#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:20:41 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179105 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/67/4306739.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4306739
loop_
_publ_author_name
'Theocharis C. Stamatatos'
'Albert Escuer'
'Khalil A. Abboud'
'Catherine P. Raptopoulou'
'Spyros P. Perlepes'
'George Christou'
_publ_section_title
;
Unusual Structural Types in Nickel Cluster Chemistry from the Use of
Pyridyl Oximes: Ni5, Ni12Na2, and Ni14 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11825
_journal_page_last               11838
_journal_paper_doi               10.1021/ic801555e
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C96 H144 N48 Na2 Ni12 O34'
_chemical_formula_weight         3265.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.327(2)
_cell_angle_beta                 108.530(2)
_cell_angle_gamma                107.775(2)
_cell_formula_units_Z            1
_cell_length_a                   13.7676(12)
_cell_length_b                   16.2729(14)
_cell_length_c                   17.5222(14)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     3328.3(5)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.14 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SMART CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.1250
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22866
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.752
_exptl_absorpt_correction_T_max  0.8659
_exptl_absorpt_correction_T_min  0.7752
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.14 (Bruker 1998)'
_exptl_crystal_colour            plates
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orange
_exptl_crystal_F_000             1686
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.761
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         14940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.761
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0122P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0645
_reflns_number_gt                8180
_reflns_number_total             14940
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic801555e_si_002_2.cif
_cod_data_source_block           st82
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4306739
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.25604(3) 0.75251(2) 0.50791(2) 0.02689(10) Uani 1 1 d . . .
Ni2 Ni 0.32204(3) 0.65807(2) 0.66875(2) 0.02622(10) Uani 1 1 d . . .
Ni3 Ni 0.61487(3) 1.01517(3) 0.78296(2) 0.02900(11) Uani 1 1 d . . .
Ni4 Ni 0.36091(3) 0.96456(2) 0.66964(2) 0.02712(10) Uani 1 1 d . . .
Ni5 Ni 0.42100(3) 0.86736(2) 0.82345(2) 0.02408(10) Uani 1 1 d . . .
Ni6 Ni 0.18807(3) 0.68524(2) 0.77977(2) 0.02686(10) Uani 1 1 d . . .
Na Na 0.44004(10) 1.06647(8) 0.95664(7) 0.0360(3) Uani 1 1 d . . .
O1 O 0.28486(17) 0.75637(13) 0.73018(13) 0.0246(5) Uani 1 1 d . . .
H1' H 0.260(2) 0.7776(18) 0.6997(16) 0.019(9) Uiso 1 1 d . . .
O2 O 0.46158(19) 0.91148(16) 0.73217(14) 0.0266(6) Uani 1 1 d . . .
H2' H 0.456(3) 0.8739(17) 0.7078(17) 0.010(10) Uiso 1 1 d . . .
O3 O 0.04894(19) 0.60947(16) 0.66518(14) 0.0344(6) Uani 1 1 d . . .
H3' H 0.067(3) 0.593(2) 0.6217(19) 0.052 Uiso 1 1 d . . .
H3" H 0.007(3) 0.628(2) 0.651(2) 0.052 Uiso 1 1 d . . .
O4 O 0.13506(17) 0.79168(12) 0.80601(11) 0.0348(5) Uani 1 1 d . . .
H4' H 0.1765 0.8349 0.8094 0.052 Uiso 1 1 d R . .
H4" H 0.0538 0.7847 0.7896 0.052 Uiso 1 1 d R . .
O5 O 0.63145(17) 1.01250(13) 0.66898(12) 0.0415(6) Uani 1 1 d . . .
H5' H 0.5801 0.9921 0.6303 0.062 Uiso 1 1 d R . .
H5" H 0.6832 0.9604 0.6397 0.062 Uiso 1 1 d R . .
O6 O 0.68575(18) 0.91886(13) 0.79336(12) 0.0433(6) Uani 1 1 d . . .
H6' H 0.6520 0.8821 0.8058 0.065 Uiso 1 1 d R . .
H6" H 0.7654 0.9396 0.8228 0.065 Uiso 1 1 d R . .
O7 O 0.16379(16) 0.59437(12) 0.56697(11) 0.0282(5) Uani 1 1 d . . .
O8 O 0.41187(16) 0.95460(12) 0.56945(11) 0.0302(5) Uani 1 1 d . . .
O9 O 0.52886(16) 0.79753(12) 0.82639(11) 0.0274(5) Uani 1 1 d . . .
O10 O 0.54682(16) 0.97847(12) 0.92389(11) 0.0271(5) Uani 1 1 d . . .
O11 O 0.31642(16) 0.94120(12) 0.82549(11) 0.0266(5) Uani 1 1 d . . .
O12 O 0.39942(16) 0.82896(13) 0.92208(11) 0.0285(5) Uani 1 1 d . . .
O13 O 0.3489(2) 1.15797(17) 1.00083(14) 0.0807(10) Uani 1 1 d . . .
H13' H 0.3888 1.1946 1.0265 0.121 Uiso 1 1 d R . .
H13" H 0.3098 1.1700 0.9566 0.121 Uiso 1 1 d R . .
O14 O -0.1044(2) 0.68345(17) 0.61077(16) 0.0823(9) Uiso 1 1 d . . .
H101 H -0.0783 0.7148 0.5776 0.123 Uiso 1 1 d R . .
N1 N 0.1100(2) 0.73685(16) 0.41226(14) 0.0285(6) Uani 1 1 d . . .
N2 N 0.1434(2) 0.63819(15) 0.51030(14) 0.0274(6) Uani 1 1 d . . .
N3 N 0.2988(2) 0.69899(17) 0.41079(14) 0.0318(7) Uani 1 1 d . . .
N4 N 0.3702(2) 0.86919(15) 0.51129(14) 0.0277(6) Uani 1 1 d . . .
N5 N 0.3799(2) 0.56199(16) 0.63051(15) 0.0328(7) Uani 1 1 d . . .
N6 N 0.4818(2) 0.71507(16) 0.76278(14) 0.0291(6) Uani 1 1 d . . .
N7 N 0.7661(2) 1.12816(16) 0.85528(15) 0.0335(7) Uani 1 1 d . . .
N8 N 0.6239(2) 1.03076(15) 0.90344(14) 0.0257(6) Uani 1 1 d . . .
N9 N 0.2623(2) 1.03281(16) 0.62907(15) 0.0334(7) Uani 1 1 d . . .
N10 N 0.2959(2) 0.97488(15) 0.76069(14) 0.0278(6) Uani 1 1 d . . .
N11 N 0.1260(2) 0.60797(16) 0.84697(15) 0.0336(7) Uani 1 1 d . . .
N12 N 0.3139(2) 0.75035(16) 0.89921(14) 0.0279(6) Uani 1 1 d . . .
N13 N 0.3829(2) 0.73573(16) 0.59890(14) 0.0266(6) Uani 1 1 d . . .
N14 N 0.4606(3) 0.73113(17) 0.58333(15) 0.0336(7) Uani 1 1 d . . .
N15 N 0.5358(3) 0.7267(2) 0.56947(18) 0.0510(8) Uani 1 1 d . . .
N16 N 0.2248(2) 0.83621(15) 0.59821(14) 0.0279(6) Uani 1 1 d . . .
N17 N 0.1304(3) 0.82936(17) 0.58216(14) 0.0319(7) Uani 1 1 d . . .
N18 N 0.0410(2) 0.82406(19) 0.56769(17) 0.0482(8) Uani 1 1 d . . .
N19 N 0.2541(2) 0.58851(16) 0.74064(15) 0.0315(7) Uani 1 1 d . . .
N20 N 0.3043(2) 0.55958(18) 0.79015(17) 0.0426(8) Uani 1 1 d . . .
N21 N 0.3515(3) 0.5302(2) 0.8360(2) 0.0755(11) Uani 1 1 d . . .
N22 N 0.5103(2) 1.08775(16) 0.74890(16) 0.0338(7) Uani 1 1 d . . .
N23 N 0.5020(3) 1.1409(2) 0.80162(19) 0.0558(10) Uani 1 1 d . . .
N24 N 0.4915(3) 1.1902(3) 0.8525(2) 0.125(2) Uani 1 1 d . . .
C1 C 0.0968(3) 0.7871(2) 0.36072(18) 0.0359(8) Uani 1 1 d . . .
H1A H 0.1598 0.8394 0.3701 0.043 Uiso 1 1 calc R . .
C2 C -0.0046(3) 0.7654(2) 0.29470(19) 0.0417(9) Uani 1 1 d . . .
H2A H -0.0116 0.8022 0.2595 0.050 Uiso 1 1 calc R . .
C3 C -0.0948(3) 0.6897(2) 0.2814(2) 0.0532(11) Uani 1 1 d . . .
H3A H -0.1650 0.6725 0.2357 0.064 Uiso 1 1 calc R . .
C4 C -0.0840(3) 0.6383(2) 0.3341(2) 0.0476(10) Uani 1 1 d . . .
H4A H -0.1467 0.5867 0.3263 0.057 Uiso 1 1 calc R . .
C5 C 0.0210(3) 0.6635(2) 0.39931(18) 0.0309(8) Uani 1 1 d . . .
C6 C 0.0411(3) 0.61232(19) 0.45792(18) 0.0308(8) Uani 1 1 d . . .
H6A H -0.0181 0.5628 0.4572 0.037 Uiso 1 1 calc R . .
C7 C 0.2546(3) 0.6114(2) 0.35706(19) 0.0361(8) Uani 1 1 d . . .
H7A H 0.2048 0.5647 0.3675 0.043 Uiso 1 1 calc R . .
C8 C 0.2796(3) 0.5874(2) 0.2874(2) 0.0436(10) Uani 1 1 d . . .
H8A H 0.2458 0.5255 0.2495 0.052 Uiso 1 1 calc R . .
C9 C 0.3537(3) 0.6541(2) 0.2740(2) 0.0535(11) Uani 1 1 d . . .
H9A H 0.3723 0.6390 0.2266 0.064 Uiso 1 1 calc R . .
C10 C 0.4016(3) 0.7439(2) 0.3296(2) 0.0470(10) Uani 1 1 d . . .
H10A H 0.4542 0.7909 0.3214 0.056 Uiso 1 1 calc R . .
C11 C 0.3718(3) 0.7641(2) 0.39718(19) 0.0335(8) Uani 1 1 d . . .
C12 C 0.4159(3) 0.8579(2) 0.45742(18) 0.0308(8) Uani 1 1 d . . .
H12A H 0.4741 0.9074 0.4571 0.037 Uiso 1 1 calc R . .
C13 C 0.3262(3) 0.4853(2) 0.5600(2) 0.0456(10) Uani 1 1 d . . .
H13A H 0.2510 0.4701 0.5230 0.055 Uiso 1 1 calc R . .
C14 C 0.3777(3) 0.4290(3) 0.5407(2) 0.0736(14) Uani 1 1 d . . .
H14A H 0.3381 0.3748 0.4913 0.088 Uiso 1 1 calc R . .
C15 C 0.4861(4) 0.4510(3) 0.5925(3) 0.0964(18) Uani 1 1 d . . .
H15A H 0.5229 0.4131 0.5785 0.116 Uiso 1 1 calc R . .
C16 C 0.5427(3) 0.5286(3) 0.6655(2) 0.0732(14) Uani 1 1 d . . .
H16A H 0.6178 0.5440 0.7029 0.088 Uiso 1 1 calc R . .
C17 C 0.4875(3) 0.5831(2) 0.6829(2) 0.0438(10) Uani 1 1 d . . .
C18 C 0.5412(3) 0.6690(2) 0.75516(19) 0.0395(9) Uani 1 1 d . . .
H18A H 0.6167 0.6900 0.7948 0.047 Uiso 1 1 calc R . .
C19 C 0.8352(3) 1.1798(2) 0.8285(2) 0.0426(9) Uani 1 1 d . . .
H19A H 0.8140 1.1671 0.7687 0.051 Uiso 1 1 calc R . .
C20 C 0.9364(3) 1.2508(2) 0.8852(2) 0.0496(10) Uani 1 1 d . . .
H20A H 0.9840 1.2859 0.8643 0.059 Uiso 1 1 calc R . .
C21 C 0.9680(3) 1.2706(2) 0.9721(2) 0.0509(10) Uani 1 1 d . . .
H21A H 1.0373 1.3192 1.0117 0.061 Uiso 1 1 calc R . .
C22 C 0.8969(3) 1.2183(2) 1.0005(2) 0.0439(9) Uani 1 1 d . . .
H22A H 0.9166 1.2305 1.0601 0.053 Uiso 1 1 calc R . .
C23 C 0.7966(3) 1.1478(2) 0.9409(2) 0.0331(8) Uani 1 1 d . . .
C24 C 0.7156(3) 1.0924(2) 0.96522(19) 0.0312(8) Uani 1 1 d . . .
H24A H 0.7292 1.1010 1.0236 0.037 Uiso 1 1 calc R . .
C25 C 0.2450(3) 1.0592(2) 0.5608(2) 0.0457(10) Uani 1 1 d . . .
H25A H 0.2863 1.0507 0.5277 0.055 Uiso 1 1 calc R . .
C26 C 0.1700(4) 1.0982(3) 0.5361(2) 0.0643(13) Uani 1 1 d . . .
H26A H 0.1593 1.1162 0.4870 0.077 Uiso 1 1 calc R . .
C27 C 0.1108(4) 1.1104(3) 0.5846(2) 0.0803(15) Uani 1 1 d . . .
H27A H 0.0589 1.1377 0.5692 0.096 Uiso 1 1 calc R . .
C28 C 0.1267(3) 1.0829(3) 0.6562(2) 0.0663(13) Uani 1 1 d . . .
H28A H 0.0857 1.0904 0.6898 0.080 Uiso 1 1 calc R . .
C29 C 0.2035(3) 1.0448(2) 0.6768(2) 0.0414(9) Uani 1 1 d . . .
C30 C 0.2250(3) 1.0123(2) 0.74900(18) 0.0366(9) Uani 1 1 d . . .
H30A H 0.1882 1.0185 0.7861 0.044 Uiso 1 1 calc R . .
C31 C 0.0311(3) 0.5340(2) 0.8178(2) 0.0458(10) Uani 1 1 d . . .
H31A H -0.0234 0.5178 0.7616 0.055 Uiso 1 1 calc R . .
C32 C 0.0087(3) 0.4799(2) 0.8661(2) 0.0644(12) Uani 1 1 d . . .
H32A H -0.0612 0.4291 0.8445 0.077 Uiso 1 1 calc R . .
C33 C 0.0892(3) 0.5009(3) 0.9459(2) 0.0672(13) Uani 1 1 d . . .
H33A H 0.0772 0.4629 0.9793 0.081 Uiso 1 1 calc R . .
C34 C 0.1860(3) 0.5761(2) 0.9766(2) 0.0523(10) Uani 1 1 d . . .
H34A H 0.2416 0.5921 1.0324 0.063 Uiso 1 1 calc R . .
C35 C 0.2041(3) 0.6298(2) 0.92692(19) 0.0384(9) Uani 1 1 d . . .
C36 C 0.3041(3) 0.7118(2) 0.95435(19) 0.0359(8) Uani 1 1 d . . .
H36A H 0.3605 0.7360 1.0111 0.043 Uiso 1 1 calc R . .
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ni1 N2 177.40(9) . . ?
N4 Ni1 N1 102.32(10) . . ?
N2 Ni1 N1 79.13(10) . . ?
N4 Ni1 N3 79.28(10) . . ?
N2 Ni1 N3 103.01(10) . . ?
N1 Ni1 N3 87.02(9) . . ?
N4 Ni1 N13 90.43(9) . . ?
N2 Ni1 N13 88.31(10) . . ?
N1 Ni1 N13 166.55(10) . . ?
N3 Ni1 N13 91.20(9) . . ?
N4 Ni1 N16 87.88(10) . . ?
N2 Ni1 N16 89.97(9) . . ?
N1 Ni1 N16 89.68(9) . . ?
N3 Ni1 N16 165.72(10) . . ?
N13 Ni1 N16 95.15(9) . . ?
O1 Ni2 N5 168.68(9) . . ?
O1 Ni2 N6 90.81(9) . . ?
N5 Ni2 N6 79.61(10) . . ?
O1 Ni2 O7 93.50(8) . . ?
N5 Ni2 O7 96.23(9) . . ?
N6 Ni2 O7 175.50(9) . . ?
O1 Ni2 N19 81.14(9) . . ?
N5 Ni2 N19 93.31(10) . . ?
N6 Ni2 N19 93.29(10) . . ?
O7 Ni2 N19 88.63(9) . . ?
O1 Ni2 N13 93.95(9) . . ?
N5 Ni2 N13 91.80(10) . . ?
N6 Ni2 N13 88.31(10) . . ?
O7 Ni2 N13 90.12(8) . . ?
N19 Ni2 N13 174.84(10) . . ?
O2 Ni3 N8 91.15(10) . . ?
O2 Ni3 O5 97.46(8) . . ?
N8 Ni3 O5 171.22(9) . . ?
O2 Ni3 N7 169.23(10) . . ?
N8 Ni3 N7 78.71(10) . . ?
O5 Ni3 N7 92.80(9) . . ?
O2 Ni3 O6 88.89(9) . . ?
N8 Ni3 O6 88.28(8) . . ?
O5 Ni3 O6 90.15(8) . . ?
N7 Ni3 O6 94.36(9) . . ?
O2 Ni3 N22 79.40(10) . . ?
N8 Ni3 N22 97.68(10) . . ?
O5 Ni3 N22 85.65(9) . . ?
N7 Ni3 N22 98.20(10) . . ?
O6 Ni3 N22 166.93(9) . . ?
O2 Ni4 N9 168.85(10) . . ?
O2 Ni4 N10 91.12(10) . . ?
N9 Ni4 N10 79.49(10) . . ?
O2 Ni4 O8 94.31(9) . . ?
N9 Ni4 O8 95.32(9) . . ?
N10 Ni4 O8 174.18(9) . . ?
O2 Ni4 N16 94.24(9) . . ?
N9 Ni4 N16 91.33(10) . . ?
N10 Ni4 N16 87.29(9) . . ?
O8 Ni4 N16 90.22(8) . . ?
O2 Ni4 N22 79.45(10) . . ?
N9 Ni4 N22 94.91(10) . . ?
N10 Ni4 N22 92.92(10) . . ?
O8 Ni4 N22 90.14(9) . . ?
N16 Ni4 N22 173.69(9) . . ?
O12 Ni5 O10 80.65(8) . . ?
O12 Ni5 O1 94.65(8) . . ?
O10 Ni5 O1 173.89(8) . . ?
O12 Ni5 O2 173.60(9) . . ?
O10 Ni5 O2 94.41(9) . . ?
O1 Ni5 O2 90.54(9) . . ?
O12 Ni5 O9 87.97(7) . . ?
O10 Ni5 O9 90.82(7) . . ?
O1 Ni5 O9 92.93(8) . . ?
O2 Ni5 O9 88.03(8) . . ?
O12 Ni5 O11 90.94(8) . . ?
O10 Ni5 O11 87.10(7) . . ?
O1 Ni5 O11 89.08(8) . . ?
O2 Ni5 O11 92.89(8) . . ?
O9 Ni5 O11 177.79(7) . . ?
O12 Ni5 Na 77.93(6) . . ?
O10 Ni5 Na 44.51(6) . . ?
O1 Ni5 Na 130.83(6) . . ?
O2 Ni5 Na 101.45(7) . . ?
O9 Ni5 Na 134.48(5) . . ?
O11 Ni5 Na 43.35(5) . . ?
O12 Ni5 Na 40.98(6) . 2_677 ?
O10 Ni5 Na 40.84(6) . 2_677 ?
O1 Ni5 Na 135.16(6) . 2_677 ?
O2 Ni5 Na 133.30(7) . 2_677 ?
O9 Ni5 Na 81.66(5) . 2_677 ?
O11 Ni5 Na 96.26(5) . 2_677 ?
Na Ni5 Na 59.41(3) . 2_677 ?
O1 Ni6 N12 90.78(9) . . ?
O1 Ni6 O3 96.42(9) . . ?
N12 Ni6 O3 172.79(10) . . ?
O1 Ni6 N11 165.18(9) . . ?
N12 Ni6 N11 78.95(10) . . ?
O3 Ni6 N11 93.89(10) . . ?
O1 Ni6 O4 90.03(8) . . ?
N12 Ni6 O4 87.20(8) . . ?
O3 Ni6 O4 93.24(8) . . ?
N11 Ni6 O4 100.00(9) . . ?
O1 Ni6 N19 80.38(9) . . ?
N12 Ni6 N19 94.72(9) . . ?
O3 Ni6 N19 86.05(9) . . ?
N11 Ni6 N19 89.76(10) . . ?
O4 Ni6 N19 170.24(9) . . ?
O10 Na O12 68.70(7) 2_677 2_677 ?
O10 Na O13 88.06(8) 2_677 . ?
O12 Na O13 85.88(8) 2_677 . ?
O10 Na O11 111.85(8) 2_677 . ?
O12 Na O11 162.23(9) 2_677 . ?
O13 Na O11 111.83(9) . . ?
O10 Na O10 88.75(8) 2_677 . ?
O12 Na O10 89.36(8) 2_677 . ?
O13 Na O10 174.99(9) . . ?
O11 Na O10 72.98(7) . . ?
O10 Na Na 45.77(5) 2_677 2_677 ?
O12 Na Na 75.18(6) 2_677 2_677 ?
O13 Na Na 133.70(8) . 2_677 ?
O11 Na Na 92.53(6) . 2_677 ?
O10 Na Na 42.98(5) . 2_677 ?
O10 Na Ni5 97.51(6) 2_677 . ?
O12 Na Ni5 124.76(7) 2_677 . ?
O13 Na Ni5 148.83(8) . . ?
O11 Na Ni5 37.90(5) . . ?
O10 Na Ni5 35.66(5) . . ?
Na Na Ni5 60.45(3) 2_677 . ?
O10 Na Ni5 34.86(5) 2_677 2_677 ?
O12 Na Ni5 34.78(5) 2_677 2_677 ?
O13 Na Ni5 80.25(6) . 2_677 ?
O11 Na Ni5 146.12(6) . 2_677 ?
O10 Na Ni5 94.94(5) . 2_677 ?
Na Na Ni5 60.14(3) 2_677 2_677 ?
Ni5 Na Ni5 120.59(3) . 2_677 ?
O10 Na H13' 87.2 2_677 . ?
O12 Na H13' 73.0 2_677 . ?
O13 Na H13' 13.6 . . ?
O11 Na H13' 124.6 . . ?
O10 Na H13' 162.1 . . ?
Na Na H13' 130.4 2_677 . ?
Ni5 Na H13' 162.2 . . ?
Ni5 Na H13' 72.1 2_677 . ?
Ni6 O1 Ni2 101.30(9) . . ?
Ni6 O1 Ni5 111.69(9) . . ?
Ni2 O1 Ni5 114.40(10) . . ?
Ni6 O1 H1' 118(2) . . ?
Ni2 O1 H1' 110(2) . . ?
Ni5 O1 H1' 102(2) . . ?
Ni4 O2 Ni3 103.21(10) . . ?
Ni4 O2 Ni5 114.51(11) . . ?
Ni3 O2 Ni5 112.30(10) . . ?
Ni4 O2 H2' 112(3) . . ?
Ni3 O2 H2' 116(3) . . ?
Ni5 O2 H2' 99(3) . . ?
Ni6 O3 H3' 112(2) . . ?
Ni6 O3 H3" 120(3) . . ?
H3' O3 H3" 107(3) . . ?
Ni6 O4 H4' 109.9 . . ?
Ni6 O4 H4" 126.2 . . ?
H4' O4 H4" 118.3 . . ?
Ni3 O5 H5' 116.5 . . ?
Ni3 O5 H5" 119.6 . . ?
H5' O5 H5" 96.2 . . ?
Ni3 O6 H6' 109.8 . . ?
Ni3 O6 H6" 119.6 . . ?
H6' O6 H6" 114.5 . . ?
N2 O7 Ni2 115.97(15) . . ?
N4 O8 Ni4 115.93(16) . . ?
N6 O9 Ni5 114.03(15) . . ?
N8 O10 Ni5 114.46(15) . . ?
N8 O10 Na 132.44(16) . 2_677 ?
Ni5 O10 Na 104.30(8) . 2_677 ?
N8 O10 Na 107.43(15) . . ?
Ni5 O10 Na 99.83(8) . . ?
Na O10 Na 91.25(8) 2_677 . ?
N10 O11 Ni5 113.21(16) . . ?
N10 O11 Na 108.69(14) . . ?
Ni5 O11 Na 98.75(8) . . ?
N12 O12 Ni5 115.18(15) . . ?
N12 O12 Na 139.61(15) . 2_677 ?
Ni5 O12 Na 104.24(9) . 2_677 ?
Na O13 H13' 102.8 . . ?
Na O13 H13" 110.0 . . ?
H13' O13 H13" 107.9 . . ?
C5 N1 C1 118.6(3) . . ?
C5 N1 Ni1 113.0(2) . . ?
C1 N1 Ni1 128.2(2) . . ?
C6 N2 O7 117.5(3) . . ?
C6 N2 Ni1 115.6(2) . . ?
O7 N2 Ni1 126.48(17) . . ?
C11 N3 C7 118.6(3) . . ?
C11 N3 Ni1 112.8(2) . . ?
C7 N3 Ni1 128.2(2) . . ?
C12 N4 O8 117.1(3) . . ?
C12 N4 Ni1 115.8(2) . . ?
O8 N4 Ni1 126.71(19) . . ?
C13 N5 C17 118.7(3) . . ?
C13 N5 Ni2 128.1(2) . . ?
C17 N5 Ni2 113.12(19) . . ?
C18 N6 O9 119.5(2) . . ?
C18 N6 Ni2 114.9(2) . . ?
O9 N6 Ni2 125.38(17) . . ?
C19 N7 C23 118.4(3) . . ?
C19 N7 Ni3 128.9(2) . . ?
C23 N7 Ni3 112.7(2) . . ?
C24 N8 O10 118.0(2) . . ?
C24 N8 Ni3 116.3(2) . . ?
O10 N8 Ni3 125.59(17) . . ?
C25 N9 C29 118.8(3) . . ?
C25 N9 Ni4 128.1(2) . . ?
C29 N9 Ni4 112.9(2) . . ?
C30 N10 O11 119.6(3) . . ?
C30 N10 Ni4 114.5(2) . . ?
O11 N10 Ni4 125.70(18) . . ?
C31 N11 C35 118.3(3) . . ?
C31 N11 Ni6 128.7(2) . . ?
C35 N11 Ni6 112.0(2) . . ?
C36 N12 O12 120.2(2) . . ?
C36 N12 Ni6 115.5(2) . . ?
O12 N12 Ni6 124.22(17) . . ?
N14 N13 Ni1 118.5(2) . . ?
N14 N13 Ni2 120.3(2) . . ?
Ni1 N13 Ni2 112.40(12) . . ?
N15 N14 N13 179.1(3) . . ?
N17 N16 Ni1 118.94(19) . . ?
N17 N16 Ni4 120.5(2) . . ?
Ni1 N16 Ni4 112.20(12) . . ?
N18 N17 N16 179.0(4) . . ?
N20 N19 Ni2 123.6(2) . . ?
N20 N19 Ni6 121.9(2) . . ?
Ni2 N19 Ni6 94.79(9) . . ?
N21 N20 N19 178.5(4) . . ?
N23 N22 Ni3 121.7(2) . . ?
N23 N22 Ni4 115.6(2) . . ?
Ni3 N22 Ni4 94.35(10) . . ?
N24 N23 N22 178.0(5) . . ?
N1 C1 C2 122.6(3) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 118.3(3) . . ?
C3 C2 H2A 120.9 . . ?
C1 C2 H2A 120.9 . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C3 C4 C5 118.6(3) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C6 115.7(3) . . ?
C4 C5 C6 122.6(3) . . ?
N2 C6 C5 116.3(3) . . ?
N2 C6 H6A 121.9 . . ?
C5 C6 H6A 121.9 . . ?
N3 C7 C8 122.1(3) . . ?
N3 C7 H7A 118.9 . . ?
C8 C7 H7A 118.9 . . ?
C9 C8 C7 118.8(3) . . ?
C9 C8 H8A 120.6 . . ?
C7 C8 H8A 120.6 . . ?
C8 C9 C10 119.8(3) . . ?
C8 C9 H9A 120.1 . . ?
C10 C9 H9A 120.1 . . ?
C11 C10 C9 118.9(3) . . ?
C11 C10 H10A 120.6 . . ?
C9 C10 H10A 120.6 . . ?
N3 C11 C10 121.8(3) . . ?
N3 C11 C12 115.9(3) . . ?
C10 C11 C12 122.3(3) . . ?
N4 C12 C11 115.9(3) . . ?
N4 C12 H12A 122.0 . . ?
C11 C12 H12A 122.0 . . ?
N5 C13 C14 121.6(3) . . ?
N5 C13 H13A 119.2 . . ?
C14 C13 H13A 119.2 . . ?
C15 C14 C13 119.6(3) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C14 C15 C16 120.0(4) . . ?
C14 C15 H15A 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C17 C16 C15 118.5(3) . . ?
C17 C16 H16A 120.8 . . ?
C15 C16 H16A 120.8 . . ?
N5 C17 C16 121.6(3) . . ?
N5 C17 C18 115.4(3) . . ?
C16 C17 C18 122.9(3) . . ?
N6 C18 C17 117.0(3) . . ?
N6 C18 H18A 121.5 . . ?
C17 C18 H18A 121.5 . . ?
N7 C19 C20 122.0(3) . . ?
N7 C19 H19A 119.0 . . ?
C20 C19 H19A 119.0 . . ?
C21 C20 C19 119.8(3) . . ?
C21 C20 H20A 120.1 . . ?
C19 C20 H20A 120.1 . . ?
C20 C21 C22 118.7(3) . . ?
C20 C21 H21A 120.6 . . ?
C22 C21 H21A 120.6 . . ?
C21 C22 C23 119.2(3) . . ?
C21 C22 H22A 120.4 . . ?
C23 C22 H22A 120.4 . . ?
N7 C23 C22 121.9(3) . . ?
N7 C23 C24 115.4(3) . . ?
C22 C23 C24 122.6(3) . . ?
N8 C24 C23 116.5(3) . . ?
N8 C24 H24A 121.7 . . ?
C23 C24 H24A 121.7 . . ?
N9 C25 C26 122.9(3) . . ?
N9 C25 H25A 118.5 . . ?
C26 C25 H25A 118.5 . . ?
C27 C26 C25 118.1(3) . . ?
C27 C26 H26A 120.9 . . ?
C25 C26 H26A 120.9 . . ?
C26 C27 C28 120.2(4) . . ?
C26 C27 H27A 119.9 . . ?
C28 C27 H27A 119.9 . . ?
C29 C28 C27 118.1(4) . . ?
C29 C28 H28A 121.0 . . ?
C27 C28 H28A 121.0 . . ?
N9 C29 C28 121.8(3) . . ?
N9 C29 C30 115.7(3) . . ?
C28 C29 C30 122.5(3) . . ?
N10 C30 C29 117.3(3) . . ?
N10 C30 H30A 121.3 . . ?
C29 C30 H30A 121.3 . . ?
N11 C31 C32 122.6(3) . . ?
N11 C31 H31A 118.7 . . ?
C32 C31 H31A 118.7 . . ?
C33 C32 C31 118.8(4) . . ?
C33 C32 H32A 120.6 . . ?
C31 C32 H32A 120.6 . . ?
C34 C33 C32 119.3(3) . . ?
C34 C33 H33A 120.4 . . ?
C32 C33 H33A 120.4 . . ?
C33 C34 C35 120.1(3) . . ?
C33 C34 H34A 120.0 . . ?
C35 C34 H34A 120.0 . . ?
N11 C35 C34 120.9(3) . . ?
N11 C35 C36 115.0(3) . . ?
C34 C35 C36 124.1(3) . . ?
N12 C36 C35 117.4(3) . . ?
N12 C36 H36A 121.3 . . ?
C35 C36 H36A 121.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 2.037(2) . ?
Ni1 N2 2.045(2) . ?
Ni1 N1 2.069(2) . ?
Ni1 N3 2.078(2) . ?
Ni1 N13 2.091(2) . ?
Ni1 N16 2.101(2) . ?
Ni2 O1 2.024(2) . ?
Ni2 N5 2.045(2) . ?
Ni2 N6 2.053(2) . ?
Ni2 O7 2.0890(18) . ?
Ni2 N19 2.110(3) . ?
Ni2 N13 2.112(2) . ?
Ni3 O2 2.021(2) . ?
Ni3 N8 2.030(2) . ?
Ni3 O5 2.074(2) . ?
Ni3 N7 2.077(2) . ?
Ni3 O6 2.094(2) . ?
Ni3 N22 2.149(3) . ?
Ni4 O2 2.009(2) . ?
Ni4 N9 2.055(2) . ?
Ni4 N10 2.064(2) . ?
Ni4 O8 2.0810(19) . ?
Ni4 N16 2.108(2) . ?
Ni4 N22 2.158(3) . ?
Ni5 O12 2.0346(19) . ?
Ni5 O10 2.0392(18) . ?
Ni5 O1 2.043(2) . ?
Ni5 O2 2.049(2) . ?
Ni5 O9 2.1226(19) . ?
Ni5 O11 2.1422(19) . ?
Ni5 Na 3.4464(12) . ?
Ni5 Na 3.4572(11) 2_677 ?
Ni6 O1 2.023(2) . ?
Ni6 N12 2.033(2) . ?
Ni6 O3 2.068(2) . ?
Ni6 N11 2.077(3) . ?
Ni6 O4 2.0950(19) . ?
Ni6 N19 2.141(2) . ?
Na O10 2.333(2) 2_677 ?
Na O12 2.339(2) 2_677 ?
Na O13 2.378(3) . ?
Na O11 2.394(2) . ?
Na O10 2.452(2) . ?
Na Na 3.421(2) 2_677 ?
Na Ni5 3.4571(11) 2_677 ?
Na H13' 2.5885 . ?
O1 H1' 0.75(2) . ?
O2 H2' 0.63(2) . ?
O3 H3' 0.89(3) . ?
O3 H3" 0.72(3) . ?
O4 H4' 0.7344 . ?
O4 H4" 1.0255 . ?
O5 H5' 0.7249 . ?
O5 H5" 1.3811 . ?
O6 H6' 0.7556 . ?
O6 H6" 0.9604 . ?
O7 N2 1.349(3) . ?
O8 N4 1.355(3) . ?
O9 N6 1.354(3) . ?
O10 N8 1.342(3) . ?
O10 Na 2.333(2) 2_677 ?
O11 N10 1.351(3) . ?
O12 N12 1.321(3) . ?
O12 Na 2.339(2) 2_677 ?
O13 H13' 0.6223 . ?
O13 H13" 0.8899 . ?
O14 H101 0.9352 . ?
N1 C5 1.338(4) . ?
N1 C1 1.348(3) . ?
N2 C6 1.286(3) . ?
N3 C11 1.342(4) . ?
N3 C7 1.350(3) . ?
N4 C12 1.301(4) . ?
N5 C13 1.352(3) . ?
N5 C17 1.359(4) . ?
N6 C18 1.283(3) . ?
N7 C19 1.339(4) . ?
N7 C23 1.357(3) . ?
N8 C24 1.291(3) . ?
N9 C25 1.331(4) . ?
N9 C29 1.360(4) . ?
N10 C30 1.286(3) . ?
N11 C31 1.330(4) . ?
N11 C35 1.357(4) . ?
N12 C36 1.279(3) . ?
N13 N14 1.205(3) . ?
N14 N15 1.154(4) . ?
N16 N17 1.203(3) . ?
N17 N18 1.146(3) . ?
N19 N20 1.201(3) . ?
N20 N21 1.148(3) . ?
N22 N23 1.184(3) . ?
N23 N24 1.143(4) . ?
C1 C2 1.383(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.369(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.376(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.397(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.467(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.380(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.364(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.384(4) . ?
C9 H9A 0.9500 . ?
C10 C11 1.379(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.467(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.370(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.361(5) . ?
C14 H14A 0.9500 . ?
C15 C16 1.384(4) . ?
C15 H15A 0.9500 . ?
C16 C17 1.377(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.457(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.383(4) . ?
C19 H19A 0.9500 . ?
C20 C21 1.376(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.383(4) . ?
C21 H21A 0.9500 . ?
C22 C23 1.384(4) . ?
C22 H22A 0.9500 . ?
C23 C24 1.445(4) . ?
C24 H24A 0.9500 . ?
C25 C26 1.375(4) . ?
C25 H25A 0.9500 . ?
C26 C27 1.374(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.396(4) . ?
C27 H27A 0.9500 . ?
C28 C29 1.374(4) . ?
C28 H28A 0.9500 . ?
C29 C30 1.453(4) . ?
C30 H30A 0.9500 . ?
C31 C32 1.380(4) . ?
C31 H31A 0.9500 . ?
C32 C33 1.371(5) . ?
C32 H32A 0.9500 . ?
C33 C34 1.354(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.384(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.445(4) . ?
C36 H36A 0.9500 . ?
