# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7278new
_database_code_depnum_ccdc_archive 'CCDC 2040401'
loop_
_audit_author_name
_audit_author_address
'Dr Thomas Weyhermueller'
;Max Planck Institute Chemische Energiekonversion
Germany
;
_audit_update_record             
;
2020-10-24 deposited with the CCDC.	2020-12-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_audit_creation_date             2011-03-09
_audit_block_code                7278
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H15 N Ni O6, 1.75(H2 O)'
_chemical_formula_sum            'C15 H18.50 N Ni O7.75'
_chemical_formula_weight         395.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.343(2)
_cell_length_b                   14.617(3)
_cell_length_c                   18.348(3)
_cell_angle_alpha                81.497(9)
_cell_angle_beta                 89.659(8)
_cell_angle_gamma                89.249(9)
_cell_volume                     3273.6(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9132
_cell_measurement_theta_min      2.4349
_cell_measurement_theta_max      66.1558

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0400
0.00 0.00 -1.00 0.0400
0.00 -1.00 0.00 0.1200
0.00 1.00 0.00 0.1500
-1.00 0.00 -1.00 0.0700
1.00 0.00 1.00 0.0500
1.00 -1.00 1.00 0.0800
2.00 2.00 1.00 0.1200
-2.00 -2.00 -1.00 0.1000

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_F_000             1644
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.114
_shelx_estimated_absorpt_T_min   0.555
_shelx_estimated_absorpt_T_max   0.849
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_absorpt_correction_T_min  0.67295
_exptl_absorpt_correction_T_max  0.88345
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_monochromator  'focusing multilayer optic'
_diffrn_measurement_device_type  'Bruker AXS X8 Proteum'
_diffrn_measurement_method       'CCD φ- and ω-scans'
_diffrn_detector_area_resol_mean 66.67
_diffrn_reflns_number            74139
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.435
_diffrn_reflns_theta_max         66.924
_diffrn_reflns_theta_full        66.924
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measured_fraction_theta_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             11191
_reflns_number_gt                9918
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PROTEUM2 (Bruker AXS, 2008)'
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0209P)²+18.3522P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11191
_refine_ls_number_parameters     964
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0643
_refine_ls_wR_factor_ref         0.1572
_refine_ls_wR_factor_gt          0.1538
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.099
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.61126(5) 0.14016(5) 0.28546(4) 0.01673(17) Uani 1 1 d . . . . .
Ni2 Ni 0.60674(6) 0.64119(5) 0.27421(4) 0.01901(18) Uani 1 1 d . . . . .
Ni3 Ni 0.89962(6) 0.38739(5) 0.27807(4) 0.01771(17) Uani 1 1 d . . . . .
Ni4 Ni 0.90537(6) -0.11133(5) 0.27769(4) 0.01776(17) Uani 1 1 d . . . . .
O101 O 0.7449(2) 0.1500(2) 0.22194(15) 0.0182(6) Uani 1 1 d . . . . .
C102 C 0.7184(3) 0.1579(3) 0.1508(2) 0.0179(8) Uani 1 1 d . . . . .
C103 C 0.7982(4) 0.1647(3) 0.0957(2) 0.0232(9) Uani 1 1 d . . . . .
H103 H 0.872593 0.164597 0.108768 0.028 Uiso 1 1 calc R U . . .
C104 C 0.7693(4) 0.1715(3) 0.0227(2) 0.0260(10) Uani 1 1 d . . . . .
H104 H 0.824005 0.176361 -0.014267 0.031 Uiso 1 1 calc R U . . .
C105 C 0.6612(4) 0.1713(3) 0.0024(2) 0.0270(10) Uani 1 1 d . . . . .
H105 H 0.642394 0.175117 -0.048098 0.032 Uiso 1 1 calc R U . . .
C106 C 0.5808(4) 0.1656(3) 0.0557(2) 0.0231(9) Uani 1 1 d . . . . .
H106 H 0.506690 0.165924 0.041969 0.028 Uiso 1 1 calc R U . . .
C107 C 0.6092(3) 0.1595(3) 0.1299(2) 0.0190(9) Uani 1 1 d . . . . .
N108 N 0.5331(3) 0.1539(2) 0.18910(19) 0.0182(7) Uani 1 1 d . . . . .
C109 C 0.4306(4) 0.1579(3) 0.1801(3) 0.0241(10) Uani 1 1 d . . . . .
H109 H 0.405917 0.166200 0.130562 0.029 Uiso 1 1 calc R U . . .
C110 C 0.3460(3) 0.1510(3) 0.2376(3) 0.0226(9) Uani 1 1 d . . . . .
C111 C 0.2397(4) 0.1572(3) 0.2107(3) 0.0274(10) Uani 1 1 d . . . . .
H111 H 0.228896 0.165977 0.158934 0.033 Uiso 1 1 calc R U . . .
C112 C 0.1499(4) 0.1510(3) 0.2565(3) 0.0296(11) Uani 1 1 d . . . . .
H112 H 0.078753 0.155555 0.236707 0.036 Uiso 1 1 calc R U . . .
C113 C 0.1663(4) 0.1380(3) 0.3320(3) 0.0285(10) Uani 1 1 d . . . . .
H113 H 0.105581 0.133376 0.364296 0.034 Uiso 1 1 calc R U . . .
C114 C 0.2696(4) 0.1317(3) 0.3610(3) 0.0264(10) Uani 1 1 d . . . . .
H114 H 0.279378 0.122970 0.412917 0.032 Uiso 1 1 calc R U . . .
C115 C 0.3596(3) 0.1380(3) 0.3144(3) 0.0223(9) Uani 1 1 d . . . . .
O116 O 0.4631(2) 0.1312(2) 0.34239(16) 0.0228(7) Uani 1 1 d . . . . .
C117 C 0.4753(4) 0.1218(3) 0.4215(2) 0.0259(10) Uani 1 1 d . . . . .
H11A H 0.440018 0.064330 0.444964 0.031 Uiso 1 1 calc R U . . .
H11B H 0.439452 0.174759 0.440160 0.031 Uiso 1 1 calc R U . . .
C118 C 0.5950(4) 0.1185(3) 0.4416(2) 0.0243(10) Uani 1 1 d . . . . .
O119 O 0.6648(2) 0.1243(2) 0.39119(16) 0.0234(7) Uani 1 1 d . . . . .
O120 O 0.6147(3) 0.1099(2) 0.50926(17) 0.0309(8) Uani 1 1 d . . . . .
O130 O 0.6054(2) 0.2815(2) 0.28335(16) 0.0210(6) Uani 1 1 d D . . . .
H131 H 0.655(3) 0.308(3) 0.258(2) 0.032 Uiso 1 1 d D U . . .
H132 H 0.600(4) 0.299(3) 0.3247(14) 0.032 Uiso 1 1 d D U . . .
O140 O 0.6131(2) -0.0004(2) 0.28909(17) 0.0222(6) Uani 1 1 d D . . . .
H141 H 0.661(3) -0.020(3) 0.262(2) 0.033 Uiso 1 1 d D U . . .
H142 H 0.596(4) -0.038(3) 0.3260(18) 0.033 Uiso 1 1 d D U . . .
O201 O 0.7503(2) 0.6523(2) 0.22053(16) 0.0226(6) Uani 1 1 d . . . . .
C202 C 0.7348(4) 0.6608(3) 0.1480(2) 0.0232(9) Uani 1 1 d . . . . .
C203 C 0.8216(4) 0.6703(3) 0.0974(3) 0.0310(11) Uani 1 1 d . . . . .
H203 H 0.893572 0.670714 0.115402 0.037 Uiso 1 1 calc R U . . .
C204 C 0.8050(4) 0.6789(4) 0.0234(3) 0.0360(12) Uani 1 1 d . . . . .
H204 H 0.865122 0.685814 -0.009380 0.043 Uiso 1 1 calc R U . . .
C205 C 0.6999(4) 0.6776(4) -0.0047(3) 0.0339(11) Uani 1 1 d . . . . .
H205 H 0.688622 0.683160 -0.056384 0.041 Uiso 1 1 calc R U . . .
C206 C 0.6137(4) 0.6681(3) 0.0427(2) 0.0266(10) Uani 1 1 d . . . . .
H206 H 0.542400 0.666184 0.023797 0.032 Uiso 1 1 calc R U . . .
C207 C 0.6291(4) 0.6613(3) 0.1186(2) 0.0226(9) Uani 1 1 d . . . . .
N208 N 0.5446(3) 0.6551(2) 0.17269(19) 0.0185(7) Uani 1 1 d . . . . .
C209 C 0.4452(4) 0.6635(3) 0.1555(2) 0.0233(9) Uani 1 1 d . . . . .
H209 H 0.429617 0.674453 0.104294 0.028 Uiso 1 1 calc R U . . .
C210 C 0.3513(3) 0.6581(3) 0.2054(2) 0.0215(9) Uani 1 1 d . . . . .
C211 C 0.2508(4) 0.6710(3) 0.1697(3) 0.0306(11) Uani 1 1 d . . . . .
H211 H 0.249401 0.684426 0.117432 0.037 Uiso 1 1 calc R U . . .
C212 C 0.1545(4) 0.6648(4) 0.2078(3) 0.0345(12) Uani 1 1 d . . . . .
H212 H 0.087536 0.673686 0.182331 0.041 Uiso 1 1 calc R U . . .
C213 C 0.1563(4) 0.6455(4) 0.2837(3) 0.0358(12) Uani 1 1 d . . . . .
H213 H 0.090137 0.640518 0.310572 0.043 Uiso 1 1 calc R U . . .
C214 C 0.2541(4) 0.6335(4) 0.3209(3) 0.0324(11) Uani 1 1 d . . . . .
H214 H 0.254387 0.619795 0.373181 0.039 Uiso 1 1 calc R U . . .
C215 C 0.3514(4) 0.6412(3) 0.2825(3) 0.0250(10) Uani 1 1 d . . . . .
O216 O 0.4499(3) 0.6306(2) 0.31863(16) 0.0268(7) Uani 1 1 d . . . . .
C217 C 0.4484(5) 0.6126(5) 0.3979(3) 0.0526(18) Uani 1 1 d . . . . .
H21A H 0.414440 0.552147 0.414586 0.063 Uiso 1 1 calc R U . . .
H21B H 0.405134 0.661120 0.417467 0.063 Uiso 1 1 calc R U . . .
C218 C 0.5640(5) 0.6118(4) 0.4268(3) 0.0434(15) Uani 1 1 d . . . . .
O219 O 0.6410(3) 0.6259(2) 0.38363(18) 0.0304(8) Uani 1 1 d . . . . .
O220 O 0.5732(4) 0.5969(4) 0.4953(2) 0.0743(17) Uani 1 1 d . . . . .
O230 O 0.5966(2) 0.7825(2) 0.27236(16) 0.0211(6) Uani 1 1 d D . . . .
H231 H 0.652(3) 0.811(3) 0.256(3) 0.032 Uiso 1 1 d D U . . .
H232 H 0.578(4) 0.803(3) 0.3109(17) 0.032 Uiso 1 1 d D U . . .
O240 O 0.6095(3) 0.4997(2) 0.28047(17) 0.0238(7) Uani 1 1 d D . . . .
H241 H 0.661(3) 0.484(4) 0.255(3) 0.036 Uiso 1 1 d D U . . .
H242 H 0.607(5) 0.473(3) 0.3242(11) 0.036 Uiso 1 1 d D U . . .
O301 O 0.7606(2) 0.4008(2) 0.22018(15) 0.0200(6) Uani 1 1 d . . . . .
C302 C 0.7822(3) 0.4077(3) 0.1483(2) 0.0204(9) Uani 1 1 d . . . . .
C303 C 0.6985(4) 0.4149(3) 0.0962(2) 0.0261(10) Uani 1 1 d . . . . .
H303 H 0.625142 0.415167 0.112187 0.031 Uiso 1 1 calc R U . . .
C304 C 0.7220(4) 0.4217(3) 0.0222(3) 0.0314(11) Uani 1 1 d . . . . .
H304 H 0.664479 0.427312 -0.012420 0.038 Uiso 1 1 calc R U . . .
C305 C 0.8284(4) 0.4204(3) -0.0029(2) 0.0313(11) Uani 1 1 d . . . . .
H305 H 0.843470 0.424030 -0.054077 0.038 Uiso 1 1 calc R U . . .
C306 C 0.9123(4) 0.4138(3) 0.0476(2) 0.0264(10) Uani 1 1 d . . . . .
H306 H 0.985216 0.412731 0.030876 0.032 Uiso 1 1 calc R U . . .
C307 C 0.8905(4) 0.4089(3) 0.1224(2) 0.0204(9) Uani 1 1 d . . . . .
N308 N 0.9694(3) 0.4031(2) 0.17894(19) 0.0200(8) Uani 1 1 d . . . . .
C309 C 1.0718(4) 0.4116(3) 0.1651(2) 0.0235(9) Uani 1 1 d . . . . .
H309 H 1.092168 0.423281 0.114558 0.028 Uiso 1 1 calc R U . . .
C310 C 1.1594(4) 0.4051(3) 0.2184(3) 0.0240(10) Uani 1 1 d . . . . .
C311 C 1.2630(4) 0.4201(3) 0.1867(3) 0.0331(11) Uani 1 1 d . . . . .
H311 H 1.269365 0.436079 0.134789 0.040 Uiso 1 1 calc R U . . .
C312 C 1.3560(4) 0.4123(4) 0.2294(3) 0.0373(12) Uani 1 1 d . . . . .
H312 H 1.425040 0.423092 0.206859 0.045 Uiso 1 1 calc R U . . .
C313 C 1.3473(4) 0.3887(3) 0.3045(3) 0.0367(12) Uani 1 1 d . . . . .
H313 H 1.410878 0.381872 0.333881 0.044 Uiso 1 1 calc R U . . .
C314 C 1.2467(4) 0.3747(3) 0.3376(3) 0.0311(11) Uani 1 1 d . . . . .
H314 H 1.241554 0.358689 0.389624 0.037 Uiso 1 1 calc R U . . .
C315 C 1.1529(4) 0.3842(3) 0.2951(3) 0.0253(10) Uani 1 1 d . . . . .
O316 O 1.0517(2) 0.3716(2) 0.32821(16) 0.0236(7) Uani 1 1 d . . . . .
C317 C 1.0450(4) 0.3541(4) 0.4078(2) 0.0304(11) Uani 1 1 d . . . . .
H31A H 1.085296 0.402044 0.428866 0.037 Uiso 1 1 calc R U . . .
H31B H 1.078303 0.293133 0.426104 0.037 Uiso 1 1 calc R U . . .
C318 C 0.9278(4) 0.3553(3) 0.4320(2) 0.0275(10) Uani 1 1 d . . . . .
O319 O 0.8535(3) 0.3694(2) 0.38537(15) 0.0242(7) Uani 1 1 d . . . . .
O320 O 0.9117(3) 0.3422(3) 0.50053(17) 0.0412(9) Uani 1 1 d . . . . .
O330 O 0.9072(2) 0.5283(2) 0.27837(16) 0.0215(6) Uani 1 1 d D . . . .
H331 H 0.851(3) 0.559(3) 0.264(3) 0.032 Uiso 1 1 d D U . . .
H332 H 0.924(4) 0.551(3) 0.3159(18) 0.032 Uiso 1 1 d D U . . .
O340 O 0.8990(2) 0.2468(2) 0.27968(16) 0.0204(6) Uani 1 1 d D . . . .
H341 H 0.853(3) 0.221(3) 0.256(3) 0.031 Uiso 1 1 d D U . . .
H342 H 0.895(4) 0.214(3) 0.3209(14) 0.031 Uiso 1 1 d D U . . .
O401 O 0.7608(2) -0.1003(2) 0.22504(15) 0.0189(6) Uani 1 1 d . . . . .
C402 C 0.7751(3) -0.0920(3) 0.1525(2) 0.0190(9) Uani 1 1 d . . . . .
C403 C 0.6878(4) -0.0843(3) 0.1038(2) 0.0236(9) Uani 1 1 d . . . . .
H403 H 0.616061 -0.083604 0.122662 0.028 Uiso 1 1 calc R U . . .
C404 C 0.7039(4) -0.0776(3) 0.0289(3) 0.0288(10) Uani 1 1 d . . . . .
H404 H 0.643201 -0.071625 -0.003134 0.035 Uiso 1 1 calc R U . . .
C405 C 0.8078(4) -0.0796(3) -0.0003(3) 0.0308(11) Uani 1 1 d . . . . .
H405 H 0.818049 -0.076504 -0.051977 0.037 Uiso 1 1 calc R U . . .
C406 C 0.8963(4) -0.0862(3) 0.0460(2) 0.0251(10) Uani 1 1 d . . . . .
H406 H 0.967532 -0.087266 0.026219 0.030 Uiso 1 1 calc R U . . .
C407 C 0.8811(3) -0.0912(3) 0.1219(2) 0.0208(9) Uani 1 1 d . . . . .
N408 N 0.9652(3) -0.0960(2) 0.17446(19) 0.0201(8) Uani 1 1 d . . . . .
C409 C 1.0658(4) -0.0879(3) 0.1557(3) 0.0249(10) Uani 1 1 d . . . . .
H409 H 1.079960 -0.079072 0.104187 0.030 Uiso 1 1 calc R U . . .
C410 C 1.1600(4) -0.0904(3) 0.2023(3) 0.0247(10) Uani 1 1 d . . . . .
C411 C 1.2594(4) -0.0803(3) 0.1640(3) 0.0288(10) Uani 1 1 d . . . . .
H411 H 1.259024 -0.073097 0.111640 0.035 Uiso 1 1 calc R U . . .
C412 C 1.3566(4) -0.0805(3) 0.1996(3) 0.0311(11) Uani 1 1 d . . . . .
H412 H 1.422564 -0.073668 0.172496 0.037 Uiso 1 1 calc R U . . .
C413 C 1.3571(4) -0.0906(3) 0.2753(3) 0.0278(10) Uani 1 1 d . . . . .
H413 H 1.424105 -0.090707 0.300560 0.033 Uiso 1 1 calc R U . . .
C414 C 1.2617(4) -0.1007(3) 0.3152(3) 0.0288(10) Uani 1 1 d . . . . .
H414 H 1.263625 -0.107013 0.367478 0.035 Uiso 1 1 calc R U . . .
C415 C 1.1625(3) -0.1015(3) 0.2793(2) 0.0220(9) Uani 1 1 d . . . . .
O416 O 1.0662(2) -0.1130(2) 0.31845(17) 0.0257(7) Uani 1 1 d . . . . .
C417 C 1.0706(4) -0.1143(3) 0.3973(2) 0.0269(10) Uani 1 1 d . . . . .
H41A H 1.104071 -0.056695 0.408169 0.032 Uiso 1 1 calc R U . . .
H41B H 1.116040 -0.167213 0.419718 0.032 Uiso 1 1 calc R U . . .
C418 C 0.9579(4) -0.1227(3) 0.4303(2) 0.0263(10) Uani 1 1 d . . . . .
O419 O 0.8769(2) -0.1292(2) 0.38787(16) 0.0240(7) Uani 1 1 d . . . . .
O420 O 0.9522(3) -0.1245(3) 0.49751(17) 0.0338(8) Uani 1 1 d . . . . .
O430 O 0.9065(2) 0.0296(2) 0.27726(16) 0.0207(6) Uani 1 1 d D . . . .
H431 H 0.849(2) 0.057(3) 0.263(3) 0.031 Uiso 1 1 d D U . . .
H432 H 0.912(4) 0.046(3) 0.3192(13) 0.031 Uiso 1 1 d D U . . .
O440 O 0.9031(2) -0.2524(2) 0.28243(16) 0.0213(6) Uani 1 1 d D . . . .
H441 H 0.853(3) -0.275(3) 0.261(3) 0.032 Uiso 1 1 d D U . . .
H442 H 0.902(4) -0.286(3) 0.3238(14) 0.032 Uiso 1 1 d D U . . .
O510 O 1.1072(3) -0.1147(2) 0.59800(17) 0.0261(7) Uani 1 1 d D . . . .
H511 H 1.062(3) -0.115(4) 0.5642(19) 0.039 Uiso 1 1 d D U . . .
H512 H 1.1700(16) -0.112(4) 0.580(2) 0.039 Uiso 1 1 d D U . . .
O520 O 0.5580(3) -0.1387(2) 0.40102(17) 0.0291(7) Uani 1 1 d D . . . .
H521 H 0.507(3) -0.133(4) 0.430(2) 0.044 Uiso 1 1 d D U . . .
H522 H 0.613(2) -0.159(4) 0.425(2) 0.044 Uiso 1 1 d D U . . .
O530 O 0.9298(3) -0.3862(2) 0.40525(16) 0.0277(7) Uani 1 1 d D . . . .
H531 H 0.975(3) -0.367(4) 0.434(2) 0.041 Uiso 1 1 d D U . . .
H532 H 0.877(3) -0.409(4) 0.430(2) 0.041 Uiso 1 1 d D U . . .
O540 O 0.5923(4) 0.3715(2) 0.40838(19) 0.0429(10) Uani 1 1 d . . . . .
O550 O 0.7233(3) -0.2321(2) 0.47556(19) 0.0348(8) Uani 1 1 d . . . . .
O560 O 0.7886(3) 0.5167(3) 0.5033(3) 0.0560(12) Uani 1 1 d . . . . .
O570 O 0.7113(4) 0.2771(4) 0.5175(3) 0.0662(13) Uani 1 1 d D . . . .
H571 H 0.696(6) 0.223(3) 0.508(5) 0.099 Uiso 1 1 d D U . . .
H572 H 0.7794(16) 0.277(5) 0.526(5) 0.099 Uiso 1 1 d D U . . .


_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 N108 2.002(4) . ?
Ni1 O101 2.008(3) . ?
Ni1 O119 2.033(3) . ?
Ni1 O140 2.045(3) . ?
Ni1 O130 2.061(3) . ?
Ni1 O116 2.097(3) . ?
Ni2 N208 2.000(4) . ?
Ni2 O201 2.019(3) . ?
Ni2 O219 2.033(3) . ?
Ni2 O240 2.054(3) . ?
Ni2 O230 2.062(3) . ?
Ni2 O216 2.095(3) . ?
Ni3 N308 1.991(4) . ?
Ni3 O301 2.015(3) . ?
Ni3 O319 2.026(3) . ?
Ni3 O340 2.051(3) . ?
Ni3 O330 2.065(3) . ?
Ni3 O316 2.090(3) . ?
Ni4 N408 2.011(4) . ?
Ni4 O401 2.027(3) . ?
Ni4 O419 2.029(3) . ?
Ni4 O440 2.051(3) . ?
Ni4 O430 2.059(3) . ?
Ni4 O416 2.125(3) . ?
O101 C102 1.335(5) . ?
C102 C103 1.401(6) . ?
C102 C107 1.403(6) . ?
C103 C104 1.378(6) . ?
C104 C105 1.387(7) . ?
C105 C106 1.384(6) . ?
C106 C107 1.397(6) . ?
C107 N108 1.426(5) . ?
N108 C109 1.277(6) . ?
C109 C110 1.474(6) . ?
C110 C111 1.402(6) . ?
C110 C115 1.404(6) . ?
C111 C112 1.382(7) . ?
C112 C113 1.386(7) . ?
C113 C114 1.382(7) . ?
C114 C115 1.393(6) . ?
C115 O116 1.376(5) . ?
O116 C117 1.447(5) . ?
C117 C118 1.524(6) . ?
C118 O120 1.254(5) . ?
C118 O119 1.255(5) . ?
O201 C202 1.333(5) . ?
C202 C203 1.408(6) . ?
C202 C207 1.414(6) . ?
C203 C204 1.362(7) . ?
C204 C205 1.400(8) . ?
C205 C206 1.366(7) . ?
C206 C207 1.396(6) . ?
C207 N208 1.429(6) . ?
N208 C209 1.269(6) . ?
C209 C210 1.468(6) . ?
C210 C215 1.398(6) . ?
C210 C211 1.405(6) . ?
C211 C212 1.373(7) . ?
C212 C213 1.378(8) . ?
C213 C214 1.387(7) . ?
C214 C215 1.387(7) . ?
C215 O216 1.385(5) . ?
O216 C217 1.439(6) . ?
C217 C218 1.524(8) . ?
C218 O219 1.234(7) . ?
C218 O220 1.249(6) . ?
O301 C302 1.333(5) . ?
C302 C303 1.404(6) . ?
C302 C307 1.415(6) . ?
C303 C304 1.378(7) . ?
C304 C305 1.389(7) . ?
C305 C306 1.386(7) . ?
C306 C307 1.389(6) . ?
C307 N308 1.420(5) . ?
N308 C309 1.292(6) . ?
C309 C310 1.456(6) . ?
C310 C315 1.397(7) . ?
C310 C311 1.408(6) . ?
C311 C312 1.387(7) . ?
C312 C313 1.374(8) . ?
C313 C314 1.384(7) . ?
C314 C315 1.393(6) . ?
C315 O316 1.389(5) . ?
O316 C317 1.447(5) . ?
C317 C318 1.511(7) . ?
C318 O319 1.252(6) . ?
C318 O320 1.258(6) . ?
O401 C402 1.330(5) . ?
C402 C403 1.397(6) . ?
C402 C407 1.419(6) . ?
C403 C404 1.376(6) . ?
C404 C405 1.390(7) . ?
C405 C406 1.382(7) . ?
C406 C407 1.396(6) . ?
C407 N408 1.415(6) . ?
N408 C409 1.289(6) . ?
C409 C410 1.444(6) . ?
C410 C415 1.398(7) . ?
C410 C411 1.410(6) . ?
C411 C412 1.369(7) . ?
C412 C413 1.375(7) . ?
C413 C414 1.381(7) . ?
C414 C415 1.395(7) . ?
C415 O416 1.384(5) . ?
O416 C417 1.445(5) . ?
C417 C418 1.513(6) . ?
C418 O420 1.232(6) . ?
C418 O419 1.284(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N108 Ni1 O101 84.03(13) . . ?
N108 Ni1 O119 170.15(13) . . ?
O101 Ni1 O119 105.81(12) . . ?
N108 Ni1 O140 89.83(14) . . ?
O101 Ni1 O140 90.32(12) . . ?
O119 Ni1 O140 89.85(13) . . ?
N108 Ni1 O130 90.20(13) . . ?
O101 Ni1 O130 91.23(12) . . ?
O119 Ni1 O130 89.86(12) . . ?
O140 Ni1 O130 178.43(12) . . ?
N108 Ni1 O116 90.45(13) . . ?
O101 Ni1 O116 174.48(12) . . ?
O119 Ni1 O116 79.71(12) . . ?
O140 Ni1 O116 89.64(12) . . ?
O130 Ni1 O116 88.79(12) . . ?
N208 Ni2 O201 83.99(13) . . ?
N208 Ni2 O219 169.47(14) . . ?
O201 Ni2 O219 106.54(13) . . ?
N208 Ni2 O240 90.95(14) . . ?
O201 Ni2 O240 91.83(12) . . ?
O219 Ni2 O240 88.91(13) . . ?
N208 Ni2 O230 90.12(13) . . ?
O201 Ni2 O230 91.47(12) . . ?
O219 Ni2 O230 89.44(13) . . ?
O240 Ni2 O230 176.61(13) . . ?
N208 Ni2 O216 89.78(13) . . ?
O201 Ni2 O216 173.77(12) . . ?
O219 Ni2 O216 79.69(13) . . ?
O240 Ni2 O216 88.03(13) . . ?
O230 Ni2 O216 88.76(13) . . ?
N308 Ni3 O301 83.98(13) . . ?
N308 Ni3 O319 170.68(14) . . ?
O301 Ni3 O319 105.34(12) . . ?
N308 Ni3 O340 90.01(13) . . ?
O301 Ni3 O340 90.74(12) . . ?
O319 Ni3 O340 89.76(12) . . ?
N308 Ni3 O330 89.84(13) . . ?
O301 Ni3 O330 91.82(12) . . ?
O319 Ni3 O330 89.97(12) . . ?
O340 Ni3 O330 177.40(12) . . ?
N308 Ni3 O316 90.41(13) . . ?
O301 Ni3 O316 174.23(12) . . ?
O319 Ni3 O316 80.27(12) . . ?
O340 Ni3 O316 87.90(12) . . ?
O330 Ni3 O316 89.51(12) . . ?
N408 Ni4 O401 83.19(13) . . ?
N408 Ni4 O419 168.43(14) . . ?
O401 Ni4 O419 108.37(12) . . ?
N408 Ni4 O440 91.20(13) . . ?
O401 Ni4 O440 90.28(12) . . ?
O419 Ni4 O440 88.45(12) . . ?
N408 Ni4 O430 90.98(13) . . ?
O401 Ni4 O430 90.40(12) . . ?
O419 Ni4 O430 89.33(12) . . ?
O440 Ni4 O430 177.78(12) . . ?
N408 Ni4 O416 89.16(13) . . ?
O401 Ni4 O416 171.77(12) . . ?
O419 Ni4 O416 79.31(12) . . ?
O440 Ni4 O416 92.94(12) . . ?
O430 Ni4 O416 86.68(12) . . ?
C102 O101 Ni1 110.6(2) . . ?
O101 C102 C103 121.1(4) . . ?
O101 C102 C107 120.2(4) . . ?
C103 C102 C107 118.6(4) . . ?
C104 C103 C102 120.3(4) . . ?
C103 C104 C105 120.8(4) . . ?
C106 C105 C104 120.0(4) . . ?
C105 C106 C107 119.6(4) . . ?
C106 C107 C102 120.6(4) . . ?
C106 C107 N108 124.2(4) . . ?
C102 C107 N108 115.1(4) . . ?
C109 N108 C107 123.7(4) . . ?
C109 N108 Ni1 126.4(3) . . ?
C107 N108 Ni1 110.0(3) . . ?
N108 C109 C110 127.5(4) . . ?
C111 C110 C115 117.5(4) . . ?
C111 C110 C109 114.5(4) . . ?
C115 C110 C109 128.1(4) . . ?
C112 C111 C110 122.7(5) . . ?
C111 C112 C113 118.3(4) . . ?
C114 C113 C112 121.1(4) . . ?
C113 C114 C115 120.2(4) . . ?
O116 C115 C114 120.9(4) . . ?
O116 C115 C110 118.7(4) . . ?
C114 C115 C110 120.3(4) . . ?
C115 O116 C117 117.8(3) . . ?
C115 O116 Ni1 128.8(3) . . ?
C117 O116 Ni1 113.2(2) . . ?
O116 C117 C118 110.1(3) . . ?
O120 C118 O119 125.5(4) . . ?
O120 C118 C117 115.3(4) . . ?
O119 C118 C117 119.2(4) . . ?
C118 O119 Ni1 117.7(3) . . ?
C202 O201 Ni2 110.2(3) . . ?
O201 C202 C203 122.1(4) . . ?
O201 C202 C207 120.8(4) . . ?
C203 C202 C207 117.1(4) . . ?
C204 C203 C202 121.7(5) . . ?
C203 C204 C205 120.5(5) . . ?
C206 C205 C204 119.4(5) . . ?
C205 C206 C207 120.8(5) . . ?
C206 C207 C202 120.4(4) . . ?
C206 C207 N208 125.3(4) . . ?
C202 C207 N208 114.2(4) . . ?
C209 N208 C207 122.4(4) . . ?
C209 N208 Ni2 126.8(3) . . ?
C207 N208 Ni2 110.6(3) . . ?
N208 C209 C210 127.7(4) . . ?
C215 C210 C211 117.8(4) . . ?
C215 C210 C209 127.8(4) . . ?
C211 C210 C209 114.4(4) . . ?
C212 C211 C210 122.1(5) . . ?
C211 C212 C213 119.1(5) . . ?
C212 C213 C214 120.5(5) . . ?
C215 C214 C213 120.5(5) . . ?
O216 C215 C214 121.4(4) . . ?
O216 C215 C210 118.6(4) . . ?
C214 C215 C210 120.0(4) . . ?
C215 O216 C217 117.9(4) . . ?
C215 O216 Ni2 129.0(3) . . ?
C217 O216 Ni2 113.2(3) . . ?
O216 C217 C218 109.6(4) . . ?
O219 C218 O220 124.2(5) . . ?
O219 C218 C217 120.3(4) . . ?
O220 C218 C217 115.5(5) . . ?
C218 O219 Ni2 117.0(3) . . ?
C302 O301 Ni3 110.0(3) . . ?
O301 C302 C303 121.1(4) . . ?
O301 C302 C307 120.8(4) . . ?
C303 C302 C307 118.1(4) . . ?
C304 C303 C302 120.4(4) . . ?
C303 C304 C305 121.2(4) . . ?
C306 C305 C304 119.3(4) . . ?
C305 C306 C307 120.5(4) . . ?
C306 C307 C302 120.4(4) . . ?
C306 C307 N308 125.5(4) . . ?
C302 C307 N308 114.1(4) . . ?
C309 N308 C307 122.5(4) . . ?
C309 N308 Ni3 126.4(3) . . ?
C307 N308 Ni3 111.0(3) . . ?
N308 C309 C310 127.0(4) . . ?
C315 C310 C311 117.6(4) . . ?
C315 C310 C309 128.3(4) . . ?
C311 C310 C309 114.1(4) . . ?
C312 C311 C310 121.7(5) . . ?
C313 C312 C311 119.4(5) . . ?
C312 C313 C314 120.4(5) . . ?
C313 C314 C315 120.3(5) . . ?
O316 C315 C314 120.6(4) . . ?
O316 C315 C310 118.9(4) . . ?
C314 C315 C310 120.5(4) . . ?
C315 O316 C317 118.8(3) . . ?
C315 O316 Ni3 128.1(3) . . ?
C317 O316 Ni3 112.8(3) . . ?
O316 C317 C318 109.9(4) . . ?
O319 C318 O320 123.7(5) . . ?
O319 C318 C317 120.5(4) . . ?
O320 C318 C317 115.8(4) . . ?
C318 O319 Ni3 116.5(3) . . ?
C402 O401 Ni4 110.7(2) . . ?
O401 C402 C403 121.9(4) . . ?
O401 C402 C407 120.5(4) . . ?
C403 C402 C407 117.6(4) . . ?
C404 C403 C402 121.2(4) . . ?
C403 C404 C405 120.7(4) . . ?
C406 C405 C404 119.8(4) . . ?
C405 C406 C407 120.0(4) . . ?
C406 C407 N408 125.1(4) . . ?
C406 C407 C402 120.6(4) . . ?
N408 C407 C402 114.3(4) . . ?
C409 N408 C407 122.3(4) . . ?
C409 N408 Ni4 126.5(3) . . ?
C407 N408 Ni4 111.2(3) . . ?
N408 C409 C410 128.8(4) . . ?
C415 C410 C411 118.0(4) . . ?
C415 C410 C409 127.6(4) . . ?
C411 C410 C409 114.5(4) . . ?
C412 C411 C410 122.2(5) . . ?
C411 C412 C413 118.9(4) . . ?
C412 C413 C414 121.0(4) . . ?
C413 C414 C415 120.4(4) . . ?
O416 C415 C414 121.2(4) . . ?
O416 C415 C410 119.2(4) . . ?
C414 C415 C410 119.6(4) . . ?
C415 O416 C417 117.7(3) . . ?
C415 O416 Ni4 128.7(3) . . ?
C417 O416 Ni4 113.0(3) . . ?
O416 C417 C418 110.5(4) . . ?
O420 C418 O419 125.0(4) . . ?
O420 C418 C417 115.9(4) . . ?
O419 C418 C417 119.1(4) . . ?
C418 O419 Ni4 117.5(3) . . ?

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
_geom_hbond_publ_flag
O130 H131 O301 0.839(10) 1.94(2) 2.742(4) 160(5) . yes
O130 H132 O540 0.839(10) 1.990(17) 2.811(5) 166(5) . yes
O140 H141 O401 0.837(10) 1.89(2) 2.693(4) 160(5) . yes
O140 H142 O520 0.836(10) 1.921(14) 2.750(4) 171(5) . yes
O230 H231 O401 0.841(10) 1.900(16) 2.725(4) 167(5) 1_565 yes
O230 H232 O520 0.840(10) 1.980(14) 2.811(4) 170(5) 1_565 yes
O240 H241 O301 0.841(10) 1.89(3) 2.678(4) 155(5) . yes
O240 H242 O540 0.839(10) 1.99(2) 2.787(5) 159(5) . yes
O330 H331 O201 0.837(10) 1.926(18) 2.743(4) 165(5) . yes
O330 H332 O530 0.836(10) 1.994(16) 2.817(4) 168(5) 1_565 yes
O340 H341 O101 0.834(10) 1.875(15) 2.699(4) 169(5) . yes
O340 H342 O510 0.837(10) 1.917(17) 2.737(4) 166(5) 2_756 yes
O430 H431 O101 0.837(10) 1.929(19) 2.740(4) 163(5) . yes
O430 H432 O510 0.839(10) 1.96(2) 2.765(4) 161(5) 2_756 yes
O440 H441 O201 0.838(10) 1.883(15) 2.711(4) 170(5) 1_545 yes
O440 H442 O530 0.839(10) 1.96(2) 2.775(4) 162(5) . yes
O510 H511 O420 0.839(10) 1.850(12) 2.685(5) 173(5) . yes
O510 H512 O119 0.838(10) 2.11(3) 2.823(4) 143(4) 2_756 yes
O520 H521 O120 0.837(10) 1.917(12) 2.751(5) 175(5) 2_656 yes
O520 H522 O550 0.839(10) 1.881(18) 2.703(5) 166(6) . yes
O530 H531 O320 0.842(10) 1.928(14) 2.762(5) 171(6) 2_756 yes
O570 H571 O120 0.857(10) 1.95(3) 2.758(6) 158(8) . yes
O570 H572 O320 0.854(10) 1.92(5) 2.661(6) 145(8) . yes

_refine_diff_density_max         1.047
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.094

# start Validation Reply Form
_vrf_PLAT306_7278new             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ..O540 Check 
RESPONSE: The hydrogen atoms in water molecules O540, O550 and O560 could not
be located reliably and were therefore ignored in the refinement.
;
_vrf_PLAT430_7278new             
;
PROBLEM: Short Inter D...A Contact  O220..O540  2.77 Ang.  
RESPONSE: Water molecule O540 is hydrogen bonded to O220.
Water molecule O550 is hydrogen bonded to O419.
Hydrogen positions at O540 and O550 could not be located reliably and 
were ignored in the refinement.
;
# end Validation Reply Form

