8 -1.9(6) . . . . ?
Ni2 O7 C25 C26 -93.8(6) . . . . ?
Ni1 O7 C25 C26 174.8(5) . . . . ?
Ni2 O7 C25 Ni1 91.4(3) . . . . ?
C31 C26 C25 O8 1.3(10) . . . . ?
C27 C26 C25 O8 -178.3(7) . . . . ?
C31 C26 C25 O7 -175.5(7) . . . . ?
C27 C26 C25 O7 4.9(10) . . . . ?
Ni2 O5 C18 O6 -18.7(10) . . . . ?
Ni2 O5 C18 C19 162.4(4) . . . . ?
Ni1 O6 C18 O5 5.0(10) . . . . ?
Ni1 O6 C18 C19 -176.1(4) . . . . ?
C31 C26 C27 C28 -1.7(11) . . . . ?
C25 C26 C27 C28 177.9(7) . . . . ?
O9 C9 C10 C11 178.6(8) . . . . ?
C8 C9 C10 C11 2.2(12) . . . . ?
C15 C14 C13 C12 3.6(13) . . . . ?
C15 C14 C13 C8 -176.4(8) . . . . ?
C9 C8 C13 C12 4.0(11) . . . . ?
C7 C8 C13 C12 -166.8(7) . . . . ?
C9 C8 C13 C14 -176.0(7) . . . . ?
C7 C8 C13 C14 13.2(11) . . . . ?
C14 C13 C12 C17 -2.7(12) . . . . ?
C8 C13 C12 C17 177.3(8) . . . . ?
C14 C13 C12 C11 178.4(8) . . . . ?
C8 C13 C12 C11 -1.6(12) . . . . ?
C24 C23 C19 C20 -0.8(12) . . . . ?
C24 C23 C19 C18 -179.9(7) . . . . ?
O5 C18 C19 C20 -159.7(7) . . . . ?
O6 C18 C19 C20 21.3(10) . . . . ?
O5 C18 C19 C23 19.4(10) . . . . ?
O6 C18 C19 C23 -159.6(7) . . . . ?
C27 C26 C31 C30 2.3(12) . . . . ?
C25 C26 C31 C30 -177.3(7) . . . . ?
O3 N2 C22 C24 -4.9(17) . . . . ?
O4 N2 C22 C24 176.1(11) . . . . ?
O3 N2 C22 C21 176.2(12) . . . . ?
O4 N2 C22 C21 -2.8(16) . . . . ?
C21 C22 C24 C23 -2.1(15) . . . . ?
N2 C22 C24 C23 179.1(9) . . . . ?
C19 C23 C24 C22 2.1(13) . . . . ?
C2 N3 C3 C4 69.0(8) . . . . ?
C1 N3 C3 C4 -175.2(7) . . . . ?
Ni1 N3 C3 C4 -57.3(7) . . . . ?
C5 C4 C3 N3 76.4(9) . . . . ?
C24 C22 C21 C20 0.8(15) . . . . ?
N2 C22 C21 C20 179.6(9) . . . . ?
C22 C21 C20 C19 0.6(14) . . . . ?
C23 C19 C20 C21 -0.6(12) . . . . ?
C18 C19 C20 C21 178.5(8) . . . . ?
C9 C10 C11 C12 0.2(14) . . . . ?
C13 C12 C11 C10 -0.5(14) . . . . ?
C17 C12 C11 C10 -179.4(9) . . . . ?
C7 N4 C5 C4 -139.2(7) . . . . ?
Ni1 N4 C5 C4 47.9(9) . . . . ?
C3 C4 C5 N4 -66.9(10) . . . . ?
C26 C31 C30 C29 -1.9(13) . . . . ?
C26 C27 C28 C29 0.9(12) . . . . ?
C31 C30 C29 C28 1.0(13) . . . . ?
C31 C30 C29 N1 179.8(7) . . . . ?
C27 C28 C29 C30 -0.5(13) . . . . ?
C27 C28 C29 N1 -179.4(7) . . . . ?
O2 N1 C29 C30 -16.5(13) . . . . ?
O1 N1 C29 C30 163.1(8) . . . . ?
O2 N1 C29 C28 162.4(9) . . . . ?
O1 N1 C29 C28 -18.0(12) . . . . ?
C13 C12 C17 C16 0.1(15) . . . . ?
C11 C12 C17 C16 179.0(10) . . . . ?
C12 C17 C16 C15 1.7(16) . . . . ?
C13 C14 C15 C16 -1.9(15) . . . . ?
C17 C16 C15 C14 -0.9(16) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C10 H10 O5 0.93 2.58 3.088(9) 114.6 3_656
C10 H10 O7 0.93 2.59 3.345(9) 138.4 3_656
C3 H3B O6 0.97 2.6 3.126(9) 114.4 .
C3 H3B O4 0.97 2.61 3.342(12) 132 3_757
C1 H1A O7 0.96 2.63 3.106(10) 111.2 .
C1 H1B O6 0.96 2.52 3.125(10) 121.1 .
C1 H1C O3 0.96 2.6 3.462(12) 149.1 2_756


# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 963146'
