# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Zheng, Wenxu'
_publ_contact_author_email       wkc@fjirsm.ac.cn

_publ_section_title              
;
Spontaneous resolution of a homochiral
helix built from tetra-nuclear nickel cluster
;
loop_
_publ_author_name
'Wenxu Zheng'
'Wei Yongqin'
'Chong-Bin Tian'
'Xueying Xiao'
'Wu Kechen'

# Attachment '- 1P.cif'

data_1P
_database_code_depnum_ccdc_archive 'CCDC 793453'
#TrackingRef '- 1P.cif'

_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H36 N12 Ni4 O24'
_chemical_formula_weight         1303.65

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   11.501(2)
_cell_length_b                   14.424(3)
_cell_length_c                   28.959(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4804.0(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7134
_cell_measurement_theta_min      2.5385
_cell_measurement_theta_max      29.1013

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2656
_exptl_absorpt_coefficient_mu    1.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83904
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_standards_number         17421
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16583
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0932
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         26.75
_reflns_number_total             9306
_reflns_number_gt                6768
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Initially the hydrogen atoms attached to the water molecules were located from the difference-Fourier maps. Then they were refined using the DFIX 0.82 0.01 and DANG 1.39 0.01 restraints to make the geometries of the water molecules reasonable. At the final cycles of refinement, the water hydrogen atoms were adjusted to D(O-H) =0.82 angstrom and then AFIX 3 to their mother O atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.027(7)
_refine_ls_number_reflns         9306
_refine_ls_number_parameters     721
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0389
_refine_ls_wR_factor_gt          0.0376
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      0.953
_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 0.47982(3) 0.72635(3) 0.131060(16) 0.02033(12) Uani 1 1 d . . .
Ni2 Ni 0.73102(3) 0.52619(3) -0.031077(17) 0.01859(12) Uani 1 1 d . . .
Ni3 Ni 0.79451(3) 0.24690(3) 0.127728(15) 0.01909(12) Uani 1 1 d . . .
Ni4 Ni 0.84679(4) 0.57096(3) 0.269936(17) 0.02266(13) Uani 1 1 d . . .
O1 O 1.08763(19) 0.2529(2) 0.07681(9) 0.0416(8) Uani 1 1 d . . .
O1W O 0.50069(19) 0.85202(16) 0.10238(8) 0.0338(7) Uani 1 1 d . . .
H1WA H 0.4719 0.8979 0.0902 0.051 Uiso 1 1 d R . .
H1WB H 0.5702 0.8643 0.1038 0.051 Uiso 1 1 d R . .
O2W O 0.65259(17) 0.43897(16) -0.07919(7) 0.0269(7) Uani 1 1 d . . .
H2WA H 0.6479 0.3828 -0.0754 0.040 Uiso 1 1 d R . .
H2WB H 0.5847 0.4560 -0.0778 0.040 Uiso 1 1 d R . .
O2 O 1.13902(19) 0.33084(19) 0.01601(9) 0.0417(8) Uani 1 1 d . . .
H2 H 1.1082 0.3694 -0.0008 0.050 Uiso 1 1 d R . .
O3W O 0.69574(17) 0.62733(16) -0.08074(8) 0.0327(7) Uani 1 1 d . . .
H3WA H 0.7242 0.6794 -0.0797 0.049 Uiso 1 1 d R . .
H3WB H 0.7103 0.6035 -0.1058 0.049 Uiso 1 1 d R . .
O3 O 1.05540(19) 0.42185(19) -0.04865(9) 0.0371(8) Uani 1 1 d . . .
O4W O 0.95478(16) 0.19408(15) 0.14337(8) 0.0278(7) Uani 1 1 d . . .
H4WA H 0.9887 0.2072 0.1674 0.042 Uiso 1 1 d R . .
H4WB H 1.0034 0.2153 0.1256 0.042 Uiso 1 1 d R . .
O4 O 0.88614(18) 0.49070(17) -0.06273(8) 0.0253(7) Uani 1 1 d . . .
O5W O 0.76816(18) 0.13220(16) 0.08719(8) 0.0322(7) Uani 1 1 d . . .
H5WB H 0.7172 0.1205 0.0683 0.048 Uiso 1 1 d R . .
H5WA H 0.8198 0.0963 0.0793 0.048 Uiso 1 1 d R . .
O5 O 0.62227(19) 0.27576(17) 0.31173(8) 0.0275(7) Uani 1 1 d . . .
O6W O 0.74298(19) 0.59453(16) 0.32738(8) 0.0335(7) Uani 1 1 d . . .
H6WA H 0.6720 0.5903 0.3259 0.050 Uiso 1 1 d R . .
H6WB H 0.7729 0.5711 0.3503 0.050 Uiso 1 1 d R . .
O6 O 0.7025(2) 0.40637(18) 0.33690(8) 0.0376(8) Uani 1 1 d . . .
O7 O 0.7168(2) 0.16633(16) 0.17806(9) 0.0275(7) Uani 1 1 d . . .
O7W O 0.97252(18) 0.52317(17) 0.31676(8) 0.0410(8) Uani 1 1 d . . .
H7WA H 1.0311 0.4940 0.3097 0.061 Uiso 1 1 d R . .
H7WB H 0.9841 0.5477 0.3419 0.061 Uiso 1 1 d R . .
O8 O 0.6370(2) 0.16616(18) 0.24722(9) 0.0473(9) Uani 1 1 d . . .
H8 H 0.6292 0.2058 0.2673 0.057 Uiso 1 1 d R . .
O9 O 0.6880(2) 0.91703(19) 0.14144(10) 0.0530(9) Uani 1 1 d . . .
O10 O 0.8048(2) 0.93738(18) 0.20018(10) 0.0528(9) Uani 1 1 d . . .
H10 H 0.8355 0.9056 0.2203 0.079 Uiso 1 1 d R . .
O11 O 0.9011(2) 0.84918(19) 0.26185(11) 0.0512(10) Uani 1 1 d . . .
O12 O 0.91320(18) 0.70141(17) 0.28115(9) 0.0275(7) Uani 1 1 d . . .
O13 O 0.32193(17) 0.71122(18) 0.09788(8) 0.0257(7) Uani 1 1 d . . .
O14 O 0.23158(19) 0.63790(19) 0.04088(9) 0.0466(9) Uani 1 1 d . . .
O15 O 0.28641(18) 0.54132(18) -0.02515(9) 0.0479(9) Uani 1 1 d . . .
H15 H 0.2607 0.5643 -0.0013 0.057 Uiso 1 1 d R . .
O16 O 0.43968(19) 0.4848(2) -0.05949(10) 0.0471(9) Uani 1 1 d . . .
N1 N 0.6333(2) 0.2972(2) 0.10539(10) 0.0217(8) Uani 1 1 d . . .
N2 N 0.8493(2) 0.31992(19) 0.06804(10) 0.0167(7) Uani 1 1 d . . .
N3 N 0.7821(2) 0.41265(19) 0.01032(10) 0.0183(7) Uani 1 1 d . . .
N4 N 0.8136(2) 0.61996(19) 0.01346(10) 0.0193(8) Uani 1 1 d . . .
N5 N 0.5888(2) 0.5765(2) 0.00609(10) 0.0178(8) Uani 1 1 d . . .
N6 N 0.5332(2) 0.6619(2) 0.06747(9) 0.0182(7) Uani 1 1 d . . .
N7 N 0.6264(2) 0.7331(2) 0.17601(10) 0.0192(8) Uani 1 1 d . . .
N8 N 0.4695(2) 0.5971(2) 0.16240(10) 0.0214(8) Uani 1 1 d . . .
N9 N 0.7264(2) 0.65346(19) 0.23028(10) 0.0175(7) Uani 1 1 d . . .
N10 N 0.9513(2) 0.5579(2) 0.21058(10) 0.0233(8) Uani 1 1 d . . .
N11 N 0.8073(2) 0.4355(2) 0.24941(10) 0.0171(7) Uani 1 1 d . . .
N12 N 0.8082(2) 0.33815(19) 0.18794(10) 0.0170(7) Uani 1 1 d . . .
C1 C 0.5277(3) 0.2718(3) 0.12102(13) 0.0324(10) Uani 1 1 d . . .
H1 H 0.5227 0.2403 0.1490 0.039 Uiso 1 1 calc R . .
C2 C 0.4255(3) 0.2910(3) 0.09696(15) 0.0367(12) Uani 1 1 d . . .
H2A H 0.3539 0.2726 0.1087 0.044 Uiso 1 1 calc R . .
C3 C 0.4323(3) 0.3372(3) 0.05598(15) 0.0350(12) Uani 1 1 d . . .
H3 H 0.3652 0.3505 0.0393 0.042 Uiso 1 1 calc R . .
C4 C 0.5407(3) 0.3644(3) 0.03943(13) 0.0256(10) Uani 1 1 d . . .
H4 H 0.5475 0.3960 0.0115 0.031 Uiso 1 1 calc R . .
C5 C 0.6376(3) 0.3436(2) 0.06535(13) 0.0170(9) Uani 1 1 d . . .
C6 C 0.7567(3) 0.3627(2) 0.04814(12) 0.0154(9) Uani 1 1 d . . .
C7 C 0.9409(3) 0.3410(2) 0.03887(13) 0.0184(9) Uani 1 1 d . . .
C8 C 0.8987(3) 0.3977(2) 0.00384(14) 0.0188(10) Uani 1 1 d . . .
C9 C 1.0607(3) 0.3058(3) 0.04592(15) 0.0293(11) Uani 1 1 d . . .
C10 C 0.9503(3) 0.4391(3) -0.03876(14) 0.0243(10) Uani 1 1 d . . .
C11 C 1.0309(3) 0.6180(3) 0.19484(15) 0.0332(11) Uani 1 1 d . . .
H11 H 1.0526 0.6672 0.2138 0.040 Uiso 1 1 calc R . .
C12 C 1.0821(3) 0.6105(3) 0.15213(16) 0.0408(13) Uani 1 1 d . . .
H12 H 1.1353 0.6548 0.1422 0.049 Uiso 1 1 calc R . .
C13 C 1.0538(3) 0.5375(3) 0.12462(16) 0.0435(12) Uani 1 1 d . . .
H13 H 1.0876 0.5310 0.0956 0.052 Uiso 1 1 calc R . .
C14 C 0.9735(3) 0.4724(3) 0.14040(13) 0.0338(11) Uani 1 1 d . . .
H14 H 0.9534 0.4218 0.1222 0.041 Uiso 1 1 calc R . .
C15 C 0.9236(3) 0.4844(3) 0.18397(13) 0.0182(9) Uani 1 1 d . . .
C16 C 0.8437(3) 0.4201(3) 0.20551(12) 0.0158(9) Uani 1 1 d . . .
C17 C 0.7458(3) 0.2991(2) 0.22334(13) 0.0172(9) Uani 1 1 d . . .
C20 C 0.7455(3) 0.3592(2) 0.26089(12) 0.0158(9) Uani 1 1 d . . .
C21 C 0.6978(3) 0.2056(3) 0.21525(14) 0.0245(10) Uani 1 1 d . . .
C22 C 0.6865(3) 0.3481(3) 0.30705(13) 0.0193(9) Uani 1 1 d . . .
C23 C 0.3838(3) 0.5339(3) 0.15816(14) 0.0308(11) Uani 1 1 d . . .
H23 H 0.3273 0.5433 0.1357 0.037 Uiso 1 1 calc R . .
C24 C 0.3758(3) 0.4565(3) 0.18535(15) 0.0404(13) Uani 1 1 d . . .
H24 H 0.3150 0.4149 0.1812 0.049 Uiso 1 1 calc R . .
C25 C 0.4587(3) 0.4404(3) 0.21915(15) 0.0395(12) Uani 1 1 d . . .
H25 H 0.4546 0.3884 0.2381 0.047 Uiso 1 1 calc R . .
C26 C 0.5481(3) 0.5046(2) 0.22365(15) 0.0313(11) Uani 1 1 d . . .
H26 H 0.6051 0.4962 0.2460 0.038 Uiso 1 1 calc R . .
C27 C 0.5522(3) 0.5800(3) 0.19522(12) 0.0166(9) Uani 1 1 d . . .
C28 C 0.6385(3) 0.6537(3) 0.19937(13) 0.0177(9) Uani 1 1 d . . .
C29 C 0.7106(3) 0.7910(3) 0.19343(13) 0.0216(9) Uani 1 1 d . . .
C30 C 0.7713(3) 0.7419(2) 0.22721(12) 0.0206(9) Uani 1 1 d . . .
C31 C 0.7327(3) 0.8862(3) 0.17657(16) 0.0312(11) Uani 1 1 d . . .
C32 C 0.8686(3) 0.7669(3) 0.25910(13) 0.0283(10) Uani 1 1 d . . .
C33 C 0.9265(3) 0.6469(3) 0.01311(14) 0.0275(11) Uani 1 1 d . . .
H33 H 0.9765 0.6209 -0.0086 0.033 Uiso 1 1 calc R . .
C34 C 0.9693(3) 0.7105(3) 0.04326(14) 0.0337(11) Uani 1 1 d . . .
H34 H 1.0467 0.7287 0.0413 0.040 Uiso 1 1 calc R . .
C35 C 0.8980(3) 0.7479(3) 0.07668(14) 0.0387(12) Uani 1 1 d . . .
H35 H 0.9265 0.7906 0.0979 0.046 Uiso 1 1 calc R . .
C36 C 0.7832(3) 0.7200(3) 0.07775(12) 0.0308(11) Uani 1 1 d . . .
H36 H 0.7326 0.7440 0.0998 0.037 Uiso 1 1 calc R . .
C37 C 0.7447(3) 0.6569(2) 0.04609(12) 0.0162(9) Uani 1 1 d . . .
C38 C 0.6223(3) 0.6293(2) 0.04191(13) 0.0163(9) Uani 1 1 d . . .
C39 C 0.4369(3) 0.6294(3) 0.04499(13) 0.0182(9) Uani 1 1 d . . .
C40 C 0.4697(3) 0.5770(2) 0.00744(12) 0.0157(9) Uani 1 1 d . . .
C41 C 0.3217(3) 0.6603(3) 0.06208(13) 0.0255(10) Uani 1 1 d . . .
C42 C 0.3990(3) 0.5302(3) -0.02765(15) 0.0299(11) Uani 1 1 d . . .
O8W O 0.5059(2) 0.5614(2) 0.33372(12) 0.0975(13) Uani 1 1 d . . .
H8WA H 0.4363 0.5685 0.3386 0.146 Uiso 1 1 d R . .
H8WB H 0.5259 0.5144 0.3475 0.146 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0197(3) 0.0254(3) 0.0160(3) -0.0009(3) 0.0001(3) 0.0021(2)
Ni2 0.0175(3) 0.0218(3) 0.0165(3) 0.0006(3) 0.0032(2) 0.0009(2)
Ni3 0.0220(2) 0.0207(3) 0.0146(3) -0.0011(3) 0.0004(2) 0.0012(2)
Ni4 0.0269(3) 0.0212(3) 0.0199(3) -0.0029(3) -0.0049(3) -0.0004(2)
O1 0.0244(15) 0.057(2) 0.043(2) 0.027(2) 0.0039(14) 0.0129(15)
O1W 0.0342(15) 0.0280(17) 0.0392(18) 0.0143(15) -0.0038(15) 0.0073(13)
O2W 0.0261(14) 0.0280(16) 0.0267(17) -0.0072(14) 0.0051(13) -0.0028(12)
O2 0.0187(15) 0.060(2) 0.047(2) 0.0175(18) 0.0111(15) 0.0106(14)
O3W 0.0454(17) 0.0242(16) 0.0286(18) 0.0020(14) 0.0058(14) -0.0055(13)
O3 0.0190(15) 0.054(2) 0.0379(19) 0.0106(17) 0.0180(14) 0.0105(14)
O4W 0.0267(14) 0.0348(17) 0.0219(17) 0.0016(14) -0.0113(12) 0.0022(12)
O4 0.0254(15) 0.0322(18) 0.0185(17) 0.0077(15) 0.0109(13) 0.0018(12)
O5W 0.0203(14) 0.0399(18) 0.0362(18) -0.0255(15) -0.0117(14) 0.0044(13)
O5 0.0373(15) 0.0293(17) 0.0157(15) 0.0001(14) 0.0108(13) -0.0127(13)
O6W 0.0344(16) 0.0450(18) 0.0211(16) 0.0004(15) -0.0059(14) 0.0031(14)
O6 0.0674(19) 0.0309(18) 0.0146(16) -0.0094(14) 0.0095(16) -0.0156(15)
O7 0.0440(17) 0.0200(15) 0.0185(16) -0.0019(14) 0.0050(15) -0.0094(14)
O7W 0.0434(16) 0.0440(19) 0.0355(19) -0.0099(17) -0.0126(15) 0.0205(16)
O8 0.079(2) 0.0343(19) 0.0283(19) -0.0082(16) 0.0229(17) -0.0335(17)
O9 0.059(2) 0.0395(19) 0.061(2) 0.0250(19) -0.0234(19) -0.0149(15)
O10 0.063(2) 0.0333(19) 0.062(2) 0.0078(18) -0.0298(18) -0.0242(16)
O11 0.0584(19) 0.0237(18) 0.072(3) -0.0017(19) -0.0412(18) -0.0158(14)
O12 0.0320(15) 0.0271(17) 0.0234(18) -0.0040(15) -0.0162(13) 0.0033(13)
O13 0.0175(14) 0.0382(18) 0.0214(16) -0.0030(14) 0.0004(13) 0.0076(12)
O14 0.0127(14) 0.078(2) 0.049(2) -0.0297(19) -0.0111(16) 0.0077(15)
O15 0.0166(14) 0.070(2) 0.057(2) -0.038(2) -0.0090(15) 0.0004(14)
O16 0.0177(15) 0.069(2) 0.054(2) -0.047(2) -0.0032(15) 0.0012(15)
N1 0.0213(18) 0.024(2) 0.020(2) 0.0027(17) 0.0069(16) 0.0021(15)
N2 0.0172(16) 0.0164(18) 0.0166(19) -0.0023(15) -0.0024(16) 0.0024(14)
N3 0.0149(17) 0.0205(18) 0.0197(19) 0.0018(16) 0.0055(16) 0.0008(14)
N4 0.0151(17) 0.0247(19) 0.018(2) -0.0017(16) -0.0019(15) 0.0012(14)
N5 0.0090(16) 0.0276(19) 0.0167(19) -0.0077(18) -0.0011(15) 0.0018(14)
N6 0.0180(17) 0.0231(19) 0.0133(18) -0.0012(16) 0.0000(16) 0.0025(14)
N7 0.0157(16) 0.0199(19) 0.0221(19) -0.0066(17) -0.0011(14) -0.0013(14)
N8 0.0158(17) 0.0263(19) 0.022(2) -0.0039(17) -0.0020(17) -0.0031(15)
N9 0.0132(16) 0.0239(18) 0.0153(18) -0.0006(17) -0.0018(16) 0.0022(14)
N10 0.0168(17) 0.024(2) 0.030(2) -0.0026(18) -0.0008(16) -0.0017(15)
N11 0.0176(16) 0.0202(18) 0.0136(18) 0.0023(16) -0.0002(15) -0.0033(14)
N12 0.0216(18) 0.0161(17) 0.0133(18) -0.0017(15) 0.0001(15) -0.0034(14)
C1 0.027(2) 0.037(2) 0.033(3) 0.010(2) 0.019(2) -0.004(2)
C2 0.018(2) 0.038(3) 0.054(3) 0.002(3) 0.010(2) -0.002(2)
C3 0.021(2) 0.043(3) 0.042(3) 0.003(3) -0.005(2) 0.002(2)
C4 0.018(2) 0.036(3) 0.022(3) 0.010(2) 0.001(2) 0.0052(19)
C5 0.015(2) 0.016(2) 0.019(2) 0.0007(19) 0.011(2) 0.0013(17)
C6 0.017(2) 0.015(2) 0.014(2) -0.0021(19) 0.0058(19) -0.0004(17)
C7 0.015(2) 0.023(2) 0.017(2) 0.006(2) 0.0052(19) 0.0009(17)
C8 0.017(2) 0.016(2) 0.024(3) -0.003(2) 0.004(2) 0.0013(17)
C9 0.022(2) 0.031(3) 0.035(3) -0.005(2) 0.004(2) -0.001(2)
C10 0.027(2) 0.021(2) 0.025(3) -0.005(2) 0.004(2) 0.0021(19)
C11 0.030(2) 0.021(2) 0.048(3) -0.007(2) -0.005(2) -0.010(2)
C12 0.032(3) 0.038(3) 0.052(4) -0.002(3) 0.017(3) -0.016(2)
C13 0.040(3) 0.052(3) 0.039(3) -0.002(3) 0.018(2) -0.012(2)
C14 0.038(2) 0.035(3) 0.028(3) -0.006(2) 0.010(2) -0.012(2)
C15 0.021(2) 0.018(2) 0.016(2) -0.002(2) -0.0031(19) 0.0006(18)
C16 0.017(2) 0.021(2) 0.009(2) 0.002(2) -0.0032(19) -0.0020(18)
C17 0.019(2) 0.017(2) 0.016(2) 0.0024(19) -0.0016(19) 0.0003(16)
C20 0.012(2) 0.020(2) 0.015(2) 0.0051(19) -0.0018(18) 0.0006(16)
C21 0.032(2) 0.023(2) 0.018(2) 0.006(2) 0.000(2) 0.0012(19)
C22 0.022(2) 0.027(2) 0.009(2) 0.007(2) 0.0037(19) 0.0056(19)
C23 0.023(2) 0.034(3) 0.035(3) -0.001(3) -0.006(2) 0.000(2)
C24 0.027(3) 0.032(3) 0.062(4) -0.010(3) -0.002(2) -0.012(2)
C25 0.036(3) 0.023(3) 0.059(3) 0.015(3) -0.003(3) 0.001(2)
C26 0.019(2) 0.023(2) 0.051(3) 0.006(2) -0.012(2) -0.0006(18)
C27 0.015(2) 0.019(2) 0.016(2) -0.004(2) -0.0017(18) 0.0012(17)
C28 0.020(2) 0.017(2) 0.016(2) -0.0019(19) 0.000(2) 0.0001(18)
C29 0.018(2) 0.026(2) 0.021(2) -0.003(2) 0.0038(19) 0.0013(19)
C30 0.022(2) 0.020(2) 0.019(2) -0.005(2) -0.0037(19) 0.0007(18)
C31 0.031(3) 0.024(3) 0.039(3) 0.004(2) -0.003(2) 0.000(2)
C32 0.028(2) 0.032(3) 0.025(3) -0.005(2) -0.008(2) -0.006(2)
C33 0.015(2) 0.028(2) 0.039(3) -0.001(2) 0.005(2) -0.0001(18)
C34 0.012(2) 0.044(3) 0.046(3) 0.002(3) 0.000(2) -0.007(2)
C35 0.027(2) 0.042(3) 0.047(3) -0.022(3) -0.006(2) -0.008(2)
C36 0.018(2) 0.045(3) 0.029(3) -0.020(2) 0.005(2) -0.002(2)
C37 0.011(2) 0.020(2) 0.017(2) -0.0007(19) -0.0050(18) 0.0012(17)
C38 0.017(2) 0.015(2) 0.016(3) -0.002(2) 0.0022(19) 0.0013(17)
C39 0.011(2) 0.026(2) 0.018(2) -0.001(2) -0.0001(19) 0.0003(17)
C40 0.0087(19) 0.020(2) 0.019(2) 0.000(2) -0.0010(19) -0.0007(17)
C41 0.024(2) 0.029(3) 0.023(3) 0.002(2) 0.006(2) 0.004(2)
C42 0.014(2) 0.035(3) 0.041(3) -0.007(3) -0.002(2) -0.001(2)
O8W 0.061(2) 0.090(3) 0.142(3) 0.013(3) -0.001(2) 0.028(2)

_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 O1W 2.008(2) . ?
Ni1 O13 2.066(2) . ?
Ni1 N8 2.077(3) . ?
Ni1 N7 2.132(3) . ?
Ni1 N6 2.152(3) . ?
Ni1 O5 2.152(2) 4_655 ?
Ni2 O4 2.070(2) . ?
Ni2 O2W 2.083(2) . ?
Ni2 N5 2.088(3) . ?
Ni2 O3W 2.088(2) . ?
Ni2 N4 2.096(3) . ?
Ni2 N3 2.113(3) . ?
Ni3 O4W 2.0453(19) . ?
Ni3 O5W 2.051(2) . ?
Ni3 O7 2.067(2) . ?
Ni3 N1 2.093(3) . ?
Ni3 N2 2.120(3) . ?
Ni3 N12 2.190(3) . ?
Ni4 O12 2.056(2) . ?
Ni4 O6W 2.076(2) . ?
Ni4 N11 2.092(3) . ?
Ni4 O7W 2.099(2) . ?
Ni4 N10 2.106(3) . ?
Ni4 N9 2.157(3) . ?
O1 C9 1.216(4) . ?
O1W H1WA 0.8201 . ?
O1W H1WB 0.8200 . ?
O2W H2WA 0.8200 . ?
O2W H2WB 0.8199 . ?
O2 C9 1.301(4) . ?
O2 H2 0.8202 . ?
O3W H3WA 0.8201 . ?
O3W H3WB 0.8201 . ?
O3 C10 1.267(4) . ?
O4W H4WA 0.8201 . ?
O4W H4WB 0.8200 . ?
O4 C10 1.258(4) . ?
O5W H5WB 0.8199 . ?
O5W H5WA 0.8201 . ?
O5 C22 1.286(4) . ?
O5 Ni1 2.152(2) 4_645 ?
O6W H6WA 0.8200 . ?
O6W H6WB 0.8199 . ?
O6 C22 1.219(4) . ?
O7 C21 1.236(4) . ?
O7W H7WA 0.8200 . ?
O7W H7WB 0.8202 . ?
O8 C21 1.293(4) . ?
O8 H8 0.8200 . ?
O9 C31 1.224(4) . ?
O10 C31 1.304(4) . ?
O10 H10 0.8199 . ?
O11 C32 1.247(4) . ?
O12 C32 1.250(4) . ?
O13 C41 1.270(4) . ?
O14 C41 1.247(4) . ?
O15 C42 1.307(3) . ?
O15 H15 0.8200 . ?
O16 C42 1.224(4) . ?
N1 C5 1.339(4) . ?
N1 C1 1.348(4) . ?
N2 C6 1.359(4) . ?
N2 C7 1.384(4) . ?
N3 C6 1.343(4) . ?
N3 C8 1.371(4) . ?
N4 C37 1.343(4) . ?
N4 C33 1.355(4) . ?
N5 C38 1.343(4) . ?
N5 C40 1.371(4) . ?
N6 C38 1.348(4) . ?
N6 C39 1.369(4) . ?
N7 C28 1.338(4) . ?
N7 C29 1.374(4) . ?
N8 C23 1.349(4) . ?
N8 C27 1.367(4) . ?
N9 C28 1.351(4) . ?
N9 C30 1.379(4) . ?
N10 C11 1.341(4) . ?
N10 C15 1.349(4) . ?
N11 C20 1.352(4) . ?
N11 C16 1.357(4) . ?
N12 C16 1.350(4) . ?
N12 C17 1.373(4) . ?
C1 C2 1.394(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.392(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.484(4) . ?
C7 C8 1.390(5) . ?
C7 C9 1.482(4) . ?
C8 C10 1.494(5) . ?
C11 C12 1.374(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.361(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.393(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.397(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.447(5) . ?
C17 C20 1.390(4) . ?
C17 C21 1.476(4) . ?
C20 C22 1.507(4) . ?
C23 C24 1.369(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.386(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.391(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.365(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.460(4) . ?
C29 C30 1.395(4) . ?
C29 C31 1.479(5) . ?
C30 C32 1.495(4) . ?
C33 C34 1.359(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.378(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.381(4) . ?
C35 H35 0.9300 . ?
C36 C37 1.366(4) . ?
C36 H36 0.9300 . ?
C37 C38 1.469(4) . ?
C39 C40 1.377(4) . ?
C39 C41 1.483(4) . ?
C40 C42 1.466(5) . ?
O8W H8WA 0.8200 . ?
O8W H8WB 0.8199 . ?

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
O1W Ni1 O13 90.46(9) . . ?
O1W Ni1 N8 176.16(10) . . ?
O13 Ni1 N8 93.34(10) . . ?
O1W Ni1 N7 96.69(11) . . ?
O13 Ni1 N7 169.65(10) . . ?
N8 Ni1 N7 79.60(11) . . ?
O1W Ni1 N6 90.09(10) . . ?
O13 Ni1 N6 78.89(10) . . ?
N8 Ni1 N6 90.15(11) . . ?
N7 Ni1 N6 108.45(10) . . ?
O1W Ni1 O5 94.86(10) . 4_655 ?
O13 Ni1 O5 85.03(9) . 4_655 ?
N8 Ni1 O5 85.98(10) . 4_655 ?
N7 Ni1 O5 86.92(9) . 4_655 ?
N6 Ni1 O5 163.22(10) . 4_655 ?
O4 Ni2 O2W 85.85(9) . . ?
O4 Ni2 N5 171.59(11) . . ?
O2W Ni2 N5 102.44(10) . . ?
O4 Ni2 O3W 92.02(9) . . ?
O2W Ni2 O3W 82.94(9) . . ?
N5 Ni2 O3W 87.72(10) . . ?
O4 Ni2 N4 92.37(10) . . ?
O2W Ni2 N4 175.95(10) . . ?
N5 Ni2 N4 79.26(11) . . ?
O3W Ni2 N4 93.50(10) . . ?
O4 Ni2 N3 79.62(10) . . ?
O2W Ni2 N3 91.82(10) . . ?
N5 Ni2 N3 101.22(11) . . ?
O3W Ni2 N3 170.47(10) . . ?
N4 Ni2 N3 91.43(11) . . ?
O4W Ni3 O5W 87.67(9) . . ?
O4W Ni3 O7 91.38(9) . . ?
O5W Ni3 O7 83.47(10) . . ?
O4W Ni3 N1 174.69(10) . . ?
O5W Ni3 N1 88.40(10) . . ?
O7 Ni3 N1 91.72(11) . . ?
O4W Ni3 N2 95.59(10) . . ?
O5W Ni3 N2 88.74(10) . . ?
O7 Ni3 N2 169.33(10) . . ?
N1 Ni3 N2 80.75(11) . . ?
O4W Ni3 N12 89.00(9) . . ?
O5W Ni3 N12 161.98(10) . . ?
O7 Ni3 N12 78.91(10) . . ?
N1 Ni3 N12 95.82(10) . . ?
N2 Ni3 N12 109.21(11) . . ?
O12 Ni4 O6W 86.40(10) . . ?
O12 Ni4 N11 168.52(10) . . ?
O6W Ni4 N11 104.81(10) . . ?
O12 Ni4 O7W 86.71(10) . . ?
O6W Ni4 O7W 86.12(9) . . ?
N11 Ni4 O7W 91.53(10) . . ?
O12 Ni4 N10 89.93(11) . . ?
O6W Ni4 N10 175.65(11) . . ?
N11 Ni4 N10 78.97(11) . . ?
O7W Ni4 N10 96.00(10) . . ?
O12 Ni4 N9 79.49(10) . . ?
O6W Ni4 N9 88.12(10) . . ?
N11 Ni4 N9 102.97(10) . . ?
O7W Ni4 N9 165.35(10) . . ?
N10 Ni4 N9 88.93(11) . . ?
Ni1 O1W H1WA 149.1 . . ?
Ni1 O1W H1WB 106.9 . . ?
H1WA O1W H1WB 103.9 . . ?
Ni2 O2W H2WA 122.5 . . ?
Ni2 O2W H2WB 101.5 . . ?
H2WA O2W H2WB 103.1 . . ?
C9 O2 H2 106.5 . . ?
Ni2 O3W H3WA 122.4 . . ?
Ni2 O3W H3WB 106.0 . . ?
H3WA O3W H3WB 109.7 . . ?
Ni3 O4W H4WA 122.0 . . ?
Ni3 O4W H4WB 109.7 . . ?
H4WA O4W H4WB 97.1 . . ?
C10 O4 Ni2 114.1(2) . . ?
Ni3 O5W H5WB 130.8 . . ?
Ni3 O5W H5WA 124.2 . . ?
H5WB O5W H5WA 101.6 . . ?
C22 O5 Ni1 131.6(2) . 4_645 ?
Ni4 O6W H6WA 121.2 . . ?
Ni4 O6W H6WB 109.8 . . ?
H6WA O6W H6WB 115.4 . . ?
C21 O7 Ni3 115.6(2) . . ?
Ni4 O7W H7WA 124.9 . . ?
Ni4 O7W H7WB 122.9 . . ?
H7WA O7W H7WB 108.0 . . ?
C21 O8 H8 105.0 . . ?
C31 O10 H10 109.2 . . ?
C32 O12 Ni4 117.3(2) . . ?
C41 O13 Ni1 116.3(2) . . ?
C42 O15 H15 117.0 . . ?
C5 N1 C1 117.4(3) . . ?
C5 N1 Ni3 114.1(2) . . ?
C1 N1 Ni3 126.9(3) . . ?
C6 N2 C7 103.8(3) . . ?
C6 N2 Ni3 109.8(2) . . ?
C7 N2 Ni3 146.4(2) . . ?
C6 N3 C8 103.9(3) . . ?
C6 N3 Ni2 144.9(2) . . ?
C8 N3 Ni2 108.4(2) . . ?
C37 N4 C33 117.2(3) . . ?
C37 N4 Ni2 114.9(2) . . ?
C33 N4 Ni2 127.9(3) . . ?
C38 N5 C40 105.1(3) . . ?
C38 N5 Ni2 111.8(2) . . ?
C40 N5 Ni2 143.1(3) . . ?
C38 N6 C39 103.5(3) . . ?
C38 N6 Ni1 146.9(2) . . ?
C39 N6 Ni1 108.9(2) . . ?
C28 N7 C29 105.1(3) . . ?
C28 N7 Ni1 110.6(2) . . ?
C29 N7 Ni1 144.0(3) . . ?
C23 N8 C27 116.7(3) . . ?
C23 N8 Ni1 127.5(3) . . ?
C27 N8 Ni1 115.2(2) . . ?
C28 N9 C30 103.6(3) . . ?
C28 N9 Ni4 146.6(2) . . ?
C30 N9 Ni4 107.8(2) . . ?
C11 N10 C15 118.4(3) . . ?
C11 N10 Ni4 127.5(3) . . ?
C15 N10 Ni4 113.7(2) . . ?
C20 N11 C16 105.0(3) . . ?
C20 N11 Ni4 143.6(2) . . ?
C16 N11 Ni4 110.6(2) . . ?
C16 N12 C17 103.6(3) . . ?
C16 N12 Ni3 148.0(3) . . ?
C17 N12 Ni3 108.1(2) . . ?
N1 C1 C2 122.6(3) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 119.0(4) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 119.2(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 118.4(4) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
N1 C5 C4 123.5(3) . . ?
N1 C5 C6 114.7(3) . . ?
C4 C5 C6 121.6(3) . . ?
N3 C6 N2 114.8(3) . . ?
N3 C6 C5 125.1(3) . . ?
N2 C6 C5 119.8(3) . . ?
N2 C7 C8 108.0(3) . . ?
N2 C7 C9 123.2(3) . . ?
C8 C7 C9 128.8(3) . . ?
N3 C8 C7 109.5(3) . . ?
N3 C8 C10 116.1(3) . . ?
C7 C8 C10 134.3(3) . . ?
O1 C9 O2 119.2(4) . . ?
O1 C9 C7 123.6(4) . . ?
O2 C9 C7 117.2(4) . . ?
O4 C10 O3 123.4(4) . . ?
O4 C10 C8 117.3(3) . . ?
O3 C10 C8 119.2(4) . . ?
N10 C11 C12 123.2(4) . . ?
N10 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C13 C12 C11 119.1(4) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 119.2(4) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C13 C14 C15 119.0(4) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
N10 C15 C14 121.1(4) . . ?
N10 C15 C16 114.0(3) . . ?
C14 C15 C16 124.8(4) . . ?
N12 C16 N11 113.8(3) . . ?
N12 C16 C15 126.2(3) . . ?
N11 C16 C15 119.7(3) . . ?
N12 C17 C20 109.3(3) . . ?
N12 C17 C21 116.8(3) . . ?
C20 C17 C21 133.8(4) . . ?
N11 C20 C17 108.3(3) . . ?
N11 C20 C22 122.7(3) . . ?
C17 C20 C22 129.0(3) . . ?
O7 C21 O8 121.2(4) . . ?
O7 C21 C17 119.4(4) . . ?
O8 C21 C17 119.4(4) . . ?
O6 C22 O5 124.8(4) . . ?
O6 C22 C20 119.2(3) . . ?
O5 C22 C20 116.0(3) . . ?
N8 C23 C24 123.2(4) . . ?
N8 C23 H23 118.4 . . ?
C24 C23 H23 118.4 . . ?
C23 C24 C25 119.8(4) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C26 117.6(4) . . ?
C24 C25 H25 121.2 . . ?
C26 C25 H25 121.2 . . ?
C27 C26 C25 120.0(4) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 N8 122.7(3) . . ?
C26 C27 C28 123.7(3) . . ?
N8 C27 C28 113.5(3) . . ?
N7 C28 N9 114.5(3) . . ?
N7 C28 C27 120.8(3) . . ?
N9 C28 C27 124.2(3) . . ?
N7 C29 C30 107.5(3) . . ?
N7 C29 C31 124.3(3) . . ?
C30 C29 C31 128.1(3) . . ?
N9 C30 C29 109.1(3) . . ?
N9 C30 C32 117.6(3) . . ?
C29 C30 C32 133.3(4) . . ?
O9 C31 O10 119.8(4) . . ?
O9 C31 C29 122.7(4) . . ?
O10 C31 C29 117.5(4) . . ?
O11 C32 O12 124.3(3) . . ?
O11 C32 C30 119.5(4) . . ?
O12 C32 C30 116.1(3) . . ?
N4 C33 C34 122.4(4) . . ?
N4 C33 H33 118.8 . . ?
C34 C33 H33 118.8 . . ?
C33 C34 C35 120.0(3) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C36 118.1(4) . . ?
C34 C35 H35 121.0 . . ?
C36 C35 H35 121.0 . . ?
C37 C36 C35 119.2(3) . . ?
C37 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
N4 C37 C36 123.0(3) . . ?
N4 C37 C38 113.6(3) . . ?
C36 C37 C38 123.1(3) . . ?
N5 C38 N6 113.9(3) . . ?
N5 C38 C37 119.4(3) . . ?
N6 C38 C37 126.1(3) . . ?
N6 C39 C40 110.0(3) . . ?
N6 C39 C41 117.5(3) . . ?
C40 C39 C41 132.4(3) . . ?
N5 C40 C39 107.5(3) . . ?
N5 C40 C42 122.1(3) . . ?
C39 C40 C42 130.4(3) . . ?
O14 C41 O13 123.6(3) . . ?
O14 C41 C39 120.0(4) . . ?
O13 C41 C39 116.4(3) . . ?
O16 C42 O15 119.1(4) . . ?
O16 C42 C40 123.8(3) . . ?
O15 C42 C40 117.1(4) . . ?
H8WA O8W H8WB 107.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O4 0.82 2.05 2.864(3) 174.8 3_465
O1W H1WB O9 0.82 1.90 2.607(3) 144.2 .
O2W H2WA O1 0.82 2.08 2.868(4) 162.1 3_455
O2W H2WB O16 0.82 1.80 2.600(3) 165.3 .
O2 H2 O3 0.82 1.69 2.481(3) 160.9 .
O3W H3WA O13 0.82 2.01 2.788(3) 159.0 3_565
O3W H3WB O6 0.82 1.94 2.701(3) 153.0 2_664
O4W H4WA O12 0.82 1.87 2.663(3) 162.2 4_745
O4W H4WB O1 0.82 1.80 2.602(3) 167.1 .
O5W H5WB O3 0.82 2.04 2.800(3) 154.2 3_455
O5W H5WA O16 0.82 1.90 2.718(3) 178.5 3
O6W H6WA O8W 0.82 1.97 2.774(3) 167.4 .
O6W H6WB O2W 0.82 2.22 3.000(3) 158.9 2_665
O7W H7WA O10 0.82 2.08 2.886(3) 169.4 4_745
O7W H7WB O4W 0.82 2.27 2.848(3) 128.2 4_755
O8 H8 O5 0.82 1.64 2.453(3) 172.7 .
O8W H8WA O7 0.82 2.31 2.995(4) 141.8 4_655
O8W H8WB O6 0.82 2.58 3.181(4) 131.5 .
O10 H10 O11 0.82 1.64 2.456(4) 175.8 .
O15 H15 O14 0.82 1.65 2.448(4) 162.6 .

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.75
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.076


data_1M
_database_code_depnum_ccdc_archive 'CCDC 864754'
#TrackingRef '- 1M.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H36 N12 Ni4 O24'
_chemical_formula_weight         1303.65

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

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   11.4952(5)
_cell_length_b                   14.4352(5)
_cell_length_c                   28.9218(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4799.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16691
_cell_measurement_theta_min      2.1125
_cell_measurement_theta_max      27.4816

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.52
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2656
_exptl_absorpt_coefficient_mu    1.648
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7929
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 28.5714
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41607
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         27.48
_reflns_number_total             10930
_reflns_number_gt                10495
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Initially the hydrogen atoms attached to the water molecules were located from the difference-Fourier maps. Then they were refined using the DFIX 0.82 0.01 and DANG 1.39 0.01 restraints to make the geometries of the water molecules reasonable. At the final cycles of refinement, the water hydrogen atoms were adjusted to D(O-H) =0.82 angstrom and then AFIX 3 to their mother O atoms.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(7)
_refine_ls_number_reflns         10930
_refine_ls_number_parameters     721
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0284
_refine_ls_wR_factor_ref         0.0515
_refine_ls_wR_factor_gt          0.0505
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.004
_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 0.52019(3) 0.27364(2) 0.868938(11) 0.02414(7) Uani 1 1 d . . .
Ni2 Ni 0.26902(3) 0.47385(2) 1.031065(12) 0.02256(7) Uani 1 1 d . . .
Ni3 Ni 0.20547(3) 0.75310(2) 0.872276(11) 0.02299(7) Uani 1 1 d . . .
Ni4 Ni 0.15321(3) 0.42905(2) 0.730079(12) 0.02661(8) Uani 1 1 d . . .
O1 O -0.08660(17) 0.74686(16) 0.92314(7) 0.0466(6) Uani 1 1 d . . .
O1W O 0.49930(18) 0.14780(12) 0.89779(6) 0.0374(5) Uani 1 1 d . . .
H1WA H 0.5281 0.1019 0.9100 0.056 Uiso 1 1 d R . .
H1WB H 0.4298 0.1355 0.8964 0.056 Uiso 1 1 d R . .
O2W O 0.34714(16) 0.56052(13) 1.07930(6) 0.0318(4) Uani 1 1 d . . .
H2WA H 0.3519 0.6167 1.0755 0.048 Uiso 1 1 d R . .
H2WB H 0.4151 0.5435 1.0779 0.048 Uiso 1 1 d R . .
O2 O -0.13884(16) 0.66865(15) 0.98439(7) 0.0459(6) Uani 1 1 d . . .
H2 H -0.1080 0.6301 1.0012 0.055 Uiso 1 1 d R . .
O3W O 0.30424(17) 0.37319(13) 1.08094(6) 0.0366(5) Uani 1 1 d . . .
H3WA H 0.2758 0.3211 1.0799 0.055 Uiso 1 1 d R . .
H3WB H 0.2896 0.3971 1.1060 0.055 Uiso 1 1 d R . .
O3 O -0.05478(16) 0.57819(15) 1.04860(7) 0.0432(6) Uani 1 1 d . . .
O4W O 0.04523(15) 0.80592(12) 0.85708(6) 0.0319(5) Uani 1 1 d . . .
H4WA H 0.0113 0.7928 0.8330 0.048 Uiso 1 1 d R . .
H4WB H -0.0034 0.7847 0.8749 0.048 Uiso 1 1 d R . .
O4 O 0.11414(15) 0.50939(13) 1.06277(6) 0.0313(5) Uani 1 1 d . . .
O5W O 0.23163(16) 0.86736(12) 0.91323(6) 0.0349(5) Uani 1 1 d . . .
H5WB H 0.2827 0.8791 0.9322 0.052 Uiso 1 1 d R . .
H5WA H 0.1800 0.9032 0.9212 0.052 Uiso 1 1 d R . .
O5 O 0.37829(17) 0.72462(13) 0.68853(6) 0.0344(5) Uani 1 1 d . . .
O6W O 0.25621(18) 0.40532(13) 0.67260(6) 0.0395(5) Uani 1 1 d . . .
H6WA H 0.3272 0.4095 0.6741 0.059 Uiso 1 1 d R . .
H6WB H 0.2263 0.4288 0.6497 0.059 Uiso 1 1 d R . .
O6 O 0.2983(2) 0.59363(13) 0.66298(6) 0.0434(6) Uani 1 1 d . . .
O7 O 0.28360(18) 0.83321(12) 0.82185(6) 0.0340(5) Uani 1 1 d . . .
O7W O 0.02765(18) 0.47687(13) 0.68302(7) 0.0448(6) Uani 1 1 d . . .
H7WA H -0.0309 0.5060 0.6901 0.067 Uiso 1 1 d R . .
H7WB H 0.0161 0.4524 0.6579 0.067 Uiso 1 1 d R . .
O8 O 0.3627(2) 0.83381(14) 0.75286(7) 0.0506(7) Uani 1 1 d . . .
H8 H 0.3705 0.7942 0.7328 0.061 Uiso 1 1 d R . .
O9 O 0.3116(2) 0.08324(15) 0.85866(8) 0.0580(7) Uani 1 1 d . . .
O10 O 0.1943(2) 0.06359(14) 0.79982(8) 0.0568(7) Uani 1 1 d . . .
H10 H 0.1637 0.0953 0.7797 0.085 Uiso 1 1 d R . .
O11 O 0.0994(2) 0.15056(14) 0.73813(8) 0.0549(7) Uani 1 1 d . . .
O12 O 0.08665(16) 0.29828(13) 0.71866(7) 0.0343(5) Uani 1 1 d . . .
O13 O 0.67813(15) 0.28931(13) 0.90206(6) 0.0309(4) Uani 1 1 d . . .
O14 O 0.76858(16) 0.36215(16) 0.95890(8) 0.0495(6) Uani 1 1 d . . .
O15 O 0.71392(16) 0.45933(15) 1.02527(8) 0.0509(6) Uani 1 1 d . . .
H15 H 0.7397 0.4364 1.0015 0.061 Uiso 1 1 d R . .
O16 O 0.56052(17) 0.51499(16) 1.05908(8) 0.0520(7) Uani 1 1 d . . .
N1 N 0.36626(18) 0.70306(15) 0.89440(7) 0.0262(5) Uani 1 1 d . . .
N2 N 0.15077(17) 0.68039(14) 0.93241(7) 0.0226(5) Uani 1 1 d . . .
N3 N 0.21830(17) 0.58796(14) 0.98980(7) 0.0225(5) Uani 1 1 d . . .
N4 N 0.18536(17) 0.38015(14) 0.98645(7) 0.0238(5) Uani 1 1 d . . .
N5 N 0.41086(17) 0.42326(15) 0.99426(7) 0.0218(4) Uani 1 1 d . . .
N6 N 0.46642(17) 0.33752(15) 0.93246(7) 0.0229(5) Uani 1 1 d . . .
N7 N 0.37361(17) 0.26673(14) 0.82426(7) 0.0236(5) Uani 1 1 d . . .
N8 N 0.53040(18) 0.40326(15) 0.83749(8) 0.0256(5) Uani 1 1 d . . .
N9 N 0.27336(19) 0.34646(14) 0.76977(7) 0.0254(5) Uani 1 1 d . . .
N10 N 0.04937(18) 0.44195(15) 0.78958(8) 0.0284(5) Uani 1 1 d . . .
N11 N 0.19295(18) 0.56434(14) 0.75086(7) 0.0229(5) Uani 1 1 d . . .
N12 N 0.19220(19) 0.66152(14) 0.81239(7) 0.0235(5) Uani 1 1 d . . .
C1 C 0.4717(2) 0.7279(2) 0.87899(10) 0.0368(7) Uani 1 1 d . . .
H1 H 0.4764 0.7592 0.8509 0.044 Uiso 1 1 calc R . .
C2 C 0.5738(2) 0.7096(2) 0.90256(11) 0.0417(8) Uani 1 1 d . . .
H2A H 0.6452 0.7280 0.8906 0.050 Uiso 1 1 calc R . .
C3 C 0.5676(2) 0.6633(2) 0.94421(11) 0.0402(8) Uani 1 1 d . . .
H3 H 0.6346 0.6507 0.9611 0.048 Uiso 1 1 calc R . .
C4 C 0.4593(2) 0.63602(19) 0.96025(10) 0.0315(7) Uani 1 1 d . . .
H4 H 0.4529 0.6042 0.9881 0.038 Uiso 1 1 calc R . .
C5 C 0.3617(2) 0.65606(17) 0.93501(9) 0.0226(5) Uani 1 1 d . . .
C6 C 0.2432(2) 0.63790(17) 0.95198(9) 0.0212(5) Uani 1 1 d . . .
C7 C 0.0597(2) 0.65917(18) 0.96108(9) 0.0230(5) Uani 1 1 d . . .
C8 C 0.1022(2) 0.60199(18) 0.99620(9) 0.0224(5) Uani 1 1 d . . .
C9 C -0.0602(2) 0.6936(2) 0.95480(10) 0.0311(6) Uani 1 1 d . . .
C10 C 0.0501(2) 0.56090(19) 1.03869(9) 0.0272(6) Uani 1 1 d . . .
C11 C -0.0303(3) 0.3818(2) 0.80524(11) 0.0403(8) Uani 1 1 d . . .
H11 H -0.0515 0.3325 0.7863 0.048 Uiso 1 1 calc R . .
C12 C -0.0821(3) 0.3895(2) 0.84788(12) 0.0466(9) Uani 1 1 d . . .
H12 H -0.1356 0.3454 0.8579 0.056 Uiso 1 1 calc R . .
C13 C -0.0534(3) 0.4636(2) 0.87546(11) 0.0461(8) Uani 1 1 d . . .
H13 H -0.0870 0.4706 0.9045 0.055 Uiso 1 1 calc R . .
C14 C 0.0262(3) 0.5274(2) 0.85936(10) 0.0388(7) Uani 1 1 d . . .
H14 H 0.0466 0.5782 0.8774 0.047 Uiso 1 1 calc R . .
C15 C 0.0754(2) 0.51509(18) 0.81603(9) 0.0252(6) Uani 1 1 d . . .
C16 C 0.1563(2) 0.58046(18) 0.79457(9) 0.0234(5) Uani 1 1 d . . .
C17 C 0.2544(2) 0.70062(17) 0.77690(8) 0.0233(5) Uani 1 1 d . . .
C20 C 0.2553(2) 0.64131(17) 0.73926(8) 0.0220(5) Uani 1 1 d . . .
C21 C 0.3015(3) 0.79358(19) 0.78484(9) 0.0303(6) Uani 1 1 d . . .
C22 C 0.3132(2) 0.65269(18) 0.69312(9) 0.0273(6) Uani 1 1 d . . .
C23 C 0.6169(2) 0.4659(2) 0.84215(10) 0.0351(7) Uani 1 1 d . . .
H23 H 0.6733 0.4559 0.8646 0.042 Uiso 1 1 calc R . .
C24 C 0.6250(3) 0.5448(2) 0.81463(12) 0.0432(8) Uani 1 1 d . . .
H24 H 0.6855 0.5866 0.8188 0.052 Uiso 1 1 calc R . .
C25 C 0.5427(3) 0.5599(2) 0.78134(12) 0.0455(9) Uani 1 1 d . . .
H25 H 0.5470 0.6117 0.7623 0.055 Uiso 1 1 calc R . .
C26 C 0.4527(2) 0.49660(18) 0.77640(11) 0.0375(7) Uani 1 1 d . . .
H26 H 0.3958 0.5055 0.7540 0.045 Uiso 1 1 calc R . .
C27 C 0.4486(2) 0.42015(18) 0.80517(9) 0.0242(6) Uani 1 1 d . . .
C28 C 0.3618(2) 0.34681(17) 0.80028(9) 0.0235(5) Uani 1 1 d . . .
C29 C 0.2887(2) 0.20964(18) 0.80647(9) 0.0263(6) Uani 1 1 d . . .
C30 C 0.2285(2) 0.25873(17) 0.77274(9) 0.0267(5) Uani 1 1 d . . .
C31 C 0.2672(3) 0.1142(2) 0.82392(11) 0.0370(7) Uani 1 1 d . . .
C32 C 0.1317(2) 0.2329(2) 0.74150(10) 0.0335(7) Uani 1 1 d . . .
C33 C 0.0736(2) 0.35299(19) 0.98709(10) 0.0314(6) Uani 1 1 d . . .
H33 H 0.0242 0.3783 1.0092 0.038 Uiso 1 1 calc R . .
C34 C 0.0292(2) 0.2893(2) 0.95641(10) 0.0369(7) Uani 1 1 d . . .
H34 H -0.0487 0.2721 0.9579 0.044 Uiso 1 1 calc R . .
C35 C 0.1014(2) 0.2512(2) 0.92339(11) 0.0415(8) Uani 1 1 d . . .
H35 H 0.0731 0.2079 0.9024 0.050 Uiso 1 1 calc R . .
C36 C 0.2170(2) 0.2786(2) 0.92208(10) 0.0354(7) Uani 1 1 d . . .
H36 H 0.2676 0.2542 0.9001 0.043 Uiso 1 1 calc R . .
C37 C 0.2558(2) 0.34321(18) 0.95425(9) 0.0232(5) Uani 1 1 d . . .
C38 C 0.3782(2) 0.37060(18) 0.95826(9) 0.0221(5) Uani 1 1 d . . .
C39 C 0.5632(2) 0.37043(18) 0.95437(9) 0.0227(5) Uani 1 1 d . . .
C40 C 0.5300(2) 0.42296(18) 0.99253(9) 0.0234(5) Uani 1 1 d . . .
C41 C 0.6776(2) 0.3399(2) 0.93795(10) 0.0290(6) Uani 1 1 d . . .
C42 C 0.6023(2) 0.4688(2) 1.02776(11) 0.0333(7) Uani 1 1 d . . .
O8W O 0.4934(2) 0.43822(19) 0.66564(11) 0.1013(11) Uani 1 1 d . . .
H8WA H 0.5631 0.4311 0.6608 0.152 Uiso 1 1 d R . .
H8WB H 0.4735 0.4853 0.6519 0.152 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.02348(15) 0.02888(17) 0.02007(17) -0.00099(14) 0.00007(14) 0.00283(14)
Ni2 0.02152(14) 0.02531(16) 0.02083(17) 0.00047(14) 0.00284(14) 0.00088(14)
Ni3 0.02608(16) 0.02483(16) 0.01806(16) -0.00034(14) 0.00005(14) 0.00084(14)
Ni4 0.02998(17) 0.02521(17) 0.02465(19) -0.00302(15) -0.00546(16) -0.00079(15)
O1 0.0305(10) 0.0617(15) 0.0475(14) 0.0181(12) 0.0028(10) 0.0135(11)
O1W 0.0389(11) 0.0331(11) 0.0403(12) 0.0128(9) -0.0039(10) 0.0044(10)
O2W 0.0329(10) 0.0328(11) 0.0296(11) -0.0030(9) 0.0007(9) -0.0043(9)
O2 0.0231(10) 0.0645(15) 0.0500(14) 0.0161(12) 0.0085(10) 0.0124(10)
O3W 0.0481(12) 0.0295(10) 0.0323(11) 0.0054(9) 0.0043(10) -0.0045(10)
O3 0.0256(10) 0.0568(14) 0.0471(14) 0.0144(12) 0.0159(10) 0.0106(10)
O4W 0.0301(10) 0.0362(11) 0.0295(11) -0.0005(8) -0.0098(9) 0.0024(9)
O4 0.0277(9) 0.0387(12) 0.0275(11) 0.0060(9) 0.0090(9) 0.0041(9)
O5W 0.0264(9) 0.0414(11) 0.0370(12) -0.0201(9) -0.0077(9) 0.0024(9)
O5 0.0451(11) 0.0360(11) 0.0221(10) 0.0013(9) 0.0112(9) -0.0125(10)
O6W 0.0436(12) 0.0483(13) 0.0266(11) 0.0012(9) 0.0010(10) 0.0045(11)
O6 0.0722(16) 0.0374(12) 0.0207(10) -0.0066(9) 0.0069(11) -0.0141(12)
O7 0.0551(13) 0.0248(10) 0.0220(10) -0.0029(8) 0.0062(10) -0.0114(10)
O7W 0.0489(13) 0.0465(13) 0.0389(13) -0.0057(11) -0.0142(11) 0.0175(12)
O8 0.0841(18) 0.0368(12) 0.0310(12) -0.0053(10) 0.0202(12) -0.0313(13)
O9 0.0723(17) 0.0425(13) 0.0591(16) 0.0233(12) -0.0266(14) -0.0161(12)
O10 0.0643(15) 0.0319(12) 0.0743(18) 0.0143(12) -0.0274(14) -0.0231(12)
O11 0.0656(15) 0.0302(12) 0.0687(17) 0.0012(12) -0.0386(14) -0.0144(11)
O12 0.0367(10) 0.0288(11) 0.0376(12) -0.0036(9) -0.0162(10) -0.0004(9)
O13 0.0221(9) 0.0419(12) 0.0285(11) -0.0055(9) 0.0005(8) 0.0056(8)
O14 0.0174(9) 0.0783(17) 0.0529(15) -0.0268(13) -0.0062(10) 0.0066(11)
O15 0.0197(9) 0.0740(16) 0.0591(15) -0.0348(13) -0.0069(10) -0.0001(11)
O16 0.0301(11) 0.0683(16) 0.0576(16) -0.0383(13) -0.0043(11) 0.0000(11)
N1 0.0242(11) 0.0298(12) 0.0245(12) 0.0017(10) 0.0075(10) 0.0014(9)
N2 0.0210(10) 0.0271(11) 0.0197(11) -0.0007(9) -0.0003(9) 0.0025(9)
N3 0.0187(10) 0.0268(11) 0.0222(11) 0.0042(9) 0.0028(9) 0.0037(9)
N4 0.0200(10) 0.0264(11) 0.0250(12) 0.0001(9) 0.0035(9) -0.0011(9)
N5 0.0175(9) 0.0262(11) 0.0217(11) -0.0035(9) 0.0004(9) 0.0008(9)
N6 0.0184(10) 0.0299(12) 0.0203(11) -0.0021(9) 0.0002(9) -0.0002(9)
N7 0.0245(10) 0.0236(11) 0.0226(11) 0.0008(9) -0.0043(9) -0.0026(9)
N8 0.0232(11) 0.0280(12) 0.0255(12) -0.0032(9) 0.0004(10) -0.0029(9)
N9 0.0263(10) 0.0249(11) 0.0249(12) 0.0002(9) -0.0050(10) 0.0010(9)
N10 0.0285(11) 0.0275(12) 0.0293(13) -0.0045(10) 0.0024(10) -0.0071(10)
N11 0.0281(10) 0.0217(11) 0.0189(11) -0.0024(9) -0.0011(9) -0.0036(9)
N12 0.0307(11) 0.0215(11) 0.0183(11) -0.0016(9) 0.0026(10) -0.0012(9)
C1 0.0305(14) 0.0430(17) 0.0367(17) 0.0081(14) 0.0146(13) -0.0022(13)
C2 0.0250(13) 0.0472(19) 0.053(2) 0.0064(16) 0.0122(15) -0.0027(14)
C3 0.0234(14) 0.0496(19) 0.047(2) 0.0027(16) -0.0015(14) 0.0027(14)
C4 0.0251(13) 0.0355(16) 0.0338(17) 0.0078(13) 0.0015(13) 0.0018(12)
C5 0.0222(12) 0.0222(13) 0.0235(14) 0.0001(10) 0.0054(11) 0.0009(10)
C6 0.0196(11) 0.0243(13) 0.0197(13) -0.0017(10) 0.0013(10) 0.0026(10)
C7 0.0189(11) 0.0279(13) 0.0221(14) -0.0015(11) 0.0016(11) 0.0017(10)
C8 0.0182(11) 0.0255(13) 0.0235(14) -0.0022(11) 0.0040(11) -0.0001(10)
C9 0.0252(13) 0.0377(16) 0.0306(16) 0.0009(13) 0.0006(12) 0.0030(12)
C10 0.0273(13) 0.0287(14) 0.0257(15) -0.0024(12) 0.0086(12) 0.0016(11)
C11 0.0351(15) 0.0321(16) 0.054(2) -0.0046(15) 0.0029(16) -0.0163(13)
C12 0.0419(18) 0.0423(19) 0.055(2) 0.0035(16) 0.0157(17) -0.0161(15)
C13 0.0447(17) 0.053(2) 0.0402(19) 0.0001(17) 0.0161(16) -0.0114(16)
C14 0.0455(17) 0.0379(16) 0.0329(17) -0.0046(13) 0.0102(14) -0.0132(15)
C15 0.0273(13) 0.0245(13) 0.0238(14) 0.0036(11) 0.0000(11) -0.0036(11)
C16 0.0236(11) 0.0254(13) 0.0214(13) 0.0007(11) 0.0004(11) 0.0000(11)
C17 0.0284(13) 0.0235(13) 0.0180(13) 0.0032(10) 0.0026(11) -0.0015(10)
C20 0.0273(13) 0.0223(12) 0.0163(12) 0.0024(10) -0.0013(11) -0.0017(10)
C21 0.0420(15) 0.0296(15) 0.0193(13) 0.0028(11) 0.0044(13) -0.0073(13)
C22 0.0322(14) 0.0302(14) 0.0194(13) 0.0024(11) 0.0010(12) 0.0019(12)
C23 0.0260(13) 0.0413(17) 0.0379(17) -0.0009(14) -0.0038(13) -0.0063(13)
C24 0.0340(15) 0.0341(17) 0.061(2) -0.0006(16) -0.0046(16) -0.0116(13)
C25 0.0404(17) 0.0286(16) 0.067(2) 0.0106(16) -0.0033(17) -0.0062(14)
C26 0.0316(15) 0.0287(15) 0.052(2) 0.0076(14) -0.0108(15) -0.0015(12)
C27 0.0214(12) 0.0228(13) 0.0283(14) -0.0024(11) -0.0012(11) -0.0001(10)
C28 0.0238(13) 0.0229(13) 0.0237(14) -0.0016(10) -0.0018(11) -0.0009(11)
C29 0.0278(13) 0.0246(13) 0.0266(14) 0.0001(11) -0.0023(12) -0.0045(11)
C30 0.0287(12) 0.0236(13) 0.0278(14) -0.0014(11) -0.0053(12) -0.0027(11)
C31 0.0365(15) 0.0298(15) 0.0447(19) 0.0054(13) -0.0053(15) -0.0065(13)
C32 0.0333(15) 0.0325(15) 0.0347(16) -0.0067(13) -0.0082(13) -0.0041(13)
C33 0.0202(12) 0.0358(16) 0.0384(17) -0.0003(13) 0.0054(12) -0.0015(12)
C34 0.0202(12) 0.0427(17) 0.0477(19) -0.0007(15) -0.0012(13) -0.0050(12)
C35 0.0297(14) 0.0482(19) 0.0466(19) -0.0112(16) -0.0047(14) -0.0102(14)
C36 0.0243(13) 0.0478(18) 0.0342(16) -0.0150(14) 0.0026(13) -0.0020(13)
C37 0.0201(12) 0.0293(14) 0.0202(13) -0.0009(11) -0.0010(10) -0.0016(11)
C38 0.0185(11) 0.0271(13) 0.0206(14) -0.0016(11) 0.0004(10) 0.0013(10)
C39 0.0157(11) 0.0289(14) 0.0236(14) 0.0010(11) -0.0018(10) 0.0014(10)
C40 0.0181(11) 0.0264(13) 0.0258(14) -0.0042(11) -0.0025(11) -0.0004(10)
C41 0.0202(12) 0.0400(16) 0.0267(15) -0.0028(12) 0.0016(11) 0.0054(12)
C42 0.0220(12) 0.0369(16) 0.0410(18) -0.0129(14) -0.0041(13) 0.0003(12)
O8W 0.0614(18) 0.086(2) 0.157(3) 0.020(2) 0.008(2) 0.0227(18)

_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 O1W 2.0133(18) . ?
Ni1 O13 2.0651(18) . ?
Ni1 N8 2.084(2) . ?
Ni1 N7 2.126(2) . ?
Ni1 N6 2.146(2) . ?
Ni1 O5 2.1505(18) 4_646 ?
Ni2 O4 2.0672(18) . ?
Ni2 O2W 2.0779(18) . ?
Ni2 N5 2.080(2) . ?
Ni2 O3W 2.0871(18) . ?
Ni2 N4 2.102(2) . ?
Ni2 N3 2.116(2) . ?
Ni3 O4W 2.0415(17) . ?
Ni3 O5W 2.0528(17) . ?
Ni3 O7 2.0666(18) . ?
Ni3 N1 2.085(2) . ?
Ni3 N2 2.127(2) . ?
Ni3 N12 2.184(2) . ?
Ni4 O12 2.0635(18) . ?
Ni4 O6W 2.0695(19) . ?
Ni4 N11 2.094(2) . ?
Ni4 O7W 2.1005(19) . ?
Ni4 N10 2.103(2) . ?
Ni4 N9 2.156(2) . ?
O1 C9 1.233(3) . ?
O1W H1WA 0.8202 . ?
O1W H1WB 0.8196 . ?
O2W H2WA 0.8199 . ?
O2W H2WB 0.8200 . ?
O2 C9 1.296(3) . ?
O2 H2 0.8200 . ?
O3W H3WA 0.8201 . ?
O3W H3WB 0.8197 . ?
O3 C10 1.264(3) . ?
O4W H4WA 0.8202 . ?
O4W H4WB 0.8199 . ?
O4 C10 1.257(3) . ?
O5W H5WB 0.8198 . ?
O5W H5WA 0.8200 . ?
O5 C22 1.287(3) . ?
O5 Ni1 2.1505(18) 4_656 ?
O6W H6WA 0.8199 . ?
O6W H6WB 0.8201 . ?
O6 C22 1.231(3) . ?
O7 C21 1.231(3) . ?
O7W H7WA 0.8198 . ?
O7W H7WB 0.8195 . ?
O8 C21 1.299(3) . ?
O8 H8 0.8197 . ?
O9 C31 1.213(3) . ?
O10 C31 1.312(3) . ?
O10 H10 0.8195 . ?
O11 C32 1.249(3) . ?
O12 C32 1.263(3) . ?
O13 C41 1.269(3) . ?
O14 C41 1.250(3) . ?
O15 C42 1.293(3) . ?
O15 H15 0.8193 . ?
O16 C42 1.223(3) . ?
N1 C1 1.340(3) . ?
N1 C5 1.357(3) . ?
N2 C6 1.351(3) . ?
N2 C7 1.370(3) . ?
N3 C6 1.341(3) . ?
N3 C8 1.362(3) . ?
N4 C33 1.343(3) . ?
N4 C37 1.344(3) . ?
N5 C38 1.343(3) . ?
N5 C40 1.370(3) . ?
N6 C38 1.347(3) . ?
N6 C39 1.366(3) . ?
N7 C28 1.355(3) . ?
N7 C29 1.377(3) . ?
N8 C27 1.348(3) . ?
N8 C23 1.350(3) . ?
N9 C28 1.346(3) . ?
N9 C30 1.370(3) . ?
N10 C15 1.338(3) . ?
N10 C11 1.341(3) . ?
N11 C16 1.353(3) . ?
N11 C20 1.364(3) . ?
N12 C16 1.343(3) . ?
N12 C17 1.372(3) . ?
C1 C2 1.383(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.379(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.386(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.369(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.472(3) . ?
C7 C8 1.397(3) . ?
C7 C9 1.476(3) . ?
C8 C10 1.490(3) . ?
C11 C12 1.374(4) . ?
C11 H11 0.9300 . ?
C12 C13 1.375(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.379(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.387(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.463(3) . ?
C17 C20 1.385(3) . ?
C17 C21 1.465(3) . ?
C20 C22 1.500(3) . ?
C23 C24 1.393(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.367(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.388(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.383(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.461(3) . ?
C29 C30 1.390(3) . ?
C29 C31 1.488(4) . ?
C30 C32 1.481(3) . ?
C33 C34 1.376(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.380(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.387(3) . ?
C35 H35 0.9300 . ?
C36 C37 1.391(3) . ?
C36 H36 0.9300 . ?
C37 C38 1.466(3) . ?
C39 C40 1.393(3) . ?
C39 C41 1.467(3) . ?
C40 C42 1.472(3) . ?
O8W H8WA 0.8196 . ?
O8W H8WB 0.8201 . ?

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
O1W Ni1 O13 90.66(8) . . ?
O1W Ni1 N8 176.17(9) . . ?
O13 Ni1 N8 93.13(8) . . ?
O1W Ni1 N7 96.61(8) . . ?
O13 Ni1 N7 169.71(8) . . ?
N8 Ni1 N7 79.72(8) . . ?
O1W Ni1 N6 89.92(8) . . ?
O13 Ni1 N6 79.00(7) . . ?
N8 Ni1 N6 90.23(8) . . ?
N7 Ni1 N6 108.19(8) . . ?
O1W Ni1 O5 95.06(8) . 4_646 ?
O13 Ni1 O5 85.26(7) . 4_646 ?
N8 Ni1 O5 85.85(8) . 4_646 ?
N7 Ni1 O5 86.84(8) . 4_646 ?
N6 Ni1 O5 163.55(8) . 4_646 ?
O4 Ni2 O2W 85.70(8) . . ?
O4 Ni2 N5 171.65(8) . . ?
O2W Ni2 N5 102.49(8) . . ?
O4 Ni2 O3W 91.91(8) . . ?
O2W Ni2 O3W 82.61(7) . . ?
N5 Ni2 O3W 87.55(8) . . ?
O4 Ni2 N4 92.17(8) . . ?
O2W Ni2 N4 175.69(8) . . ?
N5 Ni2 N4 79.55(8) . . ?
O3W Ni2 N4 93.73(8) . . ?
O4 Ni2 N3 79.61(7) . . ?
O2W Ni2 N3 91.66(8) . . ?
N5 Ni2 N3 101.58(8) . . ?
O3W Ni2 N3 170.13(8) . . ?
N4 Ni2 N3 91.64(8) . . ?
O4W Ni3 O5W 87.49(7) . . ?
O4W Ni3 O7 91.79(8) . . ?
O5W Ni3 O7 83.91(7) . . ?
O4W Ni3 N1 174.45(8) . . ?
O5W Ni3 N1 88.36(8) . . ?
O7 Ni3 N1 91.45(8) . . ?
O4W Ni3 N2 95.37(8) . . ?
O5W Ni3 N2 88.17(8) . . ?
O7 Ni3 N2 169.08(8) . . ?
N1 Ni3 N2 80.80(8) . . ?
O4W Ni3 N12 89.56(7) . . ?
O5W Ni3 N12 162.57(8) . . ?
O7 Ni3 N12 79.01(7) . . ?
N1 Ni3 N12 95.49(8) . . ?
N2 Ni3 N12 109.22(8) . . ?
O12 Ni4 O6W 86.11(8) . . ?
O12 Ni4 N11 168.57(8) . . ?
O6W Ni4 N11 105.08(8) . . ?
O12 Ni4 O7W 86.68(8) . . ?
O6W Ni4 O7W 85.82(8) . . ?
N11 Ni4 O7W 91.68(8) . . ?
O12 Ni4 N10 90.09(8) . . ?
O6W Ni4 N10 175.49(8) . . ?
N11 Ni4 N10 78.84(8) . . ?
O7W Ni4 N10 96.38(9) . . ?
O12 Ni4 N9 79.45(8) . . ?
O6W Ni4 N9 88.26(8) . . ?
N11 Ni4 N9 102.90(8) . . ?
O7W Ni4 N9 165.26(8) . . ?
N10 Ni4 N9 88.67(8) . . ?
Ni1 O1W H1WA 149.2 . . ?
Ni1 O1W H1WB 106.9 . . ?
H1WA O1W H1WB 103.9 . . ?
Ni2 O2W H2WA 122.3 . . ?
Ni2 O2W H2WB 101.4 . . ?
H2WA O2W H2WB 103.1 . . ?
C9 O2 H2 106.2 . . ?
Ni2 O3W H3WA 122.3 . . ?
Ni2 O3W H3WB 106.2 . . ?
H3WA O3W H3WB 109.7 . . ?
Ni3 O4W H4WA 121.7 . . ?
Ni3 O4W H4WB 109.9 . . ?
H4WA O4W H4WB 97.0 . . ?
C10 O4 Ni2 113.94(16) . . ?
Ni3 O5W H5WB 131.0 . . ?
Ni3 O5W H5WA 124.3 . . ?
H5WB O5W H5WA 101.6 . . ?
C22 O5 Ni1 131.36(17) . 4_656 ?
Ni4 O6W H6WA 121.0 . . ?
Ni4 O6W H6WB 109.9 . . ?
H6WA O6W H6WB 115.4 . . ?
C21 O7 Ni3 115.24(17) . . ?
Ni4 O7W H7WA 124.8 . . ?
Ni4 O7W H7WB 123.0 . . ?
H7WA O7W H7WB 108.0 . . ?
C21 O8 H8 104.5 . . ?
C31 O10 H10 109.9 . . ?
C32 O12 Ni4 116.60(17) . . ?
C41 O13 Ni1 116.01(16) . . ?
C42 O15 H15 116.6 . . ?
C1 N1 C5 117.2(2) . . ?
C1 N1 Ni3 127.34(19) . . ?
C5 N1 Ni3 113.86(16) . . ?
C6 N2 C7 104.2(2) . . ?
C6 N2 Ni3 109.53(16) . . ?
C7 N2 Ni3 146.22(17) . . ?
C6 N3 C8 103.9(2) . . ?
C6 N3 Ni2 145.07(17) . . ?
C8 N3 Ni2 107.99(17) . . ?
C33 N4 C37 118.0(2) . . ?
C33 N4 Ni2 128.08(19) . . ?
C37 N4 Ni2 113.88(16) . . ?
C38 N5 C40 104.4(2) . . ?
C38 N5 Ni2 112.11(15) . . ?
C40 N5 Ni2 143.45(18) . . ?
C38 N6 C39 103.5(2) . . ?
C38 N6 Ni1 147.51(17) . . ?
C39 N6 Ni1 108.18(16) . . ?
C28 N7 C29 104.4(2) . . ?
C28 N7 Ni1 110.51(16) . . ?
C29 N7 Ni1 144.79(18) . . ?
C27 N8 C23 117.5(2) . . ?
C27 N8 Ni1 115.19(17) . . ?
C23 N8 Ni1 126.78(19) . . ?
C28 N9 C30 104.3(2) . . ?
C28 N9 Ni4 146.19(18) . . ?
C30 N9 Ni4 107.65(16) . . ?
C15 N10 C11 118.1(3) . . ?
C15 N10 Ni4 114.27(17) . . ?
C11 N10 Ni4 127.4(2) . . ?
C16 N11 C20 104.7(2) . . ?
C16 N11 Ni4 111.14(17) . . ?
C20 N11 Ni4 143.50(18) . . ?
C16 N12 C17 103.4(2) . . ?
C16 N12 Ni3 148.50(18) . . ?
C17 N12 Ni3 107.92(16) . . ?
N1 C1 C2 123.5(3) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 H2A 120.7 . . ?
C1 C2 H2A 120.7 . . ?
C2 C3 C4 118.5(3) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 C5 C4 122.4(2) . . ?
N1 C5 C6 114.4(2) . . ?
C4 C5 C6 122.9(2) . . ?
N3 C6 N2 114.7(2) . . ?
N3 C6 C5 124.4(2) . . ?
N2 C6 C5 120.5(2) . . ?
N2 C7 C8 107.7(2) . . ?
N2 C7 C9 124.3(2) . . ?
C8 C7 C9 128.0(2) . . ?
N3 C8 C7 109.4(2) . . ?
N3 C8 C10 116.6(2) . . ?
C7 C8 C10 133.9(2) . . ?
O1 C9 O2 119.4(3) . . ?
O1 C9 C7 122.1(3) . . ?
O2 C9 C7 118.4(2) . . ?
O4 C10 O3 123.4(3) . . ?
O4 C10 C8 117.1(2) . . ?
O3 C10 C8 119.5(3) . . ?
N10 C11 C12 123.2(3) . . ?
N10 C11 H11 118.4 . . ?
C12 C11 H11 118.4 . . ?
C11 C12 C13 118.6(3) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C12 C13 C14 118.9(3) . . ?
C12 C13 H13 120.5 . . ?
C14 C13 H13 120.5 . . ?
C13 C14 C15 119.3(3) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
N10 C15 C14 121.8(2) . . ?
N10 C15 C16 114.1(2) . . ?
C14 C15 C16 124.0(3) . . ?
N12 C16 N11 114.4(2) . . ?
N12 C16 C15 126.5(2) . . ?
N11 C16 C15 118.9(2) . . ?
N12 C17 C20 109.7(2) . . ?
N12 C17 C21 116.9(2) . . ?
C20 C17 C21 133.3(2) . . ?
N11 C20 C17 107.8(2) . . ?
N11 C20 C22 122.7(2) . . ?
C17 C20 C22 129.4(2) . . ?
O7 C21 O8 120.1(3) . . ?
O7 C21 C17 120.0(2) . . ?
O8 C21 C17 119.9(2) . . ?
O6 C22 O5 124.5(3) . . ?
O6 C22 C20 119.5(2) . . ?
O5 C22 C20 116.0(2) . . ?
N8 C23 C24 122.6(3) . . ?
N8 C23 H23 118.7 . . ?
C24 C23 H23 118.7 . . ?
C25 C24 C23 119.1(3) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C24 C25 C26 118.9(3) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 H25 120.5 . . ?
C27 C26 C25 119.3(3) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
N8 C27 C26 122.5(2) . . ?
N8 C27 C28 114.3(2) . . ?
C26 C27 C28 122.9(2) . . ?
N9 C28 N7 114.1(2) . . ?
N9 C28 C27 125.6(2) . . ?
N7 C28 C27 120.0(2) . . ?
N7 C29 C30 108.1(2) . . ?
N7 C29 C31 123.0(2) . . ?
C30 C29 C31 128.8(2) . . ?
N9 C30 C29 109.1(2) . . ?
N9 C30 C32 118.5(2) . . ?
C29 C30 C32 132.4(2) . . ?
O9 C31 O10 120.2(3) . . ?
O9 C31 C29 123.5(3) . . ?
O10 C31 C29 116.2(3) . . ?
O11 C32 O12 123.3(3) . . ?
O11 C32 C30 120.7(3) . . ?
O12 C32 C30 116.0(2) . . ?
N4 C33 C34 122.8(3) . . ?
N4 C33 H33 118.6 . . ?
C34 C33 H33 118.6 . . ?
C33 C34 C35 119.3(3) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C36 118.8(3) . . ?
C34 C35 H35 120.6 . . ?
C36 C35 H35 120.6 . . ?
C35 C36 C37 118.7(3) . . ?
C35 C36 H36 120.7 . . ?
C37 C36 H36 120.7 . . ?
N4 C37 C36 122.4(2) . . ?
N4 C37 C38 114.6(2) . . ?
C36 C37 C38 122.8(2) . . ?
N5 C38 N6 114.8(2) . . ?
N5 C38 C37 118.8(2) . . ?
N6 C38 C37 125.7(2) . . ?
N6 C39 C40 109.5(2) . . ?
N6 C39 C41 118.4(2) . . ?
C40 C39 C41 131.8(2) . . ?
N5 C40 C39 107.7(2) . . ?
N5 C40 C42 122.5(2) . . ?
C39 C40 C42 129.7(2) . . ?
O14 C41 O13 122.7(2) . . ?
O14 C41 C39 121.0(2) . . ?
O13 C41 C39 116.2(2) . . ?
O16 C42 O15 119.3(3) . . ?
O16 C42 C40 122.4(2) . . ?
O15 C42 C40 118.3(3) . . ?
H8WA O8W H8WB 107.1 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O4 0.82 2.04 2.862(3) 174.6 3_557
O1W H1WB O9 0.82 1.90 2.608(3) 144.3 .
O2W H2WA O1 0.82 2.09 2.884(3) 161.9 3_567
O2W H2WB O16 0.82 1.81 2.606(3) 164.8 .
O2 H2 O3 0.82 1.68 2.467(3) 161.0 .
O3W H3WA O13 0.82 2.02 2.801(3) 159.3 3_457
O3W H3WB O6 0.82 1.94 2.692(3) 152.6 2_565
O4W H4WA O12 0.82 1.87 2.666(3) 162.4 4_556
O4W H4WB O1 0.82 1.78 2.584(3) 167.2 .
O5W H5WB O3 0.82 2.05 2.804(3) 153.9 3_567
O5W H5WA O16 0.82 1.90 2.719(3) 178.7 3_467
O5W H5WA O15 0.82 2.55 3.076(3) 123.5 3_467
O6W H6WA O8W 0.82 1.97 2.775(4) 167.1 .
O6W H6WB O2W 0.82 2.21 2.989(3) 159.0 2_564
O7W H7WA O10 0.82 2.07 2.885(3) 169.8 4_556
O7W H7WB O4W 0.82 2.27 2.852(3) 128.4 4_546
O8 H8 O5 0.82 1.63 2.445(3) 172.9 .
O10 H10 O11 0.82 1.62 2.439(3) 175.5 .
O15 H15 O14 0.82 1.67 2.459(3) 162.4 .
O8W H8WA O7 0.82 2.31 3.000(3) 141.6 4_646
O8W H8WB O6 0.82 2.57 3.173(3) 131.5 .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.064