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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H46 Mn3 N4 O22, C12 H10 N4'
_chemical_formula_sum            'C66 H56 Mn3 N8 O22'
_chemical_formula_weight         1478.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   16.899(3)
_cell_length_b                   11.245(2)
_cell_length_c                   18.736(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.504(3)
_cell_angle_gamma                90.00
_cell_volume                     3213.4(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5905
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      28.19

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1518
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7623
_exptl_absorpt_correction_T_max  0.8509
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16066
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5659
_reflns_number_gt                4598
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0800P)²+2.7743P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5659
_refine_ls_number_parameters     469
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1321
_refine_ls_wR_factor_gt          0.1197
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.61933(3) 0.69491(4) 0.18318(2) 0.02744(14) Uani 1 1 d . . .
Mn2 Mn 0.5000 0.5000 0.0000 0.02797(17) Uani 1 2 d S . .
C1 C 0.5411(2) 0.5288(3) 0.27150(18) 0.0322(7) Uani 1 1 d . . .
C2 C 0.48051(19) 0.5157(3) 0.31130(17) 0.0300(6) Uani 1 1 d . . .
C3 C 0.4685(2) 0.4053(3) 0.33740(19) 0.0358(7) Uani 1 1 d . . .
H3 H 0.5002 0.3401 0.3334 0.043 Uiso 1 1 calc R . .
C4 C 0.4089(2) 0.3926(3) 0.3696(2) 0.0388(7) Uani 1 1 d . . .
C5 C 0.3597(2) 0.4875(3) 0.3745(2) 0.0421(8) Uani 1 1 d . . .
H5 H 0.3184 0.4778 0.3945 0.051 Uiso 1 1 calc R . .
C6 C 0.3737(2) 0.5973(3) 0.3490(2) 0.0408(8) Uani 1 1 d . . .
C7 C 0.4339(2) 0.6129(3) 0.31781(19) 0.0364(7) Uani 1 1 d . . .
H7 H 0.4429 0.6877 0.3015 0.044 Uiso 1 1 calc R . .
C8 C 0.3425(3) 0.2540(3) 0.4253(2) 0.0507(9) Uani 1 1 d . . .
C9 C 0.2652(3) 0.1984(3) 0.3799(2) 0.0556(10) Uani 1 1 d . . .
H9 H 0.2476 0.1880 0.3260 0.067 Uiso 1 1 calc R . .
C10 C 0.2132(2) 0.1574(3) 0.4157(2) 0.0479(8) Uani 1 1 d . . .
H10 H 0.1603 0.1197 0.3854 0.057 Uiso 1 1 calc R . .
C11 C 0.2400(2) 0.1726(3) 0.49647(18) 0.0359(7) Uani 1 1 d . . .
C12 C 0.3166(2) 0.2321(3) 0.5401(2) 0.0473(8) Uani 1 1 d . . .
H12 H 0.3338 0.2448 0.5938 0.057 Uiso 1 1 calc R . .
C13 C 0.3688(3) 0.2735(3) 0.5052(3) 0.0568(10) Uani 1 1 d . . .
H13 H 0.4207 0.3138 0.5350 0.068 Uiso 1 1 calc R . .
C14 C 0.18536(19) 0.1192(3) 0.53458(18) 0.0337(7) Uani 1 1 d . . .
C15 C 0.2797(2) 0.7122(3) 0.3919(2) 0.0454(8) Uani 1 1 d . . .
C16 C 0.3127(2) 0.6785(3) 0.4701(2) 0.0483(9) Uani 1 1 d . . .
H16 H 0.3660 0.6386 0.4938 0.058 Uiso 1 1 calc R . .
C17 C 0.2654(2) 0.7048(3) 0.5130(2) 0.0408(8) Uani 1 1 d . . .
H17 H 0.2869 0.6817 0.5657 0.049 Uiso 1 1 calc R . .
C18 C 0.18634(19) 0.7652(3) 0.47798(17) 0.0322(6) Uani 1 1 d . . .
C19 C 0.1552(2) 0.8004(3) 0.39940(19) 0.0399(7) Uani 1 1 d . . .
H19 H 0.1028 0.8423 0.3757 0.048 Uiso 1 1 calc R . .
C20 C 0.2020(2) 0.7734(3) 0.3564(2) 0.0466(8) Uani 1 1 d . . .
H20 H 0.1809 0.7965 0.3038 0.056 Uiso 1 1 calc R . .
C21 C 0.13354(19) 0.7927(3) 0.52381(18) 0.0317(7) Uani 1 1 d . . .
C22 C 0.8229(2) 0.7284(3) 0.2602(2) 0.0452(8) Uani 1 1 d . . .
H22 H 0.8166 0.7835 0.2211 0.054 Uiso 1 1 calc R . .
C23 C 0.8983(2) 0.7025(3) 0.3225(2) 0.0429(8) Uani 1 1 d . . .
H23 H 0.9530 0.7358 0.3346 0.052 Uiso 1 1 calc R . .
C24 C 0.79248(19) 0.5963(3) 0.32652(17) 0.0344(7) Uani 1 1 d . . .
H24 H 0.7622 0.5424 0.3432 0.041 Uiso 1 1 calc R . .
C25 C 0.94059(18) 0.5577(2) 0.43416(16) 0.0311(6) Uani 1 1 d . . .
C26 C 0.9135(2) 0.5106(3) 0.48770(19) 0.0390(7) Uani 1 1 d . . .
H26 H 0.8554 0.5175 0.4793 0.047 Uiso 1 1 calc R . .
C27 C 1.0264(2) 0.5471(3) 0.44596(18) 0.0391(7) Uani 1 1 d . . .
H27 H 1.0440 0.5788 0.4093 0.047 Uiso 1 1 calc R . .
C28 C 0.4813(5) 0.9567(8) 0.2330(4) 0.143(4) Uani 1 1 d . . .
H28 H 0.5104 0.9430 0.2015 0.172 Uiso 1 1 calc R . .
C29 C 0.5144(6) 0.9624(10) 0.3071(5) 0.201(6) Uani 1 1 d . . .
H29 H 0.5738 0.9487 0.3377 0.241 Uiso 1 1 calc R . .
C30 C 0.3867(5) 0.9910(8) 0.2772(4) 0.137(3) Uani 1 1 d . . .
H30 H 0.3327 1.0030 0.2781 0.164 Uiso 1 1 calc R . .
C31 C 0.4810(3) 0.9952(3) 0.4208(3) 0.0620(11) Uani 1 1 d . . .
C32 C 0.4196(3) 0.9606(4) 0.4459(3) 0.0787(13) Uani 1 1 d . . .
H32 H 0.3648 0.9345 0.4095 0.094 Uiso 1 1 calc R . .
C33 C 0.4392(3) 0.9645(4) 0.5256(3) 0.0808(14) Uani 1 1 d . . .
H33 H 0.3977 0.9396 0.5427 0.097 Uiso 1 1 calc R . .
N1 N 0.75612(16) 0.6611(2) 0.26286(14) 0.0355(6) Uani 1 1 d . . .
N2 N 0.87935(16) 0.6171(2) 0.36523(14) 0.0331(5) Uani 1 1 d . . .
N3 N 0.4620(3) 0.9883(3) 0.3393(3) 0.0713(10) Uani 1 1 d . . .
N4 N 0.3995(5) 0.9734(6) 0.2102(4) 0.141(2) Uani 1 1 d . . .
O1 O 0.56519(16) 0.63038(19) 0.26356(14) 0.0455(6) Uani 1 1 d . . .
O2 O 0.5604(2) 0.4364(2) 0.2467(2) 0.0743(10) Uani 1 1 d . . .
O3 O 0.3240(2) 0.6975(2) 0.34492(18) 0.0689(9) Uani 1 1 d . . .
O4 O 0.4006(2) 0.2787(2) 0.3922(2) 0.0711(9) Uani 1 1 d . . .
O5 O 0.16465(14) 0.7611(2) 0.59477(12) 0.0417(5) Uani 1 1 d . . .
O6 O 0.06166(14) 0.84333(19) 0.48699(13) 0.0392(5) Uani 1 1 d D . .
O7 O 0.22147(15) 0.0921(2) 0.60579(13) 0.0484(6) Uani 1 1 d . . .
O8 O 0.10484(13) 0.1031(2) 0.48974(13) 0.0438(6) Uani 1 1 d . . .
O1W O 0.64507(16) 0.8734(2) 0.23884(15) 0.0490(6) Uani 1 1 d D . .
O2W O 0.49098(16) 0.7685(2) 0.11325(15) 0.0527(6) Uani 1 1 d D . .
O3W O 0.59200(13) 0.50947(17) 0.13063(11) 0.0288(4) Uani 1 1 d D . .
H1W H 0.6843(16) 0.881(4) 0.2836(9) 0.080 Uiso 1 1 d D . .
H4W H 0.457(2) 0.720(3) 0.0825(17) 0.080 Uiso 1 1 d D . .
H2W H 0.6022(15) 0.916(3) 0.229(2) 0.080 Uiso 1 1 d D . .
H3W H 0.481(3) 0.785(4) 0.1512(16) 0.080 Uiso 1 1 d D . .
H5W H 0.6330(15) 0.478(3) 0.1254(19) 0.080 Uiso 1 1 d D . .
H6W H 0.581(2) 0.480(3) 0.1654(18) 0.080 Uiso 1 1 d D . .
H6D H 0.041(3) 0.908(2) 0.467(2) 0.080 Uiso 1 1 d D . .


_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
Mn1 O2W 2.158(2) . ?
Mn1 O5 2.160(2) 4_675 ?
Mn1 N1 2.178(2) . ?
Mn1 O1 2.195(2) . ?
Mn1 O1W 2.217(2) . ?
Mn1 O3W 2.267(2) . ?
Mn2 O6 2.114(2) 4_675 ?
Mn2 O6 2.114(2) 2_545 ?
Mn2 O8 2.194(2) 2 ?
Mn2 O8 2.194(2) 4_665 ?
Mn2 O3W 2.268(2) . ?
Mn2 O3W 2.268(2) 3_665 ?
C1 O2 1.238(4) . ?
C1 O1 1.243(4) . ?
C1 C2 1.511(4) . ?
C2 C3 1.381(4) . ?
C2 C7 1.382(4) . ?
C3 C4 1.386(4) . ?
C3 H3 0.9300 . ?
C4 O4 1.375(4) . ?
C4 C5 1.381(4) . ?
C5 C6 1.381(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.385(4) . ?
C6 O3 1.388(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.365(6) . ?
C8 C13 1.383(5) . ?
C8 O4 1.399(4) . ?
C9 C10 1.393(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.372(5) . ?
C11 C14 1.513(4) . ?
C12 C13 1.384(5) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 O7 1.242(4) . ?
C14 O8 1.267(4) . ?
C15 C20 1.374(5) . ?
C15 C16 1.378(5) . ?
C15 O3 1.389(4) . ?
C16 C17 1.387(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.386(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.391(4) . ?
C18 C21 1.512(4) . ?
C19 C20 1.382(4) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O5 1.252(4) . ?
C21 O6 1.247(4) . ?
C22 C23 1.338(4) . ?
C22 N1 1.378(4) . ?
C22 H22 0.9300 . ?
C23 N2 1.373(4) . ?
C23 H23 0.9300 . ?
C24 N1 1.303(4) . ?
C24 N2 1.349(4) . ?
C24 H24 0.9300 . ?
C25 C27 1.374(4) . ?
C25 C26 1.375(4) . ?
C25 N2 1.427(4) . ?
C26 C27 1.382(4) 3_766 ?
C26 H26 0.9300 . ?
C27 C26 1.382(4) 3_766 ?
C27 H27 0.9300 . ?
C28 C29 1.256(10) . ?
C28 N4 1.272(9) . ?
C28 H28 0.9300 . ?
C29 N3 1.301(7) . ?
C29 C30 2.008(10) . ?
C29 H29 0.9300 . ?
C30 N3 1.303(8) . ?
C30 N4 1.378(8) . ?
C30 H30 0.9300 . ?
C31 C33 1.367(7) 3_676 ?
C31 C32 1.367(6) . ?
C31 N3 1.419(6) . ?
C32 C33 1.384(7) . ?
C32 H32 0.9300 . ?
C33 C31 1.367(7) 3_676 ?
C33 H33 0.9300 . ?
O5 Mn1 2.160(2) 4_576 ?
O6 Mn2 2.114(2) 2 ?
O6 H6D 0.824(5) . ?
O8 Mn2 2.194(2) 2_545 ?
O1W H1W 0.8200(11) . ?
O1W H2W 0.8200(11) . ?
O2W H4W 0.8201(11) . ?
O2W H3W 0.8200(11) . ?
O3W H5W 0.8201(11) . ?
O3W H6W 0.8201(11) . ?

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
O2W Mn1 O5 92.41(9) . 4_675 ?
O2W Mn1 N1 167.29(10) . . ?
O5 Mn1 N1 86.77(9) 4_675 . ?
O2W Mn1 O1 86.35(10) . . ?
O5 Mn1 O1 172.66(9) 4_675 . ?
N1 Mn1 O1 96.02(10) . . ?
O2W Mn1 O1W 83.15(9) . . ?
O5 Mn1 O1W 95.21(9) 4_675 . ?
N1 Mn1 O1W 84.29(9) . . ?
O1 Mn1 O1W 91.83(9) . . ?
O2W Mn1 O3W 97.20(8) . . ?
O5 Mn1 O3W 87.19(8) 4_675 . ?
N1 Mn1 O3W 95.43(9) . . ?
O1 Mn1 O3W 85.79(7) . . ?
O1W Mn1 O3W 177.57(8) . . ?
O6 Mn2 O6 180.00(13) 4_675 2_545 ?
O6 Mn2 O8 91.50(9) 4_675 2 ?
O6 Mn2 O8 88.50(9) 2_545 2 ?
O6 Mn2 O8 88.50(9) 4_675 4_665 ?
O6 Mn2 O8 91.50(9) 2_545 4_665 ?
O8 Mn2 O8 180.00(11) 2 4_665 ?
O6 Mn2 O3W 86.70(8) 4_675 . ?
O6 Mn2 O3W 93.30(8) 2_545 . ?
O8 Mn2 O3W 94.86(7) 2 . ?
O8 Mn2 O3W 85.14(7) 4_665 . ?
O6 Mn2 O3W 93.30(8) 4_675 3_665 ?
O6 Mn2 O3W 86.70(8) 2_545 3_665 ?
O8 Mn2 O3W 85.14(7) 2 3_665 ?
O8 Mn2 O3W 94.86(7) 4_665 3_665 ?
O3W Mn2 O3W 180.0 . 3_665 ?
O2 C1 O1 125.0(2) . . ?
O2 C1 C2 116.6(3) . . ?
O1 C1 C2 118.3(2) . . ?
C3 C2 C7 120.2(2) . . ?
C3 C2 C1 119.7(2) . . ?
C7 C2 C1 119.9(3) . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
O4 C4 C5 123.8(3) . . ?
O4 C4 C3 114.8(3) . . ?
C5 C4 C3 121.4(3) . . ?
C4 C5 C6 118.0(3) . . ?
C4 C5 H5 121.0 . . ?
C6 C5 H5 121.0 . . ?
C5 C6 C7 121.7(3) . . ?
C5 C6 O3 123.6(3) . . ?
C7 C6 O3 114.3(3) . . ?
C2 C7 C6 119.1(3) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C13 121.5(3) . . ?
C9 C8 O4 118.7(4) . . ?
C13 C8 O4 119.3(4) . . ?
C8 C9 C10 119.0(3) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C11 C10 C9 120.4(3) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C10 119.3(3) . . ?
C12 C11 C14 121.6(3) . . ?
C10 C11 C14 119.1(3) . . ?
C11 C12 C13 120.9(3) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C8 C13 C12 118.9(3) . . ?
C8 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
O7 C14 O8 124.6(3) . . ?
O7 C14 C11 119.1(3) . . ?
O8 C14 C11 116.3(3) . . ?
C20 C15 C16 121.1(3) . . ?
C20 C15 O3 114.6(3) . . ?
C16 C15 O3 124.0(3) . . ?
C15 C16 C17 119.1(3) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C18 C17 C16 120.6(3) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 119.2(3) . . ?
C17 C18 C21 121.0(3) . . ?
C19 C18 C21 119.8(3) . . ?
C20 C19 C18 120.2(3) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C15 C20 C19 119.7(3) . . ?
C15 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
O5 C21 O6 125.5(3) . . ?
O5 C21 C18 117.7(3) . . ?
O6 C21 C18 116.8(3) . . ?
C23 C22 N1 109.6(3) . . ?
C23 C22 H22 125.2 . . ?
N1 C22 H22 125.2 . . ?
C22 C23 N2 106.7(3) . . ?
C22 C23 H23 126.6 . . ?
N2 C23 H23 126.6 . . ?
N1 C24 N2 111.7(3) . . ?
N1 C24 H24 124.1 . . ?
N2 C24 H24 124.1 . . ?
C27 C25 C26 120.6(3) . . ?
C27 C25 N2 119.3(3) . . ?
C26 C25 N2 120.1(3) . . ?
C25 C26 C27 119.4(3) . 3_766 ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 3_766 . ?
C25 C27 C26 120.1(3) . 3_766 ?
C25 C27 H27 120.0 . . ?
C26 C27 H27 120.0 3_766 . ?
C29 C28 N4 105.5(5) . . ?
C29 C28 H28 127.2 . . ?
N4 C28 H28 127.3 . . ?
C28 C29 N3 117.1(7) . . ?
C28 C29 C30 77.6(5) . . ?
N3 C29 C30 39.6(3) . . ?
C28 C29 H29 121.5 . . ?
N3 C29 H29 121.4 . . ?
C30 C29 H29 160.7 . . ?
N3 C30 N4 109.6(6) . . ?
N3 C30 C29 39.5(3) . . ?
N4 C30 C29 70.1(5) . . ?
N3 C30 H30 125.2 . . ?
N4 C30 H30 125.2 . . ?
C29 C30 H30 164.5 . . ?
C33 C31 C32 119.7(5) 3_676 . ?
C33 C31 N3 120.2(4) 3_676 . ?
C32 C31 N3 120.1(5) . . ?
C31 C32 C33 119.9(5) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.0 . . ?
C31 C33 C32 120.3(4) 3_676 . ?
C31 C33 H33 119.8 3_676 . ?
C32 C33 H33 119.8 . . ?
C24 N1 C22 105.6(2) . . ?
C24 N1 Mn1 131.9(2) . . ?
C22 N1 Mn1 121.5(2) . . ?
C24 N2 C23 106.3(2) . . ?
C24 N2 C25 127.1(2) . . ?
C23 N2 C25 126.5(2) . . ?
C29 N3 C30 100.9(6) . . ?
C29 N3 C31 128.8(5) . . ?
C30 N3 C31 129.8(5) . . ?
C28 N4 C30 106.8(6) . . ?
C1 O1 Mn1 129.84(18) . . ?
C6 O3 C15 122.8(2) . . ?
C4 O4 C8 120.4(3) . . ?
C21 O5 Mn1 128.59(19) . 4_576 ?
C21 O6 Mn2 136.8(2) . 2 ?
C21 O6 H6D 141(3) . . ?
Mn2 O6 H6D 35(3) 2 . ?
C14 O8 Mn2 133.97(19) . 2_545 ?
Mn1 O1W H1W 119(3) . . ?
Mn1 O1W H2W 117(3) . . ?
H1W O1W H2W 114.6(2) . . ?
Mn1 O2W H4W 113(3) . . ?
Mn1 O2W H3W 95(3) . . ?
H4W O2W H3W 114.6(2) . . ?
Mn1 O3W Mn2 115.39(8) . . ?
Mn1 O3W H5W 115(3) . . ?
Mn2 O3W H5W 94(2) . . ?
Mn1 O3W H6W 96(3) . . ?
Mn2 O3W H6W 124(3) . . ?
H5W O3W H6W 114.6(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.068
_database_code_depnum_ccdc_archive 'CCDC 986460'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H24 Mn N8 O2, 2(C21 H13 O8)'
_chemical_formula_sum            'C66 H50 Mn N8 O18'
_chemical_formula_weight         1298.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3105(9)
_cell_length_b                   13.2138(13)
_cell_length_c                   14.0990(14)
_cell_angle_alpha                102.310(2)
_cell_angle_beta                 108.444(2)
_cell_angle_gamma                108.378(2)
_cell_volume                     1464.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4157
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      28.26

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             671
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8702
_exptl_absorpt_correction_T_max  0.9236
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7634
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5129
_reflns_number_gt                4578
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.9197P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5129
_refine_ls_number_parameters     431
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1094
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9879(3) 0.8225(2) 0.64602(18) 0.0381(5) Uani 1 1 d . . .
C2 C 0.9201(3) 0.77748(19) 0.71906(17) 0.0337(5) Uani 1 1 d . . .
C3 C 0.7580(3) 0.6995(2) 0.67924(17) 0.0375(5) Uani 1 1 d . . .
H3 H 0.6892 0.6750 0.6072 0.045 Uiso 1 1 calc R . .
C4 C 0.6984(3) 0.6579(2) 0.74757(18) 0.0389(5) Uani 1 1 d . . .
C5 C 0.7970(3) 0.6965(2) 0.85560(18) 0.0402(5) Uani 1 1 d . . .
H5 H 0.7556 0.6697 0.9016 0.048 Uiso 1 1 calc R . .
C6 C 0.9588(3) 0.7760(2) 0.89337(17) 0.0380(5) Uani 1 1 d . . .
C7 C 1.0230(3) 0.8158(2) 0.82649(18) 0.0367(5) Uani 1 1 d . . .
H7 H 1.1332 0.8674 0.8529 0.044 Uiso 1 1 calc R . .
C8 C 0.4460(3) 0.5633(2) 0.7597(2) 0.0533(7) Uani 1 1 d . . .
C9 C 0.3501(4) 0.6240(2) 0.7579(2) 0.0598(8) Uani 1 1 d . . .
H9 H 0.3548 0.6753 0.7217 0.072 Uiso 1 1 calc R . .
C10 C 0.2467(4) 0.6082(2) 0.8103(2) 0.0580(7) Uani 1 1 d . . .
H10 H 0.1783 0.6468 0.8073 0.070 Uiso 1 1 calc R . .
C11 C 0.2451(3) 0.5351(2) 0.8672(2) 0.0496(6) Uani 1 1 d . . .
C12 C 0.3424(4) 0.4749(3) 0.8684(3) 0.0626(8) Uani 1 1 d . . .
H12 H 0.3414 0.4258 0.9069 0.075 Uiso 1 1 calc R . .
C13 C 0.4418(4) 0.4874(3) 0.8126(3) 0.0670(8) Uani 1 1 d . . .
H13 H 0.5046 0.4450 0.8111 0.080 Uiso 1 1 calc R . .
C14 C 0.1402(4) 0.5205(2) 0.9268(2) 0.0539(7) Uani 1 1 d . . .
C15 C 1.0083(3) 0.8191(2) 1.07700(17) 0.0419(6) Uani 1 1 d . . .
C16 C 1.0680(3) 0.7762(2) 1.15325(18) 0.0396(5) Uani 1 1 d . . .
H16 H 1.1389 0.7409 1.1485 0.048 Uiso 1 1 calc R . .
C17 C 1.0217(3) 0.7857(2) 1.23760(18) 0.0374(5) Uani 1 1 d . . .
H17 H 1.0638 0.7584 1.2908 0.045 Uiso 1 1 calc R . .
C18 C 0.9127(3) 0.83585(19) 1.24348(16) 0.0314(5) Uani 1 1 d . . .
C19 C 0.8542(3) 0.8782(2) 1.16523(18) 0.0412(6) Uani 1 1 d . . .
H19 H 0.7804 0.9113 1.1682 0.049 Uiso 1 1 calc R . .
C20 C 0.9040(3) 0.8719(3) 1.0828(2) 0.0492(6) Uani 1 1 d . . .
H20 H 0.8674 0.9031 1.0316 0.059 Uiso 1 1 calc R . .
C21 C 0.8618(3) 0.84534(18) 1.33461(16) 0.0312(5) Uani 1 1 d . . .
C22 C 0.3385(3) 0.06139(19) 0.30239(17) 0.0343(5) Uani 1 1 d . . .
H22 H 0.2845 0.0901 0.3390 0.041 Uiso 1 1 calc R . .
C23 C 0.3370(3) 0.0711(2) 0.20906(17) 0.0368(5) Uani 1 1 d . . .
H23 H 0.2834 0.1073 0.1703 0.044 Uiso 1 1 calc R . .
C24 C 0.4854(3) -0.02186(18) 0.26172(15) 0.0279(4) Uani 1 1 d . . .
H24 H 0.5529 -0.0611 0.2639 0.034 Uiso 1 1 calc R . .
C25 C 0.4655(3) 0.00774(18) 0.08972(16) 0.0293(4) Uani 1 1 d . . .
C26 C 0.4813(3) -0.08731(19) 0.04044(17) 0.0350(5) Uani 1 1 d . . .
H26 H 0.4683 -0.1467 0.0670 0.042 Uiso 1 1 calc R . .
C27 C 0.4835(3) 0.0949(2) 0.04876(17) 0.0354(5) Uani 1 1 d . . .
H27 H 0.4720 0.1591 0.0812 0.043 Uiso 1 1 calc R . .
C28 C 0.7247(3) 0.23165(17) 0.51215(16) 0.0287(4) Uani 1 1 d . . .
H28 H 0.7579 0.1938 0.4655 0.034 Uiso 1 1 calc R . .
C29 C 0.6054(3) 0.2660(2) 0.6141(2) 0.0481(7) Uani 1 1 d . . .
H29 H 0.5390 0.2553 0.6516 0.058 Uiso 1 1 calc R . .
C30 C 0.7012(4) 0.3676(2) 0.6164(2) 0.0579(8) Uani 1 1 d . . .
H30 H 0.7131 0.4386 0.6548 0.070 Uiso 1 1 calc R . .
C31 C 0.8923(3) 0.42545(17) 0.52627(18) 0.0338(5) Uani 1 1 d . . .
C32 C 1.0299(3) 0.40982(18) 0.5228(2) 0.0382(5) Uani 1 1 d . . .
H32 H 1.0499 0.3493 0.5384 0.046 Uiso 1 1 calc R . .
C33 C 0.8616(3) 0.51530(19) 0.5040(2) 0.0399(5) Uani 1 1 d . . .
H33 H 0.7685 0.5254 0.5070 0.048 Uiso 1 1 calc R . .
Mn1 Mn 0.5000 0.0000 0.5000 0.01487(12) Uani 1 2 d S . .
N1 N 0.4315(2) 0.00296(14) 0.33569(13) 0.0274(4) Uani 1 1 d . . .
N2 N 0.4301(2) 0.01696(15) 0.18210(13) 0.0298(4) Uani 1 1 d . . .
N3 N 0.6197(2) 0.18077(14) 0.54888(13) 0.0294(4) Uani 1 1 d . . .
N4 N 0.7779(2) 0.34560(15) 0.55073(15) 0.0359(4) Uani 1 1 d . . .
O1 O 0.8702(2) 0.80998(19) 0.55876(14) 0.0532(5) Uani 1 1 d . . .
H1 H 0.9105 0.8304 0.5185 0.080 Uiso 1 1 calc R . .
O2 O 1.1348(2) 0.86299(19) 0.66767(14) 0.0607(5) Uani 1 1 d . . .
O3 O 0.5388(2) 0.57391(18) 0.69990(15) 0.0662(6) Uani 1 1 d . . .
O4 O 1.0689(2) 0.8152(2) 0.99844(13) 0.0607(6) Uani 1 1 d . . .
O5 O 0.1755(3) 0.4864(2) 1.00322(19) 0.0745(7) Uani 1 1 d . . .
O6 O 0.0147(3) 0.5439(3) 0.8952(2) 0.0860(8) Uani 1 1 d . . .
H6 H -0.0382 0.5307 0.9312 0.129 Uiso 1 1 calc R . .
O7 O 0.7269(2) 0.84880(16) 1.32268(13) 0.0440(4) Uani 1 1 d . . .
O8 O 0.96678(19) 0.84945(15) 1.42080(12) 0.0423(4) Uani 1 1 d . . .
O9 O 0.71593(19) -0.01432(14) 0.49762(12) 0.0335(3) Uani 1 1 d D . .
H1W H 0.8058(16) 0.0409(15) 0.531(2) 0.075(11) Uiso 1 1 d D . .
H2W H 0.713(3) -0.0626(16) 0.4488(16) 0.062(9) Uiso 1 1 d D . .


_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
C1 O2 1.207(3) . ?
C1 O1 1.299(3) . ?
C1 C2 1.499(3) . ?
C2 C3 1.376(3) . ?
C2 C7 1.385(3) . ?
C3 C4 1.381(3) . ?
C3 H3 0.9300 . ?
C4 O3 1.379(3) . ?
C4 C5 1.383(3) . ?
C5 C6 1.384(3) . ?
C5 H5 0.9300 . ?
C6 O4 1.375(3) . ?
C6 C7 1.376(3) . ?
C7 H7 0.9300 . ?
C8 C13 1.369(4) . ?
C8 C9 1.375(4) . ?
C8 O3 1.382(3) . ?
C9 C10 1.380(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.381(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(4) . ?
C11 C14 1.472(4) . ?
C12 C13 1.387(4) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 O5 1.244(4) . ?
C14 O6 1.271(4) . ?
C15 C16 1.366(3) . ?
C15 C20 1.376(4) . ?
C15 O4 1.392(3) . ?
C16 C17 1.382(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.389(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.379(3) . ?
C18 C21 1.498(3) . ?
C19 C20 1.377(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O7 1.231(3) . ?
C21 O8 1.273(3) . ?
C22 C23 1.345(3) . ?
C22 N1 1.373(3) . ?
C22 H22 0.9300 . ?
C23 N2 1.375(3) . ?
C23 H23 0.9300 . ?
C24 N1 1.317(3) . ?
C24 N2 1.355(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.375(3) . ?
C25 C27 1.382(3) . ?
C25 N2 1.432(3) . ?
C26 C27 1.388(3) 2_655 ?
C26 H26 0.9300 . ?
C27 C26 1.388(3) 2_655 ?
C27 H27 0.9300 . ?
C28 N3 1.315(3) . ?
C28 N4 1.348(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.344(3) . ?
C29 N3 1.365(3) . ?
C29 H29 0.9300 . ?
C30 N4 1.374(3) . ?
C30 H30 0.9300 . ?
C31 C32 1.373(3) . ?
C31 C33 1.381(3) . ?
C31 N4 1.430(3) . ?
C32 C33 1.383(3) 2_766 ?
C32 H32 0.9300 . ?
C33 C32 1.383(3) 2_766 ?
C33 H33 0.9300 . ?
Mn1 O9 2.0877(14) 2_656 ?
Mn1 O9 2.0877(14) . ?
Mn1 N3 2.1345(17) 2_656 ?
Mn1 N3 2.1345(17) . ?
Mn1 N1 2.2124(16) 2_656 ?
Mn1 N1 2.2124(16) . ?
O1 H1 0.8200 . ?
O6 H6 0.8200 . ?
O9 H1W 0.8203(11) . ?
O9 H2W 0.8203(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 125.8(2) . . ?
O2 C1 C2 122.3(2) . . ?
O1 C1 C2 111.8(2) . . ?
C3 C2 C7 120.9(2) . . ?
C3 C2 C1 120.1(2) . . ?
C7 C2 C1 119.0(2) . . ?
C2 C3 C4 119.2(2) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
O3 C4 C3 115.5(2) . . ?
O3 C4 C5 123.3(2) . . ?
C3 C4 C5 121.2(2) . . ?
C4 C5 C6 118.2(2) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
O4 C6 C7 115.5(2) . . ?
O4 C6 C5 122.5(2) . . ?
C7 C6 C5 121.8(2) . . ?
C6 C7 C2 118.6(2) . . ?
C6 C7 H7 120.7 . . ?
C2 C7 H7 120.7 . . ?
C13 C8 C9 121.5(3) . . ?
C13 C8 O3 120.0(3) . . ?
C9 C8 O3 118.3(3) . . ?
C8 C9 C10 119.4(3) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C11 119.9(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 119.9(3) . . ?
C12 C11 C14 119.5(3) . . ?
C10 C11 C14 120.6(3) . . ?
C11 C12 C13 120.3(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C8 C13 C12 118.9(3) . . ?
C8 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
O5 C14 O6 123.4(3) . . ?
O5 C14 C11 120.3(3) . . ?
O6 C14 C11 116.3(3) . . ?
C16 C15 C20 121.4(2) . . ?
C16 C15 O4 116.8(2) . . ?
C20 C15 O4 121.6(2) . . ?
C15 C16 C17 119.1(2) . . ?
C15 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C16 C17 C18 120.5(2) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C19 C18 C17 119.0(2) . . ?
C19 C18 C21 120.6(2) . . ?
C17 C18 C21 120.32(19) . . ?
C20 C19 C18 120.7(2) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C15 C20 C19 119.2(2) . . ?
C15 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
O7 C21 O8 124.9(2) . . ?
O7 C21 C18 119.87(19) . . ?
O8 C21 C18 115.20(18) . . ?
C23 C22 N1 110.08(19) . . ?
C23 C22 H22 125.0 . . ?
N1 C22 H22 125.0 . . ?
C22 C23 N2 106.56(19) . . ?
C22 C23 H23 126.7 . . ?
N2 C23 H23 126.7 . . ?
N1 C24 N2 111.47(18) . . ?
N1 C24 H24 124.3 . . ?
N2 C24 H24 124.3 . . ?
C26 C25 C27 119.20(19) . . ?
C26 C25 N2 120.83(19) . . ?
C27 C25 N2 119.97(19) . . ?
C25 C26 C27 120.2(2) . 2_655 ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 2_655 . ?
C25 C27 C26 120.6(2) . 2_655 ?
C25 C27 H27 119.7 . . ?
C26 C27 H27 119.7 2_655 . ?
N3 C28 N4 111.42(18) . . ?
N3 C28 H28 124.3 . . ?
N4 C28 H28 124.3 . . ?
C30 C29 N3 110.2(2) . . ?
C30 C29 H29 124.9 . . ?
N3 C29 H29 124.9 . . ?
C29 C30 N4 106.2(2) . . ?
C29 C30 H30 126.9 . . ?
N4 C30 H30 126.9 . . ?
C32 C31 C33 120.9(2) . . ?
C32 C31 N4 119.2(2) . . ?
C33 C31 N4 119.9(2) . . ?
C31 C32 C33 119.5(2) . 2_766 ?
C31 C32 H32 120.2 . . ?
C33 C32 H32 120.2 2_766 . ?
C31 C33 C32 119.6(2) . 2_766 ?
C31 C33 H33 120.2 . . ?
C32 C33 H33 120.2 2_766 . ?
O9 Mn1 O9 180.00(9) 2_656 . ?
O9 Mn1 N3 90.81(6) 2_656 2_656 ?
O9 Mn1 N3 89.19(6) . 2_656 ?
O9 Mn1 N3 89.19(6) 2_656 . ?
O9 Mn1 N3 90.81(6) . . ?
N3 Mn1 N3 180.00(10) 2_656 . ?
O9 Mn1 N1 88.77(6) 2_656 2_656 ?
O9 Mn1 N1 91.23(6) . 2_656 ?
N3 Mn1 N1 85.35(6) 2_656 2_656 ?
N3 Mn1 N1 94.65(6) . 2_656 ?
O9 Mn1 N1 91.23(6) 2_656 . ?
O9 Mn1 N1 88.77(6) . . ?
N3 Mn1 N1 94.65(6) 2_656 . ?
N3 Mn1 N1 85.35(6) . . ?
N1 Mn1 N1 180.0 2_656 . ?
C24 N1 C22 105.46(17) . . ?
C24 N1 Mn1 133.74(14) . . ?
C22 N1 Mn1 119.41(13) . . ?
C24 N2 C23 106.43(17) . . ?
C24 N2 C25 127.29(17) . . ?
C23 N2 C25 126.25(17) . . ?
C28 N3 C29 105.56(18) . . ?
C28 N3 Mn1 122.33(14) . . ?
C29 N3 Mn1 132.04(14) . . ?
C28 N4 C30 106.58(18) . . ?
C28 N4 C31 125.41(18) . . ?
C30 N4 C31 128.01(19) . . ?
C1 O1 H1 109.5 . . ?
C4 O3 C8 118.07(19) . . ?
C6 O4 C15 119.10(18) . . ?
C14 O6 H6 109.5 . . ?
Mn1 O9 H1W 119.8(17) . . ?
Mn1 O9 H2W 121.6(17) . . ?
H1W O9 H2W 114.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.053
_database_code_depnum_ccdc_archive 'CCDC 986461'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H17 Co N2 O8'
_chemical_formula_sum            'C27 H17 Co N2 O8'
_chemical_formula_weight         556.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.445(3)
_cell_length_b                   18.689(5)
_cell_length_c                   11.538(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.085(4)
_cell_angle_gamma                90.00
_cell_volume                     2302.7(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5859
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      28.07

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7135
_exptl_absorpt_correction_T_max  0.8181
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11774
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4053
_reflns_number_gt                3541
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0540P)²+0.7658P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4053
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0848
_refine_ls_wR_factor_gt          0.0802
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.58444(2) 0.629421(13) 0.56856(2) 0.02446(10) Uani 1 1 d . . .
O2 O 0.45157(12) 0.59740(7) 0.62765(13) 0.0321(3) Uani 1 1 d . . .
N1 N 0.52849(16) 0.62477(8) 0.38371(14) 0.0269(4) Uani 1 1 d . . .
O1 O 0.39786(14) 0.70277(7) 0.54358(13) 0.0358(3) Uani 1 1 d . . .
N2 N 0.49223(15) 0.58726(8) 0.19445(14) 0.0261(3) Uani 1 1 d . . .
C1 C 0.37651(18) 0.65047(10) 0.59793(17) 0.0263(4) Uani 1 1 d . . .
O6 O 0.01345(13) 0.76450(7) 0.64424(15) 0.0396(4) Uani 1 1 d . . .
C24 C 0.53577(17) 0.57018(10) 0.31540(17) 0.0256(4) Uani 1 1 d . . .
H24 H 0.5671 0.5254 0.3467 0.031 Uiso 1 1 calc R . .
C25 C 0.49311(17) 0.54264(10) 0.09440(16) 0.0260(4) Uani 1 1 d . . .
C5 C 0.04745(19) 0.64254(10) 0.6864(2) 0.0340(5) Uani 1 1 d . . .
H5 H -0.0251 0.6411 0.7050 0.041 Uiso 1 1 calc R . .
C23 C 0.4549(2) 0.65720(11) 0.18603(19) 0.0373(5) Uani 1 1 d . . .
H23 H 0.4208 0.6840 0.1137 0.045 Uiso 1 1 calc R . .
C4 C 0.11656(19) 0.58131(10) 0.6926(2) 0.0341(5) Uani 1 1 d . . .
C2 C 0.26199(17) 0.64679(10) 0.63043(17) 0.0256(4) Uani 1 1 d . . .
C6 C 0.08701(17) 0.70526(9) 0.65256(18) 0.0286(4) Uani 1 1 d . . .
O3 O 0.07135(17) 0.52127(8) 0.7299(2) 0.0660(6) Uani 1 1 d . . .
C7 C 0.19347(18) 0.70823(10) 0.62328(18) 0.0292(4) Uani 1 1 d . . .
H7 H 0.2187 0.7512 0.5990 0.035 Uiso 1 1 calc R . .
C26 C 0.49724(19) 0.46962(10) 0.10740(17) 0.0309(4) Uani 1 1 d . . .
H26 H 0.4951 0.4490 0.1800 0.037 Uiso 1 1 calc R . .
C3 C 0.22459(18) 0.58271(10) 0.66574(19) 0.0310(4) Uani 1 1 d . . .
H3 H 0.2714 0.5413 0.6713 0.037 Uiso 1 1 calc R . .
C15 C 0.07511(17) 0.82975(9) 0.6710(2) 0.0301(4) Uani 1 1 d . . .
C8 C 0.1294(2) 0.45528(11) 0.7368(3) 0.0421(6) Uani 1 1 d . . .
C27 C 0.49548(19) 0.57316(10) -0.01300(18) 0.0315(4) Uani 1 1 d . . .
H27 H 0.4922 0.6227 -0.0220 0.038 Uiso 1 1 calc R . .
C22 C 0.4770(2) 0.67947(11) 0.30208(19) 0.0373(5) Uani 1 1 d . . .
H22 H 0.4600 0.7251 0.3241 0.045 Uiso 1 1 calc R . .
C20 C 0.0647(2) 0.87673(11) 0.5770(2) 0.0407(5) Uani 1 1 d . . .
H20 H 0.0207 0.8642 0.4947 0.049 Uiso 1 1 calc R . .
C13 C 0.1207(2) 0.41821(12) 0.6321(3) 0.0508(6) Uani 1 1 d . . .
H13 H 0.0850 0.4394 0.5544 0.061 Uiso 1 1 calc R . .
C16 C 0.1408(2) 0.84713(11) 0.7918(2) 0.0420(5) Uani 1 1 d . . .
H16 H 0.1484 0.8144 0.8548 0.050 Uiso 1 1 calc R . .
C19 C 0.1203(2) 0.94270(11) 0.6060(2) 0.0396(5) Uani 1 1 d . . .
H19 H 0.1136 0.9750 0.5427 0.047 Uiso 1 1 calc R . .
C18 C 0.18574(17) 0.96179(10) 0.72739(19) 0.0277(4) Uani 1 1 d . . .
C17 C 0.1953(2) 0.91325(11) 0.8196(2) 0.0392(5) Uani 1 1 d . . .
H17 H 0.2393 0.9254 0.9021 0.047 Uiso 1 1 calc R . .
C21 C 0.24266(19) 1.03390(10) 0.7598(2) 0.0311(4) Uani 1 1 d . . .
O7 O 0.29655(14) 1.04890(8) 0.87205(14) 0.0394(4) Uani 1 1 d . . .
O8 O 0.23442(18) 1.07589(8) 0.67252(15) 0.0515(4) Uani 1 1 d . . .
C9 C 0.1848(2) 0.42596(11) 0.8511(2) 0.0433(6) Uani 1 1 d . . .
H9 H 0.1931 0.4525 0.9217 0.052 Uiso 1 1 calc R . .
C12 C 0.1651(2) 0.34916(12) 0.6425(2) 0.0431(5) Uani 1 1 d . . .
H12 H 0.1591 0.3235 0.5715 0.052 Uiso 1 1 calc R . .
C11 C 0.21861(18) 0.31799(10) 0.75800(19) 0.0300(4) Uani 1 1 d . . .
C10 C 0.2287(2) 0.35692(11) 0.8622(2) 0.0363(5) Uani 1 1 d . . .
H10 H 0.2654 0.3365 0.9405 0.044 Uiso 1 1 calc R . .
C14 C 0.26206(19) 0.24291(10) 0.77222(19) 0.0317(4) Uani 1 1 d . . .
O4 O 0.31844(14) 0.21881(7) 0.87664(13) 0.0387(4) Uani 1 1 d . . .
O5 O 0.2368(2) 0.20665(8) 0.67271(15) 0.0614(5) Uani 1 1 d . . .
H5A H 0.2497 0.1641 0.6900 0.092 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 1.9703(14) . ?
Co1 O7 1.9794(14) 2_646 ?
Co1 O4 1.9800(14) 2_656 ?
Co1 N1 1.9959(17) . ?
O2 C1 1.276(2) . ?
N1 C24 1.310(2) . ?
N1 C22 1.371(2) . ?
O1 C1 1.232(2) . ?
N2 C24 1.341(2) . ?
N2 C23 1.368(3) . ?
N2 C25 1.427(2) . ?
C1 C2 1.489(3) . ?
O6 C6 1.373(2) . ?
O6 C15 1.387(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.372(3) . ?
C25 C27 1.373(3) . ?
C5 C6 1.363(3) . ?
C5 C4 1.378(3) . ?
C5 H5 0.9300 . ?
C23 C22 1.337(3) . ?
C23 H23 0.9300 . ?
C4 O3 1.368(2) . ?
C4 C3 1.379(3) . ?
C2 C7 1.376(3) . ?
C2 C3 1.382(3) . ?
C6 C7 1.378(3) . ?
O3 C8 1.389(2) . ?
C7 H7 0.9300 . ?
C26 C27 1.378(3) 3_665 ?
C26 H26 0.9300 . ?
C3 H3 0.9300 . ?
C15 C16 1.364(3) . ?
C15 C20 1.367(3) . ?
C8 C9 1.356(3) . ?
C8 C13 1.365(4) . ?
C27 C26 1.378(3) 3_665 ?
C27 H27 0.9300 . ?
C22 H22 0.9300 . ?
C20 C19 1.373(3) . ?
C20 H20 0.9300 . ?
C13 C12 1.376(3) . ?
C13 H13 0.9300 . ?
C16 C17 1.369(3) . ?
C16 H16 0.9300 . ?
C19 C18 1.377(3) . ?
C19 H19 0.9300 . ?
C18 C17 1.373(3) . ?
C18 C21 1.485(3) . ?
C17 H17 0.9300 . ?
C21 O7 1.250(2) . ?
C21 O8 1.253(2) . ?
O7 Co1 1.9794(14) 2_656 ?
C9 C10 1.374(3) . ?
C9 H9 0.9300 . ?
C12 C11 1.380(3) . ?
C12 H12 0.9300 . ?
C11 C10 1.374(3) . ?
C11 C14 1.478(3) . ?
C10 H10 0.9300 . ?
C14 O4 1.229(2) . ?
C14 O5 1.274(3) . ?
O4 Co1 1.9800(14) 2_646 ?
O5 H5A 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O7 99.79(6) . 2_646 ?
O2 Co1 O4 124.07(6) . 2_656 ?
O7 Co1 O4 107.07(7) 2_646 2_656 ?
O2 Co1 N1 111.45(6) . . ?
O7 Co1 N1 104.67(6) 2_646 . ?
O4 Co1 N1 107.78(6) 2_656 . ?
C1 O2 Co1 101.53(11) . . ?
C24 N1 C22 105.78(16) . . ?
C24 N1 Co1 127.69(13) . . ?
C22 N1 Co1 126.51(13) . . ?
C24 N2 C23 106.93(15) . . ?
C24 N2 C25 126.49(16) . . ?
C23 N2 C25 126.44(16) . . ?
O1 C1 O2 121.05(17) . . ?
O1 C1 C2 121.23(17) . . ?
O2 C1 C2 117.72(16) . . ?
C6 O6 C15 116.30(14) . . ?
N1 C24 N2 111.13(16) . . ?
N1 C24 H24 124.4 . . ?
N2 C24 H24 124.4 . . ?
C26 C25 C27 120.05(17) . . ?
C26 C25 N2 120.19(17) . . ?
C27 C25 N2 119.70(17) . . ?
C6 C5 C4 119.03(18) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C22 C23 N2 106.54(17) . . ?
C22 C23 H23 126.7 . . ?
N2 C23 H23 126.7 . . ?
O3 C4 C5 115.00(18) . . ?
O3 C4 C3 123.86(17) . . ?
C5 C4 C3 121.12(18) . . ?
C7 C2 C3 120.70(18) . . ?
C7 C2 C1 118.73(17) . . ?
C3 C2 C1 120.57(17) . . ?
C5 C6 O6 117.05(17) . . ?
C5 C6 C7 121.27(18) . . ?
O6 C6 C7 121.64(17) . . ?
C4 O3 C8 121.28(16) . . ?
C2 C7 C6 119.14(17) . . ?
C2 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C25 C26 C27 120.03(18) . 3_665 ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 3_665 . ?
C4 C3 C2 118.73(17) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C16 C15 C20 121.13(19) . . ?
C16 C15 O6 119.08(18) . . ?
C20 C15 O6 119.73(19) . . ?
C9 C8 C13 121.0(2) . . ?
C9 C8 O3 117.5(2) . . ?
C13 C8 O3 121.2(2) . . ?
C25 C27 C26 119.92(18) . 3_665 ?
C25 C27 H27 120.0 . . ?
C26 C27 H27 120.0 3_665 . ?
C23 C22 N1 109.61(18) . . ?
C23 C22 H22 125.2 . . ?
N1 C22 H22 125.2 . . ?
C15 C20 C19 118.9(2) . . ?
C15 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C8 C13 C12 119.5(2) . . ?
C8 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C16 C17 119.4(2) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C20 C19 C18 121.1(2) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C17 C18 C19 118.68(18) . . ?
C17 C18 C21 119.95(19) . . ?
C19 C18 C21 121.34(18) . . ?
C18 C17 C16 120.8(2) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
O7 C21 O8 123.97(18) . . ?
O7 C21 C18 118.21(18) . . ?
O8 C21 C18 117.83(19) . . ?
C21 O7 Co1 123.43(13) . 2_656 ?
C8 C9 C10 119.9(2) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C12 C13 120.1(2) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C10 C11 C12 119.35(19) . . ?
C10 C11 C14 119.11(18) . . ?
C12 C11 C14 121.52(19) . . ?
C11 C10 C9 120.2(2) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
O4 C14 O5 123.87(19) . . ?
O4 C14 C11 119.58(18) . . ?
O5 C14 C11 116.55(18) . . ?
C14 O4 Co1 131.19(14) . 2_646 ?
C14 O5 H5A 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.045
_database_code_depnum_ccdc_archive 'CCDC 986462'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H37 N6 Ni O10'
_chemical_formula_sum            'C42 H37 N6 Ni O10'
_chemical_formula_weight         844.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.964(4)
_cell_length_b                   19.227(3)
_cell_length_c                   14.812(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.10(2)
_cell_angle_gamma                90.00
_cell_volume                     3856.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5485
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.28

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1756
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7325
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19784
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.77
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6786
_reflns_number_gt                5420
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0700P)²+1.3820P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6786
_refine_ls_number_parameters     550
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.1179
_refine_ls_wR_factor_gt          0.1109
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.77051(18) 0.06588(14) 0.82711(18) 0.0304(6) Uani 1 1 d . . .
C2 C 0.82167(18) 0.04215(14) 0.92396(18) 0.0312(6) Uani 1 1 d . . .
C3 C 0.85996(18) -0.02439(13) 0.94028(18) 0.0327(6) Uani 1 1 d . . .
H3 H 0.8533 -0.0554 0.8910 0.039 Uiso 1 1 calc R . .
C4 C 0.90816(19) -0.04522(14) 1.02945(19) 0.0331(6) Uani 1 1 d . . .
H4 H 0.9336 -0.0900 1.0398 0.040 Uiso 1 1 calc R . .
C5 C 0.91835(18) 0.00072(14) 1.10291(17) 0.0307(6) Uani 1 1 d . . .
C6 C 0.8802(2) 0.06731(14) 1.08748(19) 0.0389(7) Uani 1 1 d . . .
H6 H 0.8865 0.0983 1.1368 0.047 Uiso 1 1 calc R . .
C7 C 0.83299(19) 0.08732(14) 0.99856(19) 0.0370(6) Uani 1 1 d . . .
H7 H 0.8081 0.1323 0.9884 0.044 Uiso 1 1 calc R . .
C8 C 0.96788(19) 0.01439(13) 1.26867(17) 0.0301(6) Uani 1 1 d . . .
C9 C 1.05695(19) 0.03529(14) 1.32498(18) 0.0341(6) Uani 1 1 d . . .
H9 H 1.1160 0.0266 1.3086 0.041 Uiso 1 1 calc R . .
C10 C 1.05556(18) 0.06972(15) 1.40679(19) 0.0376(6) Uani 1 1 d . . .
C11 C 0.96880(19) 0.08258(14) 1.43225(19) 0.0347(6) Uani 1 1 d . . .
H11 H 0.9697 0.1048 1.4883 0.042 Uiso 1 1 calc R . .
C12 C 0.88021(18) 0.06221(13) 1.37371(18) 0.0313(6) Uani 1 1 d . . .
C13 C 0.87943(18) 0.02715(13) 1.29162(19) 0.0332(6) Uani 1 1 d . . .
H13 H 0.8202 0.0125 1.2526 0.040 Uiso 1 1 calc R . .
C14 C 0.78626(19) 0.08102(14) 1.3998(2) 0.0354(6) Uani 1 1 d . . .
C15 C 1.22575(19) 0.10104(17) 1.4402(2) 0.0429(7) Uani 1 1 d . . .
C16 C 1.3004(3) 0.05696(17) 1.4735(3) 0.0597(9) Uani 1 1 d . . .
H16 H 1.2928 0.0209 1.5131 0.072 Uiso 1 1 calc R . .
C17 C 1.3873(2) 0.06545(18) 1.4489(3) 0.0624(10) Uani 1 1 d . . .
H17 H 1.4384 0.0342 1.4713 0.075 Uiso 1 1 calc R . .
C18 C 1.40167(18) 0.11836(13) 1.39233(18) 0.0314(6) Uani 1 1 d . . .
C19 C 1.3259(2) 0.1635(2) 1.3602(3) 0.0661(11) Uani 1 1 d . . .
H19 H 1.3339 0.2004 1.3222 0.079 Uiso 1 1 calc R . .
C20 C 1.2371(2) 0.1544(2) 1.3842(3) 0.0774(13) Uani 1 1 d . . .
H20 H 1.1851 0.1850 1.3618 0.093 Uiso 1 1 calc R . .
C21 C 1.49701(19) 0.12542(15) 1.36542(19) 0.0348(6) Uani 1 1 d . . .
C22 C 0.90817(19) 0.18273(14) 0.6973(2) 0.0396(7) Uani 1 1 d . . .
H22 H 0.9039 0.1371 0.6760 0.048 Uiso 1 1 calc R . .
C23 C 0.8708(2) 0.28046(16) 0.7437(3) 0.0543(9) Uani 1 1 d . . .
H23 H 0.8350 0.3167 0.7611 0.065 Uiso 1 1 calc R . .
C24 C 0.9673(2) 0.28358(17) 0.7437(3) 0.0616(10) Uani 1 1 d . . .
H24 H 1.0093 0.3214 0.7611 0.074 Uiso 1 1 calc R . .
C25 C 1.08951(18) 0.20099(13) 0.7077(2) 0.0334(6) Uani 1 1 d . . .
C26 C 1.14666(19) 0.16439(15) 0.7806(2) 0.0400(7) Uani 1 1 d . . .
H26 H 1.1193 0.1514 0.8294 0.048 Uiso 1 1 calc R . .
C27 C 1.1266(2) 0.22235(15) 0.6337(2) 0.0398(7) Uani 1 1 d . . .
C28 C 1.0669(3) 0.2627(2) 0.5526(2) 0.0674(10) Uani 1 1 d . . .
H28A H 1.0058 0.2389 0.5274 0.101 Uiso 1 1 calc R . .
H28B H 1.1033 0.2667 0.5056 0.101 Uiso 1 1 calc R . .
H28C H 1.0534 0.3083 0.5730 0.101 Uiso 1 1 calc R . .
C29 C 0.5127(2) 0.08805(14) 0.7075(2) 0.0434(7) Uani 1 1 d . . .
H29 H 0.5559 0.0512 0.7077 0.052 Uiso 1 1 calc R . .
C30 C 0.4178(2) 0.08147(15) 0.7091(2) 0.0498(8) Uani 1 1 d . . .
H30 H 0.3837 0.0402 0.7110 0.060 Uiso 1 1 calc R . .
C31 C 0.45575(18) 0.19138(13) 0.70472(19) 0.0315(6) Uani 1 1 d . . .
H31 H 0.4504 0.2396 0.7026 0.038 Uiso 1 1 calc R . .
C32 C 0.28062(18) 0.16606(14) 0.70953(19) 0.0318(6) Uani 1 1 d . . .
C33 C 0.2239(2) 0.20332(15) 0.6362(2) 0.0392(7) Uani 1 1 d . . .
H33 H 0.2510 0.2161 0.5872 0.047 Uiso 1 1 calc R . .
C34 C 0.24390(19) 0.14587(15) 0.7845(2) 0.0387(7) Uani 1 1 d . . .
C35 C 0.3042(2) 0.1090(2) 0.8682(2) 0.0647(10) Uani 1 1 d . . .
H35A H 0.3279 0.0658 0.8494 0.097 Uiso 1 1 calc R . .
H35B H 0.2640 0.0999 0.9111 0.097 Uiso 1 1 calc R . .
H35C H 0.3592 0.1376 0.8979 0.097 Uiso 1 1 calc R . .
C36 C 0.6053(2) 0.25560(16) 0.51829(19) 0.0500(8) Uani 1 1 d . . .
H36 H 0.6118 0.2133 0.4899 0.060 Uiso 1 1 calc R . .
C37 C 0.5673(3) 0.31388(16) 0.4729(2) 0.0530(9) Uani 1 1 d . . .
H37 H 0.5441 0.3194 0.4089 0.064 Uiso 1 1 calc R . .
C38 C 0.61031(19) 0.33286(14) 0.62164(18) 0.0330(6) Uani 1 1 d . . .
H38 H 0.6213 0.3555 0.6787 0.040 Uiso 1 1 calc R . .
C39 C 0.53389(18) 0.43368(13) 0.52216(17) 0.0307(6) Uani 1 1 d . . .
C40 C 0.57062(19) 0.47316(14) 0.46034(18) 0.0351(6) Uani 1 1 d . . .
H40 H 0.6184 0.4539 0.4337 0.042 Uiso 1 1 calc R . .
C41 C 0.46129(19) 0.45946(14) 0.56346(18) 0.0343(6) Uani 1 1 d . . .
C42 C 0.4156(2) 0.41781(17) 0.6275(2) 0.0558(9) Uani 1 1 d . . .
H42A H 0.4057 0.3708 0.6053 0.084 Uiso 1 1 calc R . .
H42B H 0.3532 0.4379 0.6294 0.084 Uiso 1 1 calc R . .
H42C H 0.4586 0.4180 0.6889 0.084 Uiso 1 1 calc R . .
Ni1 Ni 0.68429(2) 0.190131(15) 0.70944(2) 0.02466(12) Uani 1 1 d . . .
N1 N 0.83370(15) 0.21719(11) 0.71498(15) 0.0317(5) Uani 1 1 d . . .
N2 N 0.99144(15) 0.22095(11) 0.71342(16) 0.0349(5) Uani 1 1 d . . .
N3 N 0.53736(15) 0.15714(11) 0.70529(15) 0.0310(5) Uani 1 1 d . . .
N4 N 0.38055(15) 0.14774(11) 0.70755(16) 0.0342(5) Uani 1 1 d . . .
N5 N 0.63261(15) 0.26733(11) 0.61163(14) 0.0290(5) Uani 1 1 d . . .
N6 N 0.56980(15) 0.36304(11) 0.53946(14) 0.0306(5) Uani 1 1 d . . .
O1 O 0.73430(13) 0.12666(9) 0.82126(12) 0.0370(4) Uani 1 1 d . . .
O2 O 0.76482(15) 0.02583(10) 0.76040(13) 0.0459(5) Uani 1 1 d . . .
O3 O 0.70754(13) 0.06711(11) 1.33728(15) 0.0452(5) Uani 1 1 d . . .
O4 O 0.78888(15) 0.10776(12) 1.47535(15) 0.0539(6) Uani 1 1 d . . .
O5 O 1.55638(15) 0.07544(13) 1.39124(18) 0.0601(6) Uani 1 1 d D . .
O6 O 1.51365(14) 0.17581(11) 1.32027(14) 0.0461(5) Uani 1 1 d . . .
O7 O 1.13916(14) 0.09352(15) 1.46951(15) 0.0677(8) Uani 1 1 d . . .
O8 O 0.97101(13) -0.02314(9) 1.18855(12) 0.0365(4) Uani 1 1 d . . .
O1W O 0.68527(14) 0.26346(10) 0.81442(12) 0.0360(4) Uani 1 1 d D . .
O2W O 0.69013(13) 0.11038(10) 0.61705(13) 0.0345(4) Uani 1 1 d D . .
H5AA H 1.6086(15) 0.075(2) 1.375(3) 0.080 Uiso 1 1 d D . .
H3W H 0.717(2) 0.0789(13) 0.6516(17) 0.080 Uiso 1 1 d D . .
H1W H 0.6331(14) 0.2838(17) 0.812(2) 0.080 Uiso 1 1 d D . .
H4W H 0.713(2) 0.1169(17) 0.5718(15) 0.080 Uiso 1 1 d D . .
H2W H 0.713(2) 0.2484(18) 0.8660(10) 0.080 Uiso 1 1 d D . .


_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
C1 O2 1.240(3) . ?
C1 O1 1.268(3) . ?
C1 C2 1.509(4) . ?
C2 C3 1.385(4) . ?
C2 C7 1.384(4) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(4) . ?
C4 H4 0.9300 . ?
C5 O8 1.380(3) . ?
C5 C6 1.384(4) . ?
C6 C7 1.376(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.378(4) . ?
C8 C13 1.381(4) . ?
C8 O8 1.399(3) . ?
C9 C10 1.385(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.376(4) . ?
C10 O7 1.381(3) . ?
C11 C12 1.383(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.388(4) . ?
C12 C14 1.500(4) . ?
C13 H13 0.9300 . ?
C14 O4 1.223(3) . ?
C14 O3 1.281(3) . ?
C15 C16 1.341(4) . ?
C15 C20 1.353(5) . ?
C15 O7 1.388(3) . ?
C16 C17 1.359(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.363(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.361(4) . ?
C18 C21 1.486(4) . ?
C19 C20 1.381(5) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O6 1.231(3) . ?
C21 O5 1.266(3) . ?
C22 N1 1.312(3) . ?
C22 N2 1.347(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.349(4) . ?
C23 N1 1.350(4) . ?
C23 H23 0.9300 . ?
C24 N2 1.356(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.370(4) . ?
C25 C27 1.384(4) . ?
C25 N2 1.445(3) . ?
C26 C34 1.391(4) 1_655 ?
C26 H26 0.9300 . ?
C27 C33 1.399(4) 1_655 ?
C27 C28 1.501(4) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.338(4) . ?
C29 N3 1.375(3) . ?
C29 H29 0.9300 . ?
C30 N4 1.374(4) . ?
C30 H30 0.9300 . ?
C31 N3 1.314(3) . ?
C31 N4 1.353(3) . ?
C31 H31 0.9300 . ?
C32 C33 1.378(4) . ?
C32 C34 1.387(4) . ?
C32 N4 1.446(3) . ?
C33 C27 1.399(4) 1_455 ?
C33 H33 0.9300 . ?
C34 C26 1.391(4) 1_455 ?
C34 C35 1.497(4) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.347(4) . ?
C36 N5 1.360(3) . ?
C36 H36 0.9300 . ?
C37 N6 1.360(4) . ?
C37 H37 0.9300 . ?
C38 N5 1.315(3) . ?
C38 N6 1.343(3) . ?
C38 H38 0.9300 . ?
C39 C40 1.381(4) . ?
C39 C41 1.396(4) . ?
C39 N6 1.449(3) . ?
C40 C41 1.387(4) 3_666 ?
C40 H40 0.9300 . ?
C41 C40 1.387(4) 3_666 ?
C41 C42 1.498(4) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
Ni1 O1 2.0387(17) . ?
Ni1 O2W 2.0701(18) . ?
Ni1 N5 2.077(2) . ?
Ni1 O1W 2.0966(18) . ?
Ni1 N1 2.132(2) . ?
Ni1 N3 2.134(2) . ?
O5 H5AA 0.8202(11) . ?
O1W H1W 0.8199(11) . ?
O1W H2W 0.8202(11) . ?
O2W H3W 0.8201(11) . ?
O2W H4W 0.8196(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 124.8(2) . . ?
O2 C1 C2 119.6(2) . . ?
O1 C1 C2 115.6(2) . . ?
C3 C2 C7 118.4(2) . . ?
C3 C2 C1 121.2(2) . . ?
C7 C2 C1 120.3(2) . . ?
C2 C3 C4 120.7(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 119.9(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
O8 C5 C4 116.1(2) . . ?
O8 C5 C6 123.8(2) . . ?
C4 C5 C6 120.0(2) . . ?
C7 C6 C5 119.5(3) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C2 121.6(2) . . ?
C6 C7 H7 119.2 . . ?
C2 C7 H7 119.2 . . ?
C9 C8 C13 121.9(2) . . ?
C9 C8 O8 117.0(2) . . ?
C13 C8 O8 121.0(2) . . ?
C8 C9 C10 117.8(2) . . ?
C8 C9 H9 121.1 . . ?
C10 C9 H9 121.1 . . ?
C11 C10 O7 114.4(2) . . ?
C11 C10 C9 121.8(2) . . ?
O7 C10 C9 123.9(2) . . ?
C10 C11 C12 119.3(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C13 120.1(2) . . ?
C11 C12 C14 118.4(2) . . ?
C13 C12 C14 121.5(2) . . ?
C8 C13 C12 119.0(2) . . ?
C8 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
O4 C14 O3 125.3(3) . . ?
O4 C14 C12 120.3(3) . . ?
O3 C14 C12 114.4(2) . . ?
C16 C15 C20 120.6(3) . . ?
C16 C15 O7 118.5(3) . . ?
C20 C15 O7 120.8(3) . . ?
C15 C16 C17 119.3(3) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 122.0(3) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C19 C18 C17 118.1(3) . . ?
C19 C18 C21 121.3(3) . . ?
C17 C18 C21 120.6(2) . . ?
C18 C19 C20 120.1(3) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C15 C20 C19 119.9(3) . . ?
C15 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
O6 C21 O5 124.4(3) . . ?
O6 C21 C18 121.2(2) . . ?
O5 C21 C18 114.4(2) . . ?
N1 C22 N2 112.4(2) . . ?
N1 C22 H22 123.8 . . ?
N2 C22 H22 123.8 . . ?
C24 C23 N1 110.3(3) . . ?
C24 C23 H23 124.9 . . ?
N1 C23 H23 124.8 . . ?
C23 C24 N2 106.8(3) . . ?
C23 C24 H24 126.6 . . ?
N2 C24 H24 126.6 . . ?
C26 C25 C27 121.2(2) . . ?
C26 C25 N2 117.9(2) . . ?
C27 C25 N2 120.8(2) . . ?
C25 C26 C34 122.7(3) . 1_655 ?
C25 C26 H26 118.7 . . ?
C34 C26 H26 118.7 1_655 . ?
C25 C27 C33 116.8(3) . 1_655 ?
C25 C27 C28 123.0(3) . . ?
C33 C27 C28 120.2(3) 1_655 . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N3 110.3(2) . . ?
C30 C29 H29 124.9 . . ?
N3 C29 H29 124.9 . . ?
C29 C30 N4 106.5(2) . . ?
C29 C30 H30 126.7 . . ?
N4 C30 H30 126.7 . . ?
N3 C31 N4 111.6(2) . . ?
N3 C31 H31 124.2 . . ?
N4 C31 H31 124.2 . . ?
C33 C32 C34 121.5(2) . . ?
C33 C32 N4 118.8(2) . . ?
C34 C32 N4 119.6(2) . . ?
C32 C33 C27 121.7(3) . 1_455 ?
C32 C33 H33 119.2 . . ?
C27 C33 H33 119.2 1_455 . ?
C32 C34 C26 116.2(2) . 1_455 ?
C32 C34 C35 123.6(2) . . ?
C26 C34 C35 120.2(3) 1_455 . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 N5 110.4(3) . . ?
C37 C36 H36 124.8 . . ?
N5 C36 H36 124.8 . . ?
C36 C37 N6 106.2(2) . . ?
C36 C37 H37 126.9 . . ?
N6 C37 H37 126.9 . . ?
N5 C38 N6 111.8(2) . . ?
N5 C38 H38 124.1 . . ?
N6 C38 H38 124.1 . . ?
C40 C39 C41 121.5(2) . . ?
C40 C39 N6 117.7(2) . . ?
C41 C39 N6 120.8(2) . . ?
C39 C40 C41 122.3(2) . 3_666 ?
C39 C40 H40 118.9 . . ?
C41 C40 H40 118.9 3_666 . ?
C40 C41 C39 116.3(2) 3_666 . ?
C40 C41 C42 120.0(2) 3_666 . ?
C39 C41 C42 123.7(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O1 Ni1 O2W 91.88(7) . . ?
O1 Ni1 N5 170.58(8) . . ?
O2W Ni1 N5 97.54(8) . . ?
O1 Ni1 O1W 82.01(7) . . ?
O2W Ni1 O1W 173.86(7) . . ?
N5 Ni1 O1W 88.57(8) . . ?
O1 Ni1 N1 88.66(8) . . ?
O2W Ni1 N1 90.60(8) . . ?
N5 Ni1 N1 91.31(8) . . ?
O1W Ni1 N1 88.73(8) . . ?
O1 Ni1 N3 88.97(8) . . ?
O2W Ni1 N3 87.32(8) . . ?
N5 Ni1 N3 91.38(8) . . ?
O1W Ni1 N3 93.08(8) . . ?
N1 Ni1 N3 176.79(8) . . ?
C22 N1 C23 104.8(2) . . ?
C22 N1 Ni1 133.21(19) . . ?
C23 N1 Ni1 121.95(18) . . ?
C22 N2 C24 105.7(2) . . ?
C22 N2 C25 129.4(2) . . ?
C24 N2 C25 124.8(2) . . ?
C31 N3 C29 105.2(2) . . ?
C31 N3 Ni1 132.64(18) . . ?
C29 N3 Ni1 122.06(17) . . ?
C31 N4 C30 106.4(2) . . ?
C31 N4 C32 127.6(2) . . ?
C30 N4 C32 126.1(2) . . ?
C38 N5 C36 104.9(2) . . ?
C38 N5 Ni1 131.13(17) . . ?
C36 N5 Ni1 123.65(18) . . ?
C38 N6 C37 106.7(2) . . ?
C38 N6 C39 128.1(2) . . ?
C37 N6 C39 125.2(2) . . ?
C1 O1 Ni1 131.24(17) . . ?
C21 O5 H5AA 118(3) . . ?
C10 O7 C15 118.8(2) . . ?
C5 O8 C8 119.23(19) . . ?
Ni1 O1W H1W 117(2) . . ?
Ni1 O1W H2W 112(2) . . ?
H1W O1W H2W 114.6(2) . . ?
Ni1 O2W H3W 103(2) . . ?
Ni1 O2W H4W 121(3) . . ?
H3W O2W H4W 114.6(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 986463'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C156 H114 N16 Ni5 O38'
_chemical_formula_sum            'C156 H114 N16 Ni5 O38'
_chemical_formula_weight         3114.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.5871(9)
_cell_length_b                   16.6281(11)
_cell_length_c                   17.3904(11)
_cell_angle_alpha                63.1710(10)
_cell_angle_beta                 65.8790(10)
_cell_angle_gamma                86.1310(10)
_cell_volume                     3399.8(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4846
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1606
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8423
_exptl_absorpt_correction_T_max  0.8735
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17385
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11646
_reflns_number_gt                8417
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2500P)²+1.3460P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11646
_refine_ls_number_parameters     989
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0779
_refine_ls_wR_factor_ref         0.3120
_refine_ls_wR_factor_gt          0.2600
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.688(2) 0.4115(17) 0.405(2) 0.087(11) Uani 1 1 d . . .
C2 C 0.7668(18) 0.3310(15) 0.3066(16) 0.049(6) Uani 1 1 d . . .
H2 H 0.7304 0.2760 0.3588 0.058 Uiso 1 1 calc R . .
C3 C 0.8291(15) 0.3347(13) 0.2195(16) 0.039(5) Uani 1 1 d . . .
C4 C 0.8826(16) 0.4159(14) 0.1407(15) 0.044(5) Uani 1 1 d . . .
H4 H 0.9220 0.4178 0.0821 0.053 Uiso 1 1 calc R . .
C5 C 0.8763(17) 0.4943(13) 0.1506(15) 0.042(5) Uani 1 1 d . . .
C6 C 0.8149(18) 0.4923(14) 0.2360(16) 0.053(6) Uani 1 1 d . . .
H6 H 0.8101 0.5458 0.2414 0.063 Uiso 1 1 calc R . .
C7 C 0.951(2) 0.6485(14) 0.0796(16) 0.054(6) Uani 1 1 d . . .
C8 C 1.039(2) 0.6601(16) 0.084(2) 0.060(7) Uani 1 1 d . . .
H8 H 1.0843 0.6179 0.0816 0.072 Uiso 1 1 calc R . .
C9 C 1.063(2) 0.7360(17) 0.091(2) 0.060(7) Uani 1 1 d . . .
H9 H 1.1235 0.7448 0.0929 0.072 Uiso 1 1 calc R . .
C10 C 0.9949(16) 0.7981(14) 0.0940(14) 0.041(5) Uani 1 1 d . . .
C11 C 0.9038(18) 0.7845(15) 0.0902(17) 0.050(6) Uani 1 1 d . . .
H11 H 0.8578 0.8257 0.0929 0.060 Uiso 1 1 calc R . .
C12 C 0.8820(19) 0.7095(16) 0.0825(18) 0.054(6) Uani 1 1 d . . .
H12 H 0.8218 0.7004 0.0792 0.065 Uiso 1 1 calc R . .
C13 C 1.0157(18) 0.8790(15) 0.1037(16) 0.047(5) Uani 1 1 d . . .
C14 C 0.7598(19) 0.4107(15) 0.3146(16) 0.056(7) Uani 1 1 d . . .
C15 C 0.9192(15) 0.2187(13) 0.1898(14) 0.036(4) Uani 1 1 d . . .
C16 C 0.9189(15) 0.1488(13) 0.1675(14) 0.037(4) Uani 1 1 d . . .
H16 H 0.8612 0.1305 0.1658 0.044 Uiso 1 1 calc R . .
C17 C 1.0036(15) 0.1059(13) 0.1476(14) 0.036(4) Uani 1 1 d . . .
H17 H 1.0022 0.0584 0.1336 0.043 Uiso 1 1 calc R . .
C18 C 1.0908(14) 0.1334(13) 0.1484(13) 0.033(4) Uani 1 1 d . . .
C19 C 1.0916(16) 0.2035(14) 0.1703(15) 0.041(5) Uani 1 1 d . . .
H19 H 1.1501 0.2229 0.1699 0.049 Uiso 1 1 calc R . .
C20 C 1.0056(17) 0.2453(14) 0.1927(16) 0.045(5) Uani 1 1 d . . .
H20 H 1.0058 0.2910 0.2097 0.054 Uiso 1 1 calc R . .
C21 C 1.1839(15) 0.0903(14) 0.1212(13) 0.035(4) Uani 1 1 d . . .
C22 C 0.466(3) 0.4773(19) 0.706(2) 0.094(13) Uani 1 1 d . . .
C23 C 0.429(2) 0.5053(17) 0.7839(19) 0.072(9) Uani 1 1 d . . .
C24 C 0.4404(19) 0.5960(16) 0.7592(18) 0.055(6) Uani 1 1 d . . .
H24 H 0.4692 0.6393 0.6954 0.066 Uiso 1 1 calc R . .
C25 C 0.4088(19) 0.6226(15) 0.8289(17) 0.051(6) Uani 1 1 d . . .
C26 C 0.366(2) 0.5593(15) 0.9253(17) 0.054(6) Uani 1 1 d . . .
H26 H 0.3432 0.5782 0.9720 0.065 Uiso 1 1 calc R . .
C27 C 0.357(2) 0.4691(17) 0.9492(19) 0.065(8) Uani 1 1 d . . .
C28 C 0.389(2) 0.4396(18) 0.881(2) 0.084(11) Uani 1 1 d . . .
H28 H 0.3835 0.3778 0.8981 0.100 Uiso 1 1 calc R . .
C29 C 0.277(2) 0.4282(16) 1.1134(18) 0.066(8) Uani 1 1 d . . .
C30 C 0.332(3) 0.444(2) 1.157(4) 0.099(13) Uani 1 1 d . . .
H30 H 0.4011 0.4412 1.1337 0.119 Uiso 1 1 calc R . .
C31 C 0.288(4) 0.462(2) 1.229(4) 0.106(15) Uani 1 1 d . . .
H31 H 0.3268 0.4712 1.2566 0.127 Uiso 1 1 calc R . .
C32 C 0.190(3) 0.4675(17) 1.2626(18) 0.082(11) Uani 1 1 d D . .
C33 C 0.128(2) 0.4533(18) 1.2247(17) 0.062(7) Uani 1 1 d . . .
H33 H 0.0593 0.4569 1.2498 0.075 Uiso 1 1 calc R . .
C34 C 0.173(2) 0.4335(18) 1.1485(17) 0.062(7) Uani 1 1 d . . .
H34 H 0.1337 0.4240 1.1215 0.074 Uiso 1 1 calc R . .
C35 C 0.140(3) 0.485(3) 1.347(2) 0.15(3) Uani 1 1 d D . .
C36 C 0.414(2) 0.7438(15) 0.8630(16) 0.051(6) Uani 1 1 d . . .
C37 C 0.497(2) 0.7417(15) 0.8823(18) 0.060(7) Uani 1 1 d . . .
H37 H 0.5500 0.7124 0.8600 0.072 Uiso 1 1 calc R . .
C38 C 0.5020(18) 0.7831(15) 0.9349(17) 0.047(5) Uani 1 1 d . . .
H38 H 0.5586 0.7824 0.9470 0.057 Uiso 1 1 calc R . .
C39 C 0.4207(16) 0.8253(13) 0.9688(15) 0.039(5) Uani 1 1 d . . .
C40 C 0.3351(17) 0.8195(15) 0.9545(16) 0.046(5) Uani 1 1 d . . .
H40 H 0.2783 0.8429 0.9817 0.055 Uiso 1 1 calc R . .
C41 C 0.3322(19) 0.7802(15) 0.9013(17) 0.049(6) Uani 1 1 d . . .
H41 H 0.2746 0.7783 0.8912 0.058 Uiso 1 1 calc R . .
C42 C 0.4298(16) 0.8838(14) 1.0108(14) 0.037(4) Uani 1 1 d . . .
C43 C 1.3679(16) 0.0042(15) 0.2285(14) 0.039(5) Uani 1 1 d . . .
H43 H 1.3630 0.0655 0.2111 0.047 Uiso 1 1 calc R . .
C44 C 1.3734(19) -0.1251(16) 0.2302(16) 0.049(5) Uani 1 1 d . . .
H44 H 1.3740 -0.1703 0.2125 0.058 Uiso 1 1 calc R . .
C45 C 1.3841(19) -0.1372(16) 0.3078(16) 0.049(5) Uani 1 1 d . . .
H45 H 1.3911 -0.1915 0.3536 0.058 Uiso 1 1 calc R . .
C46 C 1.3865(15) -0.0304(15) 0.3744(14) 0.039(5) Uani 1 1 d . . .
C47 C 1.3519(19) -0.0928(16) 0.4673(15) 0.050(6) Uani 1 1 d . . .
H47 H 1.3299 -0.1529 0.4866 0.060 Uiso 1 1 calc R . .
C48 C 1.349(2) -0.0673(16) 0.5328(15) 0.052(6) Uani 1 1 d . . .
H48 H 1.3250 -0.1108 0.5965 0.062 Uiso 1 1 calc R . .
C49 C 1.3822(16) 0.0212(14) 0.5076(14) 0.038(4) Uani 1 1 d . . .
C50 C 1.421(2) 0.0821(17) 0.4111(14) 0.052(6) Uani 1 1 d . . .
H50 H 1.4444 0.1421 0.3904 0.063 Uiso 1 1 calc R . .
C51 C 1.425(2) 0.0560(17) 0.3456(15) 0.055(7) Uani 1 1 d . . .
H51 H 1.4534 0.0975 0.2812 0.066 Uiso 1 1 calc R . .
C52 C 1.3728(15) 0.0501(14) 0.5794(13) 0.036(4) Uani 1 1 d . . .
C53 C 1.323(2) -0.0084(18) 0.6756(16) 0.069(9) Uani 1 1 d . . .
H53 H 1.2973 -0.0673 0.6950 0.083 Uiso 1 1 calc R . .
C54 C 1.311(2) 0.0172(18) 0.7436(17) 0.070(9) Uani 1 1 d . . .
H54 H 1.2740 -0.0234 0.8076 0.084 Uiso 1 1 calc R . .
C55 C 1.3514(16) 0.1015(14) 0.7184(14) 0.038(5) Uani 1 1 d . . .
C56 C 1.402(2) 0.1615(15) 0.6234(16) 0.054(6) Uani 1 1 d . . .
H56 H 1.4297 0.2196 0.6046 0.065 Uiso 1 1 calc R . .
C57 C 1.411(2) 0.1351(15) 0.5551(15) 0.051(6) Uani 1 1 d . . .
H57 H 1.4453 0.1767 0.4910 0.061 Uiso 1 1 calc R . .
C58 C 1.3319(18) 0.0631(15) 0.8787(15) 0.045(5) Uani 1 1 d . . .
H58 H 1.3172 0.0005 0.9036 0.054 Uiso 1 1 calc R . .
C59 C 1.3627(19) 0.2075(14) 0.7820(16) 0.049(6) Uani 1 1 d . . .
H59 H 1.3740 0.2636 0.7292 0.059 Uiso 1 1 calc R . .
C60 C 1.3596(17) 0.1929(14) 0.8658(16) 0.042(5) Uani 1 1 d . . .
H60 H 1.3686 0.2384 0.8803 0.050 Uiso 1 1 calc R . .
C61 C 0.783(3) 0.6688(19) 0.365(2) 0.092(12) Uani 1 1 d . . .
H61 H 0.7972 0.6515 0.3179 0.110 Uiso 1 1 calc R . .
C62 C 0.835(2) 0.7382(18) 0.3555(19) 0.074(9) Uani 1 1 d . . .
H62 H 0.8894 0.7784 0.3007 0.088 Uiso 1 1 calc R . .
C63 C 0.713(2) 0.6709(15) 0.4979(18) 0.064(8) Uani 1 1 d . . .
H63 H 0.6691 0.6577 0.5600 0.077 Uiso 1 1 calc R . .
C64 C 0.8198(18) 0.8059(14) 0.4631(16) 0.048(5) Uani 1 1 d . . .
C65 C 0.801(2) 0.7848(17) 0.5542(19) 0.064(7) Uani 1 1 d . . .
H65 H 0.7749 0.7255 0.6026 0.077 Uiso 1 1 calc R . .
C66 C 0.819(2) 0.8512(17) 0.5749(18) 0.061(7) Uani 1 1 d . . .
H66 H 0.8041 0.8359 0.6377 0.073 Uiso 1 1 calc R . .
C67 C 0.8599(17) 0.9398(15) 0.5051(15) 0.043(5) Uani 1 1 d . . .
C68 C 0.8829(18) 0.9580(15) 0.4122(16) 0.049(6) Uani 1 1 d . . .
H68 H 0.9128 1.0163 0.3630 0.059 Uiso 1 1 calc R . .
C69 C 0.8633(17) 0.8931(15) 0.3907(16) 0.048(5) Uani 1 1 d . . .
H69 H 0.8790 0.9076 0.3281 0.058 Uiso 1 1 calc R . .
C70 C 0.8753(16) 1.0138(15) 0.5267(15) 0.042(5) Uani 1 1 d . . .
C71 C 0.8668(19) 0.9966(16) 0.6150(16) 0.052(6) Uani 1 1 d . . .
H71 H 0.8525 0.9364 0.6621 0.062 Uiso 1 1 calc R . .
C72 C 0.8784(19) 1.0640(17) 0.6365(17) 0.054(6) Uani 1 1 d . . .
H72 H 0.8735 1.0489 0.6966 0.064 Uiso 1 1 calc R . .
C73 C 0.8973(16) 1.1540(16) 0.5692(16) 0.046(5) Uani 1 1 d . . .
C74 C 0.906(3) 1.1739(17) 0.4798(18) 0.066(8) Uani 1 1 d . . .
H74 H 0.9197 1.2342 0.4330 0.079 Uiso 1 1 calc R . .
C75 C 0.894(2) 1.1050(17) 0.4602(18) 0.063(7) Uani 1 1 d . . .
H75 H 0.8985 1.1200 0.4002 0.075 Uiso 1 1 calc R . .
C76 C 0.9501(19) 1.3120(17) 0.5282(17) 0.052(6) Uani 1 1 d . . .
H76 H 0.9744 1.3354 0.4627 0.063 Uiso 1 1 calc R . .
C77 C 0.884(2) 1.218(2) 0.6799(18) 0.066(7) Uani 1 1 d . . .
H77 H 0.8555 1.1660 0.7384 0.079 Uiso 1 1 calc R . .
C78 C 0.909(2) 1.3011(19) 0.6652(17) 0.065(7) Uani 1 1 d . . .
H78 H 0.8996 1.3164 0.7131 0.078 Uiso 1 1 calc R . .
N1 N 0.706(2) 0.6265(14) 0.4559(16) 0.080(8) Uani 1 1 d . . .
N2 N 0.7934(16) 0.7399(12) 0.4403(14) 0.056(5) Uani 1 1 d . . .
N3 N 0.9099(15) 1.2241(13) 0.5903(13) 0.048(5) Uani 1 1 d . . .
N4 N 0.9519(16) 1.3614(14) 0.5689(13) 0.053(5) Uani 1 1 d . . .
N5 N 1.3616(13) -0.0360(12) 0.1807(12) 0.040(4) Uani 1 1 d . . .
N6 N 1.3826(13) -0.0543(12) 0.3062(11) 0.039(4) Uani 1 1 d . . .
N7 N 1.3459(13) 0.1237(12) 0.7895(11) 0.040(4) Uani 1 1 d . . .
N8 N 1.3412(13) 0.1019(12) 0.9262(12) 0.039(4) Uani 1 1 d . . .
Ni1 Ni 1.34610(19) 0.03193(17) 0.05638(17) 0.0339(9) Uani 1 1 d . . .
Ni3 Ni 0.0000 0.5000 1.5000 0.0432(12) Uani 1 2 d SD . .
Ni2 Ni 0.6018(3) 0.5172(2) 0.5107(3) 0.103(2) Uani 1 1 d D . .
O1 O 0.679(3) 0.4224(14) 0.5935(15) 0.144(14) Uani 1 1 d D . .
O2 O 0.5099(16) 0.5938(10) 0.4335(12) 0.100(9) Uani 1 1 d D . .
O3 O 0.6854(16) 0.4887(11) 0.4040(13) 0.092(8) Uani 1 1 d . . .
O4 O 0.636(2) 0.3380(12) 0.4758(15) 0.120(12) Uani 1 1 d . . .
O5 O 0.5198(18) 0.5392(13) 0.6232(15) 0.109(10) Uani 1 1 d . . .
O6 O 0.440(2) 0.3992(14) 0.7264(16) 0.131(13) Uani 1 1 d . . .
O7 O 0.9298(14) 0.5741(10) 0.0689(11) 0.065(5) Uani 1 1 d . . .
O8 O 0.8301(10) 0.2544(9) 0.2120(11) 0.044(4) Uani 1 1 d . . .
O9 O 1.1786(11) 0.0151(9) 0.1216(10) 0.041(3) Uani 1 1 d . . .
O10 O 1.2685(11) 0.1304(10) 0.0987(11) 0.043(3) Uani 1 1 d . . .
O11 O 0.9533(15) 0.9236(13) 0.1259(17) 0.077(6) Uani 1 1 d . . .
O12 O 1.1112(15) 0.8947(14) 0.0865(17) 0.073(6) Uani 1 1 d . . .
H12A H 1.1163 0.9295 0.1066 0.109 Uiso 1 1 calc R . .
O13 O 0.4166(17) 0.7140(10) 0.7998(12) 0.071(6) Uani 1 1 d . . .
O14 O 0.318(2) 0.4008(13) 1.0441(15) 0.104(9) Uani 1 1 d . . .
O15 O 0.3531(11) 0.9184(10) 1.0409(11) 0.043(3) Uani 1 1 d . . .
O16 O 0.5117(12) 0.8944(11) 1.0139(11) 0.050(4) Uani 1 1 d . . .
O17 O 0.185(4) 0.482(2) 1.396(3) 0.26(3) Uani 1 1 d D . .
O18 O 0.049(3) 0.498(2) 1.3738(19) 0.21(3) Uani 1 1 d D . .
O19 O -0.122(3) 0.513(3) 1.465(2) 0.162(15) Uani 1 1 d D . .
H3W H 0.466(11) 0.625(10) 0.450(9) 0.080 Uiso 1 1 d D . .
H2W H 0.683(11) 0.420(9) 0.641(6) 0.080 Uiso 1 1 d D . .
H1W H 0.724(16) 0.390(10) 0.573(10) 0.080 Uiso 1 1 d D . .
H4W H 0.504(14) 0.586(14) 0.389(9) 0.080 Uiso 1 1 d D . .
H5W H -0.126(5) 0.529(14) 1.404(8) 0.080 Uiso 1 1 d D . .
H6W H -0.191(7) 0.481(7) 1.499(9) 0.080 Uiso 1 1 d D . .


_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
C1 O4 1.26(3) . ?
C1 O3 1.28(3) . ?
C1 C14 1.49(3) . ?
C2 C3 1.39(3) . ?
C2 C14 1.39(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.38(3) . ?
C3 O8 1.40(2) . ?
C4 C5 1.38(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.37(3) . ?
C5 O7 1.39(2) . ?
C6 C14 1.39(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.35(4) . ?
C7 C12 1.38(4) . ?
C7 O7 1.40(3) . ?
C8 C9 1.40(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.38(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.40(3) . ?
C10 C13 1.49(3) . ?
C11 C12 1.38(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 O11 1.19(3) . ?
C13 O12 1.32(3) . ?
C15 O8 1.37(2) . ?
C15 C16 1.38(3) . ?
C15 C20 1.39(3) . ?
C16 C17 1.38(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.39(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.38(3) . ?
C18 C21 1.49(3) . ?
C19 C20 1.39(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O10 1.26(2) . ?
C21 O9 1.25(2) . ?
C21 Ni1 2.512(19) . ?
C22 O6 1.22(3) . ?
C22 O5 1.27(3) . ?
C22 C23 1.51(3) . ?
C23 C24 1.37(3) . ?
C23 C28 1.41(4) . ?
C24 C25 1.37(3) . ?
C24 H24 0.9300 . ?
C25 O13 1.36(3) . ?
C25 C26 1.40(3) . ?
C26 C27 1.36(3) . ?
C26 H26 0.9300 . ?
C27 C28 1.39(4) . ?
C27 O14 1.40(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.40(5) . ?
C29 O14 1.37(3) . ?
C29 C34 1.40(4) . ?
C30 C31 1.32(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.32(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.40(4) . ?
C32 C35 1.500(4) . ?
C33 C34 1.40(3) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 O18 1.250(4) . ?
C35 O17 1.250(4) . ?
C36 C37 1.37(4) . ?
C36 C41 1.36(4) . ?
C36 O13 1.38(3) . ?
C37 C38 1.40(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.39(3) . ?
C38 H38 0.9300 . ?
C39 C40 1.39(3) . ?
C39 C42 1.50(3) . ?
C40 C41 1.37(3) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C42 O16 1.25(2) . ?
C42 O15 1.25(3) . ?
C43 N5 1.31(2) . ?
C43 N6 1.36(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.34(3) . ?
C44 N5 1.38(3) . ?
C44 H44 0.9300 . ?
C45 N6 1.37(3) . ?
C45 H45 0.9300 . ?
C46 C47 1.35(3) . ?
C46 C51 1.36(3) . ?
C46 N6 1.43(2) . ?
C47 C48 1.37(3) . ?
C47 H47 0.9300 . ?
C48 C49 1.39(3) . ?
C48 H48 0.9300 . ?
C49 C50 1.39(3) . ?
C49 C52 1.48(3) . ?
C50 C51 1.37(3) . ?
C50 H50 0.9300 . ?
C51 H51 0.9300 . ?
C52 C57 1.37(3) . ?
C52 C53 1.38(3) . ?
C53 C54 1.37(3) . ?
C53 H53 0.9300 . ?
C54 C55 1.36(3) . ?
C54 H54 0.9300 . ?
C55 C56 1.37(3) . ?
C55 N7 1.42(2) . ?
C56 C57 1.40(3) . ?
C56 H56 0.9300 . ?
C57 H57 0.9300 . ?
C58 N8 1.30(3) . ?
C58 N7 1.35(3) . ?
C58 H58 0.9300 . ?
C59 C60 1.35(3) . ?
C59 N7 1.37(3) . ?
C59 H59 0.9300 . ?
C60 N8 1.36(3) . ?
C60 H60 0.9300 . ?
C61 C62 1.33(4) . ?
C61 N1 1.38(3) . ?
C61 H61 0.9300 . ?
C62 N2 1.36(3) . ?
C62 H62 0.9300 . ?
C63 N1 1.28(3) . ?
C63 N2 1.37(3) . ?
C63 H63 0.9300 . ?
C64 C65 1.36(4) . ?
C64 C69 1.38(3) . ?
C64 N2 1.44(3) . ?
C65 C66 1.38(4) . ?
C65 H65 0.9300 . ?
C66 C67 1.38(3) . ?
C66 H66 0.9300 . ?
C67 C68 1.39(3) . ?
C67 C70 1.49(3) . ?
C68 C69 1.37(3) . ?
C68 H68 0.9300 . ?
C69 H69 0.9300 . ?
C70 C71 1.38(3) . ?
C70 C75 1.39(3) . ?
C71 C72 1.37(3) . ?
C71 H71 0.9300 . ?
C72 C73 1.38(3) . ?
C72 H72 0.9300 . ?
C73 C74 1.39(3) . ?
C73 N3 1.41(3) . ?
C74 C75 1.37(3) . ?
C74 H74 0.9300 . ?
C75 H75 0.9300 . ?
C76 N4 1.31(3) . ?
C76 N3 1.35(3) . ?
C76 H76 0.9300 . ?
C77 C78 1.33(4) . ?
C77 N3 1.40(3) . ?
C77 H77 0.9300 . ?
C78 N4 1.38(3) . ?
C78 H78 0.9300 . ?
N1 Ni2 2.04(2) . ?
N4 Ni3 2.07(2) 1_664 ?
N5 Ni1 2.040(16) . ?
N8 Ni1 2.056(17) 1_556 ?
Ni1 O15 2.015(14) 1_644 ?
Ni1 O16 2.053(15) 2_766 ?
Ni1 N8 2.056(17) 1_554 ?
Ni1 O10 2.159(14) . ?
Ni1 O9 2.209(15) . ?
Ni3 O18 2.03(2) 2_568 ?
Ni3 O18 2.03(2) . ?
Ni3 N4 2.07(2) 1_446 ?
Ni3 N4 2.07(2) 2_677 ?
Ni3 O19 2.07(4) 2_568 ?
Ni3 O19 2.07(4) . ?
Ni2 O3 2.004(16) . ?
Ni2 O5 2.018(17) . ?
Ni2 O2 2.120(19) 2_666 ?
Ni2 O2 2.22(2) . ?
Ni2 O1 2.21(3) . ?
O1 H2W 0.84(4) . ?
O1 H1W 0.89(8) . ?
O2 Ni2 2.120(19) 2_666 ?
O2 H3W 0.84(2) . ?
O2 H4W 0.86(7) . ?
O12 H12A 0.8202 . ?
O15 Ni1 2.015(14) 1_466 ?
O16 Ni1 2.053(15) 2_766 ?
O19 H5W 1.01(6) . ?
O19 H6W 0.98(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 C1 O3 124(2) . . ?
O4 C1 C14 120(2) . . ?
O3 C1 C14 116(2) . . ?
C3 C2 C14 118.9(19) . . ?
C3 C2 H2 120.6 . . ?
C14 C2 H2 120.5 . . ?
C2 C3 C4 121.5(18) . . ?
C2 C3 O8 117.6(18) . . ?
C4 C3 O8 120.7(18) . . ?
C5 C4 C3 118.8(19) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C6 C5 C4 120.7(19) . . ?
C6 C5 O7 122.7(18) . . ?
C4 C5 O7 116.4(18) . . ?
C5 C6 C14 120.2(19) . . ?
C5 C6 H6 119.9 . . ?
C14 C6 H6 119.9 . . ?
C8 C7 C12 122(2) . . ?
C8 C7 O7 119(2) . . ?
C12 C7 O7 119(2) . . ?
C7 C8 C9 119(2) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 120(2) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C11 120(2) . . ?
C9 C10 C13 122(2) . . ?
C11 C10 C13 118.7(19) . . ?
C12 C11 C10 120(2) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C7 C12 C11 119(2) . . ?
C7 C12 H12 120.4 . . ?
C11 C12 H12 120.3 . . ?
O11 C13 O12 123(2) . . ?
O11 C13 C10 124(2) . . ?
O12 C13 C10 112(2) . . ?
C2 C14 C6 120(2) . . ?
C2 C14 C1 120.8(19) . . ?
C6 C14 C1 119.1(19) . . ?
O8 C15 C16 116.1(18) . . ?
O8 C15 C20 124.5(17) . . ?
C16 C15 C20 119.4(18) . . ?
C17 C16 C15 120.6(19) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 120.4(17) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C19 C18 C17 119.2(17) . . ?
C19 C18 C21 120.8(18) . . ?
C17 C18 C21 119.9(17) . . ?
C18 C19 C20 120.6(19) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C19 C20 C15 119.8(18) . . ?
C19 C20 H20 120.1 . . ?
C15 C20 H20 120.1 . . ?
O10 C21 O9 120.3(18) . . ?
O10 C21 C18 118.9(17) . . ?
O9 C21 C18 120.8(18) . . ?
O10 C21 Ni1 59.3(10) . . ?
O9 C21 Ni1 61.5(10) . . ?
C18 C21 Ni1 173.5(14) . . ?
O6 C22 O5 125(2) . . ?
O6 C22 C23 119(2) . . ?
O5 C22 C23 116(2) . . ?
C24 C23 C28 120(2) . . ?
C24 C23 C22 119(2) . . ?
C28 C23 C22 121(2) . . ?
C25 C24 C23 120(2) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 O13 117(2) . . ?
C24 C25 C26 122(2) . . ?
O13 C25 C26 121.5(19) . . ?
C27 C26 C25 118(2) . . ?
C27 C26 H26 120.8 . . ?
C25 C26 H26 120.8 . . ?
C26 C27 C28 122(2) . . ?
C26 C27 O14 122(2) . . ?
C28 C27 O14 116(2) . . ?
C27 C28 C23 119(2) . . ?
C27 C28 H28 120.7 . . ?
C23 C28 H28 120.7 . . ?
C30 C29 O14 123(3) . . ?
C30 C29 C34 118(3) . . ?
O14 C29 C34 118(3) . . ?
C31 C30 C29 122(4) . . ?
C31 C30 H30 118.8 . . ?
C29 C30 H30 118.9 . . ?
C32 C31 C30 120(3) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C33 122(3) . . ?
C31 C32 C35 120(3) . . ?
C33 C32 C35 117(3) . . ?
C32 C33 C34 119(3) . . ?
C32 C33 H33 120.8 . . ?
C34 C33 H33 120.7 . . ?
C33 C34 C29 119(3) . . ?
C33 C34 H34 120.6 . . ?
C29 C34 H34 120.7 . . ?
O18 C35 O17 118(4) . . ?
O18 C35 C32 120(3) . . ?
O17 C35 C32 122(3) . . ?
C37 C36 C41 120(2) . . ?
C37 C36 O13 120(2) . . ?
C41 C36 O13 120(2) . . ?
C36 C37 C38 121(2) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 H37 119.5 . . ?
C39 C38 C37 118(2) . . ?
C39 C38 H38 120.7 . . ?
C37 C38 H38 120.8 . . ?
C38 C39 C40 118.9(19) . . ?
C38 C39 C42 120.4(19) . . ?
C40 C39 C42 120.4(18) . . ?
C41 C40 C39 122(2) . . ?
C41 C40 H40 119.3 . . ?
C39 C40 H40 119.2 . . ?
C36 C41 C40 120(2) . . ?
C36 C41 H41 120.2 . . ?
C40 C41 H41 120.2 . . ?
O16 C42 O15 124.7(19) . . ?
O16 C42 C39 118.6(18) . . ?
O15 C42 C39 116.7(18) . . ?
N5 C43 N6 111.9(19) . . ?
N5 C43 H43 124.0 . . ?
N6 C43 H43 124.1 . . ?
C45 C44 N5 110(2) . . ?
C45 C44 H44 125.0 . . ?
N5 C44 H44 124.9 . . ?
C44 C45 N6 107(2) . . ?
C44 C45 H45 126.6 . . ?
N6 C45 H45 126.7 . . ?
C47 C46 C51 119.8(19) . . ?
C47 C46 N6 120.5(19) . . ?
C51 C46 N6 119.7(18) . . ?
C46 C47 C48 120(2) . . ?
C46 C47 H47 120.1 . . ?
C48 C47 H47 120.1 . . ?
C47 C48 C49 122(2) . . ?
C47 C48 H48 118.8 . . ?
C49 C48 H48 118.8 . . ?
C50 C49 C48 115.8(19) . . ?
C50 C49 C52 121.9(19) . . ?
C48 C49 C52 122.3(18) . . ?
C51 C50 C49 122(2) . . ?
C51 C50 H50 119.2 . . ?
C49 C50 H50 119.2 . . ?
C46 C51 C50 120(2) . . ?
C46 C51 H51 119.8 . . ?
C50 C51 H51 119.8 . . ?
C57 C52 C53 116.2(19) . . ?
C57 C52 C49 122.7(18) . . ?
C53 C52 C49 121.1(19) . . ?
C54 C53 C52 122(2) . . ?
C54 C53 H53 118.8 . . ?
C52 C53 H53 118.8 . . ?
C55 C54 C53 121(2) . . ?
C55 C54 H54 119.7 . . ?
C53 C54 H54 119.7 . . ?
C54 C55 C56 119(2) . . ?
C54 C55 N7 119.8(19) . . ?
C56 C55 N7 121.5(19) . . ?
C55 C56 C57 120(2) . . ?
C55 C56 H56 120.0 . . ?
C57 C56 H56 120.1 . . ?
C52 C57 C56 122(2) . . ?
C52 C57 H57 119.0 . . ?
C56 C57 H57 118.9 . . ?
N8 C58 N7 112.6(19) . . ?
N8 C58 H58 123.7 . . ?
N7 C58 H58 123.7 . . ?
C60 C59 N7 106.8(18) . . ?
C60 C59 H59 126.7 . . ?
N7 C59 H59 126.6 . . ?
C59 C60 N8 110.1(18) . . ?
C59 C60 H60 124.9 . . ?
N8 C60 H60 125.0 . . ?
C62 C61 N1 109(3) . . ?
C62 C61 H61 125.4 . . ?
N1 C61 H61 125.3 . . ?
C61 C62 N2 108(2) . . ?
C61 C62 H62 126.1 . . ?
N2 C62 H62 126.1 . . ?
N1 C63 N2 112(2) . . ?
N1 C63 H63 124.1 . . ?
N2 C63 H63 124.1 . . ?
C65 C64 C69 120(2) . . ?
C65 C64 N2 122(2) . . ?
C69 C64 N2 119(2) . . ?
C64 C65 C66 120(2) . . ?
C64 C65 H65 119.9 . . ?
C66 C65 H65 119.9 . . ?
C65 C66 C67 122(2) . . ?
C65 C66 H66 119.0 . . ?
C67 C66 H66 119.0 . . ?
C66 C67 C68 116(2) . . ?
C66 C67 C70 123(2) . . ?
C68 C67 C70 120.8(19) . . ?
C69 C68 C67 122(2) . . ?
C69 C68 H68 118.8 . . ?
C67 C68 H68 118.8 . . ?
C68 C69 C64 119(2) . . ?
C68 C69 H69 120.3 . . ?
C64 C69 H69 120.3 . . ?
C71 C70 C75 116(2) . . ?
C71 C70 C67 122(2) . . ?
C75 C70 C67 122(2) . . ?
C72 C71 C70 123(2) . . ?
C72 C71 H71 118.4 . . ?
C70 C71 H71 118.4 . . ?
C73 C72 C71 120(2) . . ?
C73 C72 H72 120.0 . . ?
C71 C72 H72 120.1 . . ?
C72 C73 C74 118(2) . . ?
C72 C73 N3 121(2) . . ?
C74 C73 N3 121(2) . . ?
C75 C74 C73 120(2) . . ?
C75 C74 H74 119.8 . . ?
C73 C74 H74 119.9 . . ?
C74 C75 C70 122(2) . . ?
C74 C75 H75 118.8 . . ?
C70 C75 H75 118.9 . . ?
N4 C76 N3 114(2) . . ?
N4 C76 H76 123.2 . . ?
N3 C76 H76 123.1 . . ?
C78 C77 N3 107(2) . . ?
C78 C77 H77 126.5 . . ?
N3 C77 H77 126.5 . . ?
C77 C78 N4 111(2) . . ?
C77 C78 H78 124.7 . . ?
N4 C78 H78 124.8 . . ?
C63 N1 C61 106(2) . . ?
C63 N1 Ni2 127.4(17) . . ?
C61 N1 Ni2 127(2) . . ?
C63 N2 C62 105(2) . . ?
C63 N2 C64 126(2) . . ?
C62 N2 C64 128.0(19) . . ?
C76 N3 C77 104.5(19) . . ?
C76 N3 C73 127.5(19) . . ?
C77 N3 C73 128(2) . . ?
C76 N4 C78 104(2) . . ?
C76 N4 Ni3 125.8(16) . 1_664 ?
C78 N4 Ni3 129.8(16) . 1_664 ?
C43 N5 C44 104.9(17) . . ?
C43 N5 Ni1 122.9(15) . . ?
C44 N5 Ni1 132.1(14) . . ?
C43 N6 C45 106.4(16) . . ?
C43 N6 C46 124.0(18) . . ?
C45 N6 C46 129.4(18) . . ?
C58 N7 C59 105.5(17) . . ?
C58 N7 C55 125.4(17) . . ?
C59 N7 C55 128.9(17) . . ?
C58 N8 C60 105.0(17) . . ?
C58 N8 Ni1 123.9(15) . 1_556 ?
C60 N8 Ni1 130.5(14) . 1_556 ?
O15 Ni1 N5 91.4(6) 1_644 . ?
O15 Ni1 O16 110.0(6) 1_644 2_766 ?
N5 Ni1 O16 92.2(7) . 2_766 ?
O15 Ni1 N8 88.3(6) 1_644 1_554 ?
N5 Ni1 N8 176.0(7) . 1_554 ?
O16 Ni1 N8 84.2(7) 2_766 1_554 ?
O15 Ni1 O10 154.3(6) 1_644 . ?
N5 Ni1 O10 91.5(6) . . ?
O16 Ni1 O10 95.4(6) 2_766 . ?
N8 Ni1 O10 90.5(6) 1_554 . ?
O15 Ni1 O9 94.3(5) 1_644 . ?
N5 Ni1 O9 96.5(6) . . ?
O16 Ni1 O9 154.0(6) 2_766 . ?
N8 Ni1 O9 87.5(6) 1_554 . ?
O10 Ni1 O9 60.0(5) . . ?
O15 Ni1 C21 124.1(6) 1_644 . ?
N5 Ni1 C21 96.9(6) . . ?
O16 Ni1 C21 124.6(7) 2_766 . ?
N8 Ni1 C21 86.6(6) 1_554 . ?
O10 Ni1 C21 30.2(6) . . ?
O9 Ni1 C21 29.9(6) . . ?
O18 Ni3 O18 180.000(8) 2_568 . ?
O18 Ni3 N4 91.1(10) 2_568 1_446 ?
O18 Ni3 N4 88.9(10) . 1_446 ?
O18 Ni3 N4 88.9(10) 2_568 2_677 ?
O18 Ni3 N4 91.1(10) . 2_677 ?
N4 Ni3 N4 180.000(4) 1_446 2_677 ?
O18 Ni3 O19 72.4(16) 2_568 2_568 ?
O18 Ni3 O19 107.6(16) . 2_568 ?
N4 Ni3 O19 94.6(13) 1_446 2_568 ?
N4 Ni3 O19 85.4(13) 2_677 2_568 ?
O18 Ni3 O19 107.6(16) 2_568 . ?
O18 Ni3 O19 72.4(16) . . ?
N4 Ni3 O19 85.4(13) 1_446 . ?
N4 Ni3 O19 94.6(13) 2_677 . ?
O19 Ni3 O19 180.000(6) 2_568 . ?
O3 Ni2 O5 176.6(11) . . ?
O3 Ni2 N1 91.2(8) . . ?
O5 Ni2 N1 89.9(8) . . ?
O3 Ni2 O2 89.5(7) . 2_666 ?
O5 Ni2 O2 89.5(7) . 2_666 ?
N1 Ni2 O2 178.2(11) . 2_666 ?
O3 Ni2 O2 90.4(9) . . ?
O5 Ni2 O2 92.6(10) . . ?
N1 Ni2 O2 95.5(10) . . ?
O2 Ni2 O2 82.7(6) 2_666 . ?
O3 Ni2 O1 88.0(10) . . ?
O5 Ni2 O1 88.8(11) . . ?
N1 Ni2 O1 93.0(13) . . ?
O2 Ni2 O1 88.8(11) 2_666 . ?
O2 Ni2 O1 171.4(10) . . ?
Ni2 O1 H2W 127(3) . . ?
Ni2 O1 H1W 124(3) . . ?
H2W O1 H1W 107(7) . . ?
Ni2 O2 Ni2 97.3(6) 2_666 . ?
Ni2 O2 H3W 92(10) 2_666 . ?
Ni2 O2 H3W 126(2) . . ?
Ni2 O2 H4W 68(10) 2_666 . ?
Ni2 O2 H4W 124(3) . . ?
H3W O2 H4W 109(6) . . ?
C1 O3 Ni2 127.9(16) . . ?
C22 O5 Ni2 124.5(15) . . ?
C5 O7 C7 117.9(17) . . ?
C15 O8 C3 119.3(15) . . ?
C21 O9 Ni1 88.5(12) . . ?
C21 O10 Ni1 90.5(11) . . ?
C13 O12 H12A 109.5 . . ?
C25 O13 C36 118.2(18) . . ?
C29 O14 C27 117.1(19) . . ?
C42 O15 Ni1 128.4(14) . 1_466 ?
C42 O16 Ni1 146.5(15) . 2_766 ?
C35 O18 Ni3 110(3) . . ?
Ni3 O19 H5W 132(4) . . ?
Ni3 O19 H6W 134(4) . . ?
H5W O19 H6W 88(2) . . ?

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         1.481
_refine_diff_density_min         -2.219
_refine_diff_density_rms         0.092
_database_code_depnum_ccdc_archive 'CCDC 986464'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_z

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H15 Fe N2 O6'
_chemical_formula_weight         435.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pcca

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

_cell_length_a                   9.021(5)
_cell_length_b                   13.841(8)
_cell_length_c                   30.183(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3769(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5205
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      26.37

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6833
_exptl_absorpt_correction_T_max  0.8842
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17974
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3328
_reflns_number_gt                2726
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1080P)²+2.1053P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3328
_refine_ls_number_parameters     271
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1509
_refine_ls_wR_factor_gt          0.1377
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0000 0.4357(3) 0.2500 0.0291(9) Uani 1 2 d S . .
H1 H 0.0000 0.3685 0.2500 0.035 Uiso 1 2 calc SR . .
C2 C 0.1333(3) 0.6739(2) 0.18996(9) 0.0311(7) Uani 1 1 d . . .
C3 C 0.1920(3) 0.6788(2) 0.14317(9) 0.0333(7) Uani 1 1 d . . .
C4 C 0.3337(4) 0.6506(3) 0.13248(11) 0.0481(9) Uani 1 1 d . . .
H4 H 0.3985 0.6325 0.1550 0.058 Uiso 1 1 calc R . .
C5 C 0.3822(4) 0.6485(3) 0.08885(11) 0.0530(9) Uani 1 1 d . . .
H5 H 0.4785 0.6298 0.0820 0.064 Uiso 1 1 calc R . .
C6 C 0.2843(4) 0.6749(3) 0.05567(10) 0.0428(8) Uani 1 1 d . . .
C7 C 0.1452(4) 0.7061(3) 0.06554(11) 0.0535(10) Uani 1 1 d . . .
H7 H 0.0817 0.7258 0.0430 0.064 Uiso 1 1 calc R . .
C8 C 0.0984(4) 0.7085(3) 0.10912(11) 0.0495(9) Uani 1 1 d . . .
H8 H 0.0033 0.7301 0.1158 0.059 Uiso 1 1 calc R . .
C9 C 0.2888(4) 0.5826(3) -0.01032(10) 0.0403(8) Uani 1 1 d . . .
C10 C 0.2500 0.5000 0.01346(14) 0.0478(12) Uani 1 2 d S . .
H10 H 0.2500 0.5000 0.0443 0.057 Uiso 1 2 calc SR . .
C11 C 0.2500 0.5000 0.37091(13) 0.0326(9) Uani 1 2 d S . .
C12 C 0.2500 0.5000 0.42078(13) 0.0321(9) Uani 1 2 d S . .
C13 C 0.2090(3) 0.5831(2) 0.44419(10) 0.0354(7) Uani 1 1 d . . .
H13 H 0.1804 0.6385 0.4290 0.043 Uiso 1 1 calc R . .
C14 C 0.3462(8) 0.8307(4) 0.28236(14) 0.090(2) Uani 1 1 d . . .
H14 H 0.3385 0.8391 0.2519 0.108 Uiso 1 1 calc R . .
C15 C 0.3958(10) 0.8982(4) 0.31119(16) 0.122(3) Uani 1 1 d . . .
H15 H 0.4319 0.9592 0.3042 0.147 Uiso 1 1 calc R . .
C16 C 0.3308(4) 0.7700(3) 0.34622(12) 0.0473(9) Uani 1 1 d . . .
H16 H 0.3119 0.7272 0.3693 0.057 Uiso 1 1 calc R . .
C17 C 0.4166(5) 0.9012(3) 0.39473(14) 0.0597(11) Uani 1 1 d . . .
C18 C 0.3473(7) 0.8683(3) 0.43191(16) 0.0792(15) Uani 1 1 d . . .
H18 H 0.2757 0.8203 0.4296 0.095 Uiso 1 1 calc R . .
C19 C 0.3820(7) 0.9055(3) 0.47275(15) 0.0782(14) Uani 1 1 d . . .
H19 H 0.3360 0.8803 0.4978 0.094 Uiso 1 1 calc R . .
C20 C 0.4840(5) 0.9794(3) 0.47761(14) 0.0637(11) Uani 1 1 d . . .
C21 C 0.5470(8) 1.0123(5) 0.43987(18) 0.122(3) Uani 1 1 d . . .
H21 H 0.6156 1.0622 0.4418 0.147 Uiso 1 1 calc R . .
C22 C 0.5142(8) 0.9752(5) 0.39836(17) 0.121(3) Uani 1 1 d . . .
H22 H 0.5588 1.0008 0.3732 0.146 Uiso 1 1 calc R . .
Fe1 Fe 0.19364(5) 0.61714(3) 0.285204(12) 0.0275(2) Uani 1 1 d . . .
N1 N 0.3092(3) 0.7489(2) 0.30449(9) 0.0399(7) Uani 1 1 d . . .
N2 N 0.3826(4) 0.8592(2) 0.35236(10) 0.0571(9) Uani 1 1 d . . .
O1 O 0.2147(3) 0.57742(17) 0.35194(7) 0.0405(6) Uani 1 1 d . . .
O2 O 0.2237(3) 0.6510(2) 0.21960(7) 0.0420(6) Uani 1 1 d . . .
O3 O -0.0006(2) 0.69220(17) 0.19619(7) 0.0435(6) Uani 1 1 d . . .
O4 O 0.3301(3) 0.66730(19) 0.01138(7) 0.0546(7) Uani 1 1 d . . .
O5 O 0.1009(2) 0.47534(14) 0.27182(6) 0.0328(5) Uani 1 1 d . . .
O6 O 0.7500 1.0000 0.2970(6) 0.420(13) Uani 1 2 d SD . .
O7 O 0.0000 0.8768(8) 0.2500 0.225(5) Uani 1 2 d SD . .
H2W H 0.028(10) 0.892(5) 0.2254(11) 0.080 Uiso 1 1 d D . .
H1W H 0.735(6) 1.041(3) 0.3163(16) 0.080 Uiso 1 1 d D . .


_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
C1 O5 1.250(3) . ?
C1 O5 1.250(3) 3 ?
C1 H1 0.9300 . ?
C2 O3 1.248(4) . ?
C2 O2 1.251(4) . ?
C2 C3 1.510(4) . ?
C3 C4 1.376(5) . ?
C3 C8 1.392(4) . ?
C4 C5 1.388(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.384(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.360(5) . ?
C6 O4 1.403(4) . ?
C7 C8 1.382(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C13 1.373(4) 8_655 ?
C9 C10 1.395(4) . ?
C9 O4 1.393(4) . ?
C10 C9 1.395(4) 2_565 ?
C10 H10 0.9300 . ?
C11 O1 1.256(3) . ?
C11 O1 1.256(3) 2_565 ?
C11 C12 1.505(5) . ?
C12 C13 1.400(4) 2_565 ?
C12 C13 1.400(4) . ?
C13 C9 1.373(4) 8_656 ?
C13 H13 0.9300 . ?
C14 C15 1.353(7) . ?
C14 N1 1.355(5) . ?
C14 H14 0.9300 . ?
C15 N2 1.360(6) . ?
C15 H15 0.9300 . ?
C16 N1 1.308(4) . ?
C16 N2 1.332(5) . ?
C16 H16 0.9300 . ?
C17 C22 1.354(6) . ?
C17 C18 1.363(6) . ?
C17 N2 1.438(5) . ?
C18 C19 1.372(6) . ?
C18 H18 0.9300 . ?
C19 C20 1.384(6) . ?
C19 H19 0.9300 . ?
C20 C21 1.352(7) . ?
C20 C20 1.495(7) 5_676 ?
C21 C22 1.386(6) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
Fe1 O2 2.053(2) . ?
Fe1 O1 2.097(2) . ?
Fe1 O3 2.104(2) 3 ?
Fe1 O5 2.172(2) . ?
Fe1 N1 2.180(3) . ?
Fe1 O5 2.289(2) 2_565 ?
O3 Fe1 2.104(2) 3 ?
O5 Fe1 2.289(2) 2_565 ?
O6 H1W 0.826(13) . ?

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 C1 O5 127.9(4) . 3 ?
O5 C1 H1 116.0 . . ?
O5 C1 H1 116.0 3 . ?
O3 C2 O2 125.1(3) . . ?
O3 C2 C3 118.1(3) . . ?
O2 C2 C3 116.9(3) . . ?
C4 C3 C8 118.3(3) . . ?
C4 C3 C2 122.2(3) . . ?
C8 C3 C2 119.4(3) . . ?
C3 C4 C5 121.4(3) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 118.7(3) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C7 C6 C5 120.9(3) . . ?
C7 C6 O4 120.3(3) . . ?
C5 C6 O4 118.8(3) . . ?
C6 C7 C8 119.9(3) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.7(3) . . ?
C7 C8 H8 119.6 . . ?
C3 C8 H8 119.7 . . ?
C13 C9 C10 121.5(3) 8_655 . ?
C13 C9 O4 117.5(3) 8_655 . ?
C10 C9 O4 121.0(3) . . ?
C9 C10 C9 118.1(4) . 2_565 ?
C9 C10 H10 121.0 . . ?
C9 C10 H10 121.0 2_565 . ?
O1 C11 O1 125.7(4) . 2_565 ?
O1 C11 C12 117.13(18) . . ?
O1 C11 C12 117.13(18) 2_565 . ?
C13 C12 C13 119.4(4) 2_565 . ?
C13 C12 C11 120.31(19) 2_565 . ?
C13 C12 C11 120.31(19) . . ?
C9 C13 C12 119.8(3) 8_656 . ?
C9 C13 H13 120.1 8_656 . ?
C12 C13 H13 120.2 . . ?
C15 C14 N1 109.9(4) . . ?
C15 C14 H14 125.0 . . ?
N1 C14 H14 125.1 . . ?
C14 C15 N2 106.5(4) . . ?
C14 C15 H15 126.8 . . ?
N2 C15 H15 126.7 . . ?
N1 C16 N2 113.1(3) . . ?
N1 C16 H16 123.4 . . ?
N2 C16 H16 123.4 . . ?
C22 C17 C18 118.9(4) . . ?
C22 C17 N2 121.1(4) . . ?
C18 C17 N2 119.9(4) . . ?
C17 C18 C19 120.7(4) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C20 121.6(5) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C21 C20 C19 116.0(4) . . ?
C21 C20 C20 123.5(5) . 5_676 ?
C19 C20 C20 120.4(5) . 5_676 ?
C20 C21 C22 123.2(5) . . ?
C20 C21 H21 118.4 . . ?
C22 C21 H21 118.4 . . ?
C17 C22 C21 119.5(5) . . ?
C17 C22 H22 120.2 . . ?
C21 C22 H22 120.3 . . ?
O2 Fe1 O1 167.06(10) . . ?
O2 Fe1 O3 104.72(10) . 3 ?
O1 Fe1 O3 87.03(9) . 3 ?
O2 Fe1 O5 94.45(10) . . ?
O1 Fe1 O5 88.66(9) . . ?
O3 Fe1 O5 100.19(9) 3 . ?
O2 Fe1 N1 90.20(11) . . ?
O1 Fe1 N1 85.39(10) . . ?
O3 Fe1 N1 84.91(10) 3 . ?
O5 Fe1 N1 171.96(9) . . ?
O2 Fe1 O5 81.39(9) . 2_565 ?
O1 Fe1 O5 87.10(8) . 2_565 ?
O3 Fe1 O5 173.52(8) 3 2_565 ?
O5 Fe1 O5 76.93(9) . 2_565 ?
N1 Fe1 O5 97.34(10) . 2_565 ?
C16 N1 C14 104.6(3) . . ?
C16 N1 Fe1 121.0(2) . . ?
C14 N1 Fe1 133.2(3) . . ?
C16 N2 C15 105.7(3) . . ?
C16 N2 C17 125.0(3) . . ?
C15 N2 C17 129.3(4) . . ?
C11 O1 Fe1 133.2(2) . . ?
C2 O2 Fe1 131.4(2) . . ?
C2 O3 Fe1 137.8(2) . 3 ?
C9 O4 C6 115.6(2) . . ?
C1 O5 Fe1 140.8(2) . . ?
C1 O5 Fe1 115.9(2) . 2_565 ?
Fe1 O5 Fe1 99.23(9) . 2_565 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.069
_database_code_depnum_ccdc_archive 'CCDC 1006437'
