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

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#
#                 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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#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
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data_cmd207e4
_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Ni5(1)-MeOH '
_chemical_name_common            Ni5-MeOH
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H64 Cl2 N8 Ni5 O22'
_chemical_formula_weight         1397.46
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
_space_group_name_Hall           '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.191(2)
_cell_length_b                   12.389(3)
_cell_length_c                   12.401(3)
_cell_angle_alpha                70.12(3)
_cell_angle_beta                 63.48(3)
_cell_angle_gamma                64.17(3)
_cell_volume                     1362.0(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    150.1(2)
_cell_measurement_reflns_used    7266
_cell_measurement_theta_min      3.2841
_cell_measurement_theta_max      25.35
_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             722
_exptl_absorpt_coefficient_mu    1.880
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85835
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            10303
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         25.35
_diffrn_orient_matrix_UB_11      -0.0195679000
_diffrn_orient_matrix_UB_12      -0.0524981000
_diffrn_orient_matrix_UB_21      -0.0659540000
_diffrn_orient_matrix_UB_22      0.0301805000
_diffrn_orient_matrix_UB_23      -0.0101055000
_diffrn_orient_matrix_UB_31      0.0329522000
_diffrn_orient_matrix_UB_32      -0.0236038000
_diffrn_orient_matrix_UB_33      -0.0545760000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -64.00   14.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4216  -77.0000  -60.0000 78
  
#__ type_ start__ end____ width___ exp.time_
  2 omega  -67.00    1.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.4216  -37.0000  -60.0000 68
  
#__ type_ start__ end____ width___ exp.time_
  3 omega  -47.00  -18.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028  -77.0000  -30.0000 29
  
#__ type_ start__ end____ width___ exp.time_
  4 omega   -3.00   87.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028   77.0000 -150.0000 90
  
#__ type_ start__ end____ width___ exp.time_
  5 omega  -45.00   51.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028  -77.0000   90.0000 96
  
;
_diffrn_measurement_method       'ω scans'
_diffrn_ambient_temperature      150.1(1)
_reflns_number_total             4974
_reflns_number_gt                4541
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    SHELXS97
_computing_structure_refinement  'SHELXL-97/2 (Sheldrick,1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_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)+(0.0300P)²+3.1746P] where P=(Fo²+2Fc²)/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         4974
_refine_ls_number_parameters     366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.5000 0.5000 0.01136(11) Uani 1 2 d S . .
Ni2 Ni 0.04498(3) 0.75095(3) 0.44792(3) 0.01149(9) Uani 1 1 d . . .
Ni3 Ni 0.17863(3) 0.48160(3) 0.21033(3) 0.01083(9) Uani 1 1 d . . .
Cl1 Cl 0.55100(7) 0.32205(7) 0.32835(6) 0.02221(16) Uani 1 1 d . . .
O1 O 0.09345(19) 0.33994(16) 0.44408(15) 0.0126(4) Uani 1 1 d . . .
O2 O -0.0139(2) 0.22871(17) 0.38761(16) 0.0154(4) Uani 1 1 d . . .
O3 O 0.06394(19) 0.57735(16) 0.32708(15) 0.0130(4) Uani 1 1 d . . .
O4 O 0.2459(2) 0.61281(16) 0.12274(16) 0.0142(4) Uani 1 1 d . . .
O5 O 0.1920(2) 0.49886(18) 0.50187(17) 0.0190(4) Uani 1 1 d . . .
H5H H 0.2496 0.5362 0.4290 0.023 Uiso 1 1 calc R . .
O6 O -0.1027(2) 0.91377(17) 0.41171(17) 0.0191(4) Uani 1 1 d . . .
H6H H -0.1614 0.9597 0.4758 0.023 Uiso 1 1 calc R . .
O7 O 0.5712(5) 0.2304(3) 0.4314(3) 0.0769(12) Uani 1 1 d . . .
O8 O 0.6442(2) 0.2732(2) 0.2195(2) 0.0332(5) Uani 1 1 d . . .
O9 O 0.5750(3) 0.4226(3) 0.3321(3) 0.0569(8) Uani 1 1 d . . .
O10 O 0.4085(3) 0.3552(4) 0.3358(3) 0.0783(13) Uani 1 1 d . . .
O11 O 0.3422(2) 0.1109(2) 0.4180(2) 0.0358(6) Uani 1 1 d . . .
H11 H 0.3458 0.1783 0.4147 0.043 Uiso 1 1 calc R . .
N1 N 0.1105(2) 0.35796(19) 0.32037(18) 0.0121(4) Uani 1 1 d . . .
N2 N 0.2769(2) 0.3830(2) 0.08225(19) 0.0139(5) Uani 1 1 d . . .
N3 N 0.1019(2) 0.68049(19) 0.30267(19) 0.0127(4) Uani 1 1 d . . .
N4 N 0.2215(2) 0.8148(2) 0.34779(19) 0.0146(5) Uani 1 1 d . . .
C1 C 0.0554(3) 0.2960(2) 0.3007(2) 0.0123(5) Uani 1 1 d . . .
C2 C 0.0698(3) 0.3099(2) 0.1719(2) 0.0126(5) Uani 1 1 d . . .
C3 C -0.0252(3) 0.2782(2) 0.1558(2) 0.0161(5) Uani 1 1 d . . .
H3 H -0.0911 0.2460 0.2254 0.019 Uiso 1 1 calc R . .
C4 C -0.0257(3) 0.2926(3) 0.0401(3) 0.0196(6) Uani 1 1 d . . .
H4 H -0.0915 0.2706 0.0306 0.023 Uiso 1 1 calc R . .
C5 C 0.0702(3) 0.3391(3) -0.0611(2) 0.0203(6) Uani 1 1 d . . .
H5 H 0.0700 0.3497 -0.1406 0.024 Uiso 1 1 calc R . .
C6 C 0.1674(3) 0.3705(2) -0.0476(2) 0.0165(5) Uani 1 1 d . . .
H6 H 0.2327 0.4025 -0.1181 0.020 Uiso 1 1 calc R . .
C7 C 0.1699(3) 0.3557(2) 0.0677(2) 0.0120(5) Uani 1 1 d . . .
C8 C 0.3833(3) 0.2649(3) 0.1178(3) 0.0200(6) Uani 1 1 d . . .
H8A H 0.3340 0.2177 0.1925 0.030 Uiso 1 1 calc R . .
H8B H 0.4516 0.2822 0.1327 0.030 Uiso 1 1 calc R . .
H8C H 0.4334 0.2180 0.0514 0.030 Uiso 1 1 calc R . .
C9 C 0.3601(3) 0.4467(3) -0.0333(2) 0.0215(6) Uani 1 1 d . . .
H9A H 0.4121 0.3943 -0.0952 0.032 Uiso 1 1 calc R . .
H9B H 0.4274 0.4645 -0.0175 0.032 Uiso 1 1 calc R . .
H9C H 0.2954 0.5231 -0.0631 0.032 Uiso 1 1 calc R . .
C10 C 0.1943(3) 0.6919(2) 0.1935(2) 0.0123(5) Uani 1 1 d . . .
C11 C 0.2337(3) 0.8037(2) 0.1455(2) 0.0133(5) Uani 1 1 d . . .
C12 C 0.2531(3) 0.8540(3) 0.0224(2) 0.0170(6) Uani 1 1 d . . .
H12 H 0.2515 0.8111 -0.0273 0.020 Uiso 1 1 calc R . .
C13 C 0.2746(3) 0.9654(3) -0.0291(3) 0.0207(6) Uani 1 1 d . . .
H13 H 0.2852 0.9994 -0.1127 0.025 Uiso 1 1 calc R . .
C14 C 0.2804(3) 1.0262(3) 0.0421(3) 0.0235(6) Uani 1 1 d . . .
H14 H 0.2958 1.1023 0.0075 0.028 Uiso 1 1 calc R . .
C15 C 0.2640(3) 0.9764(3) 0.1643(3) 0.0201(6) Uani 1 1 d . . .
H15 H 0.2696 1.0187 0.2121 0.024 Uiso 1 1 calc R . .
C16 C 0.2395(3) 0.8661(2) 0.2185(2) 0.0139(5) Uani 1 1 d . . .
C17 C 0.2000(3) 0.9044(3) 0.4155(3) 0.0217(6) Uani 1 1 d . . .
H17A H 0.2853 0.9269 0.3819 0.033 Uiso 1 1 calc R . .
H17B H 0.1817 0.8679 0.5025 0.033 Uiso 1 1 calc R . .
H17C H 0.1188 0.9774 0.4068 0.033 Uiso 1 1 calc R . .
C18 C 0.3505(3) 0.7084(3) 0.3564(3) 0.0208(6) Uani 1 1 d . . .
H18A H 0.3651 0.6473 0.3141 0.031 Uiso 1 1 calc R . .
H18B H 0.3380 0.6726 0.4428 0.031 Uiso 1 1 calc R . .
H18C H 0.4331 0.7353 0.3181 0.031 Uiso 1 1 calc R . .
C19 C -0.1248(4) 0.9642(3) 0.2971(3) 0.0357(8) Uani 1 1 d . . .
H19A H -0.1396 0.9045 0.2732 0.054 Uiso 1 1 calc R . .
H19B H -0.0414 0.9841 0.2343 0.054 Uiso 1 1 calc R . .
H19C H -0.2085 1.0383 0.3053 0.054 Uiso 1 1 calc R . .
C20 C 0.2404(3) 0.4463(3) 0.6042(3) 0.0273(7) Uani 1 1 d . . .
H20A H 0.1718 0.4892 0.6726 0.041 Uiso 1 1 calc R . .
H20B H 0.3328 0.4541 0.5801 0.041 Uiso 1 1 calc R . .
H20C H 0.2494 0.3599 0.6295 0.041 Uiso 1 1 calc R . .
C21 C 0.4798(4) 0.0336(3) 0.3601(3) 0.0362(8) Uani 1 1 d . . .
H21A H 0.5505 0.0613 0.3583 0.054 Uiso 1 1 calc R . .
H21B H 0.4918 0.0361 0.2761 0.054 Uiso 1 1 calc R . .
H21C H 0.4924 -0.0501 0.4058 0.054 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
Ni1 O3 1.9643(18) 2_566 ?
Ni1 O3 1.9643(18) . ?
Ni1 O1 1.9969(19) . ?
Ni1 O1 1.9969(19) 2_566 ?
Ni1 O5 2.1527(19) . ?
Ni1 O5 2.1528(19) 2_566 ?
Ni2 N3 1.993(2) . ?
Ni2 O2 1.9960(18) 2_566 ?
Ni2 O1 2.0256(19) 2_566 ?
Ni2 O6 2.036(2) . ?
Ni2 N4 2.139(2) . ?
Ni3 O3 1.8255(19) . ?
Ni3 N1 1.859(2) . ?
Ni3 O4 1.8775(19) . ?
Ni3 N2 1.953(2) . ?
Cl1 O9 1.403(3) . ?
Cl1 O7 1.422(3) . ?
Cl1 O8 1.423(2) . ?
Cl1 O10 1.430(3) . ?
O1 N1 1.408(3) . ?
O1 Ni2 2.0256(19) 2_566 ?
O2 C1 1.290(3) . ?
O2 Ni2 1.9961(18) 2_566 ?
O3 N3 1.414(3) . ?
O4 C10 1.305(3) . ?
O5 C20 1.439(3) . ?
O5 H5H 0.9500 . ?
O6 C19 1.430(4) . ?
O6 H6H 0.9500 . ?
O11 C21 1.414(4) . ?
O11 H11 0.8400 . ?
N1 C1 1.306(3) . ?
N2 C7 1.474(3) . ?
N2 C9 1.490(3) . ?
N2 C8 1.505(4) . ?
N3 C10 1.292(3) . ?
N4 C16 1.464(3) . ?
N4 C18 1.488(4) . ?
N4 C17 1.488(3) . ?
C1 C2 1.488(3) . ?
C2 C3 1.390(4) . ?
C2 C7 1.417(4) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.390(4) . ?
C6 H6 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.485(4) . ?
C11 C12 1.393(4) . ?
C11 C16 1.412(4) . ?
C12 C13 1.386(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.388(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(4) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 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
O3 Ni1 O3 180.0 2_566 . ?
O3 Ni1 O1 92.20(8) 2_566 . ?
O3 Ni1 O1 87.80(8) . . ?
O3 Ni1 O1 87.80(8) 2_566 2_566 ?
O3 Ni1 O1 92.20(8) . 2_566 ?
O1 Ni1 O1 179.999(2) . 2_566 ?
O3 Ni1 O5 94.54(8) 2_566 . ?
O3 Ni1 O5 85.46(8) . . ?
O1 Ni1 O5 93.61(8) . . ?
O1 Ni1 O5 86.39(8) 2_566 . ?
O3 Ni1 O5 85.46(8) 2_566 2_566 ?
O3 Ni1 O5 94.54(8) . 2_566 ?
O1 Ni1 O5 86.39(8) . 2_566 ?
O1 Ni1 O5 93.61(8) 2_566 2_566 ?
O5 Ni1 O5 180.0 . 2_566 ?
N3 Ni2 O2 163.43(8) . 2_566 ?
N3 Ni2 O1 93.13(8) . 2_566 ?
O2 Ni2 O1 80.00(7) 2_566 2_566 ?
N3 Ni2 O6 100.18(9) . . ?
O2 Ni2 O6 95.58(9) 2_566 . ?
O1 Ni2 O6 96.26(8) 2_566 . ?
N3 Ni2 N4 87.13(9) . . ?
O2 Ni2 N4 96.56(8) 2_566 . ?
O1 Ni2 N4 168.26(8) 2_566 . ?
O6 Ni2 N4 95.24(9) . . ?
O3 Ni3 N1 87.96(9) . . ?
O3 Ni3 O4 84.29(8) . . ?
N1 Ni3 O4 170.25(8) . . ?
O3 Ni3 N2 171.93(9) . . ?
N1 Ni3 N2 89.88(9) . . ?
O4 Ni3 N2 98.59(9) . . ?
O9 Cl1 O7 108.2(2) . . ?
O9 Cl1 O8 112.46(16) . . ?
O7 Cl1 O8 109.04(19) . . ?
O9 Cl1 O10 110.6(2) . . ?
O7 Cl1 O10 108.3(3) . . ?
O8 Cl1 O10 108.16(15) . . ?
N1 O1 Ni1 110.05(14) . . ?
N1 O1 Ni2 110.15(14) . 2_566 ?
Ni1 O1 Ni2 103.98(8) . 2_566 ?
C1 O2 Ni2 111.41(16) . 2_566 ?
N3 O3 Ni3 112.61(14) . . ?
N3 O3 Ni1 116.04(14) . . ?
Ni3 O3 Ni1 119.29(10) . . ?
C10 O4 Ni3 109.46(16) . . ?
C20 O5 Ni1 125.54(17) . . ?
C20 O5 H5H 117.2 . . ?
Ni1 O5 H5H 117.2 . . ?
C19 O6 Ni2 124.93(18) . . ?
C19 O6 H6H 117.5 . . ?
Ni2 O6 H6H 117.5 . . ?
C21 O11 H11 109.5 . . ?
C1 N1 O1 113.9(2) . . ?
C1 N1 Ni3 126.91(18) . . ?
O1 N1 Ni3 118.32(15) . . ?
C7 N2 C9 113.2(2) . . ?
C7 N2 C8 108.8(2) . . ?
C9 N2 C8 105.8(2) . . ?
C7 N2 Ni3 107.77(16) . . ?
C9 N2 Ni3 110.61(17) . . ?
C8 N2 Ni3 110.73(16) . . ?
C10 N3 O3 110.3(2) . . ?
C10 N3 Ni2 131.84(18) . . ?
O3 N3 Ni2 115.81(14) . . ?
C16 N4 C18 109.2(2) . . ?
C16 N4 C17 112.5(2) . . ?
C18 N4 C17 108.2(2) . . ?
C16 N4 Ni2 114.14(17) . . ?
C18 N4 Ni2 106.74(16) . . ?
C17 N4 Ni2 105.73(16) . . ?
O2 C1 N1 122.9(2) . . ?
O2 C1 C2 120.0(2) . . ?
N1 C1 C2 117.1(2) . . ?
C3 C2 C7 119.2(2) . . ?
C3 C2 C1 116.4(2) . . ?
C7 C2 C1 124.4(2) . . ?
C4 C3 C2 121.4(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C7 C6 C5 120.8(3) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C6 C7 C2 118.8(2) . . ?
C6 C7 N2 121.1(2) . . ?
C2 C7 N2 120.0(2) . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 O4 122.0(2) . . ?
N3 C10 C11 118.0(2) . . ?
O4 C10 C11 119.8(2) . . ?
C12 C11 C16 119.3(2) . . ?
C12 C11 C10 116.2(2) . . ?
C16 C11 C10 124.2(2) . . ?
C13 C12 C11 121.3(3) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C14 C13 C12 119.4(3) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 120.1(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C16 121.6(3) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C15 C16 C11 118.3(2) . . ?
C15 C16 N4 121.0(2) . . ?
C11 C16 N4 120.6(2) . . ?
N4 C17 H17A 109.5 . . ?
N4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O6 C19 H19A 109.5 . . ?
O6 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O6 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O5 C20 H20A 109.5 . . ?
O5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O11 C21 H21A 109.5 . . ?
O11 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O11 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.078
_chemical_properties_physical    Hygroscopic
_exptl_crystal_preparation       'Magnetic properties'
_database_code_depnum_ccdc_archive 'CCDC 1009473'
#######################################################################
#
#                 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_cmd211e2
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Ni5(L)4(py)5](ClO4)2.1H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C61 H67 Cl2 N13 Ni5 O17'
_chemical_formula_weight         1618.71
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/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                   14.6573(4)
_cell_length_b                   15.1811(4)
_cell_length_c                   29.7812(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.552(3)
_cell_angle_gamma                90.00
_cell_volume                     6614.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9811
_cell_measurement_theta_min      2.9030
_cell_measurement_theta_max      25.35
_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3328
_exptl_absorpt_coefficient_mu    1.558
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95873
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            52717
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.9030
_diffrn_reflns_theta_max         25.35
_diffrn_orient_matrix_UB_11      0.0209052000
_diffrn_orient_matrix_UB_12      0.0111263000
_diffrn_orient_matrix_UB_21      0.0388913000
_diffrn_orient_matrix_UB_22      0.0158982000
_diffrn_orient_matrix_UB_23      0.0128757000
_diffrn_orient_matrix_UB_31      0.0200309000
_diffrn_orient_matrix_UB_32      -0.0424910000
_diffrn_orient_matrix_UB_33      -0.0004406000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -77.00   54.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653    0.0000 -180.0000 131
  
#__ type_ start__ end____ width___ exp.time_
  2 omega  -48.00   10.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653  -37.0000  -60.0000 58
  
#__ type_ start__ end____ width___ exp.time_
  3 omega  -67.00  -41.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.2653  -37.0000   30.0000 26
  
#__ type_ start__ end____ width___ exp.time_
  4 omega   30.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028 -137.0000    0.0000 57
  
#__ type_ start__ end____ width___ exp.time_
  5 omega   30.00   88.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028 -137.0000 -179.0000 58
  
#__ type_ start__ end____ width___ exp.time_
  6 omega   34.00   88.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7028  179.0000  -60.0000 54
  
;
_diffrn_measurement_method       'ω scans'
_diffrn_ambient_temperature      150(2)
_reflns_number_total             12096
_reflns_number_gt                8299
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_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)+(0.0422P)²+0.0000P] where P=(Fo²+2Fc²)/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         12096
_refine_ls_number_parameters     886
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1139
_refine_ls_wR_factor_gt          0.0993
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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 0.44145(4) 0.63110(3) 0.12387(2) 0.01520(15) Uani 1 1 d . . .
Ni2 Ni 0.60998(4) 0.49778(3) 0.09678(2) 0.01329(14) Uani 1 1 d . . .
Ni3 Ni 0.29320(4) 0.46180(3) 0.10603(2) 0.01931(16) Uani 1 1 d . . .
Ni4 Ni 0.26460(4) 0.76382(3) 0.09618(2) 0.01718(15) Uani 1 1 d . . .
Ni5 Ni 0.57735(4) 0.80711(3) 0.12519(2) 0.01459(14) Uani 1 1 d . . .
Cl1 Cl 0.06419(9) 0.84634(9) -0.07300(5) 0.0398(4) Uani 1 1 d . . .
Cl2 Cl 0.51094(11) 1.15609(9) 0.24509(6) 0.0471(4) Uani 1 1 d . . .
N1 N 0.6417(2) 0.3917(2) 0.05383(13) 0.0149(9) Uani 1 1 d . . .
N2 N 0.4848(2) 0.4501(2) 0.09639(13) 0.0166(9) Uani 1 1 d . . .
N3 N 0.6696(2) 0.4511(2) 0.15534(13) 0.0179(9) Uani 1 1 d . . .
N4 N 0.1646(2) 0.4263(2) 0.07492(15) 0.0209(10) Uani 1 1 d . . .
N5 N 0.2471(2) 0.5870(2) 0.10595(15) 0.0219(10) Uani 1 1 d . . .
N6 N 0.2664(3) 0.4257(2) 0.16974(15) 0.0233(10) Uani 1 1 d . . .
N7 N 0.2177(2) 0.8776(2) 0.07337(14) 0.0203(9) Uani 1 1 d . . .
N8 N 0.3806(2) 0.8108(2) 0.10853(14) 0.0177(9) Uani 1 1 d . . .
N9 N 0.6088(3) 0.8309(2) 0.05205(14) 0.0215(9) Uani 1 1 d . . .
N10 N 0.5657(2) 0.7842(2) 0.19535(13) 0.0186(9) Uani 1 1 d . . .
N11 N 0.6968(2) 0.8763(2) 0.14433(13) 0.0180(9) Uani 1 1 d . . .
N12 N 0.6276(2) 0.6837(2) 0.11135(13) 0.0158(9) Uani 1 1 d . . .
N13 N 0.4281(2) 0.6017(2) 0.18902(14) 0.0197(9) Uani 1 1 d . . .
O1 O 0.3643(2) 0.35542(17) 0.08775(12) 0.0217(8) Uani 1 1 d . . .
O2 O 0.41443(19) 0.51132(16) 0.10231(11) 0.0175(7) Uani 1 1 d . . .
O3 O 0.1532(2) 0.70327(17) 0.09155(12) 0.0226(8) Uani 1 1 d . . .
O4 O 0.3119(2) 0.65498(17) 0.10693(13) 0.0263(9) Uani 1 1 d . . .
O5 O 0.4908(2) 0.91326(17) 0.12660(11) 0.0194(8) Uani 1 1 d . . .
O6 O 0.45563(19) 0.75351(16) 0.10688(11) 0.0189(8) Uani 1 1 d . . .
O7 O 0.6954(2) 0.57905(17) 0.06907(11) 0.0188(7) Uani 1 1 d . . .
O8 O 0.57482(19) 0.61133(16) 0.12500(11) 0.0146(7) Uani 1 1 d . . .
O9 O 0.0702(4) 0.7712(3) -0.04401(19) 0.097(2) Uani 1 1 d . . .
O10 O 0.1472(4) 0.8791(5) -0.0762(3) 0.192(4) Uani 1 1 d . . .
O11 O 0.0210(5) 0.9134(4) -0.0487(2) 0.146(3) Uani 1 1 d . . .
O12 O 0.0071(4) 0.8371(4) -0.1113(2) 0.120(2) Uani 1 1 d . . .
O13 O 0.5330(4) 1.0723(3) 0.2285(2) 0.130(3) Uani 1 1 d . . .
O14 O 0.4272(3) 1.1451(3) 0.26716(19) 0.0858(17) Uani 1 1 d . . .
O15 O 0.4936(3) 1.2181(3) 0.21007(16) 0.0682(14) Uani 1 1 d . . .
O16 O 0.5828(3) 1.1848(3) 0.27586(15) 0.0653(14) Uani 1 1 d . . .
O17 O 0.0922(9) 0.8004(8) 0.1716(5) 0.313(6) Uiso 1 1 d . . .
C1 C 0.7425(3) 0.3911(3) 0.05154(18) 0.0221(12) Uani 1 1 d . . .
H1A H 0.7711 0.3720 0.0805 0.033 Uiso 1 1 calc R . .
H1B H 0.7637 0.4505 0.0446 0.033 Uiso 1 1 calc R . .
H1C H 0.7594 0.3503 0.0279 0.033 Uiso 1 1 calc R . .
C2 C 0.6009(3) 0.4153(3) 0.00846(16) 0.0212(11) Uani 1 1 d . . .
H2A H 0.6179 0.3710 -0.0134 0.032 Uiso 1 1 calc R . .
H2B H 0.6236 0.4732 -0.0003 0.032 Uiso 1 1 calc R . .
H2C H 0.5342 0.4174 0.0092 0.032 Uiso 1 1 calc R . .
C3 C 0.6056(3) 0.3066(2) 0.06806(15) 0.0140(10) Uani 1 1 d . . .
C4 C 0.6601(3) 0.2319(3) 0.06658(16) 0.0202(11) Uani 1 1 d . . .
H4 H 0.7206 0.2370 0.0570 0.024 Uiso 1 1 calc R . .
C5 C 0.6279(3) 0.1503(3) 0.07877(17) 0.0232(12) Uani 1 1 d . . .
H5 H 0.6666 0.1002 0.0779 0.028 Uiso 1 1 calc R . .
C6 C 0.5407(3) 0.1408(3) 0.09203(17) 0.0213(11) Uani 1 1 d . . .
H6 H 0.5183 0.0844 0.0998 0.026 Uiso 1 1 calc R . .
C7 C 0.4860(3) 0.2142(3) 0.09400(16) 0.0181(11) Uani 1 1 d . . .
H7 H 0.4256 0.2076 0.1035 0.022 Uiso 1 1 calc R . .
C8 C 0.5165(3) 0.2985(2) 0.08246(15) 0.0142(10) Uani 1 1 d . . .
C9 C 0.4503(3) 0.3720(3) 0.08845(16) 0.0153(10) Uani 1 1 d . . .
C10 C 0.1593(3) 0.3275(3) 0.0755(2) 0.0358(15) Uani 1 1 d . . .
H10A H 0.1548 0.3071 0.1065 0.054 Uiso 1 1 calc R . .
H10B H 0.2144 0.3028 0.0634 0.054 Uiso 1 1 calc R . .
H10C H 0.1054 0.3081 0.0571 0.054 Uiso 1 1 calc R . .
C11 C 0.1665(4) 0.4545(3) 0.02717(18) 0.0324(13) Uani 1 1 d . . .
H11A H 0.1085 0.4390 0.0110 0.049 Uiso 1 1 calc R . .
H11B H 0.2169 0.4248 0.0132 0.049 Uiso 1 1 calc R . .
H11C H 0.1755 0.5184 0.0259 0.049 Uiso 1 1 calc R . .
C12 C 0.0876(3) 0.4676(3) 0.09559(17) 0.0183(11) Uani 1 1 d . . .
C13 C 0.0126(3) 0.4188(3) 0.10735(17) 0.0236(12) Uani 1 1 d . . .
H13 H 0.0111 0.3572 0.1018 0.028 Uiso 1 1 calc R . .
C14 C -0.0596(3) 0.4580(3) 0.12683(18) 0.0263(12) Uani 1 1 d . . .
H14 H -0.1092 0.4228 0.1354 0.032 Uiso 1 1 calc R . .
C15 C -0.0610(3) 0.5471(3) 0.13404(19) 0.0305(13) Uani 1 1 d . . .
H15 H -0.1108 0.5739 0.1478 0.037 Uiso 1 1 calc R . .
C16 C 0.0115(3) 0.5977(3) 0.12089(18) 0.0259(12) Uani 1 1 d . . .
H16 H 0.0096 0.6599 0.1244 0.031 Uiso 1 1 calc R . .
C17 C 0.0864(3) 0.5596(3) 0.10275(17) 0.0187(11) Uani 1 1 d . . .
C18 C 0.1657(3) 0.6194(3) 0.09859(16) 0.0179(11) Uani 1 1 d . . .
C19 C 0.2576(4) 0.8868(3) 0.02823(18) 0.0346(14) Uani 1 1 d . . .
H19A H 0.2302 0.9378 0.0124 0.052 Uiso 1 1 calc R . .
H19B H 0.2446 0.8334 0.0104 0.052 Uiso 1 1 calc R . .
H19C H 0.3239 0.8950 0.0325 0.052 Uiso 1 1 calc R . .
C20 C 0.1170(3) 0.8738(3) 0.0635(2) 0.0431(16) Uani 1 1 d . . .
H20A H 0.0863 0.8721 0.0918 0.065 Uiso 1 1 calc R . .
H20B H 0.1014 0.8208 0.0459 0.065 Uiso 1 1 calc R . .
H20C H 0.0970 0.9261 0.0462 0.065 Uiso 1 1 calc R . .
C21 C 0.2459(3) 0.9545(3) 0.10127(17) 0.0193(11) Uani 1 1 d . . .
C22 C 0.1866(3) 1.0251(3) 0.10508(17) 0.0236(12) Uani 1 1 d . . .
H22 H 0.1271 1.0225 0.0906 0.028 Uiso 1 1 calc R . .
C23 C 0.2132(3) 1.0995(3) 0.12975(18) 0.0246(12) Uani 1 1 d . . .
H23 H 0.1719 1.1472 0.1320 0.030 Uiso 1 1 calc R . .
C24 C 0.2990(3) 1.1042(3) 0.15089(18) 0.0230(12) Uani 1 1 d . . .
H24 H 0.3169 1.1545 0.1682 0.028 Uiso 1 1 calc R . .
C25 C 0.3595(3) 1.0344(2) 0.14659(16) 0.0178(11) Uani 1 1 d . . .
H25 H 0.4190 1.0379 0.1611 0.021 Uiso 1 1 calc R . .
C26 C 0.3351(3) 0.9600(3) 0.12166(16) 0.0161(10) Uani 1 1 d . . .
C27 C 0.4077(3) 0.8917(3) 0.11824(16) 0.0161(10) Uani 1 1 d . . .
C28 C 0.5825(4) 0.9214(3) 0.03880(18) 0.0300(13) Uani 1 1 d . . .
H28A H 0.6180 0.9635 0.0577 0.045 Uiso 1 1 calc R . .
H28B H 0.5172 0.9300 0.0426 0.045 Uiso 1 1 calc R . .
H28C H 0.5949 0.9309 0.0072 0.045 Uiso 1 1 calc R . .
C29 C 0.5540(3) 0.7711(3) 0.02171(17) 0.0289(12) Uani 1 1 d . . .
H29A H 0.5682 0.7822 -0.0095 0.043 Uiso 1 1 calc R . .
H29B H 0.4888 0.7817 0.0250 0.043 Uiso 1 1 calc R . .
H29C H 0.5687 0.7098 0.0296 0.043 Uiso 1 1 calc R . .
C30 C 0.7052(3) 0.8127(3) 0.04854(16) 0.0191(11) Uani 1 1 d . . .
C31 C 0.7658(4) 0.8745(3) 0.03308(19) 0.0336(14) Uani 1 1 d . . .
H31 H 0.7438 0.9315 0.0250 0.040 Uiso 1 1 calc R . .
C32 C 0.8570(4) 0.8553(3) 0.0292(2) 0.0413(16) Uani 1 1 d . . .
H32 H 0.8968 0.8994 0.0191 0.050 Uiso 1 1 calc R . .
C33 C 0.8908(4) 0.7726(3) 0.0399(2) 0.0352(14) Uani 1 1 d . . .
H33 H 0.9531 0.7583 0.0364 0.042 Uiso 1 1 calc R . .
C34 C 0.8313(3) 0.7111(3) 0.05594(17) 0.0238(12) Uani 1 1 d . . .
H34 H 0.8540 0.6541 0.0635 0.029 Uiso 1 1 calc R . .
C35 C 0.7401(3) 0.7291(3) 0.06151(16) 0.0169(10) Uani 1 1 d . . .
C36 C 0.6843(3) 0.6597(3) 0.08164(15) 0.0149(10) Uani 1 1 d . . .
C37 C 0.7281(3) 0.5053(3) 0.17730(16) 0.0182(11) Uani 1 1 d . . .
H37 H 0.7406 0.5604 0.1639 0.022 Uiso 1 1 calc R . .
C38 C 0.7715(3) 0.4858(3) 0.21849(18) 0.0253(12) Uani 1 1 d . . .
H38 H 0.8136 0.5258 0.2329 0.030 Uiso 1 1 calc R . .
C39 C 0.7516(3) 0.4061(3) 0.23799(18) 0.0291(13) Uani 1 1 d . . .
H39 H 0.7808 0.3901 0.2662 0.035 Uiso 1 1 calc R . .
C40 C 0.6897(3) 0.3500(3) 0.21669(17) 0.0269(12) Uani 1 1 d . . .
H40 H 0.6741 0.2960 0.2303 0.032 Uiso 1 1 calc R . .
C41 C 0.6504(3) 0.3734(3) 0.17519(17) 0.0221(11) Uani 1 1 d . . .
H41 H 0.6087 0.3339 0.1600 0.027 Uiso 1 1 calc R . .
C42 C 0.3047(3) 0.3528(3) 0.1882(2) 0.0309(13) Uani 1 1 d . . .
H42 H 0.3427 0.3179 0.1706 0.037 Uiso 1 1 calc R . .
C43 C 0.2915(4) 0.3262(3) 0.2316(2) 0.0378(15) Uani 1 1 d . . .
H43 H 0.3193 0.2737 0.2432 0.045 Uiso 1 1 calc R . .
C44 C 0.2373(4) 0.3767(3) 0.2580(2) 0.0364(14) Uani 1 1 d . . .
H44 H 0.2276 0.3601 0.2881 0.044 Uiso 1 1 calc R . .
C45 C 0.1978(4) 0.4517(3) 0.23947(19) 0.0332(14) Uani 1 1 d . . .
H45 H 0.1599 0.4877 0.2566 0.040 Uiso 1 1 calc R . .
C46 C 0.2138(3) 0.4740(3) 0.19605(19) 0.0262(12) Uani 1 1 d . . .
H46 H 0.1864 0.5262 0.1838 0.031 Uiso 1 1 calc R . .
C47 C 0.4668(3) 0.5277(3) 0.20592(18) 0.0263(12) Uani 1 1 d . . .
H47 H 0.5008 0.4922 0.1867 0.032 Uiso 1 1 calc R . .
C48 C 0.4596(4) 0.5007(3) 0.24943(19) 0.0323(13) Uani 1 1 d . . .
H48 H 0.4875 0.4474 0.2599 0.039 Uiso 1 1 calc R . .
C49 C 0.4108(4) 0.5529(4) 0.27796(19) 0.0397(15) Uani 1 1 d . . .
H49 H 0.4051 0.5364 0.3084 0.048 Uiso 1 1 calc R . .
C50 C 0.3712(4) 0.6287(3) 0.2610(2) 0.0377(14) Uani 1 1 d . . .
H50 H 0.3376 0.6656 0.2797 0.045 Uiso 1 1 calc R . .
C51 C 0.3803(3) 0.6511(3) 0.21670(18) 0.0280(13) Uani 1 1 d . . .
H51 H 0.3517 0.7033 0.2053 0.034 Uiso 1 1 calc R . .
C52 C 0.5243(3) 0.8422(3) 0.22172(17) 0.0260(12) Uani 1 1 d . . .
H52 H 0.4948 0.8917 0.2077 0.031 Uiso 1 1 calc R . .
C53 C 0.5224(4) 0.8341(3) 0.26744(19) 0.0363(14) Uani 1 1 d . . .
H53 H 0.4922 0.8768 0.2845 0.044 Uiso 1 1 calc R . .
C54 C 0.5651(4) 0.7627(3) 0.28832(19) 0.0360(14) Uani 1 1 d . . .
H54 H 0.5641 0.7548 0.3199 0.043 Uiso 1 1 calc R . .
C55 C 0.6092(4) 0.7032(3) 0.26240(18) 0.0301(13) Uani 1 1 d . . .
H55 H 0.6400 0.6540 0.2760 0.036 Uiso 1 1 calc R . .
C56 C 0.6081(3) 0.7156(3) 0.21611(18) 0.0245(12) Uani 1 1 d . . .
H56 H 0.6386 0.6740 0.1985 0.029 Uiso 1 1 calc R . .
C57 C 0.7787(3) 0.8381(3) 0.15137(17) 0.0276(12) Uani 1 1 d . . .
H57 H 0.7818 0.7756 0.1513 0.033 Uiso 1 1 calc R . .
C58 C 0.8584(3) 0.8848(3) 0.15866(19) 0.0349(14) Uani 1 1 d . . .
H58 H 0.9152 0.8549 0.1631 0.042 Uiso 1 1 calc R . .
C59 C 0.8552(4) 0.9747(4) 0.1594(2) 0.0434(16) Uani 1 1 d . . .
H59 H 0.9096 1.0086 0.1633 0.052 Uiso 1 1 calc R . .
C60 C 0.7706(4) 1.0148(3) 0.15444(19) 0.0367(15) Uani 1 1 d . . .
H60 H 0.7659 1.0771 0.1561 0.044 Uiso 1 1 calc R . .
C61 C 0.6935(3) 0.9644(3) 0.14714(17) 0.0259(12) Uani 1 1 d . . .
H61 H 0.6357 0.9928 0.1440 0.031 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
Ni1 O6 1.941(3) . ?
Ni1 O2 1.961(3) . ?
Ni1 O4 1.968(3) . ?
Ni1 O8 1.976(3) . ?
Ni1 N13 2.012(4) . ?
Ni2 N2 1.972(3) . ?
Ni2 O7 1.975(3) . ?
Ni2 O8 1.999(3) . ?
Ni2 N3 2.029(4) . ?
Ni2 N1 2.126(3) . ?
Ni3 O2 1.939(3) . ?
Ni3 O1 2.015(3) . ?
Ni3 N5 2.017(3) . ?
Ni3 N6 2.036(4) . ?
Ni3 N4 2.118(4) . ?
Ni4 O4 1.813(3) . ?
Ni4 N8 1.859(4) . ?
Ni4 O3 1.872(3) . ?
Ni4 N7 1.964(3) . ?
Ni5 O6 2.005(3) . ?
Ni5 O5 2.053(3) . ?
Ni5 N12 2.064(3) . ?
Ni5 N11 2.091(4) . ?
Ni5 N10 2.136(4) . ?
Ni5 N9 2.283(4) . ?
Cl1 O10 1.323(5) . ?
Cl1 O12 1.379(6) . ?
Cl1 O11 1.421(6) . ?
Cl1 O9 1.430(5) . ?
Cl2 O13 1.410(5) . ?
Cl2 O15 1.416(4) . ?
Cl2 O16 1.422(4) . ?
Cl2 O14 1.437(5) . ?
N1 C3 1.469(5) . ?
N1 C1 1.483(5) . ?
N1 C2 1.488(6) . ?
N2 C9 1.305(5) . ?
N2 O2 1.408(4) . ?
N3 C37 1.330(5) . ?
N3 C41 1.357(5) . ?
N4 C12 1.461(5) . ?
N4 C11 1.487(6) . ?
N4 C10 1.502(5) . ?
N5 C18 1.297(5) . ?
N5 O4 1.402(4) . ?
N6 C42 1.343(6) . ?
N6 C46 1.350(6) . ?
N7 C21 1.477(6) . ?
N7 C20 1.488(6) . ?
N7 C19 1.505(6) . ?
N8 C27 1.318(5) . ?
N8 O6 1.405(4) . ?
N9 C30 1.450(6) . ?
N9 C28 1.474(5) . ?
N9 C29 1.482(6) . ?
N10 C56 1.345(6) . ?
N10 C52 1.348(5) . ?
N11 C57 1.338(6) . ?
N11 C61 1.341(5) . ?
N12 C36 1.303(5) . ?
N12 O8 1.418(4) . ?
N13 C47 1.342(5) . ?
N13 C51 1.343(6) . ?
O1 C9 1.284(5) . ?
O3 C18 1.301(5) . ?
O5 C27 1.271(5) . ?
O7 C36 1.293(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.390(6) . ?
C3 C8 1.404(6) . ?
C4 C5 1.383(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.368(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.406(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.496(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.389(6) . ?
C12 C17 1.414(6) . ?
C13 C14 1.372(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.371(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.487(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.388(6) . ?
C21 C26 1.409(6) . ?
C22 C23 1.390(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.392(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.493(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.390(6) . ?
C30 C35 1.413(6) . ?
C31 C32 1.380(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.380(7) . ?
C32 H32 0.9500 . ?
C33 C34 1.382(6) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.482(6) . ?
C37 C38 1.378(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.381(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.371(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.377(7) . ?
C40 H40 0.9500 . ?
C41 H41 0.9500 . ?
C42 C43 1.379(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.384(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.378(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.371(7) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C48 1.369(7) . ?
C47 H47 0.9500 . ?
C48 C49 1.392(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.371(7) . ?
C49 H49 0.9500 . ?
C50 C51 1.377(7) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.369(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.380(7) . ?
C53 H53 0.9500 . ?
C54 C55 1.374(7) . ?
C54 H54 0.9500 . ?
C55 C56 1.390(7) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C58 1.372(6) . ?
C57 H57 0.9500 . ?
C58 C59 1.366(7) . ?
C58 H58 0.9500 . ?
C59 C60 1.381(7) . ?
C59 H59 0.9500 . ?
C60 C61 1.372(6) . ?
C60 H60 0.9500 . ?
C61 H61 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
O6 Ni1 O2 145.64(14) . . ?
O6 Ni1 O4 82.75(12) . . ?
O2 Ni1 O4 85.12(12) . . ?
O6 Ni1 O8 91.61(11) . . ?
O2 Ni1 O8 92.54(11) . . ?
O4 Ni1 O8 165.97(14) . . ?
O6 Ni1 N13 118.81(14) . . ?
O2 Ni1 N13 94.63(13) . . ?
O4 Ni1 N13 97.94(15) . . ?
O8 Ni1 N13 96.03(14) . . ?
N2 Ni2 O7 147.24(15) . . ?
N2 Ni2 O8 93.17(12) . . ?
O7 Ni2 O8 79.85(11) . . ?
N2 Ni2 N3 103.17(15) . . ?
O7 Ni2 N3 109.08(14) . . ?
O8 Ni2 N3 92.77(13) . . ?
N2 Ni2 N1 87.51(14) . . ?
O7 Ni2 N1 93.07(12) . . ?
O8 Ni2 N1 167.89(13) . . ?
N3 Ni2 N1 98.85(14) . . ?
O2 Ni3 O1 78.70(11) . . ?
O2 Ni3 N5 86.71(12) . . ?
O1 Ni3 N5 159.00(14) . . ?
O2 Ni3 N6 112.82(15) . . ?
O1 Ni3 N6 99.72(14) . . ?
N5 Ni3 N6 99.84(16) . . ?
O2 Ni3 N4 150.18(15) . . ?
O1 Ni3 N4 97.97(13) . . ?
N5 Ni3 N4 87.18(14) . . ?
N6 Ni3 N4 96.98(15) . . ?
O4 Ni4 N8 88.82(13) . . ?
O4 Ni4 O3 83.57(12) . . ?
N8 Ni4 O3 170.39(15) . . ?
O4 Ni4 N7 169.83(17) . . ?
N8 Ni4 N7 91.55(15) . . ?
O3 Ni4 N7 96.98(14) . . ?
O6 Ni5 O5 77.50(11) . . ?
O6 Ni5 N12 84.26(12) . . ?
O5 Ni5 N12 160.95(14) . . ?
O6 Ni5 N11 173.71(12) . . ?
O5 Ni5 N11 96.22(13) . . ?
N12 Ni5 N11 101.95(14) . . ?
O6 Ni5 N10 94.36(13) . . ?
O5 Ni5 N10 91.17(13) . . ?
N12 Ni5 N10 95.68(14) . . ?
N11 Ni5 N10 86.08(14) . . ?
O6 Ni5 N9 91.92(13) . . ?
O5 Ni5 N9 93.25(13) . . ?
N12 Ni5 N9 81.82(13) . . ?
N11 Ni5 N9 88.03(14) . . ?
N10 Ni5 N9 172.98(14) . . ?
O10 Cl1 O12 119.5(5) . . ?
O10 Cl1 O11 102.0(5) . . ?
O12 Cl1 O11 103.1(4) . . ?
O10 Cl1 O9 108.7(4) . . ?
O12 Cl1 O9 115.4(4) . . ?
O11 Cl1 O9 106.0(4) . . ?
O13 Cl2 O15 112.1(4) . . ?
O13 Cl2 O16 109.0(3) . . ?
O15 Cl2 O16 111.3(3) . . ?
O13 Cl2 O14 106.0(4) . . ?
O15 Cl2 O14 107.2(3) . . ?
O16 Cl2 O14 111.1(3) . . ?
C3 N1 C1 112.7(3) . . ?
C3 N1 C2 110.0(3) . . ?
C1 N1 C2 107.8(4) . . ?
C3 N1 Ni2 113.3(3) . . ?
C1 N1 Ni2 106.8(3) . . ?
C2 N1 Ni2 105.8(2) . . ?
C9 N2 O2 110.1(3) . . ?
C9 N2 Ni2 133.3(3) . . ?
O2 N2 Ni2 116.5(2) . . ?
C37 N3 C41 117.9(4) . . ?
C37 N3 Ni2 115.9(3) . . ?
C41 N3 Ni2 126.0(3) . . ?
C12 N4 C11 109.9(4) . . ?
C12 N4 C10 112.5(3) . . ?
C11 N4 C10 107.7(4) . . ?
C12 N4 Ni3 113.3(3) . . ?
C11 N4 Ni3 106.0(3) . . ?
C10 N4 Ni3 107.1(3) . . ?
C18 N5 O4 109.8(3) . . ?
C18 N5 Ni3 131.5(3) . . ?
O4 N5 Ni3 117.9(2) . . ?
C42 N6 C46 116.7(5) . . ?
C42 N6 Ni3 120.3(3) . . ?
C46 N6 Ni3 123.0(3) . . ?
C21 N7 C20 112.4(4) . . ?
C21 N7 C19 108.6(3) . . ?
C20 N7 C19 105.2(4) . . ?
C21 N7 Ni4 114.9(3) . . ?
C20 N7 Ni4 110.8(3) . . ?
C19 N7 Ni4 104.1(3) . . ?
C27 N8 O6 111.0(3) . . ?
C27 N8 Ni4 131.3(3) . . ?
O6 N8 Ni4 117.6(2) . . ?
C30 N9 C28 113.5(3) . . ?
C30 N9 C29 109.4(4) . . ?
C28 N9 C29 106.6(4) . . ?
C30 N9 Ni5 107.1(3) . . ?
C28 N9 Ni5 109.8(3) . . ?
C29 N9 Ni5 110.6(3) . . ?
C56 N10 C52 116.7(4) . . ?
C56 N10 Ni5 120.9(3) . . ?
C52 N10 Ni5 122.0(3) . . ?
C57 N11 C61 117.3(4) . . ?
C57 N11 Ni5 123.6(3) . . ?
C61 N11 Ni5 119.0(3) . . ?
C36 N12 O8 111.1(3) . . ?
C36 N12 Ni5 129.8(3) . . ?
O8 N12 Ni5 116.0(2) . . ?
C47 N13 C51 117.5(4) . . ?
C47 N13 Ni1 118.9(3) . . ?
C51 N13 Ni1 123.6(3) . . ?
C9 O1 Ni3 111.2(2) . . ?
N2 O2 Ni3 115.6(2) . . ?
N2 O2 Ni1 121.2(2) . . ?
Ni3 O2 Ni1 120.54(14) . . ?
C18 O3 Ni4 110.7(3) . . ?
N5 O4 Ni4 114.6(2) . . ?
N5 O4 Ni1 120.8(2) . . ?
Ni4 O4 Ni1 124.46(15) . . ?
C27 O5 Ni5 112.3(2) . . ?
N8 O6 Ni1 119.1(2) . . ?
N8 O6 Ni5 115.1(2) . . ?
Ni1 O6 Ni5 115.18(14) . . ?
C36 O7 Ni2 112.1(3) . . ?
N12 O8 Ni1 115.7(2) . . ?
N12 O8 Ni2 112.8(2) . . ?
Ni1 O8 Ni2 113.85(13) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 119.1(4) . . ?
C4 C3 N1 119.3(4) . . ?
C8 C3 N1 121.6(3) . . ?
C5 C4 C3 121.1(4) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C6 C5 C4 120.7(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 119.0(4) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
C6 C7 C8 122.1(4) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
C3 C8 C7 118.0(4) . . ?
C3 C8 C9 126.4(4) . . ?
C7 C8 C9 115.5(4) . . ?
O1 C9 N2 123.4(4) . . ?
O1 C9 C8 119.7(3) . . ?
N2 C9 C8 116.8(4) . . ?
N4 C10 H10A 109.5 . . ?
N4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C17 118.1(4) . . ?
C13 C12 N4 121.5(4) . . ?
C17 C12 N4 120.4(4) . . ?
C14 C13 C12 121.3(4) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C15 C14 C13 120.9(4) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 118.9(4) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C17 C16 C15 121.4(4) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C12 119.4(4) . . ?
C16 C17 C18 115.0(4) . . ?
C12 C17 C18 125.0(4) . . ?
N5 C18 O3 121.2(4) . . ?
N5 C18 C17 118.1(4) . . ?
O3 C18 C17 120.5(4) . . ?
N7 C19 H19A 109.5 . . ?
N7 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N7 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N7 C20 H20A 109.5 . . ?
N7 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N7 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 119.2(4) . . ?
C22 C21 N7 120.1(4) . . ?
C26 C21 N7 120.5(4) . . ?
C21 C22 C23 120.9(5) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C24 C23 C22 120.3(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.3(4) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C26 C25 C24 121.6(4) . . ?
C26 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
C25 C26 C21 118.7(4) . . ?
C25 C26 C27 116.1(4) . . ?
C21 C26 C27 125.2(4) . . ?
O5 C27 N8 123.7(4) . . ?
O5 C27 C26 119.1(4) . . ?
N8 C27 C26 117.1(4) . . ?
N9 C28 H28A 109.5 . . ?
N9 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N9 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N9 C29 H29A 109.5 . . ?
N9 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N9 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 118.0(4) . . ?
C31 C30 N9 122.7(4) . . ?
C35 C30 N9 119.3(4) . . ?
C32 C31 C30 121.8(5) . . ?
C32 C31 H31 119.1 . . ?
C30 C31 H31 119.1 . . ?
C31 C32 C33 120.6(4) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C32 C33 C34 117.9(5) . . ?
C32 C33 H33 121.0 . . ?
C34 C33 H33 121.0 . . ?
C33 C34 C35 122.9(4) . . ?
C33 C34 H34 118.5 . . ?
C35 C34 H34 118.5 . . ?
C34 C35 C30 118.7(4) . . ?
C34 C35 C36 118.0(4) . . ?
C30 C35 C36 123.4(4) . . ?
O7 C36 N12 123.9(4) . . ?
O7 C36 C35 118.3(4) . . ?
N12 C36 C35 117.8(4) . . ?
N3 C37 C38 123.6(4) . . ?
N3 C37 H37 118.2 . . ?
C38 C37 H37 118.2 . . ?
C37 C38 C39 117.7(5) . . ?
C37 C38 H38 121.2 . . ?
C39 C38 H38 121.2 . . ?
C40 C39 C38 120.0(5) . . ?
C40 C39 H39 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C40 C41 118.9(4) . . ?
C39 C40 H40 120.5 . . ?
C41 C40 H40 120.5 . . ?
N3 C41 C40 121.9(4) . . ?
N3 C41 H41 119.0 . . ?
C40 C41 H41 119.0 . . ?
N6 C42 C43 123.1(5) . . ?
N6 C42 H42 118.5 . . ?
C43 C42 H42 118.5 . . ?
C42 C43 C44 119.3(5) . . ?
C42 C43 H43 120.4 . . ?
C44 C43 H43 120.4 . . ?
C45 C44 C43 118.1(5) . . ?
C45 C44 H44 120.9 . . ?
C43 C44 H44 120.9 . . ?
C46 C45 C44 119.4(5) . . ?
C46 C45 H45 120.3 . . ?
C44 C45 H45 120.3 . . ?
N6 C46 C45 123.4(5) . . ?
N6 C46 H46 118.3 . . ?
C45 C46 H46 118.3 . . ?
N13 C47 C48 123.4(5) . . ?
N13 C47 H47 118.3 . . ?
C48 C47 H47 118.3 . . ?
C47 C48 C49 118.6(5) . . ?
C47 C48 H48 120.7 . . ?
C49 C48 H48 120.7 . . ?
C50 C49 C48 118.4(5) . . ?
C50 C49 H49 120.8 . . ?
C48 C49 H49 120.8 . . ?
C49 C50 C51 119.8(5) . . ?
C49 C50 H50 120.1 . . ?
C51 C50 H50 120.1 . . ?
N13 C51 C50 122.4(5) . . ?
N13 C51 H51 118.8 . . ?
C50 C51 H51 118.8 . . ?
N10 C52 C53 123.9(5) . . ?
N10 C52 H52 118.0 . . ?
C53 C52 H52 118.0 . . ?
C52 C53 C54 118.8(5) . . ?
C52 C53 H53 120.6 . . ?
C54 C53 H53 120.6 . . ?
C55 C54 C53 118.6(5) . . ?
C55 C54 H54 120.7 . . ?
C53 C54 H54 120.7 . . ?
C54 C55 C56 119.4(5) . . ?
C54 C55 H55 120.3 . . ?
C56 C55 H55 120.3 . . ?
N10 C56 C55 122.5(5) . . ?
N10 C56 H56 118.8 . . ?
C55 C56 H56 118.8 . . ?
N11 C57 C58 123.2(5) . . ?
N11 C57 H57 118.4 . . ?
C58 C57 H57 118.4 . . ?
C59 C58 C57 119.3(5) . . ?
C59 C58 H58 120.4 . . ?
C57 C58 H58 120.4 . . ?
C58 C59 C60 118.1(5) . . ?
C58 C59 H59 121.0 . . ?
C60 C59 H59 121.0 . . ?
C61 C60 C59 119.7(5) . . ?
C61 C60 H60 120.1 . . ?
C59 C60 H60 120.1 . . ?
N11 C61 C60 122.3(5) . . ?
N11 C61 H61 118.9 . . ?
C60 C61 H61 118.9 . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.100
_database_code_depnum_ccdc_archive 'CCDC 1009474'
#######################################################################
#
#                 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_ni9(4)sq
_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Ni9-SO4 '
_chemical_name_common            Ni9-SO4.29H2O
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C70 H130 N20 Ni9 O57 S'
_chemical_formula_weight         2724.18
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'
S S 0.1246 0.1234 '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           orthorhombic
_symmetry_space_group_name_H-M   Ima2
_space_group_name_Hall           'I 2 -2a'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y, z'
'x+1/2, -y, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1/2, z+1/2'
'x+1, -y+1/2, z+1/2'
_cell_length_a                   29.1847(11)
_cell_length_b                   21.2385(7)
_cell_length_c                   19.7536(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     12244.1(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    214.0(9)
_cell_measurement_reflns_used    6970
_cell_measurement_theta_min      3.3570
_cell_measurement_theta_max      25.35
_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4480
_exptl_absorpt_coefficient_mu    1.431
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61718
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            52181
_diffrn_reflns_av_R_equivalents  0.1403
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.35
_diffrn_orient_matrix_UB_11      -0.0201068000
_diffrn_orient_matrix_UB_12      0.0092332000
_diffrn_orient_matrix_UB_21      -0.0061592000
_diffrn_orient_matrix_UB_22      0.0198188000
_diffrn_orient_matrix_UB_23      0.0274329000
_diffrn_orient_matrix_UB_31      0.0121789000
_diffrn_orient_matrix_UB_32      0.0252566000
_diffrn_orient_matrix_UB_33      -0.0150987000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -61.00  -35.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1403 -178.0000  -60.0000 26
  
#__ type_ start__ end____ width___ exp.time_
  2 omega   -1.00   25.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1403  -99.0000 -180.0000 26
  
#__ type_ start__ end____ width___ exp.time_
  3 omega   -6.00   91.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934   77.0000 -150.0000 97
  
#__ type_ start__ end____ width___ exp.time_
  4 omega    2.00   36.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934   57.0000  -30.0000 34
  
#__ type_ start__ end____ width___ exp.time_
  5 omega  -46.00   36.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934  -57.0000  -30.0000 82
  
#__ type_ start__ end____ width___ exp.time_
  6 omega  -47.00   37.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934  -57.0000   90.0000 84
  
#__ type_ start__ end____ width___ exp.time_
  7 omega  -44.00  -18.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934  -37.0000 -120.0000 26
  
#__ type_ start__ end____ width___ exp.time_
  8 omega   -9.00   36.00   1.0000   55.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5934   77.0000   90.0000 45
  
;
_diffrn_measurement_method       'ω scans'
_diffrn_ambient_temperature      214.0(9)
_reflns_number_total             11376
_reflns_number_gt                7684
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    SHELXS97
_computing_structure_refinement  'SHELXL-97/2 (Sheldrick,1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_refine_special_details          SQUEEZE
_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)+(0.0774P)²+0.0000P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(18)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         11376
_refine_ls_number_parameters     568
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1531
_refine_ls_wR_factor_gt          0.1455
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.964
_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 0.53669(3) 0.79555(4) 0.91405(5) 0.0334(2) Uani 1 1 d . . .
Ni2 Ni 0.52531(3) 0.92717(4) 0.99032(5) 0.0283(2) Uani 1 1 d . . .
Ni3 Ni 0.41657(3) 0.87668(4) 1.05858(5) 0.0309(2) Uani 1 1 d . . .
Ni4 Ni 0.43994(3) 0.91660(4) 0.92006(5) 0.0304(2) Uani 1 1 d . . .
Ni5 Ni 0.5000 1.0000 0.82410(7) 0.0361(4) Uani 1 2 d S . .
S1 S 0.2500 0.8628(2) 1.0260(2) 0.0674(11) Uiso 1 2 d S . .
O1 O 0.41822(19) 0.7809(2) 1.0421(3) 0.0389(14) Uani 1 1 d . . .
O2 O 0.47299(16) 0.8681(2) 0.9985(2) 0.0281(11) Uani 1 1 d . . .
O3 O 0.5101(2) 0.9310(3) 0.7593(3) 0.0488(17) Uani 1 1 d . . .
O4 O 0.5064(2) 0.9290(2) 0.8894(2) 0.0350(13) Uani 1 1 d . . .
O5 O 0.57440(18) 0.8609(2) 0.9669(2) 0.0308(12) Uani 1 1 d . . .
O6 O 0.57128(19) 0.7367(3) 0.9780(3) 0.0433(15) Uani 1 1 d . . .
O7 O 0.46270(18) 1.0632(2) 1.0881(2) 0.0278(12) Uani 1 1 d . . .
O8 O 0.44742(18) 0.9875(2) 0.9875(2) 0.0328(12) Uani 1 1 d . . .
O9 O 0.42071(19) 0.8401(3) 0.8616(2) 0.0350(13) Uani 1 1 d . . .
O10 O 0.38001(19) 0.8953(2) 0.9654(2) 0.0309(13) Uani 1 1 d . . .
O11 O 0.35734(19) 0.8750(3) 1.1117(3) 0.0435(15) Uani 1 1 d . . .
O12 O 0.4285(2) 0.9792(2) 0.8376(3) 0.0429(15) Uani 1 1 d . . .
H12A H 0.4102 1.0166 0.8504 0.051 Uiso 1 1 calc R . .
H12B H 0.4147 0.9582 0.7978 0.051 Uiso 1 1 calc R . .
O13 O 0.2899(3) 0.8255(4) 1.0303(4) 0.085(2) Uiso 1 1 d . . .
O14 O 0.2500 0.9222(8) 1.0681(10) 0.166(7) Uiso 1 2 d S . .
O15 O 0.2500 0.9064(9) 0.9636(9) 0.165(7) Uiso 1 2 d S . .
N1 N 0.4906(2) 0.7280(3) 0.8732(3) 0.049(2) Uani 1 1 d . . .
H1A H 0.4652 0.7485 0.8567 0.058 Uiso 1 1 calc R . .
H1B H 0.5046 0.7079 0.8375 0.058 Uiso 1 1 calc R . .
N2 N 0.4827(2) 0.8032(3) 0.9797(3) 0.0316(16) Uani 1 1 d . . .
N3 N 0.5859(2) 0.7840(3) 0.8355(3) 0.0346(16) Uani 1 1 d . . .
H3A H 0.6044 0.8190 0.8330 0.042 Uiso 1 1 calc R . .
H3B H 0.6041 0.7496 0.8444 0.042 Uiso 1 1 calc R . .
N4 N 0.5189(2) 0.8716(3) 0.8538(3) 0.0365(17) Uani 1 1 d . . .
N5 N 0.5808(3) 0.6349(3) 1.0539(4) 0.056(2) Uani 1 1 d . . .
H5A H 0.5757 0.5953 1.0648 0.067 Uiso 1 1 calc R . .
H5B H 0.5660 0.6519 1.0197 0.067 Uiso 1 1 calc R . .
N6 N 0.5973(2) 0.8287(3) 1.0209(3) 0.0339(16) Uani 1 1 d . . .
H6 H 0.6118 0.8499 1.0526 0.041 Uiso 1 1 calc R . .
N7 N 0.4526(2) 0.8839(3) 1.1510(3) 0.0336(16) Uani 1 1 d . . .
H7A H 0.4517 0.8456 1.1727 0.040 Uiso 1 1 calc R . .
H7B H 0.4828 0.8931 1.1420 0.040 Uiso 1 1 calc R . .
N8 N 0.4315(2) 0.9692(3) 1.0529(3) 0.0292(14) Uani 1 1 d . . .
N9 N 0.3850(7) 0.7923(10) 0.7412(7) 0.287(16) Uani 1 1 d . . .
H9A H 0.3854 0.7867 0.6971 0.344 Uiso 1 1 calc R . .
H9B H 0.4003 0.8238 0.7594 0.344 Uiso 1 1 calc R . .
N10 N 0.3607(2) 0.8462(3) 0.9334(3) 0.0363(16) Uani 1 1 d . . .
H10A H 0.3335 0.8324 0.9458 0.044 Uiso 1 1 calc R . .
C1 C 0.4759(3) 0.6802(4) 0.9235(5) 0.051(2) Uani 1 1 d . . .
C2 C 0.4810(4) 0.6186(5) 0.9095(7) 0.067(3) Uani 1 1 d . . .
H2 H 0.4976 0.6092 0.8694 0.080 Uiso 1 1 calc R . .
C3 C 0.4674(6) 0.5742(8) 0.9405(10) 0.125(8) Uani 1 1 d . . .
H3 H 0.4678 0.5330 0.9219 0.150 Uiso 1 1 calc R . .
C4 C 0.4520(6) 0.5854(6) 1.0019(11) 0.129(8) Uani 1 1 d . . .
H4 H 0.4460 0.5516 1.0321 0.155 Uiso 1 1 calc R . .
C5 C 0.4438(3) 0.6528(4) 1.0239(5) 0.057(3) Uani 1 1 d . . .
H5 H 0.4289 0.6620 1.0655 0.069 Uiso 1 1 calc R . .
C6 C 0.4576(3) 0.6979(4) 0.9840(5) 0.045(2) Uani 1 1 d . . .
C7 C 0.4518(3) 0.7657(4) 1.0033(4) 0.040(2) Uani 1 1 d . . .
C8 C 0.5633(3) 0.7756(4) 0.7752(4) 0.0315(18) Uani 1 1 d . . .
C9 C 0.5689(3) 0.7213(4) 0.7364(4) 0.0331(19) Uani 1 1 d . . .
H9 H 0.5900 0.6902 0.7517 0.040 Uiso 1 1 calc R . .
C10 C 0.5451(3) 0.7104(4) 0.6762(4) 0.040(2) Uani 1 1 d . . .
H10 H 0.5493 0.6726 0.6513 0.048 Uiso 1 1 calc R . .
C11 C 0.5153(3) 0.7562(4) 0.6542(4) 0.039(2) Uani 1 1 d . . .
H11 H 0.4985 0.7496 0.6136 0.046 Uiso 1 1 calc R . .
C12 C 0.5092(3) 0.8120(4) 0.6901(4) 0.036(2) Uani 1 1 d . . .
H12 H 0.4896 0.8440 0.6729 0.043 Uiso 1 1 calc R . .
C13 C 0.5316(3) 0.8203(4) 0.7503(4) 0.0327(18) Uani 1 1 d . . .
C14 C 0.5199(3) 0.8778(4) 0.7913(3) 0.0318(19) Uani 1 1 d . . .
C15 C 0.6112(3) 0.6695(4) 1.0897(4) 0.0356(19) Uani 1 1 d . . .
C16 C 0.6344(3) 0.6445(4) 1.1425(4) 0.051(2) Uani 1 1 d . . .
H16 H 0.6274 0.6024 1.1549 0.061 Uiso 1 1 calc R . .
C17 C 0.6676(3) 0.6753(4) 1.1800(4) 0.051(3) Uani 1 1 d . . .
H17 H 0.6822 0.6561 1.2177 0.061 Uiso 1 1 calc R . .
C18 C 0.6780(3) 0.7357(4) 1.1593(5) 0.051(2) Uani 1 1 d . . .
H18 H 0.7017 0.7576 1.1822 0.062 Uiso 1 1 calc R . .
C19 C 0.6566(3) 0.7646(4) 1.1093(4) 0.0352(19) Uani 1 1 d . . .
H19 H 0.6651 0.8064 1.0976 0.042 Uiso 1 1 calc R . .
C20 C 0.6212(3) 0.7341(4) 1.0727(3) 0.0318(18) Uani 1 1 d . . .
C21 C 0.5961(2) 0.7673(4) 1.0221(3) 0.0263(17) Uani 1 1 d . . .
C22 C 0.4353(3) 0.9286(4) 1.1930(4) 0.0345(19) Uani 1 1 d . . .
C23 C 0.4211(4) 0.9169(4) 1.2594(4) 0.053(3) Uani 1 1 d . . .
H23 H 0.4225 0.8752 1.2765 0.064 Uiso 1 1 calc R . .
C24 C 0.4059(4) 0.9625(5) 1.2992(4) 0.067(3) Uani 1 1 d . . .
H24 H 0.3964 0.9521 1.3438 0.080 Uiso 1 1 calc R . .
C25 C 0.4031(4) 1.0249(4) 1.2786(4) 0.056(3) Uani 1 1 d . . .
H25 H 0.3924 1.0570 1.3081 0.067 Uiso 1 1 calc R . .
C26 C 0.4167(3) 1.0379(4) 1.2132(4) 0.046(2) Uani 1 1 d . . .
H26 H 0.4160 1.0805 1.1985 0.055 Uiso 1 1 calc R . .
C27 C 0.4309(3) 0.9941(4) 1.1694(3) 0.0316(19) Uani 1 1 d . . .
C28 C 0.4442(3) 1.0098(3) 1.0994(3) 0.0275(17) Uani 1 1 d . . .
C29 C 0.3613(4) 0.7531(6) 0.7807(5) 0.070(3) Uani 1 1 d . . .
C30 C 0.3386(4) 0.7064(5) 0.7549(5) 0.055(3) Uani 1 1 d . . .
H30 H 0.3361 0.7022 0.7072 0.066 Uiso 1 1 calc R . .
C31 C 0.3221(7) 0.6714(7) 0.7886(7) 0.122(7) Uani 1 1 d . . .
H31 H 0.3109 0.6344 0.7672 0.147 Uiso 1 1 calc R . .
C32 C 0.3155(6) 0.6751(5) 0.8620(8) 0.122(6) Uani 1 1 d . . .
H32 H 0.2962 0.6470 0.8862 0.146 Uiso 1 1 calc R . .
C33 C 0.3382(4) 0.7199(4) 0.8909(5) 0.064(3) Uani 1 1 d . . .
H33 H 0.3388 0.7230 0.9389 0.076 Uiso 1 1 calc R . .
C34 C 0.3608(3) 0.7618(4) 0.8532(4) 0.039(2) Uani 1 1 d . . .
C35 C 0.3833(3) 0.8184(4) 0.8823(3) 0.0321(19) Uani 1 1 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
Ni1 O6 2.045(5) . ?
Ni1 N2 2.046(7) . ?
Ni1 O5 2.057(5) . ?
Ni1 N4 2.073(7) . ?
Ni1 N1 2.125(7) . ?
Ni1 N3 2.130(6) . ?
Ni2 O7 1.974(5) 2_675 ?
Ni2 O8 1.979(5) 2_675 ?
Ni2 O2 1.984(5) . ?
Ni2 O5 2.060(5) . ?
Ni2 O4 2.070(5) . ?
Ni2 Ni4 2.8609(14) . ?
Ni3 N8 2.016(6) . ?
Ni3 O11 2.023(6) . ?
Ni3 O2 2.038(5) . ?
Ni3 O1 2.061(5) . ?
Ni3 N7 2.113(6) . ?
Ni3 O10 2.163(5) . ?
Ni3 Ni4 2.9448(14) . ?
Ni4 O10 2.017(6) . ?
Ni4 O8 2.023(5) . ?
Ni4 O4 2.048(6) . ?
Ni4 O9 2.070(5) . ?
Ni4 O2 2.096(5) . ?
Ni4 O12 2.130(5) . ?
Ni5 O3 1.968(5) 2_675 ?
Ni5 O3 1.968(5) . ?
Ni5 O4 1.992(5) . ?
Ni5 O4 1.992(5) 2_675 ?
Ni5 O12 2.150(6) . ?
Ni5 O12 2.150(6) 2_675 ?
S1 O13 1.411(8) . ?
S1 O13 1.411(8) 3 ?
S1 O14 1.511(17) . ?
S1 O15 1.543(17) . ?
O1 C7 1.286(10) . ?
O2 N2 1.456(7) . ?
O3 C14 1.326(9) . ?
O4 N4 1.453(7) . ?
O5 N6 1.432(7) . ?
O6 C21 1.306(9) . ?
O7 C28 1.277(8) . ?
O7 Ni2 1.974(5) 2_675 ?
O8 N8 1.427(7) . ?
O8 Ni2 1.979(5) 2_675 ?
O9 C35 1.255(9) . ?
O10 N10 1.343(7) . ?
O12 H12A 0.9900 . ?
O12 H12B 0.9900 . ?
N1 C1 1.483(12) . ?
N1 H1A 0.9200 . ?
N1 H1B 0.9200 . ?
N2 C7 1.290(10) . ?
N3 C8 1.373(9) . ?
N3 H3A 0.9200 . ?
N3 H3B 0.9200 . ?
N4 C14 1.242(9) . ?
N5 C15 1.354(10) . ?
N5 H5A 0.8800 . ?
N5 H5B 0.8800 . ?
N6 C21 1.305(9) . ?
N6 H6 0.8800 . ?
N7 C22 1.358(10) . ?
N7 H7A 0.9200 . ?
N7 H7B 0.9200 . ?
N8 C28 1.312(9) . ?
N9 C29 1.335(18) . ?
N9 H9A 0.8800 . ?
N9 H9B 0.8800 . ?
N10 C35 1.341(9) . ?
N10 H10A 0.8800 . ?
C1 C2 1.346(13) . ?
C1 C6 1.362(14) . ?
C2 C3 1.19(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.32(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.515(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.303(13) . ?
C5 H5 0.9500 . ?
C6 C7 1.500(11) . ?
C8 C9 1.393(10) . ?
C8 C13 1.415(10) . ?
C9 C10 1.398(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.375(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.370(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.504(11) . ?
C15 C16 1.351(11) . ?
C15 C20 1.442(11) . ?
C16 C17 1.382(13) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(12) . ?
C17 H17 0.9500 . ?
C18 C19 1.319(11) . ?
C18 H18 0.9500 . ?
C19 C20 1.418(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.428(10) . ?
C22 C23 1.398(12) . ?
C22 C27 1.472(10) . ?
C23 C24 1.324(13) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.379(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.336(11) . ?
C26 H26 0.9500 . ?
C27 C28 1.475(10) . ?
C29 C30 1.296(14) . ?
C29 C34 1.445(12) . ?
C30 C31 1.107(18) . ?
C30 H30 0.9500 . ?
C31 C32 1.465(17) . ?
C31 H31 0.9500 . ?
C32 C33 1.293(15) . ?
C32 H32 0.9500 . ?
C33 C34 1.334(12) . ?
C33 H33 0.9500 . ?
C34 C35 1.486(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
O6 Ni1 N2 92.1(2) . . ?
O6 Ni1 O5 80.5(2) . . ?
N2 Ni1 O5 92.1(2) . . ?
O6 Ni1 N4 162.8(3) . . ?
N2 Ni1 N4 96.2(2) . . ?
O5 Ni1 N4 84.2(2) . . ?
O6 Ni1 N1 97.7(3) . . ?
N2 Ni1 N1 78.9(2) . . ?
O5 Ni1 N1 170.8(2) . . ?
N4 Ni1 N1 98.6(3) . . ?
O6 Ni1 N3 92.7(2) . . ?
N2 Ni1 N3 172.0(2) . . ?
O5 Ni1 N3 95.0(2) . . ?
N4 Ni1 N3 80.8(2) . . ?
N1 Ni1 N3 94.1(3) . . ?
O7 Ni2 O8 82.06(19) 2_675 2_675 ?
O7 Ni2 O2 97.0(2) 2_675 . ?
O8 Ni2 O2 153.0(2) 2_675 . ?
O7 Ni2 O5 99.6(2) 2_675 . ?
O8 Ni2 O5 109.8(2) 2_675 . ?
O2 Ni2 O5 97.0(2) . . ?
O7 Ni2 O4 171.3(2) 2_675 . ?
O8 Ni2 O4 93.6(2) 2_675 . ?
O2 Ni2 O4 83.4(2) . . ?
O5 Ni2 O4 88.99(19) . . ?
O7 Ni2 Ni4 129.59(16) 2_675 . ?
O8 Ni2 Ni4 114.09(15) 2_675 . ?
O2 Ni2 Ni4 47.11(14) . . ?
O5 Ni2 Ni4 116.30(14) . . ?
O4 Ni2 Ni4 45.69(17) . . ?
N8 Ni3 O11 103.4(2) . . ?
N8 Ni3 O2 83.1(2) . . ?
O11 Ni3 O2 172.4(2) . . ?
N8 Ni3 O1 161.5(2) . . ?
O11 Ni3 O1 94.9(2) . . ?
O2 Ni3 O1 78.5(2) . . ?
N8 Ni3 N7 82.5(2) . . ?
O11 Ni3 N7 88.7(2) . . ?
O2 Ni3 N7 96.2(2) . . ?
O1 Ni3 N7 101.3(2) . . ?
N8 Ni3 O10 83.2(2) . . ?
O11 Ni3 O10 91.3(2) . . ?
O2 Ni3 O10 85.4(2) . . ?
O1 Ni3 O10 93.31(19) . . ?
N7 Ni3 O10 165.3(2) . . ?
N8 Ni3 Ni4 67.52(16) . . ?
O11 Ni3 Ni4 133.25(15) . . ?
O2 Ni3 Ni4 45.38(14) . . ?
O1 Ni3 Ni4 97.61(16) . . ?
N7 Ni3 Ni4 131.85(18) . . ?
O10 Ni3 Ni4 43.22(15) . . ?
O10 Ni4 O8 88.18(19) . . ?
O10 Ni4 O4 168.9(2) . . ?
O8 Ni4 O4 89.8(2) . . ?
O10 Ni4 O9 80.6(2) . . ?
O8 Ni4 O9 168.8(2) . . ?
O4 Ni4 O9 101.1(2) . . ?
O10 Ni4 O2 87.71(19) . . ?
O8 Ni4 O2 80.21(19) . . ?
O4 Ni4 O2 81.18(19) . . ?
O9 Ni4 O2 98.69(19) . . ?
O10 Ni4 O12 110.1(2) . . ?
O8 Ni4 O12 93.18(19) . . ?
O4 Ni4 O12 80.9(2) . . ?
O9 Ni4 O12 91.2(2) . . ?
O2 Ni4 O12 160.9(2) . . ?
O10 Ni4 Ni2 123.87(14) . . ?
O8 Ni4 Ni2 61.84(15) . . ?
O4 Ni4 Ni2 46.31(14) . . ?
O9 Ni4 Ni2 124.63(15) . . ?
O2 Ni4 Ni2 43.89(13) . . ?
O12 Ni4 Ni2 117.31(17) . . ?
O10 Ni4 Ni3 47.28(13) . . ?
O8 Ni4 Ni3 68.14(14) . . ?
O4 Ni4 Ni3 122.09(14) . . ?
O9 Ni4 Ni3 103.27(15) . . ?
O2 Ni4 Ni3 43.78(14) . . ?
O12 Ni4 Ni3 148.70(16) . . ?
Ni2 Ni4 Ni3 76.91(4) . . ?
O3 Ni5 O3 98.9(3) 2_675 . ?
O3 Ni5 O4 176.7(3) 2_675 . ?
O3 Ni5 O4 80.97(19) . . ?
O3 Ni5 O4 80.97(19) 2_675 2_675 ?
O3 Ni5 O4 176.7(3) . 2_675 ?
O4 Ni5 O4 99.4(3) . 2_675 ?
O3 Ni5 O12 95.1(2) 2_675 . ?
O3 Ni5 O12 94.2(2) . . ?
O4 Ni5 O12 81.7(2) . . ?
O4 Ni5 O12 89.1(2) 2_675 . ?
O3 Ni5 O12 94.2(2) 2_675 2_675 ?
O3 Ni5 O12 95.1(2) . 2_675 ?
O4 Ni5 O12 89.1(2) . 2_675 ?
O4 Ni5 O12 81.7(2) 2_675 2_675 ?
O12 Ni5 O12 165.8(3) . 2_675 ?
O13 S1 O13 111.3(7) . 3 ?
O13 S1 O14 115.8(5) . . ?
O13 S1 O14 115.8(5) 3 . ?
O13 S1 O15 112.6(5) . . ?
O13 S1 O15 112.6(5) 3 . ?
O14 S1 O15 86.5(10) . . ?
C7 O1 Ni3 111.0(5) . . ?
N2 O2 Ni2 115.3(4) . . ?
N2 O2 Ni3 113.1(4) . . ?
Ni2 O2 Ni3 127.8(2) . . ?
N2 O2 Ni4 111.5(3) . . ?
Ni2 O2 Ni4 89.01(19) . . ?
Ni3 O2 Ni4 90.83(19) . . ?
C14 O3 Ni5 111.0(4) . . ?
N4 O4 Ni5 110.2(4) . . ?
N4 O4 Ni4 105.8(4) . . ?
Ni5 O4 Ni4 101.6(2) . . ?
N4 O4 Ni2 112.5(4) . . ?
Ni5 O4 Ni2 131.5(3) . . ?
Ni4 O4 Ni2 88.0(2) . . ?
N6 O5 Ni1 107.8(4) . . ?
N6 O5 Ni2 118.9(4) . . ?
Ni1 O5 Ni2 101.7(2) . . ?
C21 O6 Ni1 112.4(5) . . ?
C28 O7 Ni2 109.7(4) . 2_675 ?
N8 O8 Ni2 110.8(4) . 2_675 ?
N8 O8 Ni4 111.0(4) . . ?
Ni2 O8 Ni4 138.1(2) 2_675 . ?
C35 O9 Ni4 110.0(5) . . ?
N10 O10 Ni4 109.2(4) . . ?
N10 O10 Ni3 117.8(4) . . ?
Ni4 O10 Ni3 89.5(2) . . ?
Ni4 O12 Ni5 94.1(2) . . ?
Ni4 O12 H12A 112.9 . . ?
Ni5 O12 H12A 112.9 . . ?
Ni4 O12 H12B 112.9 . . ?
Ni5 O12 H12B 112.9 . . ?
H12A O12 H12B 110.3 . . ?
C1 N1 Ni1 113.0(5) . . ?
C1 N1 H1A 109.0 . . ?
Ni1 N1 H1A 109.0 . . ?
C1 N1 H1B 109.0 . . ?
Ni1 N1 H1B 109.0 . . ?
H1A N1 H1B 107.8 . . ?
C7 N2 O2 110.7(6) . . ?
C7 N2 Ni1 136.0(6) . . ?
O2 N2 Ni1 112.8(4) . . ?
C8 N3 Ni1 108.9(5) . . ?
C8 N3 H3A 109.9 . . ?
Ni1 N3 H3A 109.9 . . ?
C8 N3 H3B 109.9 . . ?
Ni1 N3 H3B 109.9 . . ?
H3A N3 H3B 108.3 . . ?
C14 N4 O4 113.5(6) . . ?
C14 N4 Ni1 130.3(5) . . ?
O4 N4 Ni1 116.1(4) . . ?
C15 N5 H5A 120.0 . . ?
C15 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C21 N6 O5 118.5(6) . . ?
C21 N6 H6 120.7 . . ?
O5 N6 H6 120.7 . . ?
C22 N7 Ni3 113.2(5) . . ?
C22 N7 H7A 108.9 . . ?
Ni3 N7 H7A 108.9 . . ?
C22 N7 H7B 108.9 . . ?
Ni3 N7 H7B 108.9 . . ?
H7A N7 H7B 107.8 . . ?
C28 N8 O8 111.3(6) . . ?
C28 N8 Ni3 131.5(5) . . ?
O8 N8 Ni3 112.8(4) . . ?
C29 N9 H9A 120.0 . . ?
C29 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
C35 N10 O10 119.3(6) . . ?
C35 N10 H10A 120.3 . . ?
O10 N10 H10A 120.3 . . ?
C2 C1 C6 119.4(11) . . ?
C2 C1 N1 119.7(11) . . ?
C6 C1 N1 120.9(8) . . ?
C3 C2 C1 128.8(16) . . ?
C3 C2 H2 115.6 . . ?
C1 C2 H2 115.6 . . ?
C2 C3 C4 116.4(16) . . ?
C2 C3 H3 121.8 . . ?
C4 C3 H3 121.8 . . ?
C3 C4 C5 119.2(13) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 118.2(12) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
C5 C6 C1 116.7(9) . . ?
C5 C6 C7 121.1(10) . . ?
C1 C6 C7 122.1(9) . . ?
O1 C7 N2 126.5(7) . . ?
O1 C7 C6 118.6(8) . . ?
N2 C7 C6 114.9(8) . . ?
N3 C8 C9 121.9(7) . . ?
N3 C8 C13 121.9(7) . . ?
C9 C8 C13 116.2(7) . . ?
C8 C9 C10 123.1(8) . . ?
C8 C9 H9 118.4 . . ?
C10 C9 H9 118.4 . . ?
C11 C10 C9 117.8(7) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
C10 C11 C12 121.6(8) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C13 C12 C11 119.3(7) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C8 121.9(7) . . ?
C12 C13 C14 117.6(7) . . ?
C8 C13 C14 120.5(6) . . ?
N4 C14 O3 123.9(7) . . ?
N4 C14 C13 117.1(7) . . ?
O3 C14 C13 119.0(6) . . ?
C16 C15 N5 121.3(8) . . ?
C16 C15 C20 116.8(7) . . ?
N5 C15 C20 121.8(7) . . ?
C15 C16 C17 125.3(8) . . ?
C15 C16 H16 117.3 . . ?
C17 C16 H16 117.3 . . ?
C18 C17 C16 115.7(8) . . ?
C18 C17 H17 122.1 . . ?
C16 C17 H17 122.1 . . ?
C19 C18 C17 123.4(9) . . ?
C19 C18 H18 118.3 . . ?
C17 C18 H18 118.3 . . ?
C18 C19 C20 120.8(8) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C21 120.3(7) . . ?
C19 C20 C15 117.7(7) . . ?
C21 C20 C15 122.0(7) . . ?
N6 C21 O6 120.1(7) . . ?
N6 C21 C20 119.5(7) . . ?
O6 C21 C20 120.4(7) . . ?
N7 C22 C23 124.0(7) . . ?
N7 C22 C27 120.0(7) . . ?
C23 C22 C27 116.0(7) . . ?
C24 C23 C22 121.8(8) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C25 122.9(8) . . ?
C23 C24 H24 118.6 . . ?
C25 C24 H24 118.6 . . ?
C26 C25 C24 116.7(8) . . ?
C26 C25 H25 121.6 . . ?
C24 C25 H25 121.6 . . ?
C27 C26 C25 123.7(8) . . ?
C27 C26 H26 118.1 . . ?
C25 C26 H26 118.1 . . ?
C26 C27 C22 118.7(7) . . ?
C26 C27 C28 122.1(7) . . ?
C22 C27 C28 119.1(7) . . ?
O7 C28 N8 125.5(6) . . ?
O7 C28 C27 118.4(6) . . ?
N8 C28 C27 115.7(7) . . ?
C30 C29 N9 120.9(10) . . ?
C30 C29 C34 118.8(10) . . ?
N9 C29 C34 120.3(10) . . ?
C31 C30 C29 119.9(13) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C32 128.1(16) . . ?
C30 C31 H31 116.0 . . ?
C32 C31 H31 116.0 . . ?
C33 C32 C31 114.1(14) . . ?
C33 C32 H32 122.9 . . ?
C31 C32 H32 122.9 . . ?
C32 C33 C34 119.8(10) . . ?
C32 C33 H33 120.1 . . ?
C34 C33 H33 120.1 . . ?
C33 C34 C29 118.3(8) . . ?
C33 C34 C35 122.8(7) . . ?
C29 C34 C35 118.8(8) . . ?
O9 C35 N10 120.7(7) . . ?
O9 C35 C34 123.8(7) . . ?
N10 C35 C34 115.5(7) . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.106

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.036 0.454 0.022 5034 1143 ' '
_platon_squeeze_details          
;
Electron density representing the equivalent of 29 water molecules 
per cage were removed during the SQUEEZE process 
;
_chemical_properties_physical    Hygroscopic
_exptl_crystal_preparation       'Magnetic properties'
_database_code_depnum_ccdc_archive 'CCDC 1009475'
#######################################################################
#
#                 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_cmd263e5
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Ni9]-(ClO4)2'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H116 Cl2 N20 Ni9 O52'
_chemical_formula_weight         2716.96
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   Cc
_space_group_name_Hall           'C -2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
_cell_length_a                   20.0036(7)
_cell_length_b                   25.0628(9)
_cell_length_c                   21.2234(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.320(2)
_cell_angle_gamma                90.00
_cell_volume                     10640.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5730
_cell_measurement_theta_min      3.1630
_cell_measurement_theta_max      25.35
_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5400
_exptl_absorpt_coefficient_mu    1.708
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95840
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            40644
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         25.35
_diffrn_orient_matrix_UB_11      -0.0246176000
_diffrn_orient_matrix_UB_12      0.0203886000
_diffrn_orient_matrix_UB_21      0.0145709000
_diffrn_orient_matrix_UB_22      0.0119285000
_diffrn_orient_matrix_UB_23      0.0270784000
_diffrn_orient_matrix_UB_31      0.0209616000
_diffrn_orient_matrix_UB_32      0.0156109000
_diffrn_orient_matrix_UB_33      -0.0195342000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059   77.0000  150.0000 97
  
#__ type_ start__ end____ width___ exp.time_
  2 omega   -7.00   56.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059  -99.0000  -90.0000 63
  
#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   68.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059  -99.0000   30.0000 93
  
#__ type_ start__ end____ width___ exp.time_
  4 omega   -2.00   77.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059   19.0000  120.0000 79
  
#__ type_ start__ end____ width___ exp.time_
  5 omega   59.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.9059   57.0000  -60.0000 32
  
;
_diffrn_measurement_method       'ω scans'
_diffrn_ambient_temperature      150(2)
_reflns_number_total             16130
_reflns_number_gt                12123
_reflns_threshold_expression     >2sigma(I)
_computing_structure_solution    SHELXS97
_computing_structure_refinement  'SHELXL-97/2 (Sheldrick,1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_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)+(0.0930P)²+0.0000P] where P=(Fo²+2Fc²)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.026(18)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         16130
_refine_ls_number_parameters     1236
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0693
_refine_ls_wR_factor_ref         0.1769
_refine_ls_wR_factor_gt          0.1594
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.58188(7) 0.14290(6) 0.04861(6) 0.0193(3) Uani 1 1 d . . .
Ni2 Ni 0.44356(7) 0.28234(6) 0.13732(6) 0.0191(3) Uani 1 1 d . . .
Ni3 Ni 0.44469(7) 0.17265(6) 0.01267(6) 0.0179(3) Uani 1 1 d . . .
Ni4 Ni 0.51567(7) 0.27076(6) 0.00311(6) 0.0188(3) Uani 1 1 d . . .
Ni5 Ni 0.35045(7) 0.24789(6) -0.06755(6) 0.0189(3) Uani 1 1 d . . .
Ni6 Ni 0.51309(7) 0.22391(6) -0.14035(6) 0.0182(3) Uani 1 1 d . . .
Ni7 Ni 0.44317(7) 0.32239(6) -0.14891(6) 0.0193(3) Uani 1 1 d . . .
Ni8 Ni 0.43699(7) 0.21176(6) -0.27346(6) 0.0201(3) Uani 1 1 d . . .
Ni9 Ni 0.58012(7) 0.35010(6) -0.18810(6) 0.0207(3) Uani 1 1 d . . .
Cl2 Cl 0.2116(4) 0.0792(3) -0.0005(3) 0.114(2) Uiso 1 1 d . . .
O1 O 0.5696(4) 0.1429(3) 0.1442(3) 0.0220(17) Uani 1 1 d . . .
O2 O 0.5243(4) 0.2087(3) 0.0623(3) 0.0187(16) Uani 1 1 d . . .
O3 O 0.6310(4) 0.0714(3) 0.0409(4) 0.0304(19) Uani 1 1 d . . .
O4 O 0.5083(4) 0.3235(3) 0.1940(3) 0.0216(17) Uani 1 1 d . . .
O5 O 0.4956(3) 0.3253(3) 0.0710(3) 0.0183(17) Uani 1 1 d . . .
O6 O 0.3904(4) 0.1496(3) 0.0895(3) 0.0230(18) Uani 1 1 d . . .
O7 O 0.4894(3) 0.1026(3) 0.0291(3) 0.0190(16) Uani 1 1 d . . .
O8 O 0.2870(4) 0.2564(3) 0.0034(3) 0.0261(19) Uani 1 1 d . . .
O9 O 0.4160(4) 0.2507(3) 0.0031(3) 0.0225(18) Uani 1 1 d . . .
O10 O 0.3642(4) 0.1618(3) -0.0508(3) 0.0228(18) Uani 1 1 d . . .
H10A H 0.3249 0.1449 -0.0310 0.027 Uiso 1 1 calc R . .
H10B H 0.3771 0.1421 -0.0893 0.027 Uiso 1 1 calc R . .
O11 O 0.2849(4) 0.2388(3) -0.1380(3) 0.0256(19) Uani 1 1 d . . .
O12 O 0.4141(4) 0.2444(3) -0.1387(3) 0.0212(17) Uani 1 1 d . . .
O13 O 0.3859(4) 0.3465(3) -0.2242(3) 0.0265(19) Uani 1 1 d . . .
O14 O 0.4900(4) 0.3917(3) -0.1682(3) 0.0240(18) Uani 1 1 d . . .
O15 O 0.5102(3) 0.1869(3) -0.0590(3) 0.0202(17) Uani 1 1 d . . .
O16 O 0.5208(4) 0.2854(3) -0.1990(3) 0.0171(16) Uani 1 1 d . . .
O17 O 0.6315(4) 0.4205(3) -0.1867(4) 0.034(2) Uani 1 1 d . . .
O18 O 0.6089(4) 0.2063(3) -0.1336(3) 0.0207(17) Uani 1 1 d . . .
O19 O 0.5113(3) 0.3072(3) -0.0795(3) 0.0182(16) Uani 1 1 d . . .
O20 O 0.6116(4) 0.2858(3) -0.0066(3) 0.0196(17) Uani 1 1 d . . .
O21 O 0.5005(4) 0.1714(3) -0.3312(3) 0.0245(18) Uani 1 1 d . . .
O22 O 0.4905(3) 0.1690(3) -0.2070(3) 0.0182(16) Uani 1 1 d . . .
O23 O 0.3632(4) 0.3338(3) -0.0863(3) 0.0267(19) Uani 1 1 d . . .
H23A H 0.3236 0.3501 -0.1067 0.032 Uiso 1 1 calc R . .
H23B H 0.3761 0.3543 -0.0482 0.032 Uiso 1 1 calc R . .
O24 O 0.5655(4) 0.3491(3) -0.2848(3) 0.0257(18) Uani 1 1 d . . .
O27 O 0.6700(4) 0.2014(3) -0.5392(4) 0.0307(19) Uiso 1 1 d . . .
O28 O 0.3982(4) 0.1067(3) -0.1499(4) 0.035(2) Uiso 1 1 d . . .
O29 O 0.6684(4) 0.3005(3) 0.4049(4) 0.036(2) Uiso 1 1 d . . .
O30 O 0.5539(5) -0.0023(4) 0.0996(4) 0.042(2) Uiso 1 1 d . . .
O31 O 0.4002(4) 0.3886(3) 0.0140(4) 0.036(2) Uiso 1 1 d . . .
O32 O 0.1242(5) 0.4429(4) -0.2964(4) 0.044(2) Uiso 1 1 d . . .
O33 O 0.4949(6) 0.0871(5) -0.4621(5) 0.065(3) Uiso 1 1 d . . .
O34 O 0.2410(5) 0.3638(4) -0.1240(5) 0.058(3) Uiso 1 1 d . . .
O35 O 0.1220(7) 0.0633(6) 0.1649(6) 0.087(4) Uiso 1 1 d . . .
O36 O 0.5966(6) 0.4256(5) 0.0118(5) 0.081(4) Uiso 1 1 d . . .
O37 O 0.5459(7) 0.4992(6) -0.2407(6) 0.094(4) Uiso 1 1 d . . .
O38 O 0.4711(7) 0.0381(6) -0.0739(6) 0.101(4) Uiso 1 1 d . . .
O39 O 0.3884(8) 0.4282(7) -0.7509(7) 0.111(5) Uiso 1 1 d . . .
O41 O 0.9708(9) 0.4347(8) -0.0826(8) 0.134(6) Uiso 1 1 d . . .
O42 O 0.4993(12) 0.4432(10) -0.5657(10) 0.186(9) Uiso 1 1 d . . .
O43 O 0.7022(10) 0.4600(9) -0.0791(9) 0.152(7) Uiso 1 1 d . . .
O45 O 0.4892(7) 0.4511(6) -0.0576(6) 0.097(4) Uiso 1 1 d . . .
O80 O 0.8142(10) 0.0052(8) -0.1823(9) 0.152(7) Uiso 1 1 d . . .
O54 O 0.1480(19) 0.0793(15) -0.0478(17) 0.306(17) Uiso 1 1 d . . .
O55 O 0.1905(12) 0.0345(11) 0.0441(11) 0.201(10) Uiso 1 1 d . . .
O56 O 0.2487(17) 0.0482(15) -0.0619(16) 0.291(15) Uiso 1 1 d . . .
O57 O 0.2416(10) 0.1345(9) 0.0065(9) 0.154(7) Uiso 1 1 d . . .
O61 O 0.4947(11) 0.4162(9) -0.6836(10) 0.161(8) Uiso 1 1 d . . .
H61A H 0.5285 0.4272 -0.6638 0.194 Uiso 1 1 calc R . .
O64 O 0.3753(6) 0.0893(5) -0.4000(5) 0.061(3) Uiso 1 1 d . . .
H64 H 0.3570 0.1146 -0.4194 0.074 Uiso 1 1 calc R . .
N1 N 0.5732(4) 0.1654(4) -0.0432(4) 0.021(2) Uani 1 1 d . . .
N2 N 0.6730(4) 0.1853(4) 0.0460(4) 0.020(2) Uani 1 1 d . . .
H2A H 0.6641 0.2210 0.0406 0.024 Uiso 1 1 calc R . .
H2B H 0.6948 0.1812 0.0839 0.024 Uiso 1 1 calc R . .
N3 N 0.3833(4) 0.2642(3) 0.0618(4) 0.0152(19) Uani 1 1 d . . .
N4 N 0.3649(5) 0.3409(4) 0.1503(4) 0.024(2) Uani 1 1 d . . .
H4A H 0.3744 0.3619 0.1847 0.029 Uiso 1 1 calc R . .
H4B H 0.3620 0.3626 0.1154 0.029 Uiso 1 1 calc R . .
N5 N 0.5074(4) 0.2186(3) 0.1253(4) 0.016(2) Uani 1 1 d . . .
N6 N 0.4060(5) 0.2292(4) 0.2063(4) 0.025(2) Uani 1 1 d . . .
H6A H 0.3715 0.2458 0.2271 0.030 Uiso 1 1 calc R . .
H6B H 0.3885 0.1998 0.1861 0.030 Uiso 1 1 calc R . .
N7 N 0.4601(5) 0.0804(4) 0.0837(4) 0.022(2) Uani 1 1 d . . .
H7A H 0.4742 0.0496 0.0986 0.026 Uiso 1 1 calc R . .
N8 N 0.2764(6) 0.1161(5) 0.1597(6) 0.065(4) Uani 1 1 d . . .
H8A H 0.2353 0.1179 0.1741 0.078 Uiso 1 1 calc R . .
H8B H 0.2872 0.1332 0.1250 0.078 Uiso 1 1 calc R . .
N9 N 0.6699(5) 0.3068(4) -0.1853(4) 0.025(2) Uani 1 1 d . . .
H9A H 0.6602 0.2712 -0.1802 0.030 Uiso 1 1 calc R . .
H9B H 0.6913 0.3107 -0.2233 0.030 Uiso 1 1 calc R . .
N10 N 0.5742(4) 0.3277(4) -0.0962(4) 0.020(2) Uani 1 1 d . . .
N11 N 0.2664(6) 0.3970(6) -0.2738(8) 0.093(6) Uani 1 1 d . . .
H11A H 0.2794 0.3838 -0.2373 0.112 Uiso 1 1 calc R . .
H11B H 0.2236 0.3990 -0.2831 0.112 Uiso 1 1 calc R . .
N12 N 0.4584(5) 0.4155(4) -0.2189(4) 0.029(2) Uani 1 1 d . . .
H12A H 0.4703 0.4472 -0.2324 0.035 Uiso 1 1 calc R . .
N13 N 0.3971(5) 0.2655(4) -0.3401(4) 0.025(2) Uani 1 1 d . . .
H13A H 0.3610 0.2498 -0.3598 0.030 Uiso 1 1 calc R . .
H13B H 0.3821 0.2954 -0.3195 0.030 Uiso 1 1 calc R . .
N14 N 0.5025(5) 0.2742(4) -0.2633(4) 0.022(2) Uani 1 1 d . . .
N15 N 0.5844(5) 0.1692(4) -0.4302(4) 0.030(2) Uani 1 1 d . . .
H15A H 0.5495 0.1862 -0.4151 0.036 Uiso 1 1 calc R . .
H15B H 0.5981 0.1758 -0.4688 0.036 Uiso 1 1 calc R . .
N16 N 0.5439(4) 0.1447(4) -0.2388(4) 0.021(2) Uani 1 1 d . . .
H16A H 0.5760 0.1287 -0.2174 0.025 Uiso 1 1 calc R . .
N17 N 0.3589(5) 0.1541(4) -0.2857(4) 0.023(2) Uani 1 1 d . . .
H17A H 0.3673 0.1332 -0.3205 0.028 Uiso 1 1 calc R . .
H17B H 0.3565 0.1323 -0.2510 0.028 Uiso 1 1 calc R . .
N18 N 0.3795(4) 0.2309(4) -0.1972(4) 0.019(2) Uani 1 1 d . . .
N19 N 0.5475(5) 0.3517(4) 0.1007(4) 0.026(2) Uani 1 1 d . . .
H19A H 0.5783 0.3685 0.0789 0.032 Uiso 1 1 calc R . .
N20 N 0.5872(5) 0.3320(4) 0.2958(4) 0.027(2) Uani 1 1 d . . .
H20A H 0.6000 0.3265 0.3350 0.032 Uiso 1 1 calc R . .
H20B H 0.5535 0.3138 0.2799 0.032 Uiso 1 1 calc R . .
C1 C 0.6217(5) 0.1806(4) -0.0824(5) 0.019(2) Uani 1 1 d . . .
C2 C 0.6900(5) 0.1635(4) -0.0676(5) 0.017(2) Uani 1 1 d . . .
C3 C 0.7161(6) 0.1675(5) -0.0038(6) 0.030(3) Uani 1 1 d . . .
C4 C 0.7813(6) 0.1532(5) 0.0079(5) 0.031(3) Uani 1 1 d . . .
H4 H 0.7982 0.1548 0.0498 0.037 Uiso 1 1 calc R . .
C5 C 0.8233(7) 0.1362(6) -0.0410(6) 0.042(4) Uani 1 1 d . . .
H5 H 0.8687 0.1276 -0.0326 0.050 Uiso 1 1 calc R . .
C6 C 0.7978(6) 0.1323(6) -0.1013(6) 0.039(3) Uani 1 1 d . . .
H6 H 0.8249 0.1191 -0.1345 0.047 Uiso 1 1 calc R . .
C7 C 0.7335(6) 0.1474(5) -0.1132(5) 0.034(3) Uani 1 1 d . . .
H7 H 0.7181 0.1468 -0.1556 0.040 Uiso 1 1 calc R . .
C8 C 0.3209(6) 0.2664(4) 0.0558(5) 0.022(3) Uani 1 1 d . . .
C9 C 0.2802(6) 0.2767(4) 0.1130(5) 0.021(2) Uani 1 1 d . . .
C10 C 0.2218(5) 0.2513(5) 0.1228(5) 0.023(3) Uani 1 1 d . . .
H10 H 0.2055 0.2273 0.0917 0.028 Uiso 1 1 calc R . .
C11 C 0.1850(6) 0.2594(4) 0.1767(5) 0.023(2) Uani 1 1 d . . .
H11 H 0.1437 0.2413 0.1823 0.028 Uiso 1 1 calc R . .
C12 C 0.2093(6) 0.2946(5) 0.2234(5) 0.029(3) Uani 1 1 d . . .
H12 H 0.1853 0.2996 0.2615 0.035 Uiso 1 1 calc R . .
C13 C 0.2672(5) 0.3212(4) 0.2134(5) 0.018(2) Uani 1 1 d . . .
H13 H 0.2828 0.3455 0.2446 0.022 Uiso 1 1 calc R . .
C14 C 0.3044(5) 0.3141(4) 0.1592(5) 0.020(2) Uani 1 1 d . . .
C15 C 0.5326(6) 0.1822(5) 0.1626(5) 0.024(3) Uani 1 1 d . . .
C16 C 0.5156(5) 0.1892(4) 0.2304(5) 0.017(2) Uani 1 1 d . . .
C17 C 0.5604(6) 0.1730(5) 0.2763(5) 0.026(3) Uani 1 1 d . . .
H17 H 0.6014 0.1571 0.2638 0.032 Uiso 1 1 calc R . .
C18 C 0.5477(6) 0.1791(6) 0.3390(5) 0.035(3) Uani 1 1 d . . .
H18 H 0.5787 0.1659 0.3693 0.041 Uiso 1 1 calc R . .
C19 C 0.4921(7) 0.2035(6) 0.3578(5) 0.043(4) Uani 1 1 d . . .
H19 H 0.4853 0.2095 0.4015 0.052 Uiso 1 1 calc R . .
C20 C 0.4428(6) 0.2208(6) 0.3140(5) 0.035(3) Uani 1 1 d . . .
H20 H 0.4033 0.2383 0.3278 0.042 Uiso 1 1 calc R . .
C21 C 0.4534(6) 0.2117(5) 0.2514(5) 0.027(3) Uani 1 1 d . . .
C22 C 0.4120(6) 0.1062(5) 0.1119(5) 0.028(3) Uani 1 1 d . . .
C23 C 0.3893(6) 0.0826(4) 0.1732(5) 0.022(3) Uani 1 1 d . . .
C24 C 0.3237(7) 0.0864(4) 0.1914(6) 0.034(3) Uani 1 1 d . . .
C25 C 0.3057(7) 0.0604(5) 0.2449(6) 0.037(3) Uani 1 1 d . . .
H25 H 0.2602 0.0616 0.2574 0.044 Uiso 1 1 calc R . .
C26 C 0.3502(8) 0.0324(6) 0.2817(6) 0.046(4) Uani 1 1 d . . .
H26 H 0.3353 0.0154 0.3191 0.055 Uiso 1 1 calc R . .
C27 C 0.4141(9) 0.0291(6) 0.2651(7) 0.059(5) Uani 1 1 d . . .
H27 H 0.4456 0.0098 0.2897 0.071 Uiso 1 1 calc R . .
C28 C 0.4331(7) 0.0554(6) 0.2095(5) 0.038(3) Uani 1 1 d . . .
H28 H 0.4786 0.0540 0.1971 0.046 Uiso 1 1 calc R . .
C29 C 0.6206(6) 0.3123(4) -0.0569(5) 0.024(3) Uani 1 1 d . . .
C30 C 0.6917(6) 0.3274(5) -0.0750(5) 0.026(3) Uani 1 1 d . . .
C31 C 0.7364(6) 0.3424(6) -0.0279(6) 0.041(4) Uani 1 1 d . . .
H31 H 0.7218 0.3424 0.0146 0.049 Uiso 1 1 calc R . .
C32 C 0.8022(6) 0.3573(6) -0.0408(6) 0.040(3) Uani 1 1 d . . .
H32 H 0.8321 0.3682 -0.0083 0.049 Uiso 1 1 calc R . .
C33 C 0.8216(6) 0.3555(6) -0.1028(6) 0.038(3) Uani 1 1 d . . .
H33 H 0.8653 0.3672 -0.1135 0.045 Uiso 1 1 calc R . .
C34 C 0.7795(6) 0.3373(5) -0.1504(5) 0.031(3) Uani 1 1 d . . .
H34 H 0.7952 0.3345 -0.1925 0.037 Uiso 1 1 calc R . .
C35 C 0.7142(6) 0.3231(5) -0.1361(5) 0.027(3) Uani 1 1 d . . .
C36 C 0.3154(6) 0.2294(4) -0.1896(5) 0.020(2) Uani 1 1 d . . .
C37 C 0.2747(5) 0.2196(4) -0.2480(5) 0.019(2) Uani 1 1 d . . .
C38 C 0.2194(6) 0.2482(5) -0.2585(5) 0.023(3) Uani 1 1 d . . .
H38 H 0.2044 0.2721 -0.2268 0.027 Uiso 1 1 calc R . .
C39 C 0.1834(6) 0.2439(4) -0.3139(5) 0.026(3) Uani 1 1 d . . .
H39 H 0.1438 0.2642 -0.3200 0.031 Uiso 1 1 calc R . .
C40 C 0.2052(6) 0.2102(5) -0.3598(5) 0.022(3) Uani 1 1 d . . .
H40 H 0.1813 0.2078 -0.3985 0.027 Uiso 1 1 calc R . .
C41 C 0.2621(5) 0.1793(4) -0.3506(5) 0.019(2) Uani 1 1 d . . .
H41 H 0.2769 0.1560 -0.3830 0.023 Uiso 1 1 calc R . .
C42 C 0.2975(6) 0.1823(4) -0.2940(5) 0.023(3) Uani 1 1 d . . .
C43 C 0.4095(6) 0.3883(5) -0.2464(5) 0.027(3) Uani 1 1 d . . .
C44 C 0.3807(7) 0.4135(5) -0.3071(6) 0.031(3) Uani 1 1 d . . .
C45 C 0.3139(8) 0.4149(5) -0.3170(6) 0.046(4) Uani 1 1 d . . .
C46 C 0.2906(9) 0.4402(6) -0.3711(6) 0.050(4) Uani 1 1 d . . .
H46 H 0.2438 0.4436 -0.3778 0.060 Uiso 1 1 calc R . .
C47 C 0.3319(9) 0.4596(7) -0.4130(7) 0.063(5) Uani 1 1 d . . .
H47 H 0.3149 0.4767 -0.4496 0.075 Uiso 1 1 calc R . .
C48 C 0.4011(9) 0.4550(7) -0.4039(7) 0.073(6) Uani 1 1 d . . .
H48 H 0.4305 0.4674 -0.4356 0.087 Uiso 1 1 calc R . .
C49 C 0.4262(8) 0.4336(7) -0.3516(6) 0.061(5) Uani 1 1 d . . .
H49 H 0.4731 0.4319 -0.3446 0.073 Uiso 1 1 calc R . .
C50 C 0.5261(5) 0.3098(4) -0.3007(5) 0.018(2) Uiso 1 1 d . . .
C51 C 0.5078(7) 0.3045(5) -0.3686(5) 0.029(3) Uani 1 1 d . . .
C52 C 0.4434(6) 0.2807(5) -0.3856(5) 0.029(3) Uani 1 1 d . . .
C53 C 0.4294(7) 0.2759(6) -0.4499(5) 0.036(3) Uani 1 1 d . . .
H53 H 0.3879 0.2612 -0.4631 0.043 Uiso 1 1 calc R . .
C54 C 0.4750(8) 0.2924(6) -0.4944(6) 0.047(4) Uani 1 1 d . . .
H54 H 0.4633 0.2890 -0.5376 0.057 Uiso 1 1 calc R . .
C55 C 0.5374(7) 0.3138(6) -0.4790(6) 0.043(4) Uani 1 1 d . . .
H55 H 0.5686 0.3235 -0.5106 0.051 Uiso 1 1 calc R . .
C56 C 0.5522(7) 0.3202(5) -0.4144(5) 0.034(3) Uani 1 1 d . . .
H56 H 0.5936 0.3357 -0.4022 0.041 Uiso 1 1 calc R . .
C57 C 0.5456(6) 0.1459(4) -0.3015(5) 0.020(2) Uani 1 1 d . . .
C58 C 0.6010(6) 0.1182(5) -0.3319(5) 0.027(3) Uani 1 1 d . . .
C59 C 0.6167(6) 0.1333(5) -0.3945(5) 0.027(3) Uani 1 1 d . . .
C60 C 0.6747(6) 0.1062(5) -0.4193(6) 0.039(3) Uani 1 1 d . . .
H60 H 0.6879 0.1141 -0.4612 0.047 Uiso 1 1 calc R . .
C61 C 0.7116(6) 0.0702(5) -0.3863(6) 0.032(3) Uani 1 1 d . . .
H61 H 0.7505 0.0549 -0.4044 0.039 Uiso 1 1 calc R . .
C62 C 0.6933(7) 0.0566(5) -0.3293(6) 0.038(3) Uani 1 1 d . . .
H62 H 0.7184 0.0305 -0.3069 0.045 Uiso 1 1 calc R . .
C63 C 0.6375(6) 0.0798(4) -0.3008(5) 0.027(3) Uani 1 1 d . . .
H63 H 0.6247 0.0689 -0.2597 0.032 Uiso 1 1 calc R . .
C64 C 0.5495(5) 0.3508(5) 0.1655(5) 0.020(2) Uani 1 1 d . . .
C65 C 0.6025(6) 0.3814(5) 0.1959(5) 0.029(3) Uani 1 1 d . . .
C66 C 0.6374(6) 0.4204(4) 0.1661(6) 0.031(3) Uani 1 1 d . . .
H66 H 0.6259 0.4288 0.1238 0.037 Uiso 1 1 calc R . .
C67 C 0.6899(7) 0.4491(5) 0.1952(6) 0.047(4) Uani 1 1 d . . .
H67 H 0.7127 0.4772 0.1742 0.056 Uiso 1 1 calc R . .
C68 C 0.7058(7) 0.4343(5) 0.2545(7) 0.044(4) Uani 1 1 d . . .
H68 H 0.7425 0.4513 0.2747 0.053 Uiso 1 1 calc R . .
C69 C 0.6721(7) 0.3966(5) 0.2864(6) 0.036(3) Uani 1 1 d . . .
H69 H 0.6850 0.3889 0.3285 0.043 Uiso 1 1 calc R . .
C70 C 0.6194(6) 0.3686(4) 0.2600(5) 0.024(3) Uani 1 1 d . . .
C80 C 0.4641(13) 0.3701(11) -0.6484(12) 0.126(9) Uiso 1 1 d . . .
H80A H 0.4236 0.3582 -0.6705 0.190 Uiso 1 1 calc R . .
H80B H 0.4525 0.3815 -0.6057 0.190 Uiso 1 1 calc R . .
H80C H 0.4962 0.3406 -0.6462 0.190 Uiso 1 1 calc R . .
C81 C 0.3418(9) 0.0410(8) -0.4143(8) 0.078(5) Uiso 1 1 d . . .
H81A H 0.3586 0.0126 -0.3868 0.117 Uiso 1 1 calc R . .
H81B H 0.3498 0.0315 -0.4584 0.117 Uiso 1 1 calc R . .
H81C H 0.2937 0.0456 -0.4075 0.117 Uiso 1 1 calc R . .
Cl1 Cl 0.6337(4) -0.0022(3) -0.1260(4) 0.130(2) Uiso 1 1 d D . .
O50 O 0.5859(12) -0.0350(10) -0.1657(11) 0.227(11) Uiso 1 1 d D . .
O51 O 0.6943(11) 0.0004(12) -0.1696(12) 0.248(13) Uiso 1 1 d D . .
O53 O 0.6742(18) 0.0049(18) -0.0655(12) 0.37(2) Uiso 1 1 d D . .
O52 O 0.5978(11) 0.0493(7) -0.1447(11) 0.202(10) 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
Ni1 O2 2.034(8) . ?
Ni1 N1 2.035(9) . ?
Ni1 O1 2.046(7) . ?
Ni1 O3 2.052(8) . ?
Ni1 N2 2.110(9) . ?
Ni1 O7 2.145(7) . ?
Ni1 Ni3 2.940(2) . ?
Ni2 O4 2.042(7) . ?
Ni2 N3 2.051(9) . ?
Ni2 O5 2.059(7) . ?
Ni2 N5 2.061(9) . ?
Ni2 N6 2.119(9) . ?
Ni2 N4 2.170(9) . ?
Ni3 O7 1.999(7) . ?
Ni3 O15 2.046(7) . ?
Ni3 O9 2.048(8) . ?
Ni3 O6 2.048(7) . ?
Ni3 O2 2.108(7) . ?
Ni3 O10 2.111(7) . ?
Ni3 Ni4 2.847(2) . ?
Ni4 O20 1.967(7) . ?
Ni4 O19 1.979(7) . ?
Ni4 O2 2.006(7) . ?
Ni4 O5 2.028(7) . ?
Ni4 O9 2.057(8) . ?
Ni5 O12 1.982(7) . ?
Ni5 O8 1.986(7) . ?
Ni5 O9 1.987(8) . ?
Ni5 O11 1.996(7) . ?
Ni5 O10 2.204(8) . ?
Ni5 O23 2.204(8) . ?
Ni6 O15 1.960(7) . ?
Ni6 O18 1.970(7) . ?
Ni6 O16 1.988(7) . ?
Ni6 O22 2.023(7) . ?
Ni6 O12 2.047(8) . ?
Ni6 Ni7 2.842(2) . ?
Ni7 O14 2.017(8) . ?
Ni7 O19 2.036(7) . ?
Ni7 O12 2.051(8) . ?
Ni7 O13 2.053(8) . ?
Ni7 O16 2.103(7) . ?
Ni7 O23 2.105(7) . ?
Ni7 Ni9 2.950(2) . ?
Ni8 O21 2.038(7) . ?
Ni8 N18 2.049(9) . ?
Ni8 N14 2.051(10) . ?
Ni8 O22 2.066(7) . ?
Ni8 N13 2.107(9) . ?
Ni8 N17 2.143(10) . ?
Ni9 O16 2.023(7) . ?
Ni9 N10 2.034(8) . ?
Ni9 O17 2.041(8) . ?
Ni9 O24 2.071(7) . ?
Ni9 N9 2.099(10) . ?
Ni9 O14 2.127(8) . ?
Cl2 O57 1.52(2) . ?
Cl2 O55 1.53(3) . ?
Cl2 O54 1.62(4) . ?
Cl2 O56 1.69(3) . ?
O1 C15 1.293(13) . ?
O2 N5 1.404(10) . ?
O4 C64 1.234(13) . ?
O5 N19 1.380(11) . ?
O6 C22 1.262(14) . ?
O7 N7 1.416(10) . ?
O8 C8 1.324(13) . ?
O9 N3 1.451(10) . ?
O10 H10A 0.9900 . ?
O10 H10B 0.9900 . ?
O11 C36 1.278(13) . ?
O12 N18 1.457(11) . ?
O13 C43 1.241(14) . ?
O14 N12 1.380(11) . ?
O15 N1 1.409(11) . ?
O16 N14 1.437(10) . ?
O18 C1 1.289(12) . ?
O19 N10 1.407(11) . ?
O20 C29 1.270(12) . ?
O21 C57 1.270(13) . ?
O22 N16 1.406(11) . ?
O23 H23A 0.9900 . ?
O23 H23B 0.9900 . ?
O24 C50 1.305(13) . ?
O61 C80 1.51(3) . ?
O61 H61A 0.8400 . ?
O64 C81 1.42(2) . ?
O64 H64 0.8400 . ?
N1 C1 1.337(14) . ?
N2 C3 1.438(14) . ?
N2 H2A 0.9200 . ?
N2 H2B 0.9200 . ?
N3 C8 1.254(14) . ?
N4 C14 1.397(14) . ?
N4 H4A 0.9200 . ?
N4 H4B 0.9200 . ?
N5 C15 1.307(14) . ?
N6 C21 1.415(14) . ?
N6 H6A 0.9200 . ?
N6 H6B 0.9200 . ?
N7 C22 1.306(15) . ?
N7 H7A 0.8800 . ?
N8 C24 1.377(17) . ?
N8 H8A 0.8800 . ?
N8 H8B 0.8800 . ?
N9 C35 1.424(14) . ?
N9 H9A 0.9200 . ?
N9 H9B 0.9200 . ?
N10 C29 1.303(14) . ?
N11 C45 1.40(2) . ?
N11 H11A 0.8800 . ?
N11 H11B 0.8800 . ?
N12 C43 1.326(15) . ?
N12 H12A 0.8800 . ?
N13 C52 1.394(14) . ?
N13 H13A 0.9200 . ?
N13 H13B 0.9200 . ?
N14 C50 1.286(13) . ?
N15 C59 1.340(15) . ?
N15 H15A 0.8800 . ?
N15 H15B 0.8800 . ?
N16 C57 1.331(13) . ?
N16 H16A 0.8800 . ?
N17 C42 1.428(14) . ?
N17 H17A 0.9200 . ?
N17 H17B 0.9200 . ?
N18 C36 1.293(14) . ?
N19 C64 1.376(14) . ?
N19 H19A 0.8800 . ?
N20 C70 1.356(14) . ?
N20 H20A 0.8800 . ?
N20 H20B 0.8800 . ?
C1 C2 1.464(15) . ?
C2 C7 1.367(15) . ?
C2 C3 1.451(16) . ?
C3 C4 1.372(16) . ?
C4 C5 1.406(16) . ?
C4 H4 0.9500 . ?
C5 C6 1.378(17) . ?
C5 H5 0.9500 . ?
C6 C7 1.363(17) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.488(14) . ?
C9 C10 1.348(16) . ?
C9 C14 1.439(15) . ?
C10 C11 1.377(15) . ?
C10 H10 0.9500 . ?
C11 C12 1.413(16) . ?
C11 H11 0.9500 . ?
C12 C13 1.354(15) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(14) . ?
C13 H13 0.9500 . ?
C15 C16 1.491(15) . ?
C16 C17 1.381(15) . ?
C16 C21 1.439(15) . ?
C17 C18 1.364(15) . ?
C17 H17 0.9500 . ?
C18 C19 1.334(18) . ?
C18 H18 0.9500 . ?
C19 C20 1.419(18) . ?
C19 H19 0.9500 . ?
C20 C21 1.365(16) . ?
C20 H20 0.9500 . ?
C22 C23 1.501(15) . ?
C23 C28 1.347(17) . ?
C23 C24 1.373(16) . ?
C24 C25 1.360(17) . ?
C25 C26 1.373(19) . ?
C25 H25 0.9500 . ?
C26 C27 1.33(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.405(18) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.523(15) . ?
C30 C35 1.379(15) . ?
C30 C31 1.390(17) . ?
C31 C32 1.397(17) . ?
C31 H31 0.9500 . ?
C32 C33 1.375(17) . ?
C32 H32 0.9500 . ?
C33 C34 1.389(17) . ?
C33 H33 0.9500 . ?
C34 C35 1.390(16) . ?
C34 H34 0.9500 . ?
C36 C37 1.499(14) . ?
C37 C38 1.336(15) . ?
C37 C42 1.427(14) . ?
C38 C39 1.380(15) . ?
C38 H38 0.9500 . ?
C39 C40 1.364(15) . ?
C39 H39 0.9500 . ?
C40 C41 1.389(15) . ?
C40 H40 0.9500 . ?
C41 C42 1.394(14) . ?
C41 H41 0.9500 . ?
C43 C44 1.543(16) . ?
C44 C45 1.353(19) . ?
C44 C49 1.410(19) . ?
C45 C46 1.390(18) . ?
C46 C47 1.31(2) . ?
C46 H46 0.9500 . ?
C47 C48 1.40(2) . ?
C47 H47 0.9500 . ?
C48 C49 1.33(2) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C51 1.491(15) . ?
C51 C56 1.378(17) . ?
C51 C52 1.462(18) . ?
C52 C53 1.397(16) . ?
C53 C54 1.379(18) . ?
C53 H53 0.9500 . ?
C54 C55 1.40(2) . ?
C54 H54 0.9500 . ?
C55 C56 1.411(16) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C58 1.461(15) . ?
C58 C63 1.375(16) . ?
C58 C59 1.420(16) . ?
C59 C60 1.447(16) . ?
C60 C61 1.358(17) . ?
C60 H60 0.9500 . ?
C61 C62 1.311(17) . ?
C61 H61 0.9500 . ?
C62 C63 1.400(17) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 C65 1.455(16) . ?
C65 C66 1.358(15) . ?
C65 C70 1.439(16) . ?
C66 C67 1.413(17) . ?
C66 H66 0.9500 . ?
C67 C68 1.349(18) . ?
C67 H67 0.9500 . ?
C68 C69 1.345(18) . ?
C68 H68 0.9500 . ?
C69 C70 1.380(16) . ?
C69 H69 0.9500 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
Cl1 O50 1.513(10) . ?
Cl1 O53 1.525(10) . ?
Cl1 O52 1.528(10) . ?
Cl1 O51 1.530(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 Ni1 N1 82.4(3) . . ?
O2 Ni1 O1 77.7(3) . . ?
N1 Ni1 O1 160.0(3) . . ?
O2 Ni1 O3 172.8(3) . . ?
N1 Ni1 O3 101.7(3) . . ?
O1 Ni1 O3 98.0(3) . . ?
O2 Ni1 N2 94.9(3) . . ?
N1 Ni1 N2 84.5(3) . . ?
O1 Ni1 N2 97.7(3) . . ?
O3 Ni1 N2 91.3(3) . . ?
O2 Ni1 O7 85.4(3) . . ?
N1 Ni1 O7 82.9(3) . . ?
O1 Ni1 O7 94.8(3) . . ?
O3 Ni1 O7 89.2(3) . . ?
N2 Ni1 O7 167.3(3) . . ?
O2 Ni1 Ni3 45.8(2) . . ?
N1 Ni1 Ni3 66.8(2) . . ?
O1 Ni1 Ni3 98.1(2) . . ?
O3 Ni1 Ni3 130.4(2) . . ?
N2 Ni1 Ni3 132.1(3) . . ?
O7 Ni1 Ni3 42.8(2) . . ?
O4 Ni2 N3 160.1(3) . . ?
O4 Ni2 O5 79.5(3) . . ?
N3 Ni2 O5 83.1(3) . . ?
O4 Ni2 N5 94.2(3) . . ?
N3 Ni2 N5 95.4(3) . . ?
O5 Ni2 N5 90.3(3) . . ?
O4 Ni2 N6 97.8(3) . . ?
N3 Ni2 N6 101.0(3) . . ?
O5 Ni2 N6 169.4(3) . . ?
N5 Ni2 N6 79.7(3) . . ?
O4 Ni2 N4 92.4(3) . . ?
N3 Ni2 N4 80.0(3) . . ?
O5 Ni2 N4 95.9(3) . . ?
N5 Ni2 N4 171.7(4) . . ?
N6 Ni2 N4 94.4(4) . . ?
O7 Ni3 O15 89.7(3) . . ?
O7 Ni3 O9 168.6(3) . . ?
O15 Ni3 O9 86.5(3) . . ?
O7 Ni3 O6 81.5(3) . . ?
O15 Ni3 O6 170.7(3) . . ?
O9 Ni3 O6 101.5(3) . . ?
O7 Ni3 O2 87.3(3) . . ?
O15 Ni3 O2 79.1(3) . . ?
O9 Ni3 O2 81.4(3) . . ?
O6 Ni3 O2 97.2(3) . . ?
O7 Ni3 O10 109.7(3) . . ?
O15 Ni3 O10 92.1(3) . . ?
O9 Ni3 O10 81.2(3) . . ?
O6 Ni3 O10 93.8(3) . . ?
O2 Ni3 O10 161.0(3) . . ?
O7 Ni3 Ni4 123.2(2) . . ?
O15 Ni3 Ni4 58.3(2) . . ?
O9 Ni3 Ni4 46.2(2) . . ?
O6 Ni3 Ni4 124.6(2) . . ?
O2 Ni3 Ni4 44.74(19) . . ?
O10 Ni3 Ni4 116.4(2) . . ?
O7 Ni3 Ni1 46.8(2) . . ?
O15 Ni3 Ni1 68.7(2) . . ?
O9 Ni3 Ni1 121.9(2) . . ?
O6 Ni3 Ni1 102.7(2) . . ?
O2 Ni3 Ni1 43.8(2) . . ?
O10 Ni3 Ni1 147.2(2) . . ?
Ni4 Ni3 Ni1 76.84(5) . . ?
O20 Ni4 O19 81.8(3) . . ?
O20 Ni4 O2 97.7(3) . . ?
O19 Ni4 O2 156.3(3) . . ?
O20 Ni4 O5 98.2(3) . . ?
O19 Ni4 O5 108.1(3) . . ?
O2 Ni4 O5 95.4(3) . . ?
O20 Ni4 O9 173.2(3) . . ?
O19 Ni4 O9 94.3(3) . . ?
O2 Ni4 O9 83.7(3) . . ?
O5 Ni4 O9 88.2(3) . . ?
O20 Ni4 Ni3 131.3(2) . . ?
O19 Ni4 Ni3 116.2(2) . . ?
O2 Ni4 Ni3 47.7(2) . . ?
O5 Ni4 Ni3 115.5(2) . . ?
O9 Ni4 Ni3 46.0(2) . . ?
O12 Ni5 O8 176.4(3) . . ?
O12 Ni5 O9 98.8(3) . . ?
O8 Ni5 O9 81.1(3) . . ?
O12 Ni5 O11 81.1(3) . . ?
O8 Ni5 O11 99.2(3) . . ?
O9 Ni5 O11 175.4(3) . . ?
O12 Ni5 O10 90.0(3) . . ?
O8 Ni5 O10 93.6(3) . . ?
O9 Ni5 O10 80.3(3) . . ?
O11 Ni5 O10 95.1(3) . . ?
O12 Ni5 O23 80.2(3) . . ?
O8 Ni5 O23 96.2(3) . . ?
O9 Ni5 O23 91.4(3) . . ?
O11 Ni5 O23 93.0(3) . . ?
O10 Ni5 O23 166.1(3) . . ?
O15 Ni6 O18 82.2(3) . . ?
O15 Ni6 O16 157.1(3) . . ?
O18 Ni6 O16 98.1(3) . . ?
O15 Ni6 O22 106.6(3) . . ?
O18 Ni6 O22 96.4(3) . . ?
O16 Ni6 O22 96.1(3) . . ?
O15 Ni6 O12 94.1(3) . . ?
O18 Ni6 O12 174.7(3) . . ?
O16 Ni6 O12 83.9(3) . . ?
O22 Ni6 O12 88.3(3) . . ?
O15 Ni6 Ni7 116.8(2) . . ?
O18 Ni6 Ni7 132.6(2) . . ?
O16 Ni6 Ni7 47.7(2) . . ?
O22 Ni6 Ni7 116.0(2) . . ?
O12 Ni6 Ni7 46.1(2) . . ?
O14 Ni7 O19 89.9(3) . . ?
O14 Ni7 O12 167.1(3) . . ?
O19 Ni7 O12 86.2(3) . . ?
O14 Ni7 O13 81.1(3) . . ?
O19 Ni7 O13 170.6(3) . . ?
O12 Ni7 O13 101.9(3) . . ?
O14 Ni7 O16 86.1(3) . . ?
O19 Ni7 O16 77.9(3) . . ?
O12 Ni7 O16 81.0(3) . . ?
O13 Ni7 O16 98.4(3) . . ?
O14 Ni7 O23 111.5(3) . . ?
O19 Ni7 O23 94.4(3) . . ?
O12 Ni7 O23 81.1(3) . . ?
O13 Ni7 O23 91.7(3) . . ?
O16 Ni7 O23 160.9(3) . . ?
O14 Ni7 Ni6 122.1(2) . . ?
O19 Ni7 Ni6 57.6(2) . . ?
O12 Ni7 Ni6 46.0(2) . . ?
O13 Ni7 Ni6 125.3(2) . . ?
O16 Ni7 Ni6 44.34(19) . . ?
O23 Ni7 Ni6 116.9(2) . . ?
O14 Ni7 Ni9 46.1(2) . . ?
O19 Ni7 Ni9 68.24(19) . . ?
O12 Ni7 Ni9 121.2(2) . . ?
O13 Ni7 Ni9 103.1(2) . . ?
O16 Ni7 Ni9 43.3(2) . . ?
O23 Ni7 Ni9 148.9(2) . . ?
Ni6 Ni7 Ni9 76.41(5) . . ?
O21 Ni8 N18 161.0(3) . . ?
O21 Ni8 N14 92.4(3) . . ?
N18 Ni8 N14 95.8(3) . . ?
O21 Ni8 O22 80.2(3) . . ?
N18 Ni8 O22 82.7(3) . . ?
N14 Ni8 O22 89.7(3) . . ?
O21 Ni8 N13 98.6(3) . . ?
N18 Ni8 N13 99.7(3) . . ?
N14 Ni8 N13 79.8(4) . . ?
O22 Ni8 N13 169.4(3) . . ?
O21 Ni8 N17 92.8(3) . . ?
N18 Ni8 N17 80.9(3) . . ?
N14 Ni8 N17 172.8(4) . . ?
O22 Ni8 N17 96.2(3) . . ?
N13 Ni8 N17 94.4(3) . . ?
O16 Ni9 N10 81.5(3) . . ?
O16 Ni9 O17 171.7(3) . . ?
N10 Ni9 O17 104.8(3) . . ?
O16 Ni9 O24 78.3(3) . . ?
N10 Ni9 O24 159.8(3) . . ?
O17 Ni9 O24 95.3(3) . . ?
O16 Ni9 N9 95.2(3) . . ?
N10 Ni9 N9 83.4(3) . . ?
O17 Ni9 N9 90.9(3) . . ?
O24 Ni9 N9 97.9(3) . . ?
O16 Ni9 O14 85.3(3) . . ?
N10 Ni9 O14 83.7(3) . . ?
O17 Ni9 O14 90.0(3) . . ?
O24 Ni9 O14 95.1(3) . . ?
N9 Ni9 O14 166.9(3) . . ?
O16 Ni9 Ni7 45.4(2) . . ?
N10 Ni9 Ni7 66.8(2) . . ?
O17 Ni9 Ni7 131.9(2) . . ?
O24 Ni9 Ni7 98.7(2) . . ?
N9 Ni9 Ni7 131.8(3) . . ?
O14 Ni9 Ni7 43.1(2) . . ?
O57 Cl2 O55 136.0(13) . . ?
O57 Cl2 O54 111.6(16) . . ?
O55 Cl2 O54 99.6(16) . . ?
O57 Cl2 O56 108.6(15) . . ?
O55 Cl2 O56 105.4(16) . . ?
O54 Cl2 O56 82.5(16) . . ?
C15 O1 Ni1 111.8(7) . . ?
N5 O2 Ni4 116.1(5) . . ?
N5 O2 Ni1 114.8(5) . . ?
Ni4 O2 Ni1 125.9(3) . . ?
N5 O2 Ni3 111.6(5) . . ?
Ni4 O2 Ni3 87.6(3) . . ?
Ni1 O2 Ni3 90.4(3) . . ?
C64 O4 Ni2 114.6(7) . . ?
N19 O5 Ni4 119.7(6) . . ?
N19 O5 Ni2 108.6(5) . . ?
Ni4 O5 Ni2 103.7(3) . . ?
C22 O6 Ni3 111.2(7) . . ?
N7 O7 Ni3 107.5(5) . . ?
N7 O7 Ni1 112.8(5) . . ?
Ni3 O7 Ni1 90.3(3) . . ?
C8 O8 Ni5 109.3(6) . . ?
N3 O9 Ni5 111.0(5) . . ?
N3 O9 Ni3 105.4(5) . . ?
Ni5 O9 Ni3 103.0(3) . . ?
N3 O9 Ni4 112.6(5) . . ?
Ni5 O9 Ni4 130.1(3) . . ?
Ni3 O9 Ni4 87.8(3) . . ?
Ni3 O10 Ni5 94.1(3) . . ?
Ni3 O10 H10A 112.9 . . ?
Ni5 O10 H10A 112.9 . . ?
Ni3 O10 H10B 112.9 . . ?
Ni5 O10 H10B 112.9 . . ?
H10A O10 H10B 110.3 . . ?
C36 O11 Ni5 110.4(7) . . ?
N18 O12 Ni5 110.8(5) . . ?
N18 O12 Ni6 112.5(5) . . ?
Ni5 O12 Ni6 130.5(4) . . ?
N18 O12 Ni7 105.4(5) . . ?
Ni5 O12 Ni7 102.8(3) . . ?
Ni6 O12 Ni7 87.8(3) . . ?
C43 O13 Ni7 109.4(8) . . ?
N12 O14 Ni7 108.5(6) . . ?
N12 O14 Ni9 116.2(6) . . ?
Ni7 O14 Ni9 90.7(3) . . ?
N1 O15 Ni6 111.1(5) . . ?
N1 O15 Ni3 109.3(5) . . ?
Ni6 O15 Ni3 139.4(4) . . ?
N14 O16 Ni6 115.0(5) . . ?
N14 O16 Ni9 114.3(5) . . ?
Ni6 O16 Ni9 126.6(3) . . ?
N14 O16 Ni7 112.5(5) . . ?
Ni6 O16 Ni7 88.0(3) . . ?
Ni9 O16 Ni7 91.3(3) . . ?
C1 O18 Ni6 111.2(6) . . ?
N10 O19 Ni4 110.9(5) . . ?
N10 O19 Ni7 110.2(5) . . ?
Ni4 O19 Ni7 138.9(4) . . ?
C29 O20 Ni4 109.4(7) . . ?
C57 O21 Ni8 113.3(7) . . ?
N16 O22 Ni6 117.6(6) . . ?
N16 O22 Ni8 106.8(5) . . ?
Ni6 O22 Ni8 103.7(3) . . ?
Ni7 O23 Ni5 94.0(3) . . ?
Ni7 O23 H23A 112.9 . . ?
Ni5 O23 H23A 112.9 . . ?
Ni7 O23 H23B 112.9 . . ?
Ni5 O23 H23B 112.9 . . ?
H23A O23 H23B 110.3 . . ?
C50 O24 Ni9 110.3(6) . . ?
C80 O61 H61A 109.5 . . ?
C81 O64 H64 109.5 . . ?
C1 N1 O15 113.2(8) . . ?
C1 N1 Ni1 128.0(7) . . ?
O15 N1 Ni1 113.9(6) . . ?
C3 N2 Ni1 112.7(7) . . ?
C3 N2 H2A 109.0 . . ?
Ni1 N2 H2A 109.0 . . ?
C3 N2 H2B 109.0 . . ?
Ni1 N2 H2B 109.0 . . ?
H2A N2 H2B 107.8 . . ?
C8 N3 O9 112.0(8) . . ?
C8 N3 Ni2 130.5(7) . . ?
O9 N3 Ni2 117.2(6) . . ?
C14 N4 Ni2 108.7(7) . . ?
C14 N4 H4A 109.9 . . ?
Ni2 N4 H4A 109.9 . . ?
C14 N4 H4B 109.9 . . ?
Ni2 N4 H4B 109.9 . . ?
H4A N4 H4B 108.3 . . ?
C15 N5 O2 111.0(8) . . ?
C15 N5 Ni2 134.7(7) . . ?
O2 N5 Ni2 114.0(6) . . ?
C21 N6 Ni2 115.1(7) . . ?
C21 N6 H6A 108.5 . . ?
Ni2 N6 H6A 108.5 . . ?
C21 N6 H6B 108.5 . . ?
Ni2 N6 H6B 108.5 . . ?
H6A N6 H6B 107.5 . . ?
C22 N7 O7 119.4(9) . . ?
C22 N7 H7A 120.3 . . ?
O7 N7 H7A 120.3 . . ?
C24 N8 H8A 120.0 . . ?
C24 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
C35 N9 Ni9 113.6(7) . . ?
C35 N9 H9A 108.8 . . ?
Ni9 N9 H9A 108.8 . . ?
C35 N9 H9B 108.8 . . ?
Ni9 N9 H9B 108.8 . . ?
H9A N9 H9B 107.7 . . ?
C29 N10 O19 111.4(8) . . ?
C29 N10 Ni9 130.6(7) . . ?
O19 N10 Ni9 113.5(5) . . ?
C45 N11 H11A 120.0 . . ?
C45 N11 H11B 120.0 . . ?
H11A N11 H11B 120.0 . . ?
C43 N12 O14 117.1(10) . . ?
C43 N12 H12A 121.4 . . ?
O14 N12 H12A 121.4 . . ?
C52 N13 Ni8 112.9(8) . . ?
C52 N13 H13A 109.0 . . ?
Ni8 N13 H13A 109.0 . . ?
C52 N13 H13B 109.0 . . ?
Ni8 N13 H13B 109.0 . . ?
H13A N13 H13B 107.8 . . ?
C50 N14 O16 110.9(9) . . ?
C50 N14 Ni8 134.5(7) . . ?
O16 N14 Ni8 114.1(6) . . ?
C59 N15 H15A 120.0 . . ?
C59 N15 H15B 120.0 . . ?
H15A N15 H15B 120.0 . . ?
C57 N16 O22 119.6(8) . . ?
C57 N16 H16A 120.2 . . ?
O22 N16 H16A 120.2 . . ?
C42 N17 Ni8 107.8(7) . . ?
C42 N17 H17A 110.1 . . ?
Ni8 N17 H17A 110.1 . . ?
C42 N17 H17B 110.1 . . ?
Ni8 N17 H17B 110.1 . . ?
H17A N17 H17B 108.5 . . ?
C36 N18 O12 111.6(8) . . ?
C36 N18 Ni8 130.8(7) . . ?
O12 N18 Ni8 117.4(6) . . ?
C64 N19 O5 117.9(8) . . ?
C64 N19 H19A 121.0 . . ?
O5 N19 H19A 121.0 . . ?
C70 N20 H20A 120.0 . . ?
C70 N20 H20B 120.0 . . ?
H20A N20 H20B 120.0 . . ?
O18 C1 N1 121.7(10) . . ?
O18 C1 C2 120.6(9) . . ?
N1 C1 C2 117.6(10) . . ?
C7 C2 C3 116.9(10) . . ?
C7 C2 C1 122.1(10) . . ?
C3 C2 C1 120.8(10) . . ?
C4 C3 N2 121.3(11) . . ?
C4 C3 C2 119.2(11) . . ?
N2 C3 C2 119.4(10) . . ?
C3 C4 C5 121.1(11) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 119.2(12) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C7 C6 C5 119.7(12) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C7 C2 123.8(11) . . ?
C6 C7 H7 118.1 . . ?
C2 C7 H7 118.1 . . ?
N3 C8 O8 125.6(9) . . ?
N3 C8 C9 118.2(10) . . ?
O8 C8 C9 115.9(10) . . ?
C10 C9 C14 119.4(10) . . ?
C10 C9 C8 121.6(10) . . ?
C14 C9 C8 119.0(10) . . ?
C9 C10 C11 121.8(11) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C10 C11 C12 119.4(11) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 119.2(10) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 122.1(10) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C13 C14 N4 121.4(10) . . ?
C13 C14 C9 118.0(10) . . ?
N4 C14 C9 120.6(9) . . ?
O1 C15 N5 124.7(10) . . ?
O1 C15 C16 120.9(10) . . ?
N5 C15 C16 114.3(10) . . ?
C17 C16 C21 117.1(9) . . ?
C17 C16 C15 119.8(10) . . ?
C21 C16 C15 123.2(10) . . ?
C18 C17 C16 122.1(11) . . ?
C18 C17 H17 118.9 . . ?
C16 C17 H17 118.9 . . ?
C19 C18 C17 120.2(12) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 121.5(11) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C21 C20 C19 118.3(12) . . ?
C21 C20 H20 120.8 . . ?
C19 C20 H20 120.8 . . ?
C20 C21 N6 119.9(11) . . ?
C20 C21 C16 120.5(11) . . ?
N6 C21 C16 119.3(9) . . ?
O6 C22 N7 120.3(10) . . ?
O6 C22 C23 124.1(11) . . ?
N7 C22 C23 115.5(11) . . ?
C28 C23 C24 119.5(10) . . ?
C28 C23 C22 119.7(10) . . ?
C24 C23 C22 120.7(11) . . ?
C25 C24 C23 117.4(12) . . ?
C25 C24 N8 118.8(12) . . ?
C23 C24 N8 123.7(11) . . ?
C24 C25 C26 123.1(12) . . ?
C24 C25 H25 118.5 . . ?
C26 C25 H25 118.5 . . ?
C27 C26 C25 120.1(12) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 117.3(15) . . ?
C26 C27 H27 121.4 . . ?
C28 C27 H27 121.4 . . ?
C23 C28 C27 122.6(13) . . ?
C23 C28 H28 118.7 . . ?
C27 C28 H28 118.7 . . ?
O20 C29 N10 126.1(10) . . ?
O20 C29 C30 118.6(10) . . ?
N10 C29 C30 115.3(9) . . ?
C35 C30 C31 119.0(10) . . ?
C35 C30 C29 121.9(10) . . ?
C31 C30 C29 118.9(9) . . ?
C30 C31 C32 122.4(11) . . ?
C30 C31 H31 118.8 . . ?
C32 C31 H31 118.8 . . ?
C33 C32 C31 116.7(12) . . ?
C33 C32 H32 121.7 . . ?
C31 C32 H32 121.7 . . ?
C32 C33 C34 122.3(12) . . ?
C32 C33 H33 118.8 . . ?
C34 C33 H33 118.8 . . ?
C33 C34 C35 119.4(11) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C30 C35 C34 119.9(11) . . ?
C30 C35 N9 120.5(10) . . ?
C34 C35 N9 119.6(10) . . ?
O11 C36 N18 125.4(9) . . ?
O11 C36 C37 118.7(10) . . ?
N18 C36 C37 115.8(9) . . ?
C38 C37 C42 120.3(10) . . ?
C38 C37 C36 119.6(9) . . ?
C42 C37 C36 119.9(9) . . ?
C37 C38 C39 121.8(10) . . ?
C37 C38 H38 119.1 . . ?
C39 C38 H38 119.1 . . ?
C40 C39 C38 119.4(11) . . ?
C40 C39 H39 120.3 . . ?
C38 C39 H39 120.3 . . ?
C39 C40 C41 120.7(10) . . ?
C39 C40 H40 119.7 . . ?
C41 C40 H40 119.7 . . ?
C40 C41 C42 120.2(10) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C41 C42 C37 117.6(10) . . ?
C41 C42 N17 120.7(9) . . ?
C37 C42 N17 121.2(9) . . ?
O13 C43 N12 123.2(11) . . ?
O13 C43 C44 121.4(11) . . ?
N12 C43 C44 115.3(10) . . ?
C45 C44 C49 121.9(13) . . ?
C45 C44 C43 120.3(12) . . ?
C49 C44 C43 117.8(12) . . ?
C44 C45 C46 117.8(15) . . ?
C44 C45 N11 124.4(12) . . ?
C46 C45 N11 117.5(15) . . ?
C47 C46 C45 121.3(16) . . ?
C47 C46 H46 119.3 . . ?
C45 C46 H46 119.3 . . ?
C46 C47 C48 120.1(14) . . ?
C46 C47 H47 119.9 . . ?
C48 C47 H47 119.9 . . ?
C49 C48 C47 121.2(15) . . ?
C49 C48 H48 119.4 . . ?
C47 C48 H48 119.4 . . ?
C48 C49 C44 117.4(16) . . ?
C48 C49 H49 121.3 . . ?
C44 C49 H49 121.3 . . ?
N14 C50 O24 126.0(9) . . ?
N14 C50 C51 116.4(10) . . ?
O24 C50 C51 117.5(9) . . ?
C56 C51 C52 120.8(11) . . ?
C56 C51 C50 120.1(12) . . ?
C52 C51 C50 119.1(10) . . ?
N13 C52 C53 121.4(12) . . ?
N13 C52 C51 121.9(11) . . ?
C53 C52 C51 116.6(11) . . ?
C54 C53 C52 120.8(13) . . ?
C54 C53 H53 119.6 . . ?
C52 C53 H53 119.6 . . ?
C53 C54 C55 123.3(13) . . ?
C53 C54 H54 118.3 . . ?
C55 C54 H54 118.3 . . ?
C54 C55 C56 116.9(13) . . ?
C54 C55 H55 121.6 . . ?
C56 C55 H55 121.6 . . ?
C51 C56 C55 121.4(14) . . ?
C51 C56 H56 119.3 . . ?
C55 C56 H56 119.3 . . ?
O21 C57 N16 119.0(10) . . ?
O21 C57 C58 124.0(10) . . ?
N16 C57 C58 117.0(10) . . ?
C63 C58 C59 121.1(11) . . ?
C63 C58 C57 121.5(10) . . ?
C59 C58 C57 117.3(10) . . ?
N15 C59 C58 126.9(11) . . ?
N15 C59 C60 119.7(11) . . ?
C58 C59 C60 113.4(11) . . ?
C61 C60 C59 124.0(12) . . ?
C61 C60 H60 118.0 . . ?
C59 C60 H60 118.0 . . ?
C62 C61 C60 119.6(11) . . ?
C62 C61 H61 120.2 . . ?
C60 C61 H61 120.2 . . ?
C61 C62 C63 121.3(11) . . ?
C61 C62 H62 119.4 . . ?
C63 C62 H62 119.4 . . ?
C58 C63 C62 120.4(11) . . ?
C58 C63 H63 119.8 . . ?
C62 C63 H63 119.8 . . ?
O4 C64 N19 118.8(10) . . ?
O4 C64 C65 124.3(10) . . ?
N19 C64 C65 116.9(10) . . ?
C66 C65 C70 118.7(11) . . ?
C66 C65 C64 123.3(11) . . ?
C70 C65 C64 117.9(10) . . ?
C65 C66 C67 123.2(12) . . ?
C65 C66 H66 118.4 . . ?
C67 C66 H66 118.4 . . ?
C68 C67 C66 115.9(12) . . ?
C68 C67 H67 122.1 . . ?
C66 C67 H67 122.1 . . ?
C69 C68 C67 123.2(13) . . ?
C69 C68 H68 118.4 . . ?
C67 C68 H68 118.4 . . ?
C68 C69 C70 122.4(12) . . ?
C68 C69 H69 118.8 . . ?
C70 C69 H69 118.8 . . ?
N20 C70 C69 118.7(11) . . ?
N20 C70 C65 124.8(10) . . ?
C69 C70 C65 116.5(11) . . ?
O61 C80 H80A 109.5 . . ?
O61 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
O61 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
O64 C81 H81A 109.5 . . ?
O64 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
O64 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
O50 Cl1 O53 150(2) . . ?
O50 Cl1 O52 91.2(14) . . ?
O53 Cl1 O52 112(2) . . ?
O50 Cl1 O51 100.8(16) . . ?
O53 Cl1 O51 94.8(19) . . ?
O52 Cl1 O51 100.4(15) . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.129
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.138
_database_code_depnum_ccdc_archive 'CCDC 1009476'
