# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1443519'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H54 N4 Ni4 O13'
_chemical_formula_weight         1225.87

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'

_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                   10.4566(4)
_cell_length_b                   10.8854(4)
_cell_length_c                   23.552(6)
_cell_angle_alpha                77.019(3)
_cell_angle_beta                 78.705(3)
_cell_angle_gamma                85.437(3)
_cell_volume                     2559.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25423
_cell_measurement_theta_min      2.903
_cell_measurement_theta_max      32.4862

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_F_000             1268
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_exptl_absorpt_coefficient_mu    1.520
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
face-indexed (CrysAlis RED; Oxford Diffraction, 2006)
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24294
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.905
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8985
_reflns_number_gt                5882
_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       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_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)+(0.0448P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8985
_refine_ls_number_parameters     707
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0883
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_restrained_S_all      0.928
_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
C1 C 0.5489(4) -0.0056(3) 0.65157(15) 0.0167(8) Uani 1 1 d . . . . .
C2 C 0.6797(4) 0.0174(4) 0.63254(17) 0.0256(9) Uani 1 1 d . . . . .
H2 H 0.7252 0.0483 0.6562 0.031 Uiso 1 1 calc R U . . .
C3 C 0.7438(4) -0.0051(4) 0.57843(18) 0.0317(10) Uani 1 1 d . . . . .
H3 H 0.8316 0.0126 0.5654 0.038 Uiso 1 1 calc R U . . .
C4 C 0.6779(4) -0.0535(4) 0.54384(17) 0.0316(10) Uani 1 1 d . . . . .
H4 H 0.7210 -0.0673 0.5072 0.038 Uiso 1 1 calc R U . . .
C5 C 0.5480(4) -0.0818(4) 0.56312(17) 0.0279(10) Uani 1 1 d . . . . .
H5 H 0.5046 -0.1167 0.5400 0.033 Uiso 1 1 calc R U . . .
C6 C 0.4826(4) -0.0584(3) 0.61665(16) 0.0208(9) Uani 1 1 d . . . . .
C7 C 0.2733(4) -0.1331(3) 0.61715(17) 0.0248(9) Uani 1 1 d . . . . .
H7 H 0.3023 -0.1356 0.5775 0.030 Uiso 1 1 calc R U . . .
C8 C 0.1456(4) -0.1763(3) 0.64299(17) 0.0231(9) Uani 1 1 d . . . . .
C9 C 0.0754(4) -0.2164(4) 0.60560(19) 0.0333(11) Uani 1 1 d . . . . .
H9 H 0.1148 -0.2139 0.5664 0.040 Uiso 1 1 calc R U . . .
C10 C -0.0481(4) -0.2585(4) 0.6247(2) 0.0411(12) Uani 1 1 d . . . . .
H10 H -0.0926 -0.2839 0.5990 0.049 Uiso 1 1 calc R U . . .
C11 C -0.1059(4) -0.2627(4) 0.6832(2) 0.0415(12) Uani 1 1 d . . . . .
H11 H -0.1903 -0.2910 0.6970 0.050 Uiso 1 1 calc R U . . .
C12 C -0.0409(4) -0.2262(4) 0.72087(18) 0.0306(10) Uani 1 1 d . . . . .
H12 H -0.0827 -0.2297 0.7598 0.037 Uiso 1 1 calc R U . . .
C13 C 0.0862(4) -0.1837(3) 0.70347(17) 0.0228(9) Uani 1 1 d . . . . .
C14 C 0.4323(3) 0.2440(3) 0.82187(15) 0.0161(8) Uani 1 1 d . . . . .
C15 C 0.4036(3) 0.3707(3) 0.82031(16) 0.0187(9) Uani 1 1 d . . . . .
H15 H 0.3626 0.4184 0.7905 0.022 Uiso 1 1 calc R U . . .
C16 C 0.4349(4) 0.4274(4) 0.86224(17) 0.0250(9) Uani 1 1 d . . . . .
H16 H 0.4147 0.5128 0.8606 0.030 Uiso 1 1 calc R U . . .
C17 C 0.4961(4) 0.3582(4) 0.90686(16) 0.0250(9) Uani 1 1 d . . . . .
H17 H 0.5160 0.3967 0.9354 0.030 Uiso 1 1 calc R U . . .
C18 C 0.5277(4) 0.2322(4) 0.90901(16) 0.0224(9) Uani 1 1 d . . . . .
H18 H 0.5705 0.1863 0.9386 0.027 Uiso 1 1 calc R U . . .
C19 C 0.4961(3) 0.1733(3) 0.86756(15) 0.0170(8) Uani 1 1 d . . . . .
C20 C 0.5758(3) -0.0363(3) 0.90376(16) 0.0202(9) Uani 1 1 d . . . . .
H20 H 0.5774 -0.0132 0.9393 0.024 Uiso 1 1 calc R U . . .
C21 C 0.6235(3) -0.1611(3) 0.89845(15) 0.0166(8) Uani 1 1 d . . . . .
C22 C 0.6660(4) -0.2374(4) 0.94806(17) 0.0254(9) Uani 1 1 d . . . . .
H22 H 0.6608 -0.2046 0.9817 0.031 Uiso 1 1 calc R U . . .
C23 C 0.7146(4) -0.3577(4) 0.94912(18) 0.0304(10) Uani 1 1 d . . . . .
H23 H 0.7414 -0.4060 0.9829 0.036 Uiso 1 1 calc R U . . .
C24 C 0.7235(4) -0.4069(4) 0.89892(18) 0.0287(10) Uani 1 1 d . . . . .
H24 H 0.7570 -0.4886 0.8989 0.034 Uiso 1 1 calc R U . . .
C25 C 0.6831(3) -0.3357(3) 0.84945(17) 0.0233(9) Uani 1 1 d . . . . .
H25 H 0.6893 -0.3707 0.8164 0.028 Uiso 1 1 calc R U . . .
C26 C 0.6326(3) -0.2116(3) 0.84692(16) 0.0192(9) Uani 1 1 d . . . . .
C27 C 0.1733(4) 0.1524(3) 0.66600(15) 0.0175(9) Uani 1 1 d . . . . .
C28 C 0.0425(4) 0.1329(3) 0.67048(16) 0.0234(9) Uani 1 1 d . . . . .
H28 H -0.0072 0.0970 0.7069 0.028 Uiso 1 1 calc R U . . .
C29 C -0.0143(4) 0.1670(4) 0.62066(17) 0.0299(10) Uani 1 1 d . . . . .
H29 H -0.1027 0.1548 0.6240 0.036 Uiso 1 1 calc R U . . .
C30 C 0.0573(4) 0.2184(4) 0.56639(18) 0.0315(10) Uani 1 1 d . . . . .
H30 H 0.0182 0.2379 0.5331 0.038 Uiso 1 1 calc R U . . .
C31 C 0.1870(4) 0.2412(3) 0.56125(16) 0.0235(9) Uani 1 1 d . . . . .
H31 H 0.2353 0.2774 0.5246 0.028 Uiso 1 1 calc R U . . .
C32 C 0.2458(3) 0.2100(3) 0.61095(15) 0.0174(8) Uani 1 1 d . . . . .
C33 C 0.4565(4) 0.2882(3) 0.56478(16) 0.0213(9) Uani 1 1 d . . . . .
H33 H 0.4342 0.2898 0.5283 0.026 Uiso 1 1 calc R U . . .
C34 C 0.5803(4) 0.3379(3) 0.56452(15) 0.0196(9) Uani 1 1 d . . . . .
C35 C 0.6562(4) 0.3839(4) 0.50857(17) 0.0291(10) Uani 1 1 d . . . . .
H35 H 0.6262 0.3767 0.4748 0.035 Uiso 1 1 calc R U . . .
C36 C 0.7726(4) 0.4389(4) 0.50212(18) 0.0354(11) Uani 1 1 d . . . . .
H36 H 0.8228 0.4657 0.4647 0.043 Uiso 1 1 calc R U . . .
C37 C 0.8145(4) 0.4539(4) 0.55221(18) 0.0365(11) Uani 1 1 d . . . . .
H37 H 0.8915 0.4948 0.5482 0.044 Uiso 1 1 calc R U . . .
C38 C 0.7443(4) 0.4095(4) 0.60764(18) 0.0315(10) Uani 1 1 d . . . . .
H38 H 0.7755 0.4200 0.6405 0.038 Uiso 1 1 calc R U . . .
C39 C 0.6263(4) 0.3486(3) 0.61620(16) 0.0210(9) Uani 1 1 d . . . . .
C40 C 0.2803(3) -0.1123(3) 0.86971(15) 0.0159(8) Uani 1 1 d . . . . .
C41 C 0.3154(4) -0.2385(3) 0.88808(17) 0.0244(9) Uani 1 1 d . . . . .
H41 H 0.3553 -0.2846 0.8602 0.029 Uiso 1 1 calc R U . . .
C42 C 0.2916(4) -0.2959(4) 0.94743(18) 0.0303(10) Uani 1 1 d . . . . .
H42 H 0.3167 -0.3803 0.9593 0.036 Uiso 1 1 calc R U . . .
C43 C 0.2306(4) -0.2293(4) 0.98959(18) 0.0311(10) Uani 1 1 d . . . . .
H43 H 0.2152 -0.2684 1.0296 0.037 Uiso 1 1 calc R U . . .
C44 C 0.1931(4) -0.1049(4) 0.97174(16) 0.0252(9) Uani 1 1 d . . . . .
H44 H 0.1505 -0.0604 0.9998 0.030 Uiso 1 1 calc R U . . .
C45 C 0.2179(3) -0.0449(3) 0.91247(16) 0.0189(9) Uani 1 1 d . . . . .
C46 C 0.1395(3) 0.1642(4) 0.92050(16) 0.0208(9) Uani 1 1 d . . . . .
H46 H 0.1342 0.1385 0.9613 0.025 Uiso 1 1 calc R U . . .
C47 C 0.1023(3) 0.2933(3) 0.89807(16) 0.0190(9) Uani 1 1 d . . . . .
C48 C 0.0841(4) 0.3739(4) 0.93800(17) 0.0262(10) Uani 1 1 d . . . . .
H48 H 0.0851 0.3390 0.9778 0.031 Uiso 1 1 calc R U . . .
C49 C 0.0650(4) 0.5014(4) 0.92111(18) 0.0307(10) Uani 1 1 d . . . . .
H49 H 0.0554 0.5523 0.9486 0.037 Uiso 1 1 calc R U . . .
C50 C 0.0602(4) 0.5535(4) 0.86224(18) 0.0297(10) Uani 1 1 d . . . . .
H50 H 0.0491 0.6404 0.8497 0.036 Uiso 1 1 calc R U . . .
C51 C 0.0719(4) 0.4769(4) 0.82247(17) 0.0245(9) Uani 1 1 d . . . . .
H51 H 0.0651 0.5134 0.7834 0.029 Uiso 1 1 calc R U . . .
C52 C 0.0936(3) 0.3466(3) 0.83806(16) 0.0182(9) Uani 1 1 d . . . . .
C53 C 0.4822(4) -0.3357(4) 0.71352(19) 0.0401(11) Uani 1 1 d . . . . .
H53A H 0.4120 -0.3663 0.7003 0.060 Uiso 1 1 calc R U . . .
H53B H 0.5259 -0.4052 0.7360 0.060 Uiso 1 1 calc R U . . .
H53C H 0.5429 -0.2946 0.6798 0.060 Uiso 1 1 calc R U . . .
C54 C 0.2330(4) 0.4774(4) 0.65973(17) 0.0364(11) Uani 1 1 d . . . . .
H54A H 0.3043 0.5049 0.6280 0.055 Uiso 1 1 calc R U . . .
H54B H 0.1951 0.5480 0.6761 0.055 Uiso 1 1 calc R U . . .
H54C H 0.1683 0.4424 0.6448 0.055 Uiso 1 1 calc R U . . .
C55 C -0.0633(4) -0.0404(4) 0.85869(19) 0.0403(12) Uani 1 1 d . . . . .
H55A H -0.0257 -0.1096 0.8841 0.060 Uiso 1 1 calc R U . . .
H55B H -0.1351 -0.0692 0.8458 0.060 Uiso 1 1 calc R U . . .
H55C H -0.0939 0.0248 0.8800 0.060 Uiso 1 1 calc R U . . .
N1 N 0.3526(3) -0.0911(3) 0.64308(13) 0.0192(7) Uani 1 1 d . . . . .
N2 N 0.5308(3) 0.0468(3) 0.86338(12) 0.0170(7) Uani 1 1 d . . . . .
N3 N 0.3742(3) 0.2417(3) 0.61152(12) 0.0167(7) Uani 1 1 d . . . . .
N4 N 0.1794(3) 0.0815(3) 0.88947(12) 0.0159(7) Uani 1 1 d . . . . .
O1 O 0.4811(2) 0.0227(2) 0.70269(10) 0.0174(6) Uani 1 1 d . . . . .
O2 O 0.1432(2) -0.1513(2) 0.74266(10) 0.0237(6) Uani 1 1 d . . . . .
O3 O 0.3983(2) 0.1826(2) 0.78337(10) 0.0159(5) Uani 1 1 d . . . . .
O4 O 0.5962(2) -0.1494(2) 0.79753(10) 0.0208(6) Uani 1 1 d . . . . .
O5 O 0.2364(2) 0.1176(2) 0.71296(10) 0.0162(6) Uani 1 1 d . . . . .
O6 O 0.5672(2) 0.3044(2) 0.67073(10) 0.0225(6) Uani 1 1 d D . . . .
O7 O 0.3101(2) -0.0512(2) 0.81178(10) 0.0167(6) Uani 1 1 d . . . . .
O8 O 0.1064(2) 0.2790(2) 0.79659(10) 0.0202(6) Uani 1 1 d . . . . .
O9 O 0.4309(2) -0.2472(2) 0.75017(11) 0.0265(6) Uani 1 1 d . . . . .
H9A H 0.4906 -0.2225 0.7622 0.032 Uiso 1 1 calc R U . . .
O10 O 0.6821(2) 0.1258(2) 0.74565(11) 0.0235(6) Uani 1 1 d D . . . .
O11 O 0.0331(2) 0.0081(2) 0.80830(10) 0.0234(6) Uani 1 1 d . . . . .
H11A H 0.0672 -0.0499 0.7929 0.028 Uiso 1 1 calc R U . . .
O12 O 0.2797(2) 0.3836(2) 0.70473(10) 0.0219(6) Uani 1 1 d . . . . .
H12A H 0.2176 0.3508 0.7288 0.026 Uiso 1 1 calc R U . . .
Ni1 Ni 0.31630(4) -0.08122(4) 0.72759(2) 0.01786(13) Uani 1 1 d . . . . .
Ni2 Ni 0.51702(4) 0.02115(4) 0.78479(2) 0.01647(13) Uani 1 1 d . . . . .
Ni3 Ni 0.39988(4) 0.22225(4) 0.69370(2) 0.01647(13) Uani 1 1 d . . . . .
Ni4 Ni 0.19751(4) 0.11193(4) 0.80245(2) 0.01594(13) Uani 1 1 d . . . . .
H10A H 0.661(3) 0.1937(19) 0.7230(12) 0.019 Uiso 1 1 d D U . . .
H10B H 0.730(3) 0.154(3) 0.7653(13) 0.019 Uiso 1 1 d D U . . .
C1S C 0.7936(4) 0.3731(4) 0.7826(2) 0.0517(14) Uani 1 1 d . . . . .
H1S1 H 0.8073 0.4142 0.8128 0.078 Uiso 1 1 calc R U . . .
H1S2 H 0.7024 0.3784 0.7806 0.078 Uiso 1 1 calc R U . . .
H1S3 H 0.8424 0.4137 0.7451 0.078 Uiso 1 1 calc R U . . .
O1S O 0.8355(3) 0.2453(3) 0.79620(15) 0.0471(9) Uani 1 1 d . . . . .
H1S H 0.919(2) 0.232(5) 0.799(2) 0.071 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
C1 O1 1.359(4) . ?
C1 C2 1.378(5) . ?
C1 C6 1.409(5) . ?
C2 C3 1.383(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.374(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.382(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.378(5) . ?
C5 H5 0.9300 . ?
C6 N1 1.418(5) . ?
C7 N1 1.286(4) . ?
C7 C8 1.424(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.407(5) . ?
C8 C13 1.425(5) . ?
C9 C10 1.361(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.385(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.357(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.396(5) . ?
C12 H12 0.9300 . ?
C13 O2 1.314(4) . ?
C14 O3 1.353(4) . ?
C14 C15 1.383(5) . ?
C14 C19 1.422(5) . ?
C15 C16 1.377(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.383(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.384(5) . ?
C18 H18 0.9300 . ?
C19 N2 1.416(4) . ?
C20 N2 1.290(4) . ?
C20 C21 1.434(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.400(5) . ?
C21 C26 1.424(5) . ?
C22 C23 1.363(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.388(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.368(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.404(5) . ?
C25 H25 0.9300 . ?
C26 O4 1.317(4) . ?
C27 O5 1.363(4) . ?
C27 C28 1.381(5) . ?
C27 C32 1.405(5) . ?
C28 C29 1.382(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.370(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.375(5) . ?
C30 H30 0.9300 . ?
C31 C32 1.391(5) . ?
C31 H31 0.9300 . ?
C32 N3 1.417(4) . ?
C33 N3 1.286(4) . ?
C33 C34 1.441(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.405(5) . ?
C34 C39 1.424(5) . ?
C35 C36 1.366(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.382(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.369(5) . ?
C37 H37 0.9300 . ?
C38 C39 1.406(5) . ?
C38 H38 0.9300 . ?
C39 O6 1.312(4) . ?
C40 O7 1.364(4) . ?
C40 C41 1.387(5) . ?
C40 C45 1.406(5) . ?
C41 C42 1.379(5) . ?
C41 H41 0.9300 . ?
C42 C43 1.386(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.374(5) . ?
C43 H43 0.9300 . ?
C44 C45 1.385(5) . ?
C44 H44 0.9300 . ?
C45 N4 1.418(4) . ?
C46 N4 1.279(4) . ?
C46 C47 1.437(5) . ?
C46 H46 0.9300 . ?
C47 C48 1.402(5) . ?
C47 C52 1.420(5) . ?
C48 C49 1.365(5) . ?
C48 H48 0.9300 . ?
C49 C50 1.384(5) . ?
C49 H49 0.9300 . ?
C50 C51 1.370(5) . ?
C50 H50 0.9300 . ?
C51 C52 1.396(5) . ?
C51 H51 0.9300 . ?
C52 O8 1.330(4) . ?
C53 O9 1.439(4) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 O12 1.429(4) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 O11 1.428(4) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
N1 Ni1 1.978(3) . ?
N2 Ni2 1.967(3) . ?
N3 Ni3 1.968(3) . ?
N4 Ni4 1.975(3) . ?
O1 Ni2 2.037(2) . ?
O1 Ni1 2.052(2) . ?
O1 Ni3 2.248(2) . ?
O2 Ni1 1.957(2) . ?
O3 Ni3 2.055(2) . ?
O3 Ni2 2.067(2) . ?
O3 Ni4 2.221(2) . ?
O4 Ni2 1.955(2) . ?
O5 Ni3 2.049(2) . ?
O5 Ni4 2.055(2) . ?
O5 Ni1 2.234(2) . ?
O6 Ni3 1.953(2) . ?
O7 Ni4 2.044(2) . ?
O7 Ni1 2.069(2) . ?
O7 Ni2 2.283(2) . ?
O8 Ni4 1.974(2) . ?
O9 Ni1 2.111(2) . ?
O9 H9A 0.8200 . ?
O10 Ni2 2.085(3) . ?
O10 H10A 0.850(9) . ?
O10 H10B 0.853(10) . ?
O11 Ni4 2.097(2) . ?
O11 H11A 0.8200 . ?
O12 Ni3 2.111(2) . ?
O12 H12A 0.8200 . ?
C1S O1S 1.411(5) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
O1S H1S 0.88(3) . ?

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
O1 C1 C2 122.0(3) . . ?
O1 C1 C6 118.8(3) . . ?
C2 C1 C6 119.2(3) . . ?
C1 C2 C3 120.4(4) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 H2 119.8 . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C1 119.7(4) . . ?
C5 C6 N1 125.4(3) . . ?
C1 C6 N1 114.8(3) . . ?
N1 C7 C8 126.6(4) . . ?
N1 C7 H7 116.7 . . ?
C8 C7 H7 116.7 . . ?
C9 C8 C7 116.7(4) . . ?
C9 C8 C13 118.6(4) . . ?
C7 C8 C13 124.8(3) . . ?
C10 C9 C8 122.4(4) . . ?
C10 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
C9 C10 C11 118.5(4) . . ?
C9 C10 H10 120.8 . . ?
C11 C10 H10 120.8 . . ?
C12 C11 C10 120.9(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 122.7(4) . . ?
C11 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
O2 C13 C12 119.1(3) . . ?
O2 C13 C8 123.9(3) . . ?
C12 C13 C8 116.9(3) . . ?
O3 C14 C15 123.2(3) . . ?
O3 C14 C19 118.3(3) . . ?
C15 C14 C19 118.5(3) . . ?
C16 C15 C14 120.9(3) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.4(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
C18 C17 C16 119.9(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.5(3) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 N2 125.2(3) . . ?
C18 C19 C14 119.7(3) . . ?
N2 C19 C14 114.9(3) . . ?
N2 C20 C21 125.5(3) . . ?
N2 C20 H20 117.2 . . ?
C21 C20 H20 117.2 . . ?
C22 C21 C26 118.4(3) . . ?
C22 C21 C20 116.4(3) . . ?
C26 C21 C20 125.2(3) . . ?
C23 C22 C21 122.8(4) . . ?
C23 C22 H22 118.6 . . ?
C21 C22 H22 118.6 . . ?
C22 C23 C24 118.9(4) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
C25 C24 C23 120.3(4) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 122.2(4) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
O4 C26 C25 118.4(3) . . ?
O4 C26 C21 124.1(3) . . ?
C25 C26 C21 117.5(3) . . ?
O5 C27 C28 122.8(3) . . ?
O5 C27 C32 118.0(3) . . ?
C28 C27 C32 119.2(3) . . ?
C27 C28 C29 119.7(4) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 121.2(4) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C29 C30 C31 119.9(3) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C30 C31 C32 119.9(4) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 119.9(3) . . ?
C31 C32 N3 124.1(3) . . ?
C27 C32 N3 115.8(3) . . ?
N3 C33 C34 125.2(3) . . ?
N3 C33 H33 117.4 . . ?
C34 C33 H33 117.4 . . ?
C35 C34 C39 119.0(3) . . ?
C35 C34 C33 116.3(3) . . ?
C39 C34 C33 124.6(3) . . ?
C36 C35 C34 122.1(4) . . ?
C36 C35 H35 118.9 . . ?
C34 C35 H35 118.9 . . ?
C35 C36 C37 118.8(4) . . ?
C35 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C38 C37 C36 121.0(4) . . ?
C38 C37 H37 119.5 . . ?
C36 C37 H37 119.5 . . ?
C37 C38 C39 121.8(4) . . ?
C37 C38 H38 119.1 . . ?
C39 C38 H38 119.1 . . ?
O6 C39 C38 118.2(3) . . ?
O6 C39 C34 124.6(3) . . ?
C38 C39 C34 117.1(3) . . ?
O7 C40 C41 121.6(3) . . ?
O7 C40 C45 119.5(3) . . ?
C41 C40 C45 118.9(3) . . ?
C42 C41 C40 120.4(4) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 120.7(4) . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
C44 C43 C42 119.4(4) . . ?
C44 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
C43 C44 C45 120.9(4) . . ?
C43 C44 H44 119.6 . . ?
C45 C44 H44 119.6 . . ?
C44 C45 C40 119.8(3) . . ?
C44 C45 N4 125.1(3) . . ?
C40 C45 N4 115.0(3) . . ?
N4 C46 C47 125.9(3) . . ?
N4 C46 H46 117.0 . . ?
C47 C46 H46 117.0 . . ?
C48 C47 C52 118.2(3) . . ?
C48 C47 C46 116.6(3) . . ?
C52 C47 C46 125.0(3) . . ?
C49 C48 C47 122.9(4) . . ?
C49 C48 H48 118.5 . . ?
C47 C48 H48 118.5 . . ?
C48 C49 C50 118.8(4) . . ?
C48 C49 H49 120.6 . . ?
C50 C49 H49 120.6 . . ?
C51 C50 C49 119.9(4) . . ?
C51 C50 H50 120.1 . . ?
C49 C50 H50 120.1 . . ?
C50 C51 C52 122.8(4) . . ?
C50 C51 H51 118.6 . . ?
C52 C51 H51 118.6 . . ?
O8 C52 C51 119.2(3) . . ?
O8 C52 C47 123.4(3) . . ?
C51 C52 C47 117.4(3) . . ?
O9 C53 H53A 109.5 . . ?
O9 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
O9 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O12 C54 H54A 109.5 . . ?
O12 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
O12 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O11 C55 H55A 109.5 . . ?
O11 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
O11 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C7 N1 C6 124.4(3) . . ?
C7 N1 Ni1 124.5(3) . . ?
C6 N1 Ni1 110.8(2) . . ?
C20 N2 C19 124.3(3) . . ?
C20 N2 Ni2 125.0(2) . . ?
C19 N2 Ni2 110.4(2) . . ?
C33 N3 C32 124.1(3) . . ?
C33 N3 Ni3 125.5(2) . . ?
C32 N3 Ni3 110.1(2) . . ?
C46 N4 C45 124.9(3) . . ?
C46 N4 Ni4 124.8(2) . . ?
C45 N4 Ni4 110.2(2) . . ?
C1 O1 Ni2 136.8(2) . . ?
C1 O1 Ni1 107.7(2) . . ?
Ni2 O1 Ni1 98.65(10) . . ?
C1 O1 Ni3 114.72(19) . . ?
Ni2 O1 Ni3 91.16(9) . . ?
Ni1 O1 Ni3 102.85(9) . . ?
C13 O2 Ni1 126.3(2) . . ?
C14 O3 Ni3 135.4(2) . . ?
C14 O3 Ni2 106.95(19) . . ?
Ni3 O3 Ni2 96.01(9) . . ?
C14 O3 Ni4 118.1(2) . . ?
Ni3 O3 Ni4 91.39(8) . . ?
Ni2 O3 Ni4 103.99(10) . . ?
C26 O4 Ni2 125.6(2) . . ?
C27 O5 Ni3 107.4(2) . . ?
C27 O5 Ni4 138.1(2) . . ?
Ni3 O5 Ni4 96.53(9) . . ?
C27 O5 Ni1 114.68(19) . . ?
Ni3 O5 Ni1 103.42(9) . . ?
Ni4 O5 Ni1 91.57(8) . . ?
C39 O6 Ni3 125.7(2) . . ?
C40 O7 Ni4 107.1(2) . . ?
C40 O7 Ni1 140.2(2) . . ?
Ni4 O7 Ni1 96.82(9) . . ?
C40 O7 Ni2 113.59(19) . . ?
Ni4 O7 Ni2 102.58(9) . . ?
Ni1 O7 Ni2 90.74(9) . . ?
C52 O8 Ni4 123.6(2) . . ?
C53 O9 Ni1 127.4(2) . . ?
C53 O9 H9A 109.5 . . ?
Ni1 O9 H9A 103.3 . . ?
Ni2 O10 H10A 110(2) . . ?
Ni2 O10 H10B 124(2) . . ?
H10A O10 H10B 101(3) . . ?
C55 O11 Ni4 129.7(2) . . ?
C55 O11 H11A 109.5 . . ?
Ni4 O11 H11A 100.3 . . ?
C54 O12 Ni3 127.6(2) . . ?
C54 O12 H12A 109.5 . . ?
Ni3 O12 H12A 100.4 . . ?
O2 Ni1 N1 93.77(11) . . ?
O2 Ni1 O1 168.81(9) . . ?
N1 Ni1 O1 82.76(11) . . ?
O2 Ni1 O7 96.98(9) . . ?
N1 Ni1 O7 169.08(11) . . ?
O1 Ni1 O7 86.33(9) . . ?
O2 Ni1 O9 100.52(10) . . ?
N1 Ni1 O9 91.47(11) . . ?
O1 Ni1 O9 90.23(9) . . ?
O7 Ni1 O9 88.44(9) . . ?
O2 Ni1 O5 92.96(9) . . ?
N1 Ni1 O5 95.85(10) . . ?
O1 Ni1 O5 76.89(9) . . ?
O7 Ni1 O5 81.74(8) . . ?
O9 Ni1 O5 164.21(9) . . ?
O4 Ni2 N2 94.35(11) . . ?
O4 Ni2 O1 95.70(9) . . ?
N2 Ni2 O1 169.69(11) . . ?
O4 Ni2 O3 167.54(10) . . ?
N2 Ni2 O3 82.64(10) . . ?
O1 Ni2 O3 87.05(9) . . ?
O4 Ni2 O10 100.29(10) . . ?
N2 Ni2 O10 90.99(11) . . ?
O1 Ni2 O10 89.49(10) . . ?
O3 Ni2 O10 91.88(10) . . ?
O4 Ni2 O7 92.76(9) . . ?
N2 Ni2 O7 95.97(10) . . ?
O1 Ni2 O7 81.25(9) . . ?
O3 Ni2 O7 75.60(8) . . ?
O10 Ni2 O7 164.71(9) . . ?
O6 Ni3 N3 94.04(11) . . ?
O6 Ni3 O5 172.59(10) . . ?
N3 Ni3 O5 83.23(11) . . ?
O6 Ni3 O3 95.97(9) . . ?
N3 Ni3 O3 169.89(11) . . ?
O5 Ni3 O3 86.66(9) . . ?
O6 Ni3 O12 97.70(10) . . ?
N3 Ni3 O12 91.94(10) . . ?
O5 Ni3 O12 89.29(9) . . ?
O3 Ni3 O12 88.16(9) . . ?
O6 Ni3 O1 96.84(9) . . ?
N3 Ni3 O1 95.40(10) . . ?
O5 Ni3 O1 76.62(9) . . ?
O3 Ni3 O1 81.99(9) . . ?
O12 Ni3 O1 163.20(9) . . ?
O8 Ni4 N4 93.47(11) . . ?
O8 Ni4 O7 172.75(9) . . ?
N4 Ni4 O7 83.73(10) . . ?
O8 Ni4 O5 95.81(9) . . ?
N4 Ni4 O5 170.59(10) . . ?
O7 Ni4 O5 86.87(9) . . ?
O8 Ni4 O11 96.77(10) . . ?
N4 Ni4 O11 92.51(11) . . ?
O7 Ni4 O11 90.04(9) . . ?
O5 Ni4 O11 87.96(9) . . ?
O8 Ni4 O3 96.20(9) . . ?
N4 Ni4 O3 95.15(10) . . ?
O7 Ni4 O3 77.46(9) . . ?
O5 Ni4 O3 82.32(8) . . ?
O11 Ni4 O3 164.50(9) . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C1S O1S H1S 115(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
C2 H2 O10 0.93 2.39 3.152(5) 138.9 .
C15 H15 O12 0.93 2.46 3.208(4) 137.3 .
C28 H28 O11 0.93 2.47 3.210(4) 136.4 .
C41 H41 O9 0.93 2.51 3.256(5) 137.8 .
O9 H9A O4 0.82 1.83 2.637(3) 167.9 .
O11 H11A O2 0.82 1.83 2.630(3) 166.5 .
O12 H12A O8 0.82 1.84 2.636(3) 164.8 .
O10 H10A O6 0.850(9) 1.884(13) 2.693(3) 159(3) .
O10 H10B O1S 0.853(10) 1.890(13) 2.731(4) 168(3) .
O1S H1S O8 0.88(3) 2.053(19) 2.887(4) 157(4) 1_655

_refine_diff_density_max         0.741
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1443520'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H86 N6 Ni4 O12'
_chemical_formula_weight         1486.32

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'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.5714(6)
_cell_length_b                   15.1014(10)
_cell_length_c                   21.0065(13)
_cell_angle_alpha                90
_cell_angle_beta                 111.223(4)
_cell_angle_gamma                90
_cell_volume                     3717.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    24423
_cell_measurement_theta_min      2.872
_cell_measurement_theta_max      32.224

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    1.059
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
;
face-indexed (CrysAlis RED; Oxford Diffraction, 2006)
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23490
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.891
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6517
_reflns_number_gt                4863
_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       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_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)+(0.0587P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6517
_refine_ls_number_parameters     472
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0898
_refine_ls_wR_factor_gt          0.0868
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_restrained_S_all      0.968
_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 0.84116(2) 0.08950(2) 0.90131(2) 0.03049(10) Uani 1 1 d . . . . .
Ni2 Ni 1.06312(2) -0.00987(2) 0.94743(2) 0.02968(10) Uani 1 1 d . . . . .
O1 O 0.76073(14) 0.19855(12) 0.85267(9) 0.0429(5) Uani 1 1 d . . . . .
O2 O 0.90205(13) -0.02825(12) 0.94886(8) 0.0296(4) Uani 1 1 d . . . . .
O3 O 0.85749(13) 0.12398(11) 1.00526(8) 0.0344(4) Uani 1 1 d . . . . .
O4 O 1.00959(13) 0.11420(11) 0.92125(8) 0.0332(4) Uani 1 1 d . . . . .
O5 O 1.00137(13) -0.05395(12) 0.84824(8) 0.0346(4) Uani 1 1 d . . . . .
O6 O 0.84414(13) 0.03220(11) 0.81063(8) 0.0319(4) Uani 1 1 d . . . . .
N1 N 0.6932(4) 0.0209(3) 0.8792(2) 0.0347(12) Uani 0.719(4) 1 d D . P A 1
N2 N 0.78246(17) -0.01703(17) 1.05327(10) 0.0395(6) Uani 1 1 d . . . . .
C1 C 0.6523(5) 0.2110(5) 0.8459(4) 0.0457(13) Uani 0.719(4) 1 d . . P A 1
C2 C 0.6142(4) 0.3006(4) 0.8330(3) 0.0458(13) Uani 0.719(4) 1 d . . P A 1
H2 H 0.6673 0.3455 0.8331 0.055 Uiso 0.719(4) 1 calc R U P A 1
C3 C 0.5013(4) 0.3239(4) 0.8202(2) 0.0499(12) Uani 0.719(4) 1 d . . P A 1
H3 H 0.4783 0.3841 0.8119 0.060 Uiso 0.719(4) 1 calc R U P A 1
C4 C 0.4239(4) 0.2608(4) 0.8196(2) 0.0559(12) Uani 0.719(4) 1 d . . P A 1
H4 H 0.3471 0.2776 0.8109 0.067 Uiso 0.719(4) 1 calc R U P A 1
C5 C 0.4535(4) 0.1748(4) 0.8309(2) 0.0539(14) Uani 0.719(4) 1 d . . P A 1
H5 H 0.3971 0.1320 0.8292 0.065 Uiso 0.719(4) 1 calc R U P A 1
C6 C 0.5678(4) 0.1472(4) 0.8455(2) 0.0424(12) Uani 0.719(4) 1 d D . P A 1
C7 C 0.5928(3) 0.0562(3) 0.85791(16) 0.0382(9) Uani 0.719(4) 1 d D . P A 1
H7 H 0.5299 0.0173 0.8499 0.046 Uiso 0.719(4) 1 calc R U P A 1
C8 C 0.7143(5) -0.0716(3) 0.8864(3) 0.0339(11) Uani 0.719(4) 1 d . . P A 1
C9 C 0.6336(3) -0.1377(4) 0.8569(2) 0.0454(11) Uani 0.719(4) 1 d . . P A 1
H9 H 0.5559 -0.1227 0.8327 0.054 Uiso 0.719(4) 1 calc R U P A 1
C10 C 0.6678(4) -0.2234(4) 0.8632(2) 0.0499(13) Uani 0.719(4) 1 d . . P A 1
H10 H 0.6124 -0.2683 0.8444 0.060 Uiso 0.719(4) 1 calc R U P A 1
C11 C 0.7810(4) -0.2479(3) 0.8963(2) 0.0432(10) Uani 0.719(4) 1 d . . P A 1
H11 H 0.8025 -0.3085 0.9000 0.052 Uiso 0.719(4) 1 calc R U P A 1
C12 C 0.8623(4) -0.1821(4) 0.9239(3) 0.0336(10) Uani 0.719(4) 1 d . . P A 1
H12 H 0.9408 -0.1969 0.9453 0.040 Uiso 0.719(4) 1 calc R U P A 1
C13 C 0.8282(9) -0.0985(8) 0.9198(5) 0.0249(12) Uani 0.719(4) 1 d . . P A 1
C14 C 0.76107(19) 0.13413(18) 1.01708(11) 0.0335(6) Uani 1 1 d . . . . .
C15 C 0.7040(2) 0.21539(19) 1.00501(12) 0.0420(7) Uani 1 1 d . . . . .
H15 H 0.7352 0.2648 0.9899 0.050 Uiso 1 1 calc R U . . .
C16 C 0.6002(2) 0.2235(2) 1.01540(14) 0.0543(9) Uani 1 1 d . . . . .
H16 H 0.5604 0.2782 1.0064 0.065 Uiso 1 1 calc R U . B 1
C17 C 0.5557(2) 0.1522(3) 1.03864(13) 0.0558(9) Uani 1 1 d . . . . .
H17 H 0.4856 0.1584 1.0457 0.067 Uiso 1 1 calc R U . . .
C18 C 0.6116(2) 0.0727(2) 1.05152(13) 0.0488(8) Uani 1 1 d . . . . .
H18 H 0.5804 0.0241 1.0676 0.059 Uiso 1 1 calc R U . . .
C19 C 0.7131(2) 0.06302(19) 1.04126(12) 0.0378(6) Uani 1 1 d . . . . .
C20 C 0.7461(2) -0.0919(2) 1.06068(12) 0.0457(7) Uani 1 1 d . . . . .
H20 H 0.6703 -0.0952 1.0601 0.055 Uiso 1 1 calc R U . . .
C21 C 1.1920(2) 0.17220(19) 0.93010(12) 0.0384(6) Uani 1 1 d . . . . .
C22 C 1.2551(2) 0.2512(2) 0.93140(13) 0.0543(8) Uani 1 1 d . . . . .
H22 H 1.3326 0.2462 0.9354 0.065 Uiso 1 1 calc R U . . .
C23 C 1.2088(3) 0.3329(2) 0.92723(15) 0.0625(9) Uani 1 1 d . . . . .
H23 H 1.2537 0.3842 0.9293 0.075 Uiso 1 1 calc R U . . .
C24 C 1.0962(3) 0.3409(2) 0.91999(15) 0.0572(8) Uani 1 1 d . . . . .
H24 H 1.0631 0.3981 0.9163 0.069 Uiso 1 1 calc R U . . .
C25 C 1.0312(2) 0.26775(19) 0.91800(12) 0.0430(7) Uani 1 1 d . . . . .
H25 H 0.9534 0.2754 0.9128 0.052 Uiso 1 1 calc R U . . .
C26 C 1.0751(2) 0.18258(17) 0.92336(11) 0.0321(6) Uani 1 1 d . . . . .
C27 C 0.9072(2) -0.02896(18) 0.80455(12) 0.0342(6) Uani 1 1 d . . . . .
C28 C 0.8653(3) -0.0792(3) 0.73743(16) 0.0763(11) Uani 1 1 d . . . . .
H28A H 0.9018 -0.1376 0.7439 0.114 Uiso 1 1 calc R U . . .
H28B H 0.8847 -0.0460 0.7031 0.114 Uiso 1 1 calc R U . . .
H28C H 0.7823 -0.0865 0.7220 0.114 Uiso 1 1 calc R U . . .
N3 N 0.20232(18) 0.71665(17) 0.77133(11) 0.0496(6) Uani 1 1 d . . . . .
H3A H 0.2175 0.7066 0.7283 0.059 Uiso 1 1 calc R U . . .
C29 C 0.0766(2) 0.7020(2) 0.75423(16) 0.0562(8) Uani 1 1 d . . . . .
H29A H 0.0343 0.7446 0.7182 0.067 Uiso 1 1 calc R U . C 1
H29B H 0.0573 0.6418 0.7348 0.067 Uiso 1 1 calc R U . C 1
C30A C 0.0347(3) 0.7109(2) 0.8118(2) 0.0714(10) Uani 0.735(6) 1 d . . P D 1
H30A H 0.0426 0.7723 0.8295 0.086 Uiso 0.735(6) 1 calc R U P D 1
H30B H 0.0743 0.6697 0.8497 0.086 Uiso 0.735(6) 1 calc R U P D 1
C30B C 0.0347(3) 0.7109(2) 0.8118(2) 0.0714(10) Uani 0.265(6) 1 d . . P D 2
H30C H -0.0489 0.7200 0.7912 0.086 Uiso 0.265(6) 1 calc R U P D 2
H30D H 0.0675 0.7665 0.8360 0.086 Uiso 0.265(6) 1 calc R U P D 2
C31A C -0.0928(5) 0.6848(4) 0.7746(4) 0.111(3) Uani 0.735(6) 1 d . . P D 1
H31A H -0.1281 0.7251 0.7362 0.167 Uiso 0.735(6) 1 calc R U P D 1
H31B H -0.1331 0.6889 0.8066 0.167 Uiso 0.735(6) 1 calc R U P D 1
H31C H -0.0972 0.6239 0.7576 0.167 Uiso 0.735(6) 1 calc R U P D 1
C32 C 0.2400(3) 0.8087(2) 0.79406(14) 0.0561(8) Uani 1 1 d . . . . .
H32A H 0.3228 0.8135 0.8035 0.067 Uiso 1 1 calc R U . . .
H32B H 0.2279 0.8203 0.8373 0.067 Uiso 1 1 calc R U . . .
C33 C 0.1786(3) 0.8785(2) 0.74300(16) 0.0632(9) Uani 1 1 d . . . . .
H33A H 0.1000 0.8852 0.7424 0.076 Uiso 1 1 calc R U . . .
H33B H 0.1738 0.8598 0.6968 0.076 Uiso 1 1 calc R U . . .
C34 C 0.2400(4) 0.9661(3) 0.76049(18) 0.0844(12) Uani 1 1 d . . . . .
H34A H 0.2418 0.9859 0.8053 0.127 Uiso 1 1 calc R U . . .
H34B H 0.1998 1.0101 0.7258 0.127 Uiso 1 1 calc R U . . .
H34C H 0.3182 0.9593 0.7617 0.127 Uiso 1 1 calc R U . . .
C35 C 0.2724(2) 0.6508(2) 0.82213(14) 0.0535(8) Uani 1 1 d . . . . .
H35A H 0.2786 0.6703 0.8683 0.064 Uiso 1 1 calc R U . . .
H35B H 0.2320 0.5932 0.8131 0.064 Uiso 1 1 calc R U . . .
C36 C 0.3888(3) 0.6374(3) 0.82172(19) 0.0832(12) Uani 1 1 d . . . . .
H36A H 0.4300 0.6946 0.8311 0.100 Uiso 1 1 calc R U . . .
H36B H 0.3832 0.6176 0.7757 0.100 Uiso 1 1 calc R U . . .
C37 C 0.4566(3) 0.5701(3) 0.8736(2) 0.0878(12) Uani 1 1 d . . . . .
H37A H 0.4783 0.5953 0.9196 0.132 Uiso 1 1 calc R U . . .
H37B H 0.5256 0.5543 0.8647 0.132 Uiso 1 1 calc R U . . .
H37C H 0.4101 0.5170 0.8703 0.132 Uiso 1 1 calc R U . . .
C31B C 0.0570(9) 0.6318(8) 0.8726(5) 0.053(4) Uani 0.265(6) 1 d . . P D 2
H31D H 0.0228 0.6505 0.9055 0.079 Uiso 0.265(6) 1 calc R U P D 2
H31E H 0.0219 0.5762 0.8511 0.079 Uiso 0.265(6) 1 calc R U P D 2
H31F H 0.1392 0.6230 0.8962 0.079 Uiso 0.265(6) 1 calc R U P D 2
C6B C 0.7090(14) -0.0970(7) 0.8862(9) 0.0424(12) Uani 0.281(4) 1 d DG . P A 2
C5B C 0.6487(8) -0.1755(9) 0.8655(7) 0.0539(14) Uani 0.281(4) 1 d G . P A 2
H5B H 0.5680 -0.1743 0.8436 0.065 Uiso 0.281(4) 1 calc R U P A 2
C4B C 0.7064(10) -0.2559(7) 0.8768(6) 0.0559(12) Uani 0.281(4) 1 d G . P A 2
H4B H 0.6652 -0.3096 0.8627 0.067 Uiso 0.281(4) 1 calc R U P A 2
C3B C 0.8245(10) -0.2577(8) 0.9089(6) 0.0499(12) Uani 0.281(4) 1 d G . P A 2
H3B H 0.8639 -0.3127 0.9167 0.060 Uiso 0.281(4) 1 calc R U P A 2
C1B C 0.8847(8) -0.1792(11) 0.9296(9) 0.0457(13) Uani 0.281(4) 1 d G . P A 2
H1B H 0.9654 -0.1839 0.9501 0.055 Uiso 0.281(4) 1 calc R U P A 2
C2B C 0.836(3) -0.090(3) 0.9231(19) 0.0458(13) Uani 0.281(4) 1 d G . P A 2
C7B C 0.6402(9) -0.0180(7) 0.8681(5) 0.0382(9) Uani 0.281(4) 1 d D . P A 2
H7B H 0.5597 -0.0250 0.8487 0.046 Uiso 0.281(4) 1 calc R U P A 2
N1B N 0.6791(13) 0.0590(8) 0.8762(8) 0.0347(12) Uani 0.281(4) 1 d D . P A 2
C8B C 0.5988(9) 0.1356(7) 0.8508(6) 0.0339(11) Uani 0.281(4) 1 d G . P A 2
C9B C 0.4836(9) 0.1377(6) 0.8415(5) 0.0454(11) Uani 0.281(4) 1 d G . P A 2
H9B H 0.4466 0.0855 0.8480 0.054 Uiso 0.281(4) 1 calc R U P A 2
C10B C 0.4224(7) 0.2162(8) 0.8227(5) 0.0499(13) Uani 0.281(4) 1 d G . P A 2
H10B H 0.3437 0.2176 0.8163 0.060 Uiso 0.281(4) 1 calc R U P A 2
C11B C 0.4766(10) 0.2926(6) 0.8132(6) 0.0432(10) Uani 0.281(4) 1 d G . P A 2
H11B H 0.4348 0.3462 0.8003 0.052 Uiso 0.281(4) 1 calc R U P A 2
C12B C 0.5918(10) 0.2905(7) 0.8225(8) 0.0336(10) Uani 0.281(4) 1 d G . P A 2
H12B H 0.6288 0.3427 0.8160 0.040 Uiso 0.281(4) 1 calc R U P A 2
C13B C 0.6529(7) 0.2120(9) 0.8413(8) 0.0249(12) Uani 0.281(4) 1 d G . P A 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 N1B 1.965(15) . ?
Ni1 O1 2.0076(18) . ?
Ni1 N1 2.030(5) . ?
Ni1 O4 2.0387(15) . ?
Ni1 O2 2.0474(17) . ?
Ni1 O6 2.1050(16) . ?
Ni1 O3 2.1810(16) . ?
Ni2 N2 1.989(2) 3_757 ?
Ni2 O4 1.9994(17) . ?
Ni2 O5 2.0534(16) . ?
Ni2 O2 2.0549(16) . ?
Ni2 O3 2.0580(17) 3_757 ?
Ni2 O2 2.1396(15) 3_757 ?
O1 C13B 1.305(9) . ?
O1 C1 1.332(5) . ?
O2 C2B 1.23(4) . ?
O2 C13 1.396(10) . ?
O2 Ni2 2.1396(15) 3_757 ?
O3 C14 1.331(3) . ?
O3 Ni2 2.0580(17) 3_757 ?
O4 C26 1.312(3) . ?
O5 C27 1.265(3) . ?
O6 C27 1.253(3) . ?
N1 C7 1.292(5) . ?
N1 C8 1.419(6) . ?
N2 C20 1.250(3) . ?
N2 C19 1.458(4) . ?
N2 Ni2 1.989(2) 3_757 ?
C1 C2 1.429(6) . ?
C1 C6 1.432(7) . ?
C2 C3 1.390(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.360(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.348(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.418(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.413(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.398(6) . ?
C8 C13 1.407(13) . ?
C9 C10 1.355(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.389(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.392(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.327(14) . ?
C12 H12 0.9500 . ?
C14 C15 1.397(4) . ?
C14 C19 1.413(4) . ?
C15 C16 1.404(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.368(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.377(4) . ?
C18 H18 0.9500 . ?
C20 C21 1.416(4) 3_757 ?
C20 H20 0.9500 . ?
C21 C20 1.416(4) 3_757 ?
C21 C22 1.428(4) . ?
C21 C26 1.432(3) . ?
C22 C23 1.354(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.373(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.366(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.388(4) . ?
C25 H25 0.9500 . ?
C27 C28 1.518(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N3 C32 1.490(4) . ?
N3 C35 1.491(4) . ?
N3 C29 1.505(3) . ?
N3 H3A 1.0000 . ?
C29 C30B 1.491(4) . ?
C29 C30A 1.491(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30A C31A 1.558(6) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
C30B C31B 1.695(10) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C32 C33 1.502(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.509(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.481(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.508(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C6B C5B 1.3900 . ?
C6B C2B 1.51(4) . ?
C6B C7B 1.441(12) . ?
C5B C4B 1.3900 . ?
C5B H5B 0.9500 . ?
C4B C3B 1.3900 . ?
C4B H4B 0.9500 . ?
C3B C1B 1.3900 . ?
C3B H3B 0.9500 . ?
C1B C2B 1.47(4) . ?
C1B H1B 0.9500 . ?
C7B N1B 1.249(14) . ?
C7B H7B 0.9500 . ?
N1B C8B 1.501(16) . ?
C8B C9B 1.3900 . ?
C8B C13B 1.3900 . ?
C9B C10B 1.3900 . ?
C9B H9B 0.9500 . ?
C10B C11B 1.3900 . ?
C10B H10B 0.9500 . ?
C11B C12B 1.3900 . ?
C11B H11B 0.9500 . ?
C12B C13B 1.3900 . ?
C12B H12B 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1B Ni1 O1 76.9(4) . . ?
O1 Ni1 N1 92.93(12) . . ?
N1B Ni1 O4 175.3(4) . . ?
O1 Ni1 O4 104.40(7) . . ?
N1 Ni1 O4 159.66(12) . . ?
N1B Ni1 O2 95.5(4) . . ?
O1 Ni1 O2 172.39(7) . . ?
N1 Ni1 O2 79.54(12) . . ?
O4 Ni1 O2 83.20(6) . . ?
N1B Ni1 O6 91.0(4) . . ?
O1 Ni1 O6 92.71(7) . . ?
N1 Ni1 O6 84.14(14) . . ?
O4 Ni1 O6 84.47(6) . . ?
O2 Ni1 O6 87.62(6) . . ?
N1B Ni1 O3 92.1(5) . . ?
O1 Ni1 O3 99.28(7) . . ?
N1 Ni1 O3 95.60(15) . . ?
O4 Ni1 O3 92.08(6) . . ?
O2 Ni1 O3 80.55(6) . . ?
O6 Ni1 O3 168.01(6) . . ?
N2 Ni2 O4 92.22(9) 3_757 . ?
N2 Ni2 O5 94.03(7) 3_757 . ?
O4 Ni2 O5 93.37(7) . . ?
N2 Ni2 O2 175.96(9) 3_757 . ?
O4 Ni2 O2 83.99(7) . . ?
O5 Ni2 O2 87.62(6) . . ?
N2 Ni2 O3 82.56(8) 3_757 3_757 ?
O4 Ni2 O3 166.80(6) . 3_757 ?
O5 Ni2 O3 99.07(7) . 3_757 ?
O2 Ni2 O3 100.84(7) . 3_757 ?
N2 Ni2 O2 96.44(7) 3_757 3_757 ?
O4 Ni2 O2 87.27(6) . 3_757 ?
O5 Ni2 O2 169.49(6) . 3_757 ?
O2 Ni2 O2 82.00(7) . 3_757 ?
O3 Ni2 O2 81.31(6) 3_757 3_757 ?
C13B O1 Ni1 121.3(6) . . ?
C1 O1 Ni1 118.5(3) . . ?
C2B O2 Ni1 111.5(17) . . ?
C13 O2 Ni1 112.0(5) . . ?
C2B O2 Ni2 127.2(17) . . ?
C13 O2 Ni2 126.8(5) . . ?
Ni1 O2 Ni2 94.12(7) . . ?
C2B O2 Ni2 120.5(17) . 3_757 ?
C13 O2 Ni2 120.5(4) . 3_757 ?
Ni1 O2 Ni2 99.54(7) . 3_757 ?
Ni2 O2 Ni2 97.99(7) . 3_757 ?
C14 O3 Ni2 108.75(15) . 3_757 ?
C14 O3 Ni1 116.88(13) . . ?
Ni2 O3 Ni1 97.87(7) 3_757 . ?
C26 O4 Ni2 125.71(15) . . ?
C26 O4 Ni1 138.07(16) . . ?
Ni2 O4 Ni1 96.10(7) . . ?
C27 O5 Ni2 123.39(16) . . ?
C27 O6 Ni1 127.90(15) . . ?
C7 N1 C8 124.3(5) . . ?
C7 N1 Ni1 124.6(3) . . ?
C8 N1 Ni1 111.0(3) . . ?
C20 N2 C19 123.3(2) . . ?
C20 N2 Ni2 126.0(2) . 3_757 ?
C19 N2 Ni2 110.69(17) . 3_757 ?
O1 C1 C2 114.4(6) . . ?
O1 C1 C6 129.3(5) . . ?
C2 C1 C6 116.1(4) . . ?
C3 C2 C1 121.6(4) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 121.5(4) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C6 121.0(5) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 117.8(4) . . ?
C7 C6 C1 122.5(4) . . ?
C5 C6 C1 119.6(4) . . ?
N1 C7 C6 126.2(4) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
C9 C8 C13 117.3(6) . . ?
C9 C8 N1 125.3(5) . . ?
C13 C8 N1 117.0(5) . . ?
C10 C9 C8 119.0(4) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
C9 C10 C11 122.3(4) . . ?
C9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C10 C11 C12 118.9(4) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C13 C12 C11 118.7(6) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 O2 123.1(8) . . ?
C12 C13 C8 123.6(7) . . ?
O2 C13 C8 113.2(9) . . ?
O3 C14 C15 120.6(2) . . ?
O3 C14 C19 121.0(2) . . ?
C15 C14 C19 118.4(2) . . ?
C14 C15 C16 119.5(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 120.6(3) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 120.1(3) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C14 121.1(3) . . ?
C18 C19 N2 126.2(3) . . ?
C14 C19 N2 112.7(2) . . ?
N2 C20 C21 125.7(3) . 3_757 ?
N2 C20 H20 117.1 . . ?
C21 C20 H20 117.1 3_757 . ?
C20 C21 C22 116.0(3) 3_757 . ?
C20 C21 C26 126.9(2) 3_757 . ?
C22 C21 C26 117.0(3) . . ?
C23 C22 C21 122.5(3) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C22 C23 C24 119.3(3) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C25 C24 C23 120.9(3) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
C24 C25 C26 122.0(3) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
O4 C26 C25 120.0(2) . . ?
O4 C26 C21 121.8(2) . . ?
C25 C26 C21 118.2(2) . . ?
O6 C27 O5 127.3(2) . . ?
O6 C27 C28 116.3(2) . . ?
O5 C27 C28 116.3(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32 N3 C35 110.9(2) . . ?
C32 N3 C29 113.5(2) . . ?
C35 N3 C29 111.7(2) . . ?
C32 N3 H3A 106.8 . . ?
C35 N3 H3A 106.8 . . ?
C29 N3 H3A 106.8 . . ?
C30B C29 N3 116.2(3) . . ?
C30A C29 N3 116.2(3) . . ?
C30A C29 H29A 108.2 . . ?
N3 C29 H29A 108.2 . . ?
C30A C29 H29B 108.2 . . ?
N3 C29 H29B 108.2 . . ?
H29A C29 H29B 107.4 . . ?
C29 C30A C31A 99.8(3) . . ?
C29 C30A H30A 111.8 . . ?
C31A C30A H30A 111.8 . . ?
C29 C30A H30B 111.8 . . ?
C31A C30A H30B 111.8 . . ?
H30A C30A H30B 109.5 . . ?
C29 C30B C31B 122.4(5) . . ?
C29 C30B H30C 106.7 . . ?
C31B C30B H30C 106.7 . . ?
C29 C30B H30D 106.7 . . ?
C31B C30B H30D 106.7 . . ?
H30C C30B H30D 106.6 . . ?
C30A C31A H31A 109.5 . . ?
C30A C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C30A C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
N3 C32 C33 113.8(2) . . ?
N3 C32 H32A 108.8 . . ?
C33 C32 H32A 108.8 . . ?
N3 C32 H32B 108.8 . . ?
C33 C32 H32B 108.8 . . ?
H32A C32 H32B 107.7 . . ?
C32 C33 C34 110.9(3) . . ?
C32 C33 H33A 109.5 . . ?
C34 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N3 114.6(3) . . ?
C36 C35 H35A 108.6 . . ?
N3 C35 H35A 108.6 . . ?
C36 C35 H35B 108.6 . . ?
N3 C35 H35B 108.6 . . ?
H35A C35 H35B 107.6 . . ?
C35 C36 C37 112.9(3) . . ?
C35 C36 H36A 109.0 . . ?
C37 C36 H36A 109.0 . . ?
C35 C36 H36B 109.0 . . ?
C37 C36 H36B 109.0 . . ?
H36A C36 H36B 107.8 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C30B C31B H31D 109.5 . . ?
C30B C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C30B C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C5B C6B C2B 125.5(16) . . ?
C5B C6B C7B 114.6(12) . . ?
C2B C6B C7B 119.9(18) . . ?
C6B C5B C4B 120.0 . . ?
C6B C5B H5B 120.0 . . ?
C4B C5B H5B 120.0 . . ?
C3B C4B C5B 120.0 . . ?
C3B C4B H4B 120.0 . . ?
C5B C4B H4B 120.0 . . ?
C1B C3B C4B 120.0 . . ?
C1B C3B H3B 120.0 . . ?
C4B C3B H3B 120.0 . . ?
C3B C1B C2B 126.6(15) . . ?
C3B C1B H1B 116.7 . . ?
C2B C1B H1B 116.7 . . ?
O2 C2B C1B 118(3) . . ?
O2 C2B C6B 134(3) . . ?
C1B C2B C6B 108(3) . . ?
N1B C7B C6B 124.5(11) . . ?
N1B C7B H7B 117.7 . . ?
C6B C7B H7B 117.7 . . ?
C7B N1B C8B 119.3(12) . . ?
C7B N1B Ni1 124.9(10) . . ?
C8B N1B Ni1 114.4(8) . . ?
C9B C8B C13B 120.0 . . ?
C9B C8B N1B 126.9(10) . . ?
C13B C8B N1B 112.9(10) . . ?
C10B C9B C8B 120.0 . . ?
C10B C9B H9B 120.0 . . ?
C8B C9B H9B 120.0 . . ?
C11B C10B C9B 120.0 . . ?
C11B C10B H10B 120.0 . . ?
C9B C10B H10B 120.0 . . ?
C12B C11B C10B 120.0 . . ?
C12B C11B H11B 120.0 . . ?
C10B C11B H11B 120.0 . . ?
C11B C12B C13B 120.0 . . ?
C11B C12B H12B 120.0 . . ?
C13B C12B H12B 120.0 . . ?
O1 C13B C12B 128.0(10) . . ?
O1 C13B C8B 112.0(9) . . ?
C12B C13B C8B 120.0 . . ?

_refine_diff_density_max         0.642
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.060

