# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Scott Dalgarno'
_publ_contact_author_email       S.J.DALGARNO@HW.AC.UK

_publ_section_title              
;
Magnetism in metal-organic capsules
;
loop_
_publ_author_name
'Scott Dalgarno'
'Jerry L Atwood'
'Euan Brechin'
'Ross Inglis'
'Andrew Mossine'
;
M.J.Paterson
;
'Nicholas P. Power'
'Simon J. Teat'

# Attachment '742756.cif'

data_CoDimerPy
_database_code_depnum_ccdc_archive 'CCDC 742756'
#TrackingRef '742756.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C162 H154 Co8 N18 O24'
_chemical_formula_weight         3208.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020 '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'
O O -0.0041 0.0074 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.1760 1.1404 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fddd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   18.6001(8)
_cell_length_b                   28.4944(11)
_cell_length_c                   54.266(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     28761(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      .
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             13280
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_process_details   'SADABS 2004 Bruker AXS, Madison, WI'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean .
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            26582
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         21.44
_reflns_number_total             3163
_reflns_number_gt                2163
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINTv7.34a'
_computing_data_reduction        'Bruker SAINTv7.34a'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed v2.0 (Barbour, 2005)'
_computing_publication_material  'local program'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. The FLAT instruction
was applied to a pyridine of crystallisation that is disordered
over four positions (C70-C75). It was not possible to determine which atom
was the nitrogen of this ring and as this is the case, all have been
modelled as carbon. This gives rise to difference in calculated and
reported formulae. SIMU instructions were also applied to two other
pyridines of crystallisation, C44 - N49 and N31 - C34. The encapsulated
pyridine molecule was restrained using SIMU and DELU commands, and the
DFIX instruction was used on one of the pyrogallol4arene hydroxyl groups.
Crystals were weakly diffracting. As this was the case, a strategy of
collecting both low and high angle shells was employed. Despite this
stategy, and long exposure times, a low data:parameter ratio resulted.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+343.5622P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3163
_refine_ls_number_parameters     482
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1572
_refine_ls_wR_factor_gt          0.1341
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.053
_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
Co1 Co 0.6250 0.44741(5) 0.1250 0.0446(5) Uani 1 2 d S . .
O1 O 0.5190(3) 0.46231(17) 0.11411(10) 0.0453(15) Uani 1 1 d . A 1
C1 C 0.4175(5) 0.5461(3) 0.16644(16) 0.048(2) Uani 1 1 d . . .
Co2 Co 0.62408(7) 0.50491(4) 0.062277(19) 0.0491(4) Uani 1 1 d . . .
O2 O 0.5201(3) 0.52694(19) 0.19270(10) 0.0518(15) Uani 1 1 d D . .
C2 C 0.4835(5) 0.5250(3) 0.17053(15) 0.043(2) Uani 1 1 d . A .
Co3 Co 0.6250 0.6250 0.03750(3) 0.0581(6) Uani 1 2 d S . .
O3 O 0.5175(3) 0.49290(19) 0.07203(10) 0.0514(15) Uani 1 1 d . A 2
C3 C 0.5177(5) 0.4997(3) 0.15221(15) 0.042(2) Uani 1 1 d . . .
C4 C 0.4829(5) 0.4918(3) 0.12998(15) 0.045(2) Uani 1 1 d . A .
C5 C 0.4167(5) 0.5121(3) 0.12508(15) 0.045(2) Uani 1 1 d . . .
C6 C 0.3863(5) 0.5402(3) 0.14321(16) 0.047(2) Uani 1 1 d . A .
H6 H 0.3426 0.5560 0.1397 0.056 Uiso 1 1 calc R . .
C7 C 0.3823(5) 0.5069(3) 0.09979(15) 0.049(2) Uani 1 1 d . A .
H7 H 0.3979 0.4754 0.0937 0.059 Uiso 1 1 calc R . .
C8 C 0.4158(5) 0.5424(3) 0.08183(15) 0.051(2) Uani 1 1 d . . .
O9 O 0.5191(3) 0.64554(19) 0.03975(9) 0.0530(16) Uani 1 1 d . A .
C9 C 0.4815(5) 0.5339(3) 0.07031(16) 0.050(2) Uani 1 1 d . A .
O10 O 0.5857(3) 0.48404(17) 0.15571(9) 0.0450(14) Uani 1 1 d . . .
C10 C 0.5129(5) 0.5697(3) 0.05656(15) 0.053(2) Uani 1 1 d . . .
C11 C 0.4809(6) 0.6131(3) 0.05358(15) 0.051(2) Uani 1 1 d . A .
C12 C 0.4153(5) 0.6228(3) 0.06499(15) 0.047(2) Uani 1 1 d . . .
C13 C 0.3842(5) 0.5874(3) 0.07926(15) 0.055(2) Uani 1 1 d . A .
H13 H 0.3403 0.5937 0.0876 0.066 Uiso 1 1 calc R . .
C14 C 0.3826(5) 0.6720(3) 0.06377(15) 0.052(2) Uani 1 1 d . . .
H14 H 0.3979 0.6852 0.0475 0.062 Uiso 1 1 calc R . .
C15 C 0.3019(6) 0.5056(4) 0.09957(18) 0.081(3) Uani 1 1 d . . .
H15A H 0.2852 0.5017 0.0824 0.097 Uiso 1 1 calc R A .
H15B H 0.2833 0.5360 0.1057 0.097 Uiso 1 1 calc R . .
O16 O 0.5816(3) 0.56281(18) 0.04737(10) 0.0536(16) Uani 1 1 d . A .
C16 C 0.2701(6) 0.4658(4) 0.11541(19) 0.097(4) Uani 1 1 d . A .
H16A H 0.2932 0.4360 0.1110 0.146 Uiso 1 1 calc R . .
H16B H 0.2182 0.4635 0.1124 0.146 Uiso 1 1 calc R . .
H16C H 0.2785 0.4725 0.1329 0.146 Uiso 1 1 calc R . .
C17 C 0.3010(5) 0.6724(3) 0.06343(17) 0.064(3) Uani 1 1 d . . .
H17A H 0.2838 0.6501 0.0507 0.077 Uiso 1 1 calc R A .
H17B H 0.2829 0.6616 0.0796 0.077 Uiso 1 1 calc R . .
C18 C 0.2705(6) 0.7207(3) 0.05804(19) 0.082(3) Uani 1 1 d . A .
H18A H 0.2833 0.7422 0.0714 0.123 Uiso 1 1 calc R . .
H18B H 0.2181 0.7186 0.0567 0.123 Uiso 1 1 calc R . .
H18C H 0.2904 0.7324 0.0425 0.123 Uiso 1 1 calc R . .
N19 N 0.6220(5) 0.3897(2) 0.09845(12) 0.0463(18) Uani 1 1 d . A .
C20 C 0.6817(6) 0.3660(3) 0.09509(18) 0.065(3) Uani 1 1 d . . .
H20 H 0.7220 0.3732 0.1051 0.078 Uiso 1 1 calc R A .
C21 C 0.6883(6) 0.3314(4) 0.07768(19) 0.074(3) Uani 1 1 d . A .
H21 H 0.7326 0.3153 0.0757 0.089 Uiso 1 1 calc R . .
C22 C 0.6305(7) 0.3204(3) 0.06327(18) 0.069(3) Uani 1 1 d . . .
H22 H 0.6334 0.2958 0.0515 0.083 Uiso 1 1 calc R A .
C23 C 0.5692(6) 0.3451(3) 0.06599(17) 0.065(3) Uani 1 1 d . A .
H23 H 0.5287 0.3389 0.0558 0.078 Uiso 1 1 calc R . .
C24 C 0.5666(6) 0.3796(3) 0.08387(18) 0.059(3) Uani 1 1 d . . .
H24 H 0.5233 0.3969 0.0858 0.071 Uiso 1 1 calc R A .
N25 N 0.6305(5) 0.4540(3) 0.03598(13) 0.058(2) Uani 1 1 d . A .
C26 C 0.6883(7) 0.4288(4) 0.03346(17) 0.075(3) Uani 1 1 d . . .
H26 H 0.7279 0.4355 0.0439 0.090 Uiso 1 1 calc R A .
C27 C 0.6959(8) 0.3927(4) 0.0164(2) 0.101(4) Uani 1 1 d . A .
H27 H 0.7391 0.3750 0.0153 0.121 Uiso 1 1 calc R . .
C28 C 0.6397(11) 0.3838(5) 0.0017(2) 0.122(6) Uani 1 1 d . . .
H28 H 0.6436 0.3599 -0.0104 0.147 Uiso 1 1 calc R A .
C29 C 0.5770(9) 0.4084(6) 0.0039(2) 0.132(6) Uani 1 1 d . A .
H29 H 0.5364 0.4015 -0.0062 0.158 Uiso 1 1 calc R . .
C30 C 0.5753(7) 0.4441(5) 0.0215(2) 0.098(4) Uani 1 1 d . . .
H30 H 0.5327 0.4621 0.0232 0.117 Uiso 1 1 calc R A .
N31 N 0.6250 0.6250 -0.00101(19) 0.071(3) Uani 1 2 d SU . .
C32 C 0.6100(6) 0.5870(4) -0.01341(19) 0.094(3) Uani 1 1 d U . .
H32 H 0.6000 0.5590 -0.0045 0.113 Uiso 1 1 calc R A .
C33 C 0.6079(6) 0.5856(5) -0.0397(2) 0.102(3) Uani 1 1 d U A .
H33 H 0.5948 0.5578 -0.0483 0.122 Uiso 1 1 calc R . .
C34 C 0.6250 0.6250 -0.0520(3) 0.100(4) Uani 1 2 d SU . .
H34 H 0.6250 0.6250 -0.0695 0.121 Uiso 1 2 calc SR A .
N40 N 0.8750 0.3750 0.0909(2) 0.086(4) Uani 1 2 d S . .
C41 C 0.8661(6) 0.4151(3) 0.0778(2) 0.075(3) Uani 1 1 d . . .
H41 H 0.8586 0.4439 0.0862 0.090 Uiso 1 1 calc R . .
C42 C 0.8678(6) 0.4146(4) 0.0526(2) 0.089(3) Uani 1 1 d . . .
H42 H 0.8637 0.4433 0.0438 0.107 Uiso 1 1 calc R . .
C43 C 0.8750 0.3750 0.0402(3) 0.092(5) Uani 1 2 d S . .
H43 H 0.8750 0.3750 0.0227 0.110 Uiso 1 2 calc SR . .
C44 C 0.5988(11) 0.2469(7) 0.0012(3) 0.148(4) Uani 1 1 d U . .
H44 H 0.6281 0.2630 -0.0104 0.178 Uiso 1 1 calc R . .
C45 C 0.6241(11) 0.2091(6) 0.0131(3) 0.145(4) Uani 1 1 d U . .
H45 H 0.6704 0.1973 0.0091 0.174 Uiso 1 1 calc R . .
C46 C 0.5858(10) 0.1884(6) 0.0302(3) 0.134(4) Uani 1 1 d U . .
H46 H 0.6055 0.1618 0.0383 0.161 Uiso 1 1 calc R . .
C47 C 0.5199(10) 0.2031(6) 0.0367(3) 0.136(4) Uani 1 1 d U . .
H47 H 0.4951 0.1881 0.0498 0.164 Uiso 1 1 calc R . .
C48 C 0.4878(10) 0.2406(6) 0.0241(3) 0.144(4) Uani 1 1 d U . .
H48 H 0.4404 0.2508 0.0277 0.173 Uiso 1 1 calc R . .
N49 N 0.5304(10) 0.2621(5) 0.0059(2) 0.156(4) Uani 1 1 d U . .
N60 N 0.620(3) 0.624(3) 0.0903(3) 0.092(7) Uiso 0.25 1 d PGU B -1
C61 C 0.686(3) 0.623(2) 0.1018(6) 0.086(9) Uiso 0.25 1 d PGU B -1
H61 H 0.7286 0.6176 0.0924 0.103 Uiso 0.25 1 calc PR B -1
C62 C 0.691(2) 0.6314(11) 0.1270(6) 0.075(8) Uiso 0.25 1 d PGU B -1
H62 H 0.7371 0.6309 0.1348 0.090 Uiso 0.25 1 calc PR B -1
C63 C 0.630(3) 0.6399(10) 0.1407(3) 0.092(9) Uiso 0.25 1 d PGU B -1
H63 H 0.6332 0.6453 0.1579 0.110 Uiso 0.25 1 calc PR B -1
C64 C 0.563(2) 0.6406(9) 0.1292(6) 0.089(9) Uiso 0.25 1 d PGU B -1
H64 H 0.5208 0.6464 0.1386 0.107 Uiso 0.25 1 calc PR B -1
C65 C 0.558(2) 0.633(2) 0.1040(7) 0.097(9) Uiso 0.25 1 d PGU B -1
H65 H 0.5122 0.6331 0.0961 0.116 Uiso 0.25 1 calc PR B -1
C70 C 0.133(3) 0.6770(14) 0.1186(6) 0.15(3) Uiso 0.25 1 d PGD C -1
H70 H 0.1388 0.7054 0.1096 0.186 Uiso 0.25 1 calc PR C -1
C71 C 0.136(3) 0.6777(12) 0.1442(6) 0.16(3) Uiso 0.25 1 d PGD C -1
H71 H 0.1427 0.7065 0.1527 0.189 Uiso 0.25 1 calc PR C -1
C72 C 0.128(3) 0.6362(14) 0.1574(5) 0.139(19) Uiso 0.25 1 d PGD C -1
H72 H 0.1295 0.6366 0.1749 0.167 Uiso 0.25 1 calc PR C -1
C73 C 0.118(2) 0.5940(13) 0.1450(6) 0.12(2) Uiso 0.25 1 d PGD C -1
H73 H 0.1124 0.5656 0.1540 0.144 Uiso 0.25 1 calc PR C -1
C74 C 0.115(3) 0.5934(14) 0.1194(6) 0.20(3) Uiso 0.25 1 d PGD C -1
H74 H 0.1085 0.5645 0.1109 0.236 Uiso 0.25 1 calc PR C -1
C75 C 0.123(3) 0.6349(16) 0.1062(5) 0.14(2) Uiso 0.25 1 d PGD C -1
H75 H 0.1217 0.6344 0.0887 0.164 Uiso 0.25 1 calc PR C -1
H101 H 0.5170 0.5555 0.1998 0.06(3) Uiso 1 1 d GD C -1
H100 H 0.5092 0.4746 0.0968 0.16(5) Uiso 1 1 d G C 1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0636(11) 0.0346(9) 0.0355(9) 0.000 0.0024(9) 0.000
O1 0.067(4) 0.035(3) 0.034(3) -0.002(3) 0.006(3) -0.008(3)
C1 0.070(7) 0.031(5) 0.044(6) 0.003(5) 0.009(5) -0.004(5)
Co2 0.0692(9) 0.0419(7) 0.0362(7) 0.0007(5) -0.0010(6) -0.0023(7)
O2 0.077(4) 0.041(4) 0.037(4) -0.002(3) -0.001(3) -0.001(3)
C2 0.062(7) 0.030(5) 0.039(6) 0.002(5) 0.004(5) -0.002(5)
Co3 0.0713(13) 0.0455(11) 0.0575(11) 0.000 0.000 -0.0065(10)
O3 0.070(4) 0.039(4) 0.045(3) 0.001(3) -0.001(3) 0.006(3)
C3 0.060(7) 0.031(5) 0.035(6) 0.002(4) 0.006(5) -0.003(5)
C4 0.065(7) 0.038(5) 0.033(6) 0.001(4) 0.008(5) -0.001(5)
C5 0.057(6) 0.036(5) 0.042(6) 0.003(5) 0.000(5) -0.007(5)
C6 0.052(6) 0.040(5) 0.048(6) 0.000(5) 0.004(5) -0.003(5)
C7 0.055(7) 0.044(5) 0.050(6) -0.001(4) -0.001(5) -0.002(5)
C8 0.068(7) 0.043(6) 0.041(6) 0.004(5) -0.005(5) -0.011(5)
O9 0.078(4) 0.047(4) 0.033(3) 0.004(3) 0.000(3) -0.007(3)
C9 0.063(7) 0.047(7) 0.041(5) 0.002(5) 0.006(5) -0.006(6)
O10 0.064(4) 0.038(3) 0.033(3) -0.001(3) -0.002(3) 0.006(3)
C10 0.062(7) 0.056(7) 0.042(6) -0.001(5) 0.006(5) 0.002(6)
C11 0.072(7) 0.042(7) 0.039(6) -0.002(5) -0.008(5) 0.000(6)
C12 0.068(7) 0.040(6) 0.033(5) -0.002(5) -0.010(5) 0.001(6)
C13 0.061(6) 0.063(7) 0.041(5) -0.008(5) -0.005(5) -0.013(6)
C14 0.058(7) 0.052(6) 0.045(5) 0.000(4) -0.005(5) -0.003(5)
C15 0.099(10) 0.084(8) 0.061(7) -0.002(6) -0.006(6) -0.008(7)
O16 0.067(4) 0.047(4) 0.047(4) 0.004(3) 0.007(3) 0.002(3)
C16 0.101(9) 0.114(9) 0.077(8) 0.021(7) -0.013(7) -0.053(8)
C17 0.071(8) 0.060(7) 0.060(6) -0.011(5) -0.009(5) 0.006(6)
C18 0.087(8) 0.062(7) 0.096(8) -0.010(6) -0.030(7) 0.012(6)
N19 0.064(5) 0.032(4) 0.043(4) 0.000(3) -0.003(5) -0.001(4)
C20 0.076(8) 0.049(6) 0.070(7) -0.021(6) -0.015(6) 0.012(6)
C21 0.072(8) 0.078(8) 0.074(7) -0.021(7) -0.012(7) 0.030(6)
C22 0.094(9) 0.053(6) 0.061(7) -0.015(5) -0.006(7) 0.005(7)
C23 0.081(8) 0.053(6) 0.060(7) -0.011(6) -0.014(6) 0.002(6)
C24 0.075(7) 0.044(6) 0.058(6) -0.009(5) 0.002(6) 0.004(5)
N25 0.072(6) 0.055(5) 0.046(5) -0.006(4) -0.005(5) -0.006(5)
C26 0.115(10) 0.056(7) 0.053(7) -0.023(6) -0.008(6) -0.002(7)
C27 0.145(13) 0.077(9) 0.082(9) -0.026(8) 0.011(9) -0.001(8)
C28 0.169(16) 0.127(13) 0.070(10) -0.058(9) 0.038(11) -0.039(12)
C29 0.132(14) 0.199(17) 0.064(9) -0.052(11) 0.004(9) -0.034(13)
C30 0.101(10) 0.125(11) 0.067(8) -0.031(8) -0.001(8) -0.006(8)
N31 0.093(7) 0.070(7) 0.050(6) 0.000 0.000 -0.012(7)
C32 0.121(7) 0.093(7) 0.068(6) -0.011(5) 0.001(5) -0.012(6)
C33 0.121(7) 0.115(8) 0.071(6) -0.017(6) 0.000(6) -0.014(7)
C34 0.105(9) 0.123(11) 0.074(9) 0.000 0.000 -0.013(10)
N40 0.093(10) 0.072(9) 0.093(9) 0.000 0.000 -0.009(8)
C41 0.089(8) 0.049(7) 0.088(9) -0.007(6) 0.018(7) 0.011(6)
C42 0.111(10) 0.074(8) 0.083(9) 0.020(7) -0.006(8) -0.005(8)
C43 0.144(16) 0.093(14) 0.037(9) 0.000 0.000 -0.029(13)
C44 0.209(11) 0.151(9) 0.084(7) -0.033(7) -0.006(8) 0.006(9)
C45 0.196(11) 0.148(9) 0.091(8) -0.036(7) -0.018(8) 0.010(9)
C46 0.193(11) 0.119(8) 0.091(8) -0.020(7) -0.018(8) 0.002(8)
C47 0.199(11) 0.116(8) 0.095(8) -0.015(7) 0.004(8) -0.015(9)
C48 0.200(11) 0.133(9) 0.100(8) -0.030(7) -0.004(8) -0.008(8)
N49 0.220(11) 0.152(8) 0.095(7) -0.032(6) -0.022(8) -0.005(8)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O10 2.098(5) 4_655 ?
Co1 O10 2.098(5) . ?
Co1 O1 2.102(6) 4_655 ?
Co1 O1 2.102(6) . ?
Co1 N19 2.186(6) . ?
Co1 N19 2.186(6) 4_655 ?
O1 C4 1.377(9) . ?
O1 H100 1.0185 . ?
C1 C2 1.386(12) . ?
C1 C6 1.398(11) . ?
C1 C14 1.548(11) 3_565 ?
Co2 O10 1.983(5) 4_655 ?
Co2 O16 2.000(5) . ?
Co2 N25 2.039(8) . ?
Co2 O3 2.081(6) . ?
Co2 O2 2.083(6) 4_655 ?
O2 C2 1.383(9) . ?
O2 Co2 2.083(6) 4_655 ?
O2 H101 0.9027 . ?
C2 C3 1.382(11) . ?
Co3 O16 2.020(5) 2_665 ?
Co3 O16 2.020(5) . ?
Co3 O9 2.059(6) 2_665 ?
Co3 O9 2.059(6) . ?
Co3 N31 2.090(10) . ?
O3 C9 1.350(10) . ?
O3 H100 1.4502 . ?
C3 O10 1.356(10) . ?
C3 C4 1.387(11) . ?
C4 C5 1.388(11) . ?
C5 C6 1.387(11) . ?
C5 C7 1.521(11) . ?
C6 H6 0.9500 . ?
C7 C15 1.497(12) . ?
C7 C8 1.536(11) . ?
C7 H7 1.0000 . ?
C8 C9 1.394(12) . ?
C8 C13 1.417(12) . ?
O9 C11 1.386(10) . ?
C9 C10 1.392(12) . ?
O10 Co2 1.983(5) 4_655 ?
C10 C11 1.382(12) . ?
C10 O16 1.387(10) . ?
C11 C12 1.397(12) . ?
C12 C13 1.398(11) . ?
C12 C14 1.528(12) . ?
C13 H13 0.9500 . ?
C14 C17 1.519(11) . ?
C14 C1 1.548(11) 3_565 ?
C14 H14 1.0000 . ?
C15 C16 1.541(13) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.515(12) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N19 C20 1.312(11) . ?
N19 C24 1.331(11) . ?
C20 C21 1.371(12) . ?
C20 H20 0.9500 . ?
C21 C22 1.367(13) . ?
C21 H21 0.9500 . ?
C22 C23 1.347(12) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(12) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
N25 C26 1.300(12) . ?
N25 C30 1.322(13) . ?
C26 C27 1.390(14) . ?
C26 H26 0.9500 . ?
C27 C28 1.338(18) . ?
C27 H27 0.9500 . ?
C28 C29 1.366(19) . ?
C28 H28 0.9500 . ?
C29 C30 1.399(17) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
N31 C32 1.306(11) . ?
N31 C32 1.306(11) 2_665 ?
C32 C33 1.430(15) . ?
C32 H32 0.9500 . ?
C33 C34 1.343(14) . ?
C33 H33 0.9500 . ?
C34 C33 1.343(14) 2_665 ?
C34 H34 0.9500 . ?
N40 C41 1.357(12) . ?
N40 C41 1.357(12) 14_655 ?
C41 C42 1.367(14) . ?
C41 H41 0.9500 . ?
C42 C43 1.318(13) . ?
C42 H42 0.9500 . ?
C43 C42 1.318(13) 14_655 ?
C43 H43 0.9500 . ?
C44 C45 1.34(2) . ?
C44 N49 1.37(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.31(2) . ?
C45 H45 0.9500 . ?
C46 C47 1.34(2) . ?
C46 H46 0.9500 . ?
C47 C48 1.40(2) . ?
C47 H47 0.9500 . ?
C48 N49 1.407(19) . ?
C48 H48 0.9500 . ?
N60 C61 1.3900 . ?
N60 C65 1.3900 . ?
C61 C62 1.3900 . ?
C61 H61 0.9500 . ?
C62 C63 1.3900 . ?
C62 H62 0.9500 . ?
C63 C64 1.3900 . ?
C63 H63 0.9500 . ?
C64 C65 1.3900 . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
C70 C71 1.3900 . ?
C70 C75 1.3900 . ?
C70 H70 0.9500 . ?
C71 C72 1.3900 . ?
C71 H71 0.9500 . ?
C72 C73 1.3900 . ?
C72 H72 0.9500 . ?
C73 C74 1.3900 . ?
C73 H73 0.9500 . ?
C74 C75 1.3900 . ?
C74 H74 0.9500 . ?
C75 H75 0.9500 . ?

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
O10 Co1 O10 120.3(3) 4_655 . ?
O10 Co1 O1 78.2(2) 4_655 4_655 ?
O10 Co1 O1 90.2(2) . 4_655 ?
O10 Co1 O1 90.2(2) 4_655 . ?
O10 Co1 O1 78.2(2) . . ?
O1 Co1 O1 156.7(3) 4_655 . ?
O10 Co1 N19 81.9(2) 4_655 . ?
O10 Co1 N19 152.7(3) . . ?
O1 Co1 N19 111.2(3) 4_655 . ?
O1 Co1 N19 86.7(3) . . ?
O10 Co1 N19 152.7(3) 4_655 4_655 ?
O10 Co1 N19 81.9(2) . 4_655 ?
O1 Co1 N19 86.7(3) 4_655 4_655 ?
O1 Co1 N19 111.2(3) . 4_655 ?
N19 Co1 N19 82.5(3) . 4_655 ?
C4 O1 Co1 113.8(5) . . ?
C4 O1 H100 106.2 . . ?
Co1 O1 H100 119.8 . . ?
C2 C1 C6 117.3(8) . . ?
C2 C1 C14 121.0(8) . 3_565 ?
C6 C1 C14 121.6(9) . 3_565 ?
O10 Co2 O16 138.7(2) 4_655 . ?
O10 Co2 N25 112.2(3) 4_655 . ?
O16 Co2 N25 109.1(3) . . ?
O10 Co2 O3 95.0(2) 4_655 . ?
O16 Co2 O3 82.1(2) . . ?
N25 Co2 O3 96.7(3) . . ?
O10 Co2 O2 81.2(2) 4_655 4_655 ?
O16 Co2 O2 94.1(2) . 4_655 ?
N25 Co2 O2 93.9(3) . 4_655 ?
O3 Co2 O2 169.4(2) . 4_655 ?
C2 O2 Co2 109.9(5) . 4_655 ?
C2 O2 H101 112.2 . . ?
Co2 O2 H101 112.8 4_655 . ?
C3 C2 O2 114.8(8) . . ?
C3 C2 C1 121.2(8) . . ?
O2 C2 C1 123.9(8) . . ?
O16 Co3 O16 149.3(3) 2_665 . ?
O16 Co3 O9 81.4(2) 2_665 2_665 ?
O16 Co3 O9 96.7(2) . 2_665 ?
O16 Co3 O9 96.7(2) 2_665 . ?
O16 Co3 O9 81.4(2) . . ?
O9 Co3 O9 173.2(3) 2_665 . ?
O16 Co3 N31 105.37(16) 2_665 . ?
O16 Co3 N31 105.37(16) . . ?
O9 Co3 N31 93.40(15) 2_665 . ?
O9 Co3 N31 93.40(15) . . ?
C9 O3 Co2 108.2(5) . . ?
C9 O3 H100 108.8 . . ?
Co2 O3 H100 113.4 . . ?
O10 C3 C2 120.0(8) . . ?
O10 C3 C4 120.2(8) . . ?
C2 C3 C4 119.8(9) . . ?
O1 C4 C3 114.6(8) . . ?
O1 C4 C5 124.6(8) . . ?
C3 C4 C5 120.8(8) . . ?
C4 C5 C6 117.8(8) . . ?
C4 C5 C7 120.4(8) . . ?
C6 C5 C7 121.7(8) . . ?
C5 C6 C1 122.8(8) . . ?
C5 C6 H6 118.6 . . ?
C1 C6 H6 118.6 . . ?
C15 C7 C5 115.5(7) . . ?
C15 C7 C8 114.6(8) . . ?
C5 C7 C8 109.8(7) . . ?
C15 C7 H7 105.3 . . ?
C5 C7 H7 105.3 . . ?
C8 C7 H7 105.3 . . ?
C9 C8 C13 118.4(8) . . ?
C9 C8 C7 121.7(8) . . ?
C13 C8 C7 119.4(9) . . ?
C11 O9 Co3 109.4(5) . . ?
O3 C9 C8 123.6(8) . . ?
O3 C9 C10 117.6(9) . . ?
C8 C9 C10 118.8(9) . . ?
C3 O10 Co2 112.1(5) . 4_655 ?
C3 O10 Co1 112.2(5) . . ?
Co2 O10 Co1 135.6(3) 4_655 . ?
C11 C10 O16 118.8(9) . . ?
C11 C10 C9 122.6(9) . . ?
O16 C10 C9 118.4(9) . . ?
C10 C11 O9 116.1(9) . . ?
C10 C11 C12 120.1(9) . . ?
O9 C11 C12 123.7(8) . . ?
C13 C12 C11 117.6(8) . . ?
C13 C12 C14 121.5(9) . . ?
C11 C12 C14 120.7(8) . . ?
C12 C13 C8 122.5(9) . . ?
C12 C13 H13 118.7 . . ?
C8 C13 H13 118.7 . . ?
C17 C14 C12 113.9(7) . . ?
C17 C14 C1 115.0(7) . 3_565 ?
C12 C14 C1 109.9(7) . 3_565 ?
C17 C14 H14 105.7 . . ?
C12 C14 H14 105.7 . . ?
C1 C14 H14 105.7 3_565 . ?
C7 C15 C16 113.5(9) . . ?
C7 C15 H15A 108.9 . . ?
C16 C15 H15A 108.9 . . ?
C7 C15 H15B 108.9 . . ?
C16 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C10 O16 Co2 109.6(5) . . ?
C10 O16 Co3 109.9(5) . . ?
Co2 O16 Co3 132.3(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C14 112.6(8) . . ?
C18 C17 H17A 109.1 . . ?
C14 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C14 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 N19 C24 117.4(7) . . ?
C20 N19 Co1 117.2(6) . . ?
C24 N19 Co1 125.1(7) . . ?
N19 C20 C21 122.8(9) . . ?
N19 C20 H20 118.6 . . ?
C21 C20 H20 118.6 . . ?
C22 C21 C20 119.2(9) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C23 C22 C21 119.0(9) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 118.5(9) . . ?
C22 C23 H23 120.8 . . ?
C24 C23 H23 120.8 . . ?
N19 C24 C23 123.0(9) . . ?
N19 C24 H24 118.5 . . ?
C23 C24 H24 118.5 . . ?
C26 N25 C30 117.5(9) . . ?
C26 N25 Co2 121.0(7) . . ?
C30 N25 Co2 121.4(8) . . ?
N25 C26 C27 124.3(11) . . ?
N25 C26 H26 117.9 . . ?
C27 C26 H26 117.9 . . ?
C28 C27 C26 117.2(14) . . ?
C28 C27 H27 121.4 . . ?
C26 C27 H27 121.4 . . ?
C27 C28 C29 121.3(13) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C28 C29 C30 116.7(13) . . ?
C28 C29 H29 121.6 . . ?
C30 C29 H29 121.6 . . ?
N25 C30 C29 123.0(13) . . ?
N25 C30 H30 118.5 . . ?
C29 C30 H30 118.5 . . ?
C32 N31 C32 117.9(13) . 2_665 ?
C32 N31 Co3 121.0(6) . . ?
C32 N31 Co3 121.0(6) 2_665 . ?
N31 C32 C33 122.9(11) . . ?
N31 C32 H32 118.5 . . ?
C33 C32 H32 118.5 . . ?
C34 C33 C32 117.8(13) . . ?
C34 C33 H33 121.1 . . ?
C32 C33 H33 121.1 . . ?
C33 C34 C33 120.6(17) 2_665 . ?
C33 C34 H34 119.7 2_665 . ?
C33 C34 H34 119.7 . . ?
C41 N40 C41 116.6(13) . 14_655 ?
N40 C41 C42 120.9(10) . . ?
N40 C41 H41 119.6 . . ?
C42 C41 H41 119.6 . . ?
C43 C42 C41 121.3(11) . . ?
C43 C42 H42 119.3 . . ?
C41 C42 H42 119.3 . . ?
C42 C43 C42 118.9(14) 14_655 . ?
C42 C43 H43 120.5 14_655 . ?
C42 C43 H43 120.5 . . ?
C45 C44 N49 119(2) . . ?
C45 C44 H44 120.3 . . ?
N49 C44 H44 120.3 . . ?
C46 C45 C44 121(2) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C47 122.8(19) . . ?
C45 C46 H46 118.6 . . ?
C47 C46 H46 118.6 . . ?
C46 C47 C48 120.0(18) . . ?
C46 C47 H47 120.0 . . ?
C48 C47 H47 120.0 . . ?
C47 C48 N49 115.7(18) . . ?
C47 C48 H48 122.1 . . ?
N49 C48 H48 122.1 . . ?
C44 N49 C48 121.1(18) . . ?
C61 N60 C65 120.0 . . ?
C62 C61 N60 120.0 . . ?
C62 C61 H61 120.0 . . ?
N60 C61 H61 120.0 . . ?
C61 C62 C63 120.0 . . ?
C61 C62 H62 120.0 . . ?
C63 C62 H62 120.0 . . ?
C64 C63 C62 120.0 . . ?
C64 C63 H63 120.0 . . ?
C62 C63 H63 120.0 . . ?
C63 C64 C65 120.0 . . ?
C63 C64 H64 120.0 . . ?
C65 C64 H64 120.0 . . ?
C64 C65 N60 120.0 . . ?
C64 C65 H65 120.0 . . ?
N60 C65 H65 120.0 . . ?
C71 C70 C75 120.0 . . ?
C71 C70 H70 120.0 . . ?
C75 C70 H70 120.0 . . ?
C72 C71 C70 120.0 . . ?
C72 C71 H71 120.0 . . ?
C70 C71 H71 120.0 . . ?
C71 C72 C73 120.0 . . ?
C71 C72 H72 120.0 . . ?
C73 C72 H72 120.0 . . ?
C74 C73 C72 120.0 . . ?
C74 C73 H73 120.0 . . ?
C72 C73 H73 120.0 . . ?
C73 C74 C75 120.0 . . ?
C73 C74 H74 120.0 . . ?
C75 C74 H74 120.0 . . ?
C74 C75 C70 120.0 . . ?
C74 C75 H75 120.0 . . ?
C70 C75 H75 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        21.44
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.071

# Attachment '742757.cif'

data_Ni8PgC2MeCNPy
_database_code_depnum_ccdc_archive 'CCDC 742757'
#TrackingRef '742757.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C161 H155 N19 Ni8 O24'
_chemical_formula_weight         3209.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.1906 1.3024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fddd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   19.7468(9)
_cell_length_b                   27.6774(13)
_cell_length_c                   53.647(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     29320(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             13360
_exptl_absorpt_coefficient_mu    1.346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7746
_exptl_absorpt_correction_T_max  0.8771
_exptl_absorpt_process_details   'SADABS 2004 Bruker AXS, Madison, WI'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77490
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean .
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            39692
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_limit_l_max       66
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         28.98
_reflns_number_total             7504
_reflns_number_gt                5462
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX 2'
_computing_cell_refinement       'Bruker SAINTv7.34a'
_computing_data_reduction        'Bruker SAINTv7.34a'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed v2.0 (Barbour, 2005)'
_computing_publication_material  'local program'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. A disordered ligated pyri-
dine molecule has been modelled over two positions, each with half occup-
ancy. The FLAT and SAME instructions were applied to the disordered
pyridine N47 - C52. The SIMU instruction was also applied to three pyridi-
ne rings, N31 - C36, N37 - C42 and N47 - C52. Pyrogallol[4]arene upper rim
hydroxyl H atoms were located from the difference map. These OH distances
were constrained using the DFIX command.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+217.5138P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7504
_refine_ls_number_parameters     534
_refine_ls_number_restraints     131
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0630
_refine_ls_wR_factor_ref         0.2007
_refine_ls_wR_factor_gt          0.1806
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.6250 0.30925(3) 0.1250 0.0346(2) Uani 1 2 d S . .
O1 O 0.71945(15) 0.22177(11) 0.19153(5) 0.0362(7) Uani 1 1 d . . .
C1 C 0.8185(2) 0.20494(16) 0.16566(8) 0.0372(9) Uani 1 1 d . . .
Ni2 Ni 0.62604(3) 0.00370(2) 0.187525(10) 0.03459(18) Uani 1 1 d . . .
O2 O 0.65750(15) 0.26652(10) 0.15441(5) 0.0349(6) Uani 1 1 d . . .
C2 C 0.7548(2) 0.22573(15) 0.16967(7) 0.0364(9) Uani 1 1 d . . .
Ni3 Ni 0.6250 0.1250 0.210959(14) 0.0348(2) Uani 1 2 d S . .
H100 H 0.721(4) 0.286(3) 0.0989(5) 0.10(3) Uiso 1 1 d D . .
H101 H 0.729(4) 0.1709(13) 0.2047(12) 0.09(3) Uiso 1 1 d D . .
O3 O 0.72411(16) 0.29567(11) 0.11330(6) 0.0377(7) Uani 1 1 d D . .
C3 C 0.7224(2) 0.25262(15) 0.15114(8) 0.0351(9) Uani 1 1 d . . .
O4 O 0.72404(15) -0.01241(11) 0.17894(5) 0.0375(7) Uani 1 1 d . . .
C4 C 0.7570(2) 0.26409(15) 0.12917(8) 0.0359(9) Uani 1 1 d . . .
O5 O 0.66901(15) 0.05788(11) 0.20679(5) 0.0367(7) Uani 1 1 d . C .
C5 C 0.8199(2) 0.24352(16) 0.12420(8) 0.0389(10) Uani 1 1 d . . .
O6 O 0.72488(16) 0.14437(11) 0.21144(5) 0.0376(7) Uani 1 1 d D C .
C6 C 0.8486(2) 0.21364(15) 0.14246(8) 0.0373(10) Uani 1 1 d . . .
H6 H 0.8907 0.1985 0.1389 0.045 Uiso 1 1 calc R . .
C7 C 0.8520(3) -0.00010(17) 0.15157(9) 0.0427(11) Uani 1 1 d . . .
H7 H 0.8354 -0.0320 0.1579 0.051 Uiso 1 1 calc R . .
C8 C 0.8223(2) 0.03805(16) 0.16924(8) 0.0377(10) Uani 1 1 d . . .
C9 C 0.7606(2) 0.02932(15) 0.18151(8) 0.0356(9) Uani 1 1 d . C .
C10 C 0.7311(2) 0.06539(15) 0.19606(7) 0.0359(9) Uani 1 1 d . . .
C11 C 0.7608(2) 0.11090(16) 0.19774(8) 0.0367(9) Uani 1 1 d . C .
C12 C 0.8207(2) 0.12154(16) 0.18525(8) 0.0379(10) Uani 1 1 d . . .
C13 C 0.8505(2) 0.08386(16) 0.17138(8) 0.0385(10) Uani 1 1 d . C .
H13 H 0.8920 0.0901 0.1630 0.046 Uiso 1 1 calc R . .
C14 C 0.8502(2) 0.17236(17) 0.18578(9) 0.0424(10) Uani 1 1 d . C .
H14 H 0.8364 0.1865 0.2022 0.051 Uiso 1 1 calc R . .
C15 C 0.9279(3) -0.0030(2) 0.15225(10) 0.0563(13) Uani 1 1 d . . .
H15A H 0.9430 -0.0070 0.1697 0.068 Uiso 1 1 calc R . .
H15B H 0.9472 0.0276 0.1458 0.068 Uiso 1 1 calc R . .
C16 C 0.9542(3) -0.0454(2) 0.13651(12) 0.0676(17) Uani 1 1 d . . .
H16A H 0.9321 -0.0753 0.1419 0.101 Uiso 1 1 calc R . .
H16B H 1.0033 -0.0483 0.1387 0.101 Uiso 1 1 calc R . .
H16C H 0.9439 -0.0395 0.1189 0.101 Uiso 1 1 calc R . .
C17 C 0.9277(3) 0.1715(2) 0.18595(11) 0.0573(13) Uani 1 1 d . . .
H17A H 0.9431 0.1471 0.1982 0.069 Uiso 1 1 calc R C .
H17B H 0.9439 0.1613 0.1693 0.069 Uiso 1 1 calc R . .
C18 C 0.9589(3) 0.2194(2) 0.19232(15) 0.078(2) Uani 1 1 d . C .
H18A H 0.9478 0.2429 0.1793 0.117 Uiso 1 1 calc R . .
H18B H 1.0082 0.2158 0.1934 0.117 Uiso 1 1 calc R . .
H18C H 0.9411 0.2307 0.2083 0.117 Uiso 1 1 calc R . .
N19 N 0.6132(2) 0.36474(13) 0.09864(7) 0.0383(8) Uani 1 1 d D . .
C20 C 0.5538(3) 0.38439(17) 0.09443(9) 0.0486(12) Uani 1 1 d D . .
H20 H 0.5161 0.3736 0.1039 0.058 Uiso 1 1 calc R . .
C21 C 0.5436(3) 0.4200(2) 0.07680(11) 0.0601(14) Uani 1 1 d D . .
H21 H 0.4996 0.4331 0.0743 0.072 Uiso 1 1 calc R . .
C22 C 0.5968(3) 0.4363(2) 0.06305(10) 0.0605(14) Uani 1 1 d D . .
H22 H 0.5905 0.4609 0.0509 0.073 Uiso 1 1 calc R . .
C23 C 0.6589(3) 0.41689(18) 0.06691(9) 0.0514(12) Uani 1 1 d D . .
H23 H 0.6969 0.4278 0.0576 0.062 Uiso 1 1 calc R . .
C24 C 0.6659(3) 0.38078(17) 0.08464(9) 0.0474(12) Uani 1 1 d D . .
H24 H 0.7093 0.3667 0.0871 0.057 Uiso 1 1 calc R . .
N25 N 0.6170(2) -0.04819(15) 0.21374(7) 0.0447(10) Uani 1 1 d D . .
C26 C 0.6681(4) -0.0605(3) 0.22857(11) 0.0768(19) Uani 1 1 d D . .
H26 H 0.7091 -0.0425 0.2277 0.092 Uiso 1 1 calc R . .
C27 C 0.6637(5) -0.0990(3) 0.24543(13) 0.091(2) Uani 1 1 d D . .
H27 H 0.7018 -0.1081 0.2552 0.109 Uiso 1 1 calc R . .
C28 C 0.6041(5) -0.1230(3) 0.24760(14) 0.092(3) Uani 1 1 d D . .
H28 H 0.5998 -0.1490 0.2591 0.111 Uiso 1 1 calc R . .
C29 C 0.5515(4) -0.1097(2) 0.23343(12) 0.0777(19) Uani 1 1 d D . .
H29 H 0.5089 -0.1253 0.2353 0.093 Uiso 1 1 calc R . .
C30 C 0.5595(3) -0.07320(19) 0.21617(10) 0.0571(14) Uani 1 1 d D . .
H30 H 0.5226 -0.0655 0.2055 0.068 Uiso 1 1 calc R . .
N31 N 0.6250 0.1250 0.24970(10) 0.0441(13) Uani 1 2 d SU . .
C32 C 0.6049(8) 0.1635(8) 0.2628(4) 0.058(3) Uani 0.50 1 d PU A 2
H32 H 0.5893 0.1908 0.2537 0.070 Uiso 0.50 1 calc PR A 2
C33 C 0.6051(8) 0.1667(7) 0.2885(3) 0.064(3) Uani 0.50 1 d PU A 2
H33 H 0.5925 0.1955 0.2969 0.077 Uiso 0.50 1 calc PR A 2
C34 C 0.6250 0.1250 0.30129(15) 0.075(2) Uani 1 2 d SU . .
H34 H 0.6250 0.1250 0.3190 0.089 Uiso 1 2 calc SR A 1
C35 C 0.5833(8) 0.1548(7) 0.2624(4) 0.058(3) Uani 0.50 1 d PU A 1
H35 H 0.5553 0.1765 0.2534 0.069 Uiso 0.50 1 calc PR A 1
C36 C 0.5802(8) 0.1547(7) 0.2884(3) 0.067(3) Uani 0.50 1 d PU A 1
H36 H 0.5484 0.1743 0.2971 0.081 Uiso 0.50 1 calc PR A 1
N37 N 0.4755(5) 0.2360(3) -0.00635(18) 0.136(3) Uiso 1 1 d DU . .
C38 C 0.5196(6) 0.2595(4) -0.0246(2) 0.144(4) Uiso 1 1 d DU . .
H38 H 0.5659 0.2511 -0.0266 0.173 Uiso 1 1 calc R . .
C39 C 0.4886(5) 0.2949(4) -0.03861(19) 0.119(3) Uiso 1 1 d DU . .
H39 H 0.5129 0.3099 -0.0518 0.143 Uiso 1 1 calc R . .
C40 C 0.4270(6) 0.3078(4) -0.0341(2) 0.137(3) Uiso 1 1 d DU . .
H40 H 0.4079 0.3330 -0.0439 0.164 Uiso 1 1 calc R . .
C41 C 0.3891(6) 0.2876(5) -0.0166(2) 0.150(4) Uiso 1 1 d DU . .
H41 H 0.3445 0.2985 -0.0131 0.180 Uiso 1 1 calc R . .
C42 C 0.4163(6) 0.2526(4) -0.0046(2) 0.127(3) Uiso 1 1 d DU . .
H42 H 0.3879 0.2371 0.0072 0.152 Uiso 1 1 calc R . .
N43 N 0.3750 0.3750 0.08753(14) 0.0628(18) Uani 1 2 d S . .
C44 C 0.3914(3) 0.33427(19) 0.07472(11) 0.0561(13) Uani 1 1 d . . .
H44 H 0.4038 0.3057 0.0834 0.067 Uiso 1 1 calc R . .
C45 C 0.3898(3) 0.3350(2) 0.04917(13) 0.0687(17) Uani 1 1 d . . .
H45 H 0.3995 0.3063 0.0402 0.082 Uiso 1 1 calc R . .
C46 C 0.3750 0.3750 0.03689(17) 0.069(2) Uani 1 2 d S . .
H46 H 0.3750 0.3750 0.0192 0.083 Uiso 1 2 calc SR . .
N47 N 1.1032(10) 0.2025(7) 0.0998(4) 0.087(5) Uani 0.25 1 d PDU B -1
C48 C 1.0605(10) 0.1640(8) 0.1024(5) 0.084(5) Uani 0.25 1 d PDU B -1
H48 H 1.0435 0.1479 0.0880 0.101 Uiso 0.25 1 calc PR B -1
C49 C 1.0423(10) 0.1487(8) 0.1252(5) 0.079(5) Uani 0.25 1 d PDU B -1
H49 H 1.0125 0.1220 0.1271 0.095 Uiso 0.25 1 calc PR B -1
C50 C 1.0669(11) 0.1718(8) 0.1453(5) 0.091(5) Uani 0.25 1 d PDU B -1
H50 H 1.0543 0.1607 0.1614 0.110 Uiso 0.25 1 calc PR B -1
C51 C 1.1086(12) 0.2097(8) 0.1435(4) 0.085(5) Uani 0.25 1 d PDU B -1
H51 H 1.1252 0.2259 0.1578 0.102 Uiso 0.25 1 calc PR B -1
C52 C 1.1260(13) 0.2241(7) 0.1199(4) 0.077(5) Uani 0.25 1 d PDU B -1
H52 H 1.1559 0.2508 0.1181 0.093 Uiso 0.25 1 calc PR B -1
N53 N 0.628(3) 0.1235(11) 0.16939(16) 0.063(4) Uani 0.50 1 d P C -1
C54 C 0.6724(5) 0.1262(3) 0.15231(17) 0.0377(19) Uani 0.50 1 d P C -1
C55 C 0.7184(5) 0.1229(5) 0.13150(14) 0.046(2) Uani 0.50 1 d P C -1
H55A H 0.7631 0.1128 0.1374 0.068 Uiso 0.50 1 calc PR C -1
H55B H 0.7220 0.1545 0.1234 0.068 Uiso 0.50 1 calc PR C -1
H55C H 0.7012 0.0991 0.1195 0.068 Uiso 0.50 1 calc PR C -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0443(5) 0.0316(4) 0.0278(4) 0.000 0.0041(3) 0.000
O1 0.0408(17) 0.0380(16) 0.0298(15) -0.0051(12) 0.0025(12) 0.0055(13)
C1 0.041(2) 0.034(2) 0.037(2) -0.0091(17) 0.0010(18) -0.0020(18)
Ni2 0.0425(3) 0.0346(3) 0.0266(3) 0.0009(2) -0.0037(2) 0.0065(2)
O2 0.0396(16) 0.0354(15) 0.0297(14) -0.0006(11) 0.0042(12) 0.0040(13)
C2 0.042(2) 0.038(2) 0.029(2) -0.0082(17) 0.0025(17) -0.0035(19)
Ni3 0.0418(5) 0.0368(4) 0.0259(4) 0.000 0.000 0.0088(3)
O3 0.0463(18) 0.0369(16) 0.0298(16) -0.0025(13) 0.0033(13) -0.0041(13)
C3 0.041(2) 0.033(2) 0.031(2) -0.0068(16) 0.0015(17) -0.0013(18)
O4 0.0442(17) 0.0361(16) 0.0323(15) -0.0027(12) -0.0029(13) 0.0079(13)
C4 0.043(2) 0.032(2) 0.032(2) -0.0034(16) -0.0017(18) -0.0026(18)
O5 0.0415(17) 0.0401(16) 0.0285(14) -0.0019(12) -0.0021(12) 0.0075(13)
C5 0.040(2) 0.041(2) 0.036(2) -0.0121(18) 0.0039(18) -0.0085(19)
O6 0.0466(18) 0.0364(17) 0.0297(15) -0.0049(12) 0.0003(13) 0.0090(14)
C6 0.036(2) 0.036(2) 0.039(2) -0.0130(18) -0.0014(18) -0.0022(18)
C7 0.048(3) 0.042(2) 0.038(2) -0.0119(19) -0.005(2) 0.014(2)
C8 0.042(2) 0.042(2) 0.029(2) -0.0052(17) -0.0058(17) 0.0101(19)
C9 0.039(2) 0.037(2) 0.030(2) 0.0011(17) -0.0062(17) 0.0082(18)
C10 0.042(2) 0.040(2) 0.0253(19) -0.0029(16) -0.0061(17) 0.0092(19)
C11 0.041(2) 0.042(2) 0.028(2) -0.0062(17) -0.0042(17) 0.0098(19)
C12 0.039(2) 0.044(2) 0.031(2) -0.0035(18) -0.0049(17) 0.0050(19)
C13 0.039(2) 0.045(2) 0.032(2) -0.0052(18) -0.0048(18) 0.005(2)
C14 0.042(2) 0.043(2) 0.041(2) -0.0113(19) -0.005(2) 0.003(2)
C15 0.057(3) 0.061(3) 0.050(3) -0.007(2) -0.002(2) 0.010(3)
C16 0.066(4) 0.076(4) 0.061(4) -0.011(3) -0.007(3) 0.026(3)
C17 0.055(3) 0.059(3) 0.059(3) -0.005(3) -0.005(3) 0.003(3)
C18 0.064(4) 0.059(4) 0.112(6) -0.003(4) -0.022(4) -0.007(3)
N19 0.051(2) 0.0317(18) 0.0325(18) -0.0026(14) 0.0014(16) -0.0030(16)
C20 0.058(3) 0.041(3) 0.046(3) 0.010(2) 0.010(2) 0.003(2)
C21 0.064(4) 0.055(3) 0.061(3) 0.022(3) 0.002(3) 0.008(3)
C22 0.081(4) 0.050(3) 0.051(3) 0.019(2) 0.001(3) 0.001(3)
C23 0.063(3) 0.050(3) 0.041(3) 0.008(2) 0.003(2) -0.011(3)
C24 0.058(3) 0.043(3) 0.041(2) 0.003(2) 0.002(2) -0.012(2)
N25 0.061(3) 0.045(2) 0.0286(18) 0.0037(16) -0.0023(17) 0.0135(19)
C26 0.086(5) 0.098(5) 0.047(3) 0.024(3) -0.017(3) 0.007(4)
C27 0.112(6) 0.106(6) 0.054(4) 0.026(4) -0.015(4) 0.024(5)
C28 0.123(7) 0.090(5) 0.065(4) 0.041(4) 0.015(4) 0.014(5)
C29 0.109(6) 0.063(4) 0.061(4) 0.021(3) 0.009(4) -0.004(4)
C30 0.077(4) 0.044(3) 0.050(3) 0.010(2) 0.000(3) 0.000(3)
N31 0.046(3) 0.058(3) 0.029(2) 0.000 0.000 0.013(3)
C32 0.071(6) 0.070(6) 0.034(4) -0.005(4) -0.004(5) 0.022(5)
C33 0.076(7) 0.079(6) 0.037(4) -0.010(4) -0.002(5) 0.021(5)
C34 0.088(6) 0.100(6) 0.036(3) 0.000 0.000 0.034(5)
C35 0.066(6) 0.073(6) 0.035(4) 0.002(4) 0.003(5) 0.031(5)
C36 0.079(7) 0.086(6) 0.037(4) -0.002(4) 0.008(5) 0.035(5)
N43 0.066(4) 0.052(4) 0.070(5) 0.000 0.000 -0.005(3)
C44 0.058(3) 0.039(3) 0.072(4) -0.004(2) -0.003(3) 0.002(2)
C45 0.079(4) 0.057(4) 0.070(4) -0.018(3) 0.005(3) 0.001(3)
C46 0.085(6) 0.075(6) 0.047(4) 0.000 0.000 -0.005(5)
N47 0.074(9) 0.077(9) 0.111(12) 0.017(9) -0.023(9) -0.013(8)
C48 0.062(9) 0.085(10) 0.105(12) 0.006(9) -0.025(9) -0.010(8)
C49 0.047(9) 0.088(10) 0.102(12) -0.006(9) -0.002(9) 0.004(8)
C50 0.071(10) 0.097(10) 0.107(12) -0.009(10) 0.018(9) 0.018(8)
C51 0.074(10) 0.074(10) 0.108(13) -0.012(9) 0.000(10) 0.019(9)
C52 0.070(9) 0.060(8) 0.102(13) 0.005(9) -0.011(10) 0.004(9)
N53 0.092(8) 0.057(6) 0.041(4) -0.032(9) -0.015(12) 0.042(5)
C54 0.044(5) 0.032(4) 0.037(5) -0.005(4) -0.011(4) 0.006(4)
C55 0.054(5) 0.054(6) 0.028(6) -0.006(7) -0.001(3) 0.002(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 2.073(3) 4_655 ?
Ni1 O2 2.073(3) . ?
Ni1 O3 2.089(3) 4_655 ?
Ni1 O3 2.089(3) . ?
Ni1 N19 2.101(4) 4_655 ?
Ni1 N19 2.101(4) . ?
O1 C2 1.369(5) . ?
O1 Ni2 2.016(3) 2_655 ?
C1 C2 1.399(6) . ?
C1 C6 1.401(6) . ?
C1 C14 1.540(7) . ?
Ni2 O2 1.977(3) 2_655 ?
Ni2 O5 2.009(3) . ?
Ni2 O1 2.016(3) 2_655 ?
Ni2 N25 2.018(4) . ?
Ni2 O4 2.039(3) . ?
O2 C3 1.350(5) . ?
O2 Ni2 1.977(3) 2_655 ?
C2 C3 1.397(6) . ?
Ni3 O6 2.044(3) . ?
Ni3 O6 2.044(3) 2_655 ?
Ni3 O5 2.063(3) 2_655 ?
Ni3 O5 2.063(3) . ?
Ni3 N31 2.079(5) . ?
Ni3 N53 2.231(9) 2_655 ?
Ni3 N53 2.231(9) . ?
O3 C4 1.382(5) . ?
O3 H100 0.822(10) . ?
C3 C4 1.399(6) . ?
O4 C9 1.369(5) . ?
C4 C5 1.392(7) . ?
O5 C10 1.370(5) . ?
C5 C6 1.402(7) . ?
C5 C7 1.532(6) 3 ?
O6 C11 1.379(5) . ?
O6 H101 0.822(10) . ?
C6 H6 0.9500 . ?
C7 C15 1.500(7) . ?
C7 C5 1.532(6) 3 ?
C7 C8 1.536(6) . ?
C7 H7 1.0000 . ?
C8 C13 1.389(6) . ?
C8 C9 1.406(6) . ?
C9 C10 1.395(6) . ?
C10 C11 1.393(6) . ?
C11 C12 1.391(7) . ?
C12 C13 1.409(6) . ?
C12 C14 1.523(6) . ?
C13 H13 0.9500 . ?
C14 C17 1.529(7) . ?
C14 H14 1.0000 . ?
C15 C16 1.536(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.502(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N19 C20 1.313(6) . ?
N19 C24 1.358(6) . ?
C20 C21 1.381(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.361(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.355(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(7) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
N25 C26 1.329(7) . ?
N25 C30 1.336(7) . ?
C26 C27 1.401(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.356(12) . ?
C27 H27 0.9500 . ?
C28 C29 1.339(11) . ?
C28 H28 0.9500 . ?
C29 C30 1.379(7) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
N31 C32 1.34(2) . ?
N31 C32 1.34(2) 2_655 ?
N31 C35 1.350(19) . ?
N31 C35 1.350(19) 2_655 ?
C32 C33 1.38(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.400(19) . ?
C33 H33 0.9500 . ?
C34 C36 1.390(18) . ?
C34 C36 1.390(18) 2_655 ?
C34 C33 1.400(19) 2_655 ?
C34 H34 0.9500 . ?
C35 C36 1.40(2) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
N37 C42 1.261(11) . ?
N37 C38 1.462(12) . ?
C38 C39 1.379(12) . ?
C38 H38 0.9500 . ?
C39 C40 1.290(12) . ?
C39 H39 0.9500 . ?
C40 C41 1.327(12) . ?
C40 H40 0.9500 . ?
C41 C42 1.280(12) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
N43 C44 1.359(6) 14 ?
N43 C44 1.359(6) . ?
C44 C45 1.371(9) . ?
C44 H44 0.9500 . ?
C45 C46 1.321(8) . ?
C45 H45 0.9500 . ?
C46 C45 1.321(8) 14 ?
C46 H46 0.9500 . ?
N47 C52 1.315(18) . ?
N47 C48 1.368(18) . ?
C48 C49 1.344(19) . ?
C48 H48 0.9500 . ?
C49 C50 1.34(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.34(2) . ?
C50 H50 0.9500 . ?
C51 C52 1.37(2) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
N53 C54 1.27(4) . ?
C54 C55 1.441(13) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?

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 Ni1 O2 110.44(16) 4_655 . ?
O2 Ni1 O3 80.57(12) 4_655 4_655 ?
O2 Ni1 O3 87.63(12) . 4_655 ?
O2 Ni1 O3 87.63(12) 4_655 . ?
O2 Ni1 O3 80.57(12) . . ?
O3 Ni1 O3 159.27(17) 4_655 . ?
O2 Ni1 N19 164.47(13) 4_655 4_655 ?
O2 Ni1 N19 82.56(12) . 4_655 ?
O3 Ni1 N19 91.90(14) 4_655 4_655 ?
O3 Ni1 N19 103.30(14) . 4_655 ?
O2 Ni1 N19 82.56(12) 4_655 . ?
O2 Ni1 N19 164.47(13) . . ?
O3 Ni1 N19 103.30(14) 4_655 . ?
O3 Ni1 N19 91.90(14) . . ?
N19 Ni1 N19 86.04(19) 4_655 . ?
C2 O1 Ni2 111.0(3) . 2_655 ?
C2 C1 C6 116.6(4) . . ?
C2 C1 C14 119.9(4) . . ?
C6 C1 C14 123.4(4) . . ?
O2 Ni2 O5 144.59(12) 2_655 . ?
O2 Ni2 O1 82.98(12) 2_655 2_655 ?
O5 Ni2 O1 95.10(12) . 2_655 ?
O2 Ni2 N25 113.29(15) 2_655 . ?
O5 Ni2 N25 102.11(15) . . ?
O1 Ni2 N25 94.77(14) 2_655 . ?
O2 Ni2 O4 93.04(12) 2_655 . ?
O5 Ni2 O4 83.02(12) . . ?
O1 Ni2 O4 170.34(12) 2_655 . ?
N25 Ni2 O4 94.89(14) . . ?
C3 O2 Ni2 110.7(3) . 2_655 ?
C3 O2 Ni1 111.0(2) . . ?
Ni2 O2 Ni1 137.87(16) 2_655 . ?
O1 C2 C3 114.7(4) . . ?
O1 C2 C1 123.8(4) . . ?
C3 C2 C1 121.4(4) . . ?
O6 Ni3 O6 178.54(17) . 2_655 ?
O6 Ni3 O5 99.89(12) . 2_655 ?
O6 Ni3 O5 80.28(12) 2_655 2_655 ?
O6 Ni3 O5 80.28(12) . . ?
O6 Ni3 O5 99.89(12) 2_655 . ?
O5 Ni3 O5 167.56(16) 2_655 . ?
O6 Ni3 N31 89.27(8) . . ?
O6 Ni3 N31 89.27(8) 2_655 . ?
O5 Ni3 N31 96.22(8) 2_655 . ?
O5 Ni3 N31 96.22(8) . . ?
O6 Ni3 N53 92.1(12) . 2_655 ?
O6 Ni3 N53 89.3(12) 2_655 2_655 ?
O5 Ni3 N53 82.1(9) 2_655 2_655 ?
O5 Ni3 N53 85.4(9) . 2_655 ?
N31 Ni3 N53 178.0(12) . 2_655 ?
O6 Ni3 N53 89.3(12) . . ?
O6 Ni3 N53 92.1(12) 2_655 . ?
O5 Ni3 N53 85.4(9) 2_655 . ?
O5 Ni3 N53 82.1(9) . . ?
N31 Ni3 N53 178.0(12) . . ?
N53 Ni3 N53 4(2) 2_655 . ?
C4 O3 Ni1 111.6(3) . . ?
C4 O3 H100 114(6) . . ?
Ni1 O3 H100 106(6) . . ?
O2 C3 C2 119.6(4) . . ?
O2 C3 C4 120.5(4) . . ?
C2 C3 C4 119.8(4) . . ?
C9 O4 Ni2 107.1(2) . . ?
O3 C4 C5 124.0(4) . . ?
O3 C4 C3 115.7(4) . . ?
C5 C4 C3 120.3(4) . . ?
C10 O5 Ni2 105.9(2) . . ?
C10 O5 Ni3 106.6(2) . . ?
Ni2 O5 Ni3 123.36(15) . . ?
C4 C5 C6 117.9(4) . . ?
C4 C5 C7 119.6(4) . 3 ?
C6 C5 C7 122.2(4) . 3 ?
C11 O6 Ni3 108.3(3) . . ?
C11 O6 H101 109(5) . . ?
Ni3 O6 H101 108(5) . . ?
C1 C6 C5 123.4(4) . . ?
C1 C6 H6 118.3 . . ?
C5 C6 H6 118.3 . . ?
C15 C7 C5 116.2(4) . 3 ?
C15 C7 C8 113.8(4) . . ?
C5 C7 C8 108.5(3) 3 . ?
C15 C7 H7 105.8 . . ?
C5 C7 H7 105.8 3 . ?
C8 C7 H7 105.8 . . ?
C13 C8 C9 117.7(4) . . ?
C13 C8 C7 121.7(4) . . ?
C9 C8 C7 120.2(4) . . ?
O4 C9 C10 116.1(4) . . ?
O4 C9 C8 123.7(4) . . ?
C10 C9 C8 120.1(4) . . ?
O5 C10 C11 119.2(4) . . ?
O5 C10 C9 120.0(4) . . ?
C11 C10 C9 120.5(4) . . ?
O6 C11 C12 123.5(4) . . ?
O6 C11 C10 115.1(4) . . ?
C12 C11 C10 121.3(4) . . ?
C11 C12 C13 116.9(4) . . ?
C11 C12 C14 120.8(4) . . ?
C13 C12 C14 122.3(4) . . ?
C8 C13 C12 123.5(4) . . ?
C8 C13 H13 118.2 . . ?
C12 C13 H13 118.2 . . ?
C12 C14 C17 111.6(4) . . ?
C12 C14 C1 111.8(4) . . ?
C17 C14 C1 114.9(4) . . ?
C12 C14 H14 105.9 . . ?
C17 C14 H14 105.9 . . ?
C1 C14 H14 105.9 . . ?
C7 C15 C16 111.4(5) . . ?
C7 C15 H15A 109.3 . . ?
C16 C15 H15A 109.3 . . ?
C7 C15 H15B 109.3 . . ?
C16 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C14 113.4(5) . . ?
C18 C17 H17A 108.9 . . ?
C14 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
C14 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 N19 C24 117.0(4) . . ?
C20 N19 Ni1 121.2(3) . . ?
C24 N19 Ni1 121.7(3) . . ?
N19 C20 C21 123.0(5) . . ?
N19 C20 H20 118.5 . . ?
C21 C20 H20 118.5 . . ?
C22 C21 C20 119.6(5) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C23 C22 C21 119.0(5) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 118.8(5) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
N19 C24 C23 122.5(5) . . ?
N19 C24 H24 118.7 . . ?
C23 C24 H24 118.7 . . ?
C26 N25 C30 117.0(5) . . ?
C26 N25 Ni2 122.2(4) . . ?
C30 N25 Ni2 120.8(3) . . ?
N25 C26 C27 122.3(7) . . ?
N25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
C28 C27 C26 118.8(7) . . ?
C28 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
C29 C28 C27 119.3(6) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 119.5(7) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
N25 C30 C29 122.9(6) . . ?
N25 C30 H30 118.6 . . ?
C29 C30 H30 118.6 . . ?
C32 N31 C32 116.5(19) . 2_655 ?
C32 N31 C35 21.0(11) . . ?
C32 N31 C35 113.7(7) 2_655 . ?
C32 N31 C35 113.7(7) . 2_655 ?
C32 N31 C35 21.0(11) 2_655 2_655 ?
C35 N31 C35 119.3(18) . 2_655 ?
C32 N31 Ni3 121.8(10) . . ?
C32 N31 Ni3 121.8(10) 2_655 . ?
C35 N31 Ni3 120.4(9) . . ?
C35 N31 Ni3 120.4(9) 2_655 . ?
N31 C32 C33 125.2(16) . . ?
N31 C32 H32 117.4 . . ?
C33 C32 H32 117.4 . . ?
C32 C33 C34 115.9(14) . . ?
C32 C33 H33 122.1 . . ?
C34 C33 H33 122.1 . . ?
C36 C34 C36 120.5(15) . 2_655 ?
C36 C34 C33 24.6(9) . . ?
C36 C34 C33 115.0(8) 2_655 . ?
C36 C34 C33 115.0(8) . 2_655 ?
C36 C34 C33 24.6(9) 2_655 2_655 ?
C33 C34 C33 121.2(16) . 2_655 ?
C36 C34 H34 119.7 . . ?
C36 C34 H34 119.7 2_655 . ?
C33 C34 H34 119.4 . . ?
C33 C34 H34 119.4 2_655 . ?
N31 C35 C36 122.0(15) . . ?
N31 C35 H35 119.0 . . ?
C36 C35 H35 119.0 . . ?
C34 C36 C35 118.0(13) . . ?
C34 C36 H36 121.0 . . ?
C35 C36 H36 121.0 . . ?
C42 N37 C38 116.1(10) . . ?
C39 C38 N37 114.6(10) . . ?
C39 C38 H38 122.7 . . ?
N37 C38 H38 122.7 . . ?
C40 C39 C38 120.9(11) . . ?
C40 C39 H39 119.5 . . ?
C38 C39 H39 119.5 . . ?
C39 C40 C41 123.2(12) . . ?
C39 C40 H40 118.4 . . ?
C41 C40 H40 118.4 . . ?
C42 C41 C40 116.0(12) . . ?
C42 C41 H41 122.0 . . ?
C40 C41 H41 122.0 . . ?
N37 C42 C41 128.9(12) . . ?
N37 C42 H42 115.5 . . ?
C41 C42 H42 115.5 . . ?
C44 N43 C44 119.3(8) 14 . ?
N43 C44 C45 119.2(6) . . ?
N43 C44 H44 120.4 . . ?
C45 C44 H44 120.4 . . ?
C46 C45 C44 121.1(6) . . ?
C46 C45 H45 119.5 . . ?
C44 C45 H45 119.5 . . ?
C45 C46 C45 120.2(9) 14 . ?
C45 C46 H46 119.9 14 . ?
C45 C46 H46 119.9 . . ?
C52 N47 C48 118.8(19) . . ?
C49 C48 N47 120.1(19) . . ?
C49 C48 H48 119.9 . . ?
N47 C48 H48 119.9 . . ?
C48 C49 C50 119(2) . . ?
C48 C49 H49 120.5 . . ?
C50 C49 H49 120.5 . . ?
C51 C50 C49 122(2) . . ?
C51 C50 H50 118.8 . . ?
C49 C50 H50 118.8 . . ?
C50 C51 C52 117(2) . . ?
C50 C51 H51 121.6 . . ?
C52 C51 H51 121.6 . . ?
N47 C52 C51 123(2) . . ?
N47 C52 H52 118.6 . . ?
C51 C52 H52 118.6 . . ?
C54 N53 Ni3 138(3) . . ?
N53 C54 C55 171.8(16) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.98
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.103