# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1519306'
_audit_update_record             
;
2016-11-25 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C6 H24 N6 Ni), 8(C H O2), 3(C2 H6 O)'
_chemical_formula_sum            'C38 H122 N24 Ni4 O19'
_chemical_formula_weight         1454.43

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'
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'
H H 0.0000 0.0000 '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                   9.7670(4)
_cell_length_b                   15.3025(5)
_cell_length_c                   12.9080(5)
_cell_angle_alpha                90
_cell_angle_beta                 111.908(5)
_cell_angle_gamma                90
_cell_volume                     1789.90(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    200
_cell_measurement_reflns_used    3287
_cell_measurement_theta_min      4.6970
_cell_measurement_theta_max      70.6200
_cell_oxdiff_twin_number         2
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -0.9997 0.0287 0.0007 0.0750 1.0001 0.0064 0.0005 -0.0099 -0.9990



_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_F_000             782
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    1.814
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.41280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14254
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.689
_diffrn_reflns_theta_max         62.492
_diffrn_reflns_theta_full        62.500
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_orient_matrix_UB_11      0.1539636000
_diffrn_orient_matrix_UB_12      0.0381404000
_diffrn_orient_matrix_UB_13      0.0214524000
_diffrn_orient_matrix_UB_21      -0.0688357000
_diffrn_orient_matrix_UB_22      0.0910706000
_diffrn_orient_matrix_UB_23      -0.0355665000
_diffrn_orient_matrix_UB_31      0.0199181000
_diffrn_orient_matrix_UB_32      0.0200209000
_diffrn_orient_matrix_UB_33      0.1218067000
_diffrn_oxdiff_twin_integration_method simultaneous
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.8858 6057 2143
2 0.1142 6054 2143

_reflns_number_total             5911
_reflns_number_gt                3549
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;

_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1568P)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         5911
_refine_ls_number_parameters     256
_refine_ls_number_restraints     186
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.2365
_refine_ls_wR_factor_gt          0.2240
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.019
_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 0.2393(8) 0.1497(3) 0.0904(6) 0.0600(15) Uani 1 1 d . U . . .
H1A H 0.1391 0.1492 0.0357 0.072 Uiso 1 1 calc R U . . .
H1B H 0.2529 0.0985 0.1376 0.072 Uiso 1 1 calc R U . . .
C2 C 0.3481(8) 0.1484(3) 0.0323(6) 0.0625(16) Uani 1 1 d . U . . .
H2A H 0.4483 0.1473 0.0870 0.075 Uiso 1 1 calc R U . . .
H2B H 0.3330 0.0967 -0.0142 0.075 Uiso 1 1 calc R U . . .
C3 C 0.0543(6) 0.4279(4) -0.1014(5) 0.0529(13) Uani 1 1 d . U . . .
H3A H 0.0626 0.4803 -0.0572 0.063 Uiso 1 1 calc R U . . .
H3B H -0.0418 0.4279 -0.1615 0.063 Uiso 1 1 calc R U . . .
C4 C 0.1746(6) 0.4267(3) -0.1489(4) 0.0461(12) Uani 1 1 d . U . . .
H4A H 0.1637 0.3757 -0.1960 0.055 Uiso 1 1 calc R U . . .
H4B H 0.1677 0.4784 -0.1940 0.055 Uiso 1 1 calc R U . . .
C5 C 0.5628(6) 0.4167(4) 0.2250(5) 0.0574(14) Uani 1 1 d . U . . .
H5A H 0.5663 0.4671 0.1805 0.069 Uiso 1 1 calc R U . . .
H5B H 0.6579 0.4113 0.2858 0.069 Uiso 1 1 calc R U . . .
C6 C 0.4434(6) 0.4290(4) 0.2712(4) 0.0552(13) Uani 1 1 d . U . . .
H6A H 0.4464 0.3816 0.3219 0.066 Uiso 1 1 calc R U . . .
H6B H 0.4587 0.4835 0.3123 0.066 Uiso 1 1 calc R U . . .
C7 C 0.3560(6) 0.6602(3) 0.1061(5) 0.0510(13) Uani 1 1 d D U . . .
H7B H 0.2825 0.6785 0.1307 0.061 Uiso 1 1 calc R U . . .
N1 N 0.2655(5) 0.2298(2) 0.1585(4) 0.0486(10) Uani 1 1 d . U . . .
H1C H 0.3511 0.2225 0.2270 0.058 Uiso 1 1 calc R U . . .
H1D H 0.1807 0.2426 0.1779 0.058 Uiso 1 1 calc R U . . .
N2 N 0.3244(5) 0.2277(2) -0.0370(3) 0.0455(10) Uani 1 1 d . U . . .
H2C H 0.2361 0.2217 -0.1038 0.055 Uiso 1 1 calc R U . . .
H2D H 0.4077 0.2376 -0.0591 0.055 Uiso 1 1 calc R U . . .
N3 N 0.0702(5) 0.3500(3) -0.0312(4) 0.0494(10) Uani 1 1 d . U . . .
H3C H 0.0299 0.2991 -0.0773 0.059 Uiso 1 1 calc R U . . .
H3D H 0.0181 0.3580 0.0191 0.059 Uiso 1 1 calc R U . . .
N4 N 0.3194(4) 0.4244(3) -0.0549(3) 0.0431(9) Uani 1 1 d . U . . .
H4C H 0.3437 0.4817 -0.0208 0.052 Uiso 1 1 calc R U . . .
H4D H 0.3963 0.4068 -0.0811 0.052 Uiso 1 1 calc R U . . .
N5 N 0.5326(5) 0.3375(3) 0.1555(4) 0.0550(11) Uani 1 1 d . U . . .
H5C H 0.5634 0.2860 0.2023 0.066 Uiso 1 1 calc R U . . .
H5D H 0.5862 0.3393 0.1057 0.066 Uiso 1 1 calc R U . . .
N6 N 0.2986(5) 0.4304(3) 0.1778(3) 0.0464(10) Uani 1 1 d . U . . .
H6C H 0.2811 0.4873 0.1423 0.056 Uiso 1 1 calc R U . . .
H6D H 0.2204 0.4185 0.2051 0.056 Uiso 1 1 calc R U . . .
O1 O 0.3245(8) 0.5987(3) 0.0420(5) 0.112(2) Uani 1 1 d D U . . .
C8 C -0.0404(14) 0.3275(7) 0.2373(12) 0.054(3) Uani 0.70(2) 1 d D U P A 3
H8A H -0.1100 0.3638 0.1868 0.065 Uiso 0.70(2) 1 calc R U P A 3
O3 O 0.0786(10) 0.3374(8) 0.2458(10) 0.092(3) Uani 0.70(2) 1 d D U P A 3
O4 O -0.0901(11) 0.2722(7) 0.2890(9) 0.115(5) Uani 0.70(2) 1 d D U P A 3
C8' C -0.020(5) 0.340(2) 0.259(6) 0.12(2) Uani 0.30(2) 1 d D U P A 4
H8' H -0.1107 0.3625 0.2543 0.149 Uiso 0.30(2) 1 calc R U P A 4
O3' O 0.071(2) 0.3895(19) 0.270(3) 0.103(8) Uani 0.30(2) 1 d D U P A 4
O4' O -0.009(3) 0.2603(13) 0.2540(19) 0.093(8) Uani 0.30(2) 1 d D U P A 4
O2 O 0.4688(5) 0.7003(4) 0.1417(4) 0.0849(14) Uani 1 1 d D U . . .
O7 O -0.269(3) 0.178(2) 0.145(3) 0.089(8) Uani 0.31(3) 1 d D U P B 1
H7A H -0.2003 0.1746 0.2051 0.134 Uiso 0.31(3) 1 calc R U P B 1
C9 C -0.270(3) 0.1024(18) 0.077(3) 0.063(9) Uani 0.31(3) 1 d D U P B 1
H9A H -0.3563 0.1029 0.0086 0.075 Uiso 0.31(3) 1 calc R U P B 1
H9B H -0.2700 0.0491 0.1176 0.075 Uiso 0.31(3) 1 calc R U P B 1
C10 C -0.136(2) 0.108(2) 0.052(2) 0.059(7) Uani 0.31(3) 1 d D U P B 1
H10A H -0.1371 0.0624 0.0002 0.089 Uiso 0.31(3) 1 calc R U P B 1
H10B H -0.0507 0.1001 0.1198 0.089 Uiso 0.31(3) 1 calc R U P B 1
H10C H -0.1308 0.1636 0.0203 0.089 Uiso 0.31(3) 1 calc R U P B 1
O7' O -0.2832(18) 0.1376(14) 0.1656(12) 0.073(5) Uani 0.44(3) 1 d D U P B 2
H7' H -0.2071 0.1540 0.2154 0.110 Uiso 0.44(3) 1 calc R U P B 2
C9' C -0.257(4) 0.128(2) 0.061(2) 0.096(10) Uani 0.44(3) 1 d D U P B 2
H9'1 H -0.3474 0.1086 0.0023 0.116 Uiso 0.44(3) 1 calc R U P B 2
H9'2 H -0.2302 0.1838 0.0396 0.116 Uiso 0.44(3) 1 calc R U P B 2
C10' C -0.142(2) 0.0655(16) 0.0714(18) 0.070(5) Uani 0.44(3) 1 d D U P B 2
H10D H -0.1303 0.0600 0.0009 0.105 Uiso 0.44(3) 1 calc R U P B 2
H10E H -0.1674 0.0097 0.0930 0.105 Uiso 0.44(3) 1 calc R U P B 2
H10F H -0.0507 0.0854 0.1270 0.105 Uiso 0.44(3) 1 calc R U P B 2
Ni1 Ni 0.30129(8) 0.33296(5) 0.06175(6) 0.0394(4) Uani 1 1 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 N1 1.475(7) . ?
C1 C2 1.513(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.474(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.470(7) . ?
C3 C4 1.515(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.481(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N5 1.470(7) . ?
C5 C6 1.507(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N6 1.477(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O2 1.193(7) . ?
C7 O1 1.215(7) . ?
C7 H7B 0.9300 . ?
N1 Ni1 2.121(4) . ?
N1 H1C 0.9700 . ?
N1 H1D 0.9700 . ?
N2 Ni1 2.117(4) . ?
N2 H2C 0.9700 . ?
N2 H2D 0.9700 . ?
N3 Ni1 2.140(4) . ?
N3 H3C 0.9700 . ?
N3 H3D 0.9700 . ?
N4 Ni1 2.110(4) . ?
N4 H4C 0.9700 . ?
N4 H4D 0.9700 . ?
N5 Ni1 2.129(5) . ?
N5 H5C 0.9700 . ?
N5 H5D 0.9700 . ?
N6 Ni1 2.120(4) . ?
N6 H6C 0.9700 . ?
N6 H6D 0.9700 . ?
C8 O3 1.137(13) . ?
C8 O4 1.280(13) . ?
C8 H8A 0.9300 . ?
C8' O3' 1.13(3) . ?
C8' O4' 1.24(3) . ?
C8' H8' 0.9300 . ?
O7 C9 1.45(3) . ?
O7 H7A 0.8200 . ?
C9 C10 1.46(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
O7' C9' 1.47(2) . ?
O7' H7' 0.8200 . ?
C9' C10' 1.44(2) . ?
C9' H9'1 0.9700 . ?
C9' H9'2 0.9700 . ?
C10' H10D 0.9600 . ?
C10' H10E 0.9600 . ?
C10' H10F 0.9600 . ?

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
N1 C1 C2 108.0(4) . . ?
N1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
N1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
N2 C2 C1 108.0(5) . . ?
N2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
N2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
N3 C3 C4 108.7(4) . . ?
N3 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
N3 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.3 . . ?
N4 C4 C3 108.4(4) . . ?
N4 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
N4 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
N5 C5 C6 109.6(4) . . ?
N5 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N5 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
N6 C6 C5 109.0(4) . . ?
N6 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
N6 C6 H6B 109.9 . . ?
C5 C6 H6B 109.9 . . ?
H6A C6 H6B 108.3 . . ?
O2 C7 O1 128.6(6) . . ?
O2 C7 H7B 115.7 . . ?
O1 C7 H7B 115.7 . . ?
C1 N1 Ni1 107.3(3) . . ?
C1 N1 H1C 110.3 . . ?
Ni1 N1 H1C 110.3 . . ?
C1 N1 H1D 110.3 . . ?
Ni1 N1 H1D 110.3 . . ?
H1C N1 H1D 108.5 . . ?
C2 N2 Ni1 106.8(3) . . ?
C2 N2 H2C 110.4 . . ?
Ni1 N2 H2C 110.4 . . ?
C2 N2 H2D 110.4 . . ?
Ni1 N2 H2D 110.4 . . ?
H2C N2 H2D 108.6 . . ?
C3 N3 Ni1 106.9(3) . . ?
C3 N3 H3C 110.3 . . ?
Ni1 N3 H3C 110.3 . . ?
C3 N3 H3D 110.3 . . ?
Ni1 N3 H3D 110.3 . . ?
H3C N3 H3D 108.6 . . ?
C4 N4 Ni1 107.0(3) . . ?
C4 N4 H4C 110.3 . . ?
Ni1 N4 H4C 110.3 . . ?
C4 N4 H4D 110.3 . . ?
Ni1 N4 H4D 110.3 . . ?
H4C N4 H4D 108.6 . . ?
C5 N5 Ni1 107.6(3) . . ?
C5 N5 H5C 110.2 . . ?
Ni1 N5 H5C 110.2 . . ?
C5 N5 H5D 110.2 . . ?
Ni1 N5 H5D 110.2 . . ?
H5C N5 H5D 108.5 . . ?
C6 N6 Ni1 107.8(3) . . ?
C6 N6 H6C 110.1 . . ?
Ni1 N6 H6C 110.1 . . ?
C6 N6 H6D 110.1 . . ?
Ni1 N6 H6D 110.1 . . ?
H6C N6 H6D 108.5 . . ?
O3 C8 O4 127.7(12) . . ?
O3 C8 H8A 116.1 . . ?
O4 C8 H8A 116.1 . . ?
O3' C8' O4' 126(4) . . ?
O3' C8' H8' 117.0 . . ?
O4' C8' H8' 117.0 . . ?
C9 O7 H7A 109.5 . . ?
O7 C9 C10 107(2) . . ?
O7 C9 H9A 110.4 . . ?
C10 C9 H9A 110.4 . . ?
O7 C9 H9B 110.4 . . ?
C10 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9' O7' H7' 109.5 . . ?
C10' C9' O7' 112(2) . . ?
C10' C9' H9'1 109.1 . . ?
O7' C9' H9'1 109.1 . . ?
C10' C9' H9'2 109.1 . . ?
O7' C9' H9'2 109.1 . . ?
H9'1 C9' H9'2 107.8 . . ?
C9' C10' H10D 109.5 . . ?
C9' C10' H10E 109.5 . . ?
H10D C10' H10E 109.5 . . ?
C9' C10' H10F 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?
N4 Ni1 N2 91.07(16) . . ?
N4 Ni1 N6 93.69(16) . . ?
N2 Ni1 N6 172.81(16) . . ?
N4 Ni1 N1 171.65(16) . . ?
N2 Ni1 N1 82.33(16) . . ?
N6 Ni1 N1 93.38(17) . . ?
N4 Ni1 N5 91.75(16) . . ?
N2 Ni1 N5 92.19(17) . . ?
N6 Ni1 N5 82.28(17) . . ?
N1 Ni1 N5 93.60(18) . . ?
N4 Ni1 N3 82.59(16) . . ?
N2 Ni1 N3 94.71(17) . . ?
N6 Ni1 N3 91.25(17) . . ?
N1 Ni1 N3 92.82(17) . . ?
N5 Ni1 N3 171.14(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 -59.0(7) . . . . ?
N3 C3 C4 N4 -58.1(5) . . . . ?
N5 C5 C6 N6 -55.2(6) . . . . ?
C2 C1 N1 Ni1 42.0(6) . . . . ?
C1 C2 N2 Ni1 44.4(6) . . . . ?
C4 C3 N3 Ni1 41.1(5) . . . . ?
C3 C4 N4 Ni1 43.6(4) . . . . ?
C6 C5 N5 Ni1 40.2(5) . . . . ?
C5 C6 N6 Ni1 40.7(5) . . . . ?

_refine_diff_density_max         0.951
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.119




# start Validation Reply Form
_vrf_PLAT029_shelx               
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.955 Note  
RESPONSE: Crystals undergo of phase transition below ca. 180 K. Despite this,
crystals were found to be twinned, at least into three different domains.
By data integration, two domains were taken into account. Reflections at higher
theta angles were not only comparatively weak, they did even overlap
with each other significantly. 
Therefore, the number of data for refinement were restricted.
;
# end Validation Reply Form



_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1519308'
_audit_update_record             
;
2016-11-25 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H26 N6 Ni, 2(C H O2)'
_chemical_formula_sum            'C10 H28 N6 Ni O4'
_chemical_formula_weight         355.09

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'
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'
H H 0.0000 0.0000 '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                   13.2477(5)
_cell_length_b                   8.7413(3)
_cell_length_c                   13.7152(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.087(3)
_cell_angle_gamma                90
_cell_volume                     1587.2(1)
_cell_formula_units_Z            4
_cell_measurement_temperature    110
_cell_measurement_reflns_used    2942
_cell_measurement_theta_min      4.0940
_cell_measurement_theta_max      27.6560

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_F_000             760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.32
_exptl_absorpt_coefficient_mu    1.248
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.95165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         1
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6343
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.972
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2801
_reflns_number_gt                2530
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0268P)²+2.8514P] 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         2801
_refine_ls_number_parameters     230
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.0792
_refine_ls_wR_factor_gt          0.0772
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.003
_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 0.5853(2) 0.1524(3) 0.4007(2) 0.0250(6) Uani 1 1 d . . . . .
H1A H 0.5950 0.1300 0.3324 0.030 Uiso 1 1 calc R U . . .
H1B H 0.5184 0.1178 0.4168 0.030 Uiso 1 1 calc R U . . .
C2 C 0.6635(2) 0.0685(3) 0.4628(2) 0.0273(7) Uani 1 1 d . . . . .
H2A H 0.6463 0.0747 0.5308 0.033 Uiso 1 1 calc R U . . .
H2B H 0.6644 -0.0385 0.4442 0.033 Uiso 1 1 calc R U . . .
C3 C 0.8438(2) 0.0962(3) 0.5179(2) 0.0260(6) Uani 1 1 d . . . . .
H3A H 0.8621 -0.0104 0.5098 0.031 Uiso 1 1 calc R U . . .
H3B H 0.8225 0.1101 0.5843 0.031 Uiso 1 1 calc R U . . .
C4 C 0.9334(2) 0.1952(3) 0.5008(2) 0.0284(7) Uani 1 1 d . . . . .
H4A H 0.9828 0.1825 0.5541 0.034 Uiso 1 1 calc R U . . .
H4B H 0.9644 0.1640 0.4410 0.034 Uiso 1 1 calc R U . . .
C7 C 0.7723(2) 0.5728(3) 0.28130(18) 0.0196(6) Uani 1 1 d . . . . .
H7A H 0.7042 0.5951 0.2570 0.024 Uiso 1 1 calc R U . . .
H7B H 0.8187 0.6004 0.2311 0.024 Uiso 1 1 calc R U . . .
C8 C 0.7959(2) 0.6662(3) 0.37292(18) 0.0176(6) Uani 1 1 d . . . . .
H8A H 0.8664 0.6542 0.3933 0.021 Uiso 1 1 calc R U . . .
H8B H 0.7829 0.7738 0.3606 0.021 Uiso 1 1 calc R U . . .
C9 C 0.7505(2) 0.6652(3) 0.54858(18) 0.0194(6) Uani 1 1 d . . . . .
H9A H 0.7305 0.7715 0.5538 0.023 Uiso 1 1 calc R U . . .
H9B H 0.8220 0.6571 0.5659 0.023 Uiso 1 1 calc R U . . .
C10 C 0.6895(2) 0.5665(3) 0.61559(18) 0.0219(6) Uani 1 1 d . . . . .
H10A H 0.7034 0.5964 0.6829 0.026 Uiso 1 1 calc R U . . .
H10B H 0.6180 0.5813 0.6009 0.026 Uiso 1 1 calc R U . . .
C11 C 0.9435(2) 0.4952(4) 0.7467(2) 0.0322(8) Uani 1 1 d . . . . .
H11 H 0.9756 0.5363 0.8021 0.039 Uiso 1 1 calc R U . . .
C12 C 0.5025(2) 0.7789(3) 0.33180(18) 0.0189(6) Uani 1 1 d . . . . .
H12 H 0.5574 0.8114 0.2968 0.023 Uiso 1 1 calc R U . . .
N1 N 0.59351(16) 0.3195(3) 0.41712(16) 0.0161(5) Uani 1 1 d D . . . .
N2 N 0.76202(18) 0.1346(3) 0.45052(18) 0.0237(5) Uani 1 1 d D . . . .
N3 N 0.90367(16) 0.3576(3) 0.49347(16) 0.0157(5) Uani 1 1 d D . . . .
N4 N 0.78158(17) 0.4083(3) 0.30304(15) 0.0173(5) Uani 1 1 d D . . . .
N5 N 0.73036(16) 0.6093(2) 0.44893(15) 0.0145(5) Uani 1 1 d D . . . .
N6 N 0.71583(17) 0.4047(3) 0.60257(15) 0.0180(5) Uani 1 1 d D . . . .
O1 O 0.98213(15) 0.5268(3) 0.67042(14) 0.0310(5) Uani 1 1 d . . . . .
O2 O 0.86827(17) 0.4170(3) 0.76211(16) 0.0433(6) Uani 1 1 d . . . . .
O3 O 0.52172(14) 0.6840(2) 0.39727(14) 0.0247(5) Uani 1 1 d . . . . .
O4 O 0.42038(14) 0.8359(2) 0.30705(14) 0.0257(5) Uani 1 1 d . . . . .
Ni1 Ni 0.74636(2) 0.37238(4) 0.45255(2) 0.01212(11) Uani 1 1 d . . . . .
H1 H 0.571(2) 0.369(3) 0.3624(16) 0.026(8) Uiso 1 1 d D . . . .
H2 H 0.556(2) 0.344(3) 0.4691(16) 0.021(8) Uiso 1 1 d D . . . .
H3 H 0.786(4) 0.100(6) 0.390(2) 0.106(19) Uiso 1 1 d D . . . .
H4 H 0.942(2) 0.399(3) 0.4478(17) 0.021(8) Uiso 1 1 d D . . . .
H5 H 0.916(2) 0.408(3) 0.5503(15) 0.018(7) Uiso 1 1 d D . . . .
H6 H 0.7713(19) 0.384(4) 0.644(2) 0.042(10) Uiso 1 1 d D . . . .
H7 H 0.6630(19) 0.345(3) 0.623(2) 0.035(9) Uiso 1 1 d D . . . .
H8 H 0.6647(14) 0.632(3) 0.430(2) 0.018(7) Uiso 1 1 d D . . . .
H9 H 0.737(2) 0.355(4) 0.263(2) 0.039(10) Uiso 1 1 d D . . . .
H10 H 0.8471(15) 0.380(4) 0.294(2) 0.034(9) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.481(4) . ?
C1 C2 1.507(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.442(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.439(4) . ?
C3 C4 1.494(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N3 1.475(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 N4 1.473(4) . ?
C7 C8 1.522(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N5 1.468(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N5 1.467(3) . ?
C9 C10 1.515(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N6 1.470(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O1 1.213(3) . ?
C11 O2 1.233(4) . ?
C11 H11 0.9300 . ?
C12 O4 1.233(3) . ?
C12 O3 1.242(3) . ?
C12 H12 0.9300 . ?
N1 Ni1 2.116(2) . ?
N1 H1 0.909(18) . ?
N1 H2 0.908(17) . ?
N2 Ni1 2.089(2) . ?
N2 H3 0.954(19) . ?
N3 Ni1 2.142(2) . ?
N3 H4 0.901(17) . ?
N3 H5 0.904(17) . ?
N4 Ni1 2.143(2) . ?
N4 H9 0.922(18) . ?
N4 H10 0.916(18) . ?
N5 Ni1 2.082(2) . ?
N5 H8 0.920(17) . ?
N6 Ni1 2.130(2) . ?
N6 H6 0.932(18) . ?
N6 H7 0.922(18) . ?

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
N1 C1 C2 110.4(2) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 110.2(2) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 110.3(2) . . ?
N2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
N3 C4 C3 110.9(2) . . ?
N3 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N3 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
N4 C7 C8 110.1(2) . . ?
N4 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
N4 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
N5 C8 C7 107.2(2) . . ?
N5 C8 H8A 110.3 . . ?
C7 C8 H8A 110.3 . . ?
N5 C8 H8B 110.3 . . ?
C7 C8 H8B 110.3 . . ?
H8A C8 H8B 108.5 . . ?
N5 C9 C10 107.0(2) . . ?
N5 C9 H9A 110.3 . . ?
C10 C9 H9A 110.3 . . ?
N5 C9 H9B 110.3 . . ?
C10 C9 H9B 110.3 . . ?
H9A C9 H9B 108.6 . . ?
N6 C10 C9 109.9(2) . . ?
N6 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
N6 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
O1 C11 O2 130.0(3) . . ?
O1 C11 H11 115.0 . . ?
O2 C11 H11 115.0 . . ?
O4 C12 O3 128.6(3) . . ?
O4 C12 H12 115.7 . . ?
O3 C12 H12 115.7 . . ?
C1 N1 Ni1 108.33(17) . . ?
C1 N1 H1 108.8(19) . . ?
Ni1 N1 H1 112(2) . . ?
C1 N1 H2 108.3(19) . . ?
Ni1 N1 H2 108.1(19) . . ?
H1 N1 H2 111(3) . . ?
C3 N2 C2 119.7(2) . . ?
C3 N2 Ni1 107.25(17) . . ?
C2 N2 Ni1 107.83(18) . . ?
C3 N2 H3 103(3) . . ?
C2 N2 H3 108(3) . . ?
Ni1 N2 H3 111(3) . . ?
C4 N3 Ni1 109.31(16) . . ?
C4 N3 H4 106.2(19) . . ?
Ni1 N3 H4 111.5(19) . . ?
C4 N3 H5 111.8(18) . . ?
Ni1 N3 H5 109.7(18) . . ?
H4 N3 H5 108(3) . . ?
C7 N4 Ni1 108.49(16) . . ?
C7 N4 H9 109(2) . . ?
Ni1 N4 H9 110(2) . . ?
C7 N4 H10 108(2) . . ?
Ni1 N4 H10 109(2) . . ?
H9 N4 H10 112(3) . . ?
C9 N5 C8 117.2(2) . . ?
C9 N5 Ni1 107.09(15) . . ?
C8 N5 Ni1 106.96(16) . . ?
C9 N5 H8 108.9(18) . . ?
C8 N5 H8 107.9(18) . . ?
Ni1 N5 H8 108.5(18) . . ?
C10 N6 Ni1 107.41(16) . . ?
C10 N6 H6 107(2) . . ?
Ni1 N6 H6 113(2) . . ?
C10 N6 H7 109(2) . . ?
Ni1 N6 H7 113(2) . . ?
H6 N6 H7 107(3) . . ?
N5 Ni1 N2 177.87(9) . . ?
N5 Ni1 N1 96.67(9) . . ?
N2 Ni1 N1 82.77(9) . . ?
N5 Ni1 N6 82.44(9) . . ?
N2 Ni1 N6 99.63(9) . . ?
N1 Ni1 N6 92.12(9) . . ?
N5 Ni1 N3 99.42(8) . . ?
N2 Ni1 N3 81.21(9) . . ?
N1 Ni1 N3 163.83(9) . . ?
N6 Ni1 N3 88.40(8) . . ?
N5 Ni1 N4 81.79(8) . . ?
N2 Ni1 N4 96.18(9) . . ?
N1 Ni1 N4 92.99(9) . . ?
N6 Ni1 N4 163.88(9) . . ?
N3 Ni1 N4 90.91(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 -50.5(3) . . . . ?
N2 C3 C4 N3 48.1(3) . . . . ?
N4 C7 C8 N5 -53.9(3) . . . . ?
N5 C9 C10 N6 56.4(3) . . . . ?
C2 C1 N1 Ni1 30.7(3) . . . . ?
C4 C3 N2 C2 -171.2(3) . . . . ?
C4 C3 N2 Ni1 -48.1(3) . . . . ?
C1 C2 N2 C3 166.2(3) . . . . ?
C1 C2 N2 Ni1 43.4(3) . . . . ?
C3 C4 N3 Ni1 -22.9(3) . . . . ?
C8 C7 N4 Ni1 29.5(2) . . . . ?
C10 C9 N5 C8 -168.1(2) . . . . ?
C10 C9 N5 Ni1 -48.1(2) . . . . ?
C7 C8 N5 C9 170.5(2) . . . . ?
C7 C8 N5 Ni1 50.4(2) . . . . ?
C9 C10 N6 Ni1 -34.8(2) . . . . ?

_refine_diff_density_max         0.902
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.067

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1519307'
_audit_update_record             
;
2016-11-25 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H38 N4 Ni2 O9'
_chemical_formula_sum            'C16 H38 N4 Ni2 O9'
_chemical_formula_weight         547.92

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   26.9488(11)
_cell_length_b                   13.7861(5)
_cell_length_c                   27.4426(14)
_cell_angle_alpha                90
_cell_angle_beta                 108.680(5)
_cell_angle_gamma                90
_cell_volume                     9658.4(8)
_cell_formula_units_Z            16
_cell_measurement_temperature    100
_cell_measurement_reflns_used    7945
_cell_measurement_theta_min      2.9501
_cell_measurement_theta_max      28.0887


_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_F_000             4640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_exptl_absorpt_coefficient_mu    1.610
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.93654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_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  'oxford gemini s'
_diffrn_measurement_method       'ω scans'
_diffrn_standards_number         1
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  5
_diffrn_standards_decay_%        0
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23504
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.057
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             8424
_reflns_number_gt                6864
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0415P)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         8424
_refine_ls_number_parameters     585
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0906
_refine_ls_wR_factor_gt          0.0843
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      8.148
_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_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
C2 C 0.92052(11) -0.3668(2) 0.72293(11) 0.0204(7) Uani 1 1 d . . . . .
H2A H 0.9474 -0.4123 0.7314 0.024 Uiso 1 1 calc R U . . .
C1 C 0.90293(10) -0.1041(2) 0.67967(11) 0.0182(6) Uani 1 1 d . . . . .
H1A H 0.9203 -0.0493 0.6738 0.022 Uiso 1 1 calc R U . . .
C8 C 0.91594(11) -0.0657(2) 0.84640(11) 0.0235(7) Uani 1 1 d . . . . .
H8A H 0.9269 -0.0181 0.8259 0.028 Uiso 1 1 calc R U . . .
H8B H 0.9337 -0.0514 0.8824 0.028 Uiso 1 1 calc R U . . .
C3 C 0.79873(11) -0.3501(2) 0.78605(12) 0.0230(7) Uani 1 1 d . . . . .
H3A H 0.7890 -0.3884 0.8094 0.028 Uiso 1 1 calc DR U . . .
C9 C 0.93437(12) -0.2312(2) 0.87698(11) 0.0265(7) Uani 1 1 d . . . . .
H9A H 0.9008 -0.2357 0.8821 0.040 Uiso 1 1 calc R U . . .
H9B H 0.9598 -0.2075 0.9078 0.040 Uiso 1 1 calc R U . . .
H9C H 0.9447 -0.2942 0.8689 0.040 Uiso 1 1 calc R U . . .
C20 C 0.87730(13) 0.3526(2) 0.49099(12) 0.0300(8) Uani 1 1 d . . . . .
H20 H 0.8525 0.3874 0.4656 0.036 Uiso 1 1 calc R U . . .
C13 C 0.84361(11) -0.4161(2) 0.55550(11) 0.0213(7) Uani 1 1 d . . . . .
H13A H 0.8670 -0.4595 0.5802 0.026 Uiso 1 1 calc R U . . .
H13B H 0.8445 -0.4333 0.5215 0.026 Uiso 1 1 calc R U . . .
C17 C 0.98764(11) 0.1317(2) 0.67405(11) 0.0211(7) Uani 1 1 d . . . . .
H17 H 0.9933 0.0865 0.7004 0.025 Uiso 1 1 calc R U . . .
C23 C 1.11310(13) 0.4389(2) 0.68740(12) 0.0306(8) Uani 1 1 d . . . . .
H23A H 1.1479 0.4561 0.7096 0.037 Uiso 1 1 calc R U . . .
H23B H 1.0884 0.4841 0.6939 0.037 Uiso 1 1 calc R U . . .
C18 C 0.94048(11) 0.3912(2) 0.64740(11) 0.0203(7) Uani 1 1 d . . . . .
H18 H 0.9305 0.4462 0.6615 0.024 Uiso 1 1 calc R U . . .
C15 C 0.80562(12) -0.4869(2) 0.64463(11) 0.0242(7) Uani 1 1 d . . . . .
H15A H 0.8413 -0.5003 0.6473 0.036 Uiso 1 1 calc R U . . .
H15B H 0.7844 -0.5429 0.6314 0.036 Uiso 1 1 calc R U . . .
H15C H 0.8036 -0.4712 0.6780 0.036 Uiso 1 1 calc R U . . .
C5 C 0.77375(11) -0.1005(2) 0.77385(12) 0.0247(7) Uani 1 1 d . . . . .
H5A H 0.7714 -0.1559 0.7942 0.037 Uiso 1 1 calc R U . . .
H5B H 0.7552 -0.1135 0.7383 0.037 Uiso 1 1 calc R U . . .
H5C H 0.7586 -0.0452 0.7849 0.037 Uiso 1 1 calc R U . . .
C24 C 1.11097(12) 0.4469(2) 0.63227(12) 0.0326(8) Uani 1 1 d . . . . .
H24A H 1.1192 0.5128 0.6253 0.039 Uiso 1 1 calc R U . . .
H24B H 1.1370 0.4042 0.6262 0.039 Uiso 1 1 calc R U . . .
C10 C 0.98275(11) -0.1595(2) 0.82767(11) 0.0253(7) Uani 1 1 d . . . . .
H10A H 0.9815 -0.1164 0.7998 0.038 Uiso 1 1 calc R U . . .
H10B H 0.9928 -0.2231 0.8201 0.038 Uiso 1 1 calc R U . . .
H10C H 1.0079 -0.1360 0.8588 0.038 Uiso 1 1 calc R U . . .
C6 C 0.83061(11) 0.00514(19) 0.74835(12) 0.0250(7) Uani 1 1 d . . . . .
H6A H 0.8126 -0.0093 0.7129 0.038 Uiso 1 1 calc R U . . .
H6B H 0.8663 0.0218 0.7525 0.038 Uiso 1 1 calc R U . . .
H6C H 0.8138 0.0587 0.7590 0.038 Uiso 1 1 calc R U . . .
C22 C 1.08476(12) 0.3422(2) 0.74617(11) 0.0322(8) Uani 1 1 d . . . . .
H22A H 1.0761 0.2781 0.7543 0.048 Uiso 1 1 calc R U . . .
H22B H 1.0548 0.3838 0.7404 0.048 Uiso 1 1 calc R U . . .
H22C H 1.1132 0.3671 0.7743 0.048 Uiso 1 1 calc R U . . .
C19 C 1.07701(13) 0.1545(2) 0.57077(13) 0.0285(8) Uani 1 1 d . . . . .
H19 H 1.1050 0.1205 0.5662 0.034 Uiso 1 1 calc R U . . .
C11 C 0.83884(12) -0.2526(2) 0.52181(11) 0.0248(7) Uani 1 1 d . . . . .
H11A H 0.8506 -0.1871 0.5300 0.037 Uiso 1 1 calc R U . . .
H11B H 0.8013 -0.2548 0.5119 0.037 Uiso 1 1 calc R U . . .
H11C H 0.8500 -0.2755 0.4939 0.037 Uiso 1 1 calc R U . . .
C32 C 0.93022(13) 0.0068(2) 0.55593(12) 0.0306(8) Uani 1 1 d . . . . .
H32A H 0.9646 0.0288 0.5580 0.046 Uiso 1 1 calc R U . . .
H32B H 0.9214 -0.0495 0.5342 0.046 Uiso 1 1 calc R U . . .
H32C H 0.9296 -0.0095 0.5897 0.046 Uiso 1 1 calc R U . . .
C4 C 0.74799(11) -0.1306(2) 0.59752(12) 0.0245(7) Uani 1 1 d . . . . .
H4A H 0.7260 -0.0927 0.5714 0.029 Uiso 1 1 calc DR U . . .
C7 C 0.85756(11) -0.0589(2) 0.83538(11) 0.0261(7) Uani 1 1 d . . . . .
H7A H 0.8468 -0.1047 0.8569 0.031 Uiso 1 1 calc R U . . .
H7B H 0.8485 0.0058 0.8435 0.031 Uiso 1 1 calc R U . . .
C25 C 1.02202(12) 0.5032(2) 0.59017(12) 0.0254(7) Uani 1 1 d . . . . .
H25A H 0.9882 0.4845 0.5674 0.038 Uiso 1 1 calc R U . . .
H25B H 1.0350 0.5573 0.5757 0.038 Uiso 1 1 calc R U . . .
H25C H 1.0190 0.5214 0.6229 0.038 Uiso 1 1 calc R U . . .
C12 C 0.91914(11) -0.3107(2) 0.58002(11) 0.0259(7) Uani 1 1 d . . . . .
H12A H 0.9353 -0.3503 0.6096 0.039 Uiso 1 1 calc R U . . .
H12B H 0.9307 -0.2448 0.5873 0.039 Uiso 1 1 calc R U . . .
H12C H 0.9288 -0.3342 0.5514 0.039 Uiso 1 1 calc R U . . .
C26 C 1.06343(13) 0.3989(2) 0.54575(12) 0.0309(8) Uani 1 1 d . . . . .
H26A H 1.0869 0.3453 0.5486 0.046 Uiso 1 1 calc R U . . .
H26B H 1.0768 0.4548 0.5332 0.046 Uiso 1 1 calc R U . . .
H26C H 1.0296 0.3826 0.5223 0.046 Uiso 1 1 calc R U . . .
C14 C 0.78834(11) -0.4278(2) 0.55753(11) 0.0221(7) Uani 1 1 d . . . . .
H14A H 0.7649 -0.3851 0.5324 0.027 Uiso 1 1 calc R U . . .
H14B H 0.7767 -0.4940 0.5489 0.027 Uiso 1 1 calc R U . . .
C16 C 0.73118(11) -0.3863(2) 0.60659(12) 0.0263(7) Uani 1 1 d . . . . .
H16A H 0.7177 -0.3323 0.5842 0.039 Uiso 1 1 calc R U . . .
H16B H 0.7296 -0.3721 0.6403 0.039 Uiso 1 1 calc R U . . .
H16C H 0.7106 -0.4429 0.5933 0.039 Uiso 1 1 calc R U . . .
C21 C 1.14613(12) 0.2749(2) 0.70999(13) 0.0312(8) Uani 1 1 d . . . . .
H21A H 1.1570 0.2711 0.6800 0.047 Uiso 1 1 calc R U . . .
H21B H 1.1371 0.2113 0.7187 0.047 Uiso 1 1 calc R U . . .
H21C H 1.1742 0.3006 0.7382 0.047 Uiso 1 1 calc R U . . .
C31 C 0.89393(17) 0.1029(2) 0.48204(13) 0.0506(11) Uani 1 1 d . . . . .
H31A H 0.9285 0.1241 0.4841 0.076 Uiso 1 1 calc R U . . .
H31B H 0.8690 0.1523 0.4659 0.076 Uiso 1 1 calc R U . . .
H31C H 0.8857 0.0444 0.4621 0.076 Uiso 1 1 calc R U . . .
C29 C 0.8238(2) 0.0716(4) 0.5723(3) 0.029(2) Uani 0.579(11) 1 d D . P A 1
H29A H 0.8434 0.0304 0.6006 0.035 Uiso 0.579(11) 1 calc R U P A 1
H29B H 0.7872 0.0536 0.5635 0.035 Uiso 0.579(11) 1 calc R U P A 1
C29' C 0.8044(3) 0.1123(6) 0.5448(3) 0.022(3) Uani 0.421(11) 1 d D . P A 2
H29C H 0.7778 0.0725 0.5518 0.026 Uiso 0.421(11) 1 calc R U P A 2
H29D H 0.7871 0.1536 0.5157 0.026 Uiso 0.421(11) 1 calc R U P A 2
C30 C 0.83977(14) 0.0516(3) 0.53140(18) 0.0686(15) Uani 1 1 d D . . . .
H30A H 0.8148 0.0803 0.5011 0.082 Uiso 1 1 calc R U . A 1
H30B H 0.8383 -0.0181 0.5264 0.082 Uiso 1 1 calc R U . A 1
C27 C 0.78971(14) 0.2489(3) 0.57332(18) 0.0690(14) Uani 1 1 d D . . . .
H27A H 0.7854 0.2645 0.5381 0.104 Uiso 1 1 calc R U . . .
H27B H 0.8000 0.3060 0.5941 0.104 Uiso 1 1 calc R U . . .
H27C H 0.7572 0.2250 0.5759 0.104 Uiso 1 1 calc R U . . .
N8 N 0.89183(9) 0.08444(17) 0.53416(9) 0.0228(6) Uani 1 1 d D . . . .
N3 N 0.86145(9) -0.31492(16) 0.56733(9) 0.0194(5) Uani 1 1 d . . . . .
N4 N 0.78639(9) -0.40418(16) 0.60964(9) 0.0188(5) Uani 1 1 d . . . . .
N1 N 0.82934(9) -0.08059(16) 0.78016(9) 0.0188(5) Uani 1 1 d . . . . .
N2 N 0.93088(9) -0.16399(16) 0.83429(9) 0.0189(5) Uani 1 1 d . . . . .
N5 N 1.10031(9) 0.33880(17) 0.69955(9) 0.0213(6) Uani 1 1 d . . . . .
N7 N 0.82958(10) 0.17544(17) 0.59100(9) 0.0254(6) Uani 1 1 d D . . . .
N6 N 1.05874(9) 0.42074(16) 0.59712(9) 0.0204(5) Uani 1 1 d . . . . .
O15 O 1.03328(9) 0.13667(16) 0.53933(9) 0.0409(6) Uani 1 1 d . . . . .
O8 O 0.74706(8) -0.11240(15) 0.64135(8) 0.0301(5) Uani 1 1 d . . . . .
O18 O 0.97370(8) 0.25317(16) 0.56798(8) 0.0200(5) Uani 1 1 d D . . . .
O10 O 1.02730(8) 0.17584(14) 0.67260(8) 0.0245(5) Uani 1 1 d . . . . .
O9 O 0.81208(7) -0.23981(14) 0.69464(7) 0.0181(4) Uani 1 1 d D . . . .
O2 O 0.87914(7) -0.15165(13) 0.64040(7) 0.0212(5) Uani 1 1 d . . . . .
O4 O 0.89635(7) -0.35832(14) 0.67593(7) 0.0218(5) Uani 1 1 d . . . . .
O1 O 0.90687(7) -0.11908(13) 0.72552(7) 0.0188(4) Uani 1 1 d . . . . .
O17 O 0.85978(8) 0.29115(14) 0.51476(8) 0.0254(5) Uani 1 1 d . . . . .
O12 O 0.98867(7) 0.37835(13) 0.65918(7) 0.0206(4) Uani 1 1 d . . . . .
O13 O 0.90349(7) 0.34122(14) 0.61939(7) 0.0230(5) Uani 1 1 d . . . . .
O14 O 1.08828(8) 0.21230(14) 0.60770(8) 0.0254(5) Uani 1 1 d . . . . .
O7 O 0.77439(8) -0.19302(14) 0.58325(7) 0.0221(5) Uani 1 1 d . . . . .
O11 O 0.94118(8) 0.13896(14) 0.64532(7) 0.0243(5) Uani 1 1 d . . . . .
O6 O 0.77459(8) -0.36572(15) 0.74055(8) 0.0294(5) Uani 1 1 d . . . . .
O5 O 0.83440(8) -0.29058(13) 0.80565(8) 0.0229(5) Uani 1 1 d . . . . .
O16 O 0.92391(9) 0.37290(16) 0.49716(9) 0.0382(6) Uani 1 1 d . . . . .
O3 O 0.91380(7) -0.32311(14) 0.76018(7) 0.0219(5) Uani 1 1 d . . . . .
Ni1 Ni 0.87061(2) -0.20446(2) 0.76443(2) 0.01521(10) Uani 1 1 d . . . . .
Ni2 Ni 0.83595(2) -0.27551(2) 0.63151(2) 0.01616(10) Uani 1 1 d . . . . .
Ni3 Ni 1.03709(2) 0.29518(2) 0.63292(2) 0.01665(10) Uani 1 1 d . . . . .
Ni4 Ni 0.90325(2) 0.21536(2) 0.58060(2) 0.01786(10) Uani 1 1 d D . . . .
C28 C 0.83318(15) 0.1555(4) 0.64429(15) 0.0733(15) Uani 1 1 d D . . . .
H28A H 0.8590 0.1062 0.6580 0.110 Uiso 1 1 calc R U . . .
H28B H 0.7998 0.1337 0.6456 0.110 Uiso 1 1 calc R U . . .
H28C H 0.8431 0.2137 0.6643 0.110 Uiso 1 1 calc R U . . .
H1 H 0.7966(13) -0.2876(19) 0.7093(13) 0.057(12) Uiso 1 1 d D . . . .
H2 H 0.7871(12) -0.190(2) 0.6798(14) 0.066(13) Uiso 1 1 d D . . . .
H3 H 0.9932(17) 0.203(3) 0.5547(16) 0.071(14) Uiso 1 1 d . . . . .
H4 H 0.9630(13) 0.295(2) 0.5478(13) 0.031(11) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 O3 1.249(3) . ?
C2 O4 1.251(3) . ?
C2 H2A 0.9300 . ?
C1 O1 1.246(3) . ?
C1 O2 1.249(3) . ?
C1 H1A 0.9300 . ?
C8 N2 1.481(3) . ?
C8 C7 1.507(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C3 O6 1.228(3) . ?
C3 O5 1.248(3) . ?
C3 H3A 0.9300 . ?
C9 N2 1.473(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C20 O16 1.244(4) . ?
C20 O17 1.251(4) . ?
C20 H20 0.9300 . ?
C13 N3 1.478(3) . ?
C13 C14 1.517(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C17 O10 1.241(3) . ?
C17 O11 1.252(3) . ?
C17 H17 0.9300 . ?
C23 N5 1.486(4) . ?
C23 C24 1.499(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C18 O12 1.246(3) . ?
C18 O13 1.252(3) . ?
C18 H18 0.9300 . ?
C15 N4 1.473(3) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C5 N1 1.478(3) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C24 N6 1.474(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C10 N2 1.468(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C6 N1 1.476(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C22 N5 1.469(4) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C19 O15 1.242(4) . ?
C19 O14 1.248(4) . ?
C19 H19 0.9300 . ?
C11 N3 1.477(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C32 N8 1.476(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C4 O8 1.237(3) . ?
C4 O7 1.256(3) . ?
C4 H4A 0.9300 . ?
C7 N1 1.492(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C25 N6 1.479(3) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C12 N3 1.482(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C26 N6 1.486(4) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C14 N4 1.484(3) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 N4 1.484(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C21 N5 1.468(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C31 N8 1.472(4) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C29 C30 1.351(6) . ?
C29 N7 1.513(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29' C30 1.402(8) . ?
C29' N7 1.508(7) . ?
C29' H29C 0.9700 . ?
C29' H29D 0.9700 . ?
C30 N8 1.453(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C27 N7 1.442(4) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
N8 Ni4 2.174(2) . ?
N3 Ni2 2.155(2) . ?
N4 Ni2 2.186(2) . ?
N1 Ni1 2.156(2) . ?
N2 Ni1 2.152(2) . ?
N5 Ni3 2.148(2) . ?
N7 C28 1.460(4) . ?
N7 Ni4 2.165(2) . ?
N6 Ni3 2.161(2) . ?
O18 Ni4 2.102(2) . ?
O18 Ni3 2.116(2) . ?
O18 H3 1.00(4) . ?
O18 H4 0.79(3) . ?
O10 Ni3 2.0363(19) . ?
O9 Ni2 2.091(2) . ?
O9 Ni1 2.1115(19) . ?
O9 H1 0.937(18) . ?
O9 H2 0.959(18) . ?
O2 Ni2 2.0368(19) . ?
O4 Ni2 2.0414(19) . ?
O1 Ni1 2.0369(19) . ?
O17 Ni4 2.0910(19) . ?
O12 Ni3 2.0346(19) . ?
O13 Ni4 2.0345(19) . ?
O14 Ni3 2.073(2) . ?
O7 Ni2 2.0957(19) . ?
O11 Ni4 2.0361(19) . ?
O5 Ni1 2.0850(19) . ?
O3 Ni1 2.0325(19) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 C2 O4 129.4(3) . . ?
O3 C2 H2A 115.3 . . ?
O4 C2 H2A 115.3 . . ?
O1 C1 O2 129.7(3) . . ?
O1 C1 H1A 115.2 . . ?
O2 C1 H1A 115.2 . . ?
N2 C8 C7 110.7(2) . . ?
N2 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
O6 C3 O5 129.6(3) . . ?
O6 C3 H3A 115.2 . . ?
O5 C3 H3A 115.2 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O16 C20 O17 127.9(3) . . ?
O16 C20 H20 116.0 . . ?
O17 C20 H20 116.0 . . ?
N3 C13 C14 110.3(2) . . ?
N3 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
N3 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
O10 C17 O11 129.7(3) . . ?
O10 C17 H17 115.2 . . ?
O11 C17 H17 115.2 . . ?
N5 C23 C24 111.0(2) . . ?
N5 C23 H23A 109.4 . . ?
C24 C23 H23A 109.4 . . ?
N5 C23 H23B 109.4 . . ?
C24 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
O12 C18 O13 129.7(3) . . ?
O12 C18 H18 115.1 . . ?
O13 C18 H18 115.1 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N6 C24 C23 111.3(3) . . ?
N6 C24 H24A 109.4 . . ?
C23 C24 H24A 109.4 . . ?
N6 C24 H24B 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N5 C22 H22A 109.5 . . ?
N5 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N5 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O15 C19 O14 128.4(3) . . ?
O15 C19 H19 115.8 . . ?
O14 C19 H19 115.8 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N8 C32 H32A 109.5 . . ?
N8 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N8 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O8 C4 O7 129.2(3) . . ?
O8 C4 H4A 115.4 . . ?
O7 C4 H4A 115.4 . . ?
N1 C7 C8 110.6(2) . . ?
N1 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N6 C25 H25A 109.5 . . ?
N6 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N6 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N6 C26 H26A 109.5 . . ?
N6 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N6 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N4 C14 C13 110.5(2) . . ?
N4 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C21 H21A 109.5 . . ?
N5 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N5 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N8 C31 H31A 109.5 . . ?
N8 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N8 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C29 N7 116.8(5) . . ?
C30 C29 H29A 108.1 . . ?
N7 C29 H29A 108.1 . . ?
C30 C29 H29B 108.1 . . ?
N7 C29 H29B 108.1 . . ?
H29A C29 H29B 107.3 . . ?
C30 C29' N7 113.9(5) . . ?
C30 C29' H29C 108.8 . . ?
N7 C29' H29C 108.8 . . ?
C30 C29' H29D 108.8 . . ?
N7 C29' H29D 108.8 . . ?
H29C C29' H29D 107.7 . . ?
C29 C30 N8 116.8(4) . . ?
C29' C30 N8 121.7(4) . . ?
C29 C30 H30A 108.1 . . ?
N8 C30 H30A 108.1 . . ?
C29 C30 H30B 108.1 . . ?
N8 C30 H30B 108.1 . . ?
H30A C30 H30B 107.3 . . ?
N7 C27 H27A 109.5 . . ?
N7 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N7 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C30 N8 C31 109.9(3) . . ?
C30 N8 C32 109.6(3) . . ?
C31 N8 C32 106.2(2) . . ?
C30 N8 Ni4 104.03(19) . . ?
C31 N8 Ni4 112.56(18) . . ?
C32 N8 Ni4 114.57(18) . . ?
C11 N3 C13 110.2(2) . . ?
C11 N3 C12 107.1(2) . . ?
C13 N3 C12 109.4(2) . . ?
C11 N3 Ni2 113.04(17) . . ?
C13 N3 Ni2 104.55(16) . . ?
C12 N3 Ni2 112.54(17) . . ?
C15 N4 C14 110.2(2) . . ?
C15 N4 C16 107.6(2) . . ?
C14 N4 C16 109.1(2) . . ?
C15 N4 Ni2 113.10(17) . . ?
C14 N4 Ni2 103.63(16) . . ?
C16 N4 Ni2 113.20(17) . . ?
C6 N1 C5 107.1(2) . . ?
C6 N1 C7 109.9(2) . . ?
C5 N1 C7 108.9(2) . . ?
C6 N1 Ni1 113.87(17) . . ?
C5 N1 Ni1 113.44(17) . . ?
C7 N1 Ni1 103.54(16) . . ?
C10 N2 C9 107.7(2) . . ?
C10 N2 C8 109.1(2) . . ?
C9 N2 C8 110.5(2) . . ?
C10 N2 Ni1 112.20(17) . . ?
C9 N2 Ni1 112.55(17) . . ?
C8 N2 Ni1 104.79(16) . . ?
C21 N5 C22 107.8(2) . . ?
C21 N5 C23 111.1(2) . . ?
C22 N5 C23 108.5(2) . . ?
C21 N5 Ni3 112.74(18) . . ?
C22 N5 Ni3 112.37(17) . . ?
C23 N5 Ni3 104.29(17) . . ?
C27 N7 C28 105.8(3) . . ?
C27 N7 C29' 92.1(4) . . ?
C28 N7 C29' 127.0(4) . . ?
C27 N7 C29 124.5(4) . . ?
C28 N7 C29 97.4(4) . . ?
C27 N7 Ni4 113.1(2) . . ?
C28 N7 Ni4 114.2(2) . . ?
C29' N7 Ni4 102.7(3) . . ?
C29 N7 Ni4 101.2(2) . . ?
C24 N6 C25 110.8(2) . . ?
C24 N6 C26 108.5(2) . . ?
C25 N6 C26 106.9(2) . . ?
C24 N6 Ni3 103.81(17) . . ?
C25 N6 Ni3 114.04(17) . . ?
C26 N6 Ni3 112.76(17) . . ?
Ni4 O18 Ni3 117.21(10) . . ?
Ni4 O18 H3 120(2) . . ?
Ni3 O18 H3 97(2) . . ?
Ni4 O18 H4 99(3) . . ?
Ni3 O18 H4 114(2) . . ?
H3 O18 H4 111(3) . . ?
C17 O10 Ni3 132.34(19) . . ?
Ni2 O9 Ni1 117.86(9) . . ?
Ni2 O9 H1 119(2) . . ?
Ni1 O9 H1 94(2) . . ?
Ni2 O9 H2 100(2) . . ?
Ni1 O9 H2 116(2) . . ?
H1 O9 H2 110(3) . . ?
C1 O2 Ni2 131.24(19) . . ?
C2 O4 Ni2 136.11(19) . . ?
C1 O1 Ni1 136.50(18) . . ?
C20 O17 Ni4 126.1(2) . . ?
C18 O12 Ni3 136.17(19) . . ?
C18 O13 Ni4 131.22(19) . . ?
C19 O14 Ni3 127.4(2) . . ?
C4 O7 Ni2 125.96(19) . . ?
C17 O11 Ni4 135.41(19) . . ?
C3 O5 Ni1 124.81(19) . . ?
C2 O3 Ni1 132.16(18) . . ?
O3 Ni1 O1 93.17(8) . . ?
O3 Ni1 O5 87.07(8) . . ?
O1 Ni1 O5 178.85(8) . . ?
O3 Ni1 O9 92.14(8) . . ?
O1 Ni1 O9 90.13(8) . . ?
O5 Ni1 O9 90.99(8) . . ?
O3 Ni1 N2 88.68(8) . . ?
O1 Ni1 N2 88.01(8) . . ?
O5 Ni1 N2 90.87(8) . . ?
O9 Ni1 N2 178.00(8) . . ?
O3 Ni1 N1 172.18(8) . . ?
O1 Ni1 N1 90.69(8) . . ?
O5 Ni1 N1 88.94(8) . . ?
O9 Ni1 N1 94.65(8) . . ?
N2 Ni1 N1 84.65(8) . . ?
O2 Ni2 O4 94.67(8) . . ?
O2 Ni2 O9 91.09(8) . . ?
O4 Ni2 O9 92.01(8) . . ?
O2 Ni2 O7 85.82(8) . . ?
O4 Ni2 O7 177.66(8) . . ?
O9 Ni2 O7 90.27(8) . . ?
O2 Ni2 N3 89.41(8) . . ?
O4 Ni2 N3 86.84(8) . . ?
O9 Ni2 N3 178.78(8) . . ?
O7 Ni2 N3 90.88(8) . . ?
O2 Ni2 N4 171.43(8) . . ?
O4 Ni2 N4 90.59(8) . . ?
O9 Ni2 N4 95.48(8) . . ?
O7 Ni2 N4 88.65(8) . . ?
N3 Ni2 N4 84.13(9) . . ?
O12 Ni3 O10 93.33(8) . . ?
O12 Ni3 O14 178.34(8) . . ?
O10 Ni3 O14 86.98(8) . . ?
O12 Ni3 O18 90.93(8) . . ?
O10 Ni3 O18 91.22(8) . . ?
O14 Ni3 O18 90.70(8) . . ?
O12 Ni3 N5 87.96(8) . . ?
O10 Ni3 N5 88.52(8) . . ?
O14 Ni3 N5 90.41(9) . . ?
O18 Ni3 N5 178.85(9) . . ?
O12 Ni3 N6 90.40(8) . . ?
O10 Ni3 N6 172.10(8) . . ?
O14 Ni3 N6 89.10(8) . . ?
O18 Ni3 N6 95.69(9) . . ?
N5 Ni3 N6 84.64(9) . . ?
O13 Ni4 O11 93.91(8) . . ?
O13 Ni4 O17 86.15(8) . . ?
O11 Ni4 O17 176.34(8) . . ?
O13 Ni4 O18 91.32(8) . . ?
O11 Ni4 O18 92.55(9) . . ?
O17 Ni4 O18 91.11(9) . . ?
O13 Ni4 N7 89.84(9) . . ?
O11 Ni4 N7 88.78(9) . . ?
O17 Ni4 N7 87.55(9) . . ?
O18 Ni4 N7 178.17(9) . . ?
O13 Ni4 N8 172.30(8) . . ?
O11 Ni4 N8 91.10(8) . . ?
O17 Ni4 N8 88.48(8) . . ?
O18 Ni4 N8 94.31(9) . . ?
N7 Ni4 N8 84.41(9) . . ?
N7 C28 H28A 109.5 . . ?
N7 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N7 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N5 C23 C24 N6 58.7(3) . . . . ?
N2 C8 C7 N1 -59.2(3) . . . . ?
N3 C13 C14 N4 -60.6(3) . . . . ?
N7 C29 C30 C29' -57.9(6) . . . . ?
N7 C29 C30 N8 50.4(8) . . . . ?
N7 C29' C30 C29 56.1(6) . . . . ?
N7 C29' C30 N8 -39.2(9) . . . . ?
C29 C30 N8 C31 -151.7(5) . . . . ?
C29' C30 N8 C31 -105.5(6) . . . . ?
C29 C30 N8 C32 91.9(5) . . . . ?
C29' C30 N8 C32 138.2(6) . . . . ?
C29 C30 N8 Ni4 -31.0(5) . . . . ?
C29' C30 N8 Ni4 15.3(6) . . . . ?
C14 C13 N3 C11 -78.8(3) . . . . ?
C14 C13 N3 C12 163.7(2) . . . . ?
C14 C13 N3 Ni2 43.0(2) . . . . ?
C13 C14 N4 C15 -79.5(3) . . . . ?
C13 C14 N4 C16 162.6(2) . . . . ?
C13 C14 N4 Ni2 41.7(2) . . . . ?
C8 C7 N1 C6 -78.8(3) . . . . ?
C8 C7 N1 C5 164.2(2) . . . . ?
C8 C7 N1 Ni1 43.2(3) . . . . ?
C7 C8 N2 C10 160.2(2) . . . . ?
C7 C8 N2 C9 -81.6(3) . . . . ?
C7 C8 N2 Ni1 39.9(3) . . . . ?
C24 C23 N5 C21 81.4(3) . . . . ?
C24 C23 N5 C22 -160.2(2) . . . . ?
C24 C23 N5 Ni3 -40.3(3) . . . . ?
C30 C29' N7 C27 152.6(6) . . . . ?
C30 C29' N7 C28 -95.8(6) . . . . ?
C30 C29' N7 C29 -53.4(6) . . . . ?
C30 C29' N7 Ni4 38.3(7) . . . . ?
C30 C29 N7 C27 90.7(6) . . . . ?
C30 C29 N7 C28 -154.3(5) . . . . ?
C30 C29 N7 C29' 58.6(7) . . . . ?
C30 C29 N7 Ni4 -37.7(6) . . . . ?
C23 C24 N6 C25 81.1(3) . . . . ?
C23 C24 N6 C26 -161.9(3) . . . . ?
C23 C24 N6 Ni3 -41.7(3) . . . . ?
O11 C17 O10 Ni3 12.0(5) . . . . ?
O1 C1 O2 Ni2 -0.4(4) . . . . ?
O3 C2 O4 Ni2 0.6(5) . . . . ?
O2 C1 O1 Ni1 -13.8(5) . . . . ?
O16 C20 O17 Ni4 9.6(5) . . . . ?
O13 C18 O12 Ni3 15.1(5) . . . . ?
O12 C18 O13 Ni4 1.0(5) . . . . ?
O15 C19 O14 Ni3 3.7(5) . . . . ?
O8 C4 O7 Ni2 -10.3(5) . . . . ?
O10 C17 O11 Ni4 3.7(5) . . . . ?
O6 C3 O5 Ni1 -6.7(4) . . . . ?
O4 C2 O3 Ni1 -11.5(5) . . . . ?

_refine_diff_density_max         0.579
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.077

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1519309'
_audit_update_record             
;
2016-11-25 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C11 H25 N3 Ni O4), H2 O'

_chemical_formula_sum            'C22 H52 N6 Ni2 O9'
_chemical_formula_weight         662.11

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      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

_cell_length_a                   30.8174(7)
_cell_length_b                   8.5618(4)
_cell_length_c                   13.1881(6)
_cell_angle_alpha                90
_cell_angle_beta                 119.006(3)
_cell_angle_gamma                90
_cell_volume                     3043.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    110
_cell_measurement_reflns_used    6672
_cell_measurement_theta_min      3.0150
_cell_measurement_theta_max      28.0747


_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.291
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.82318
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10743
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.023
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.924
_reflns_number_total             4941
_reflns_number_gt                4739
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_max     0.848
_reflns_Friedel_fraction_full    0.848

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0270P)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_abs_structure_details 
;
 Flack x determined using 2061 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.007(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4941
_refine_ls_number_parameters     360
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0587
_refine_ls_wR_factor_gt          0.0575
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.001

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 0.40787(14) 0.2935(5) 0.5899(3) 0.0209(9) Uani 1 1 d . . . . .
H2A H 0.3962 0.2825 0.5107 0.025 Uiso 1 1 calc R U . . .
C2 C 0.38266(14) 0.6168(5) 0.7253(4) 0.0205(9) Uani 1 1 d . . . . .
H2N H 0.3870 0.6089 0.6605 0.025 Uiso 1 1 calc R U . . .
C3 C 0.36071(14) 0.1933(5) 0.8369(4) 0.0279(10) Uani 1 1 d . . . . .
H3A H 0.3494 0.1536 0.7600 0.042 Uiso 1 1 calc R U . . .
H3B H 0.3477 0.2965 0.8323 0.042 Uiso 1 1 calc R U . . .
H3C H 0.3494 0.1261 0.8775 0.042 Uiso 1 1 calc R U . . .
C4 C 0.43190(16) 0.2632(5) 1.0169(3) 0.0270(9) Uani 1 1 d . . . . .
H4A H 0.4188 0.3667 1.0101 0.040 Uiso 1 1 calc R U . . .
H4B H 0.4675 0.2671 1.0595 0.040 Uiso 1 1 calc R U . . .
H4C H 0.4199 0.1976 1.0569 0.040 Uiso 1 1 calc R U . . .
C5 C 0.43571(14) 0.0395(4) 0.9083(3) 0.0237(9) Uani 1 1 d . . . . .
H5A H 0.4168 -0.0144 0.8350 0.028 Uiso 1 1 calc R U . . .
H5B H 0.4328 -0.0189 0.9677 0.028 Uiso 1 1 calc R U . . .
C6 C 0.48948(14) 0.0490(5) 0.9380(3) 0.0220(9) Uani 1 1 d . . . . .
H6A H 0.5087 0.0980 1.0132 0.026 Uiso 1 1 calc R U . . .
H6B H 0.5025 -0.0554 0.9420 0.026 Uiso 1 1 calc R U . . .
C7 C 0.48734(15) 0.0360(5) 0.7525(4) 0.0265(10) Uani 1 1 d . . . . .
H7A H 0.4556 -0.0144 0.7211 0.040 Uiso 1 1 calc R U . . .
H7B H 0.5131 -0.0415 0.7816 0.040 Uiso 1 1 calc R U . . .
H7C H 0.4890 0.0957 0.6928 0.040 Uiso 1 1 calc R U . . .
C8 C 0.54284(13) 0.2189(5) 0.8956(3) 0.0226(9) Uani 1 1 d . . . . .
H8A H 0.5474 0.2569 0.8322 0.027 Uiso 1 1 calc R U . . .
H8B H 0.5688 0.1435 0.9390 0.027 Uiso 1 1 calc R U . . .
C9 C 0.54723(14) 0.3537(5) 0.9738(3) 0.0221(9) Uani 1 1 d . . . . .
H9A H 0.5463 0.3147 1.0418 0.026 Uiso 1 1 calc R U . . .
H9B H 0.5788 0.4062 0.9995 0.026 Uiso 1 1 calc R U . . .
C10 C 0.51760(15) 0.5674(5) 0.8362(4) 0.0236(10) Uani 1 1 d . . . . .
H10A H 0.5202 0.5044 0.7792 0.035 Uiso 1 1 calc R U . . .
H10B H 0.5484 0.6207 0.8826 0.035 Uiso 1 1 calc R U . . .
H10C H 0.4915 0.6426 0.7981 0.035 Uiso 1 1 calc R U . . .
C11 C 0.50178(14) 0.5693(5) 0.9960(3) 0.0246(9) Uani 1 1 d . . . . .
H11A H 0.4747 0.6407 0.9554 0.037 Uiso 1 1 calc R U . . .
H11B H 0.5320 0.6271 1.0389 0.037 Uiso 1 1 calc R U . . .
H11C H 0.4957 0.5074 1.0486 0.037 Uiso 1 1 calc R U . . .
C12 C 0.64265(15) 0.1223(5) 0.5436(4) 0.0265(9) Uani 1 1 d . . . . .
H12 H 0.6278 0.1056 0.4640 0.032 Uiso 1 1 calc R U . . .
C13 C 0.60860(16) -0.0766(6) 0.7205(4) 0.0317(12) Uani 1 1 d . . . . .
H13 H 0.6125 -0.1009 0.6567 0.038 Uiso 1 1 calc R U . . .
C14 C 0.62288(14) 0.4194(5) 0.7631(4) 0.0264(10) Uani 1 1 d . . . . .
H14A H 0.5971 0.3437 0.7440 0.040 Uiso 1 1 calc R U . . .
H14B H 0.6237 0.4498 0.6940 0.040 Uiso 1 1 calc R U . . .
H14C H 0.6165 0.5095 0.7972 0.040 Uiso 1 1 calc R U . . .
C15 C 0.66823(15) 0.3091(5) 0.9519(3) 0.0234(9) Uani 1 1 d . . . . .
H15A H 0.6419 0.2353 0.9320 0.035 Uiso 1 1 calc R U . . .
H15B H 0.6617 0.4015 0.9835 0.035 Uiso 1 1 calc R U . . .
H15C H 0.6990 0.2638 1.0084 0.035 Uiso 1 1 calc R U . . .
C16 C 0.71137(14) 0.4654(4) 0.8765(3) 0.0211(9) Uani 1 1 d . . . . .
H16A H 0.7402 0.4354 0.9488 0.025 Uiso 1 1 calc R U . . .
H16B H 0.7004 0.5670 0.8876 0.025 Uiso 1 1 calc R U . . .
C17 C 0.72578(14) 0.4763(4) 0.7816(3) 0.0206(9) Uani 1 1 d . . . . .
H17A H 0.6988 0.5226 0.7129 0.025 Uiso 1 1 calc R U . . .
H17B H 0.7546 0.5432 0.8072 0.025 Uiso 1 1 calc R U . . .
C18 C 0.73920(16) 0.3309(5) 0.6438(4) 0.0242(9) Uani 1 1 d . . . . .
H18A H 0.7076 0.3647 0.5825 0.036 Uiso 1 1 calc R U . . .
H18B H 0.7471 0.2303 0.6249 0.036 Uiso 1 1 calc R U . . .
H18C H 0.7643 0.4047 0.6529 0.036 Uiso 1 1 calc R U . . .
C19 C 0.78553(13) 0.0879(5) 0.8515(3) 0.0216(9) Uani 1 1 d . . . . .
H19A H 0.7794 0.0442 0.7778 0.026 Uiso 1 1 calc R U . . .
H19B H 0.8175 0.0504 0.9111 0.026 Uiso 1 1 calc R U . . .
C20 C 0.78637(13) 0.2642(5) 0.8459(3) 0.0189(8) Uani 1 1 d . . . . .
H20A H 0.7933 0.3083 0.9200 0.023 Uiso 1 1 calc R U . . .
H20B H 0.8123 0.2975 0.8289 0.023 Uiso 1 1 calc R U . . .
C21 C 0.73702(17) -0.1327(5) 0.8520(5) 0.0372(13) Uani 1 1 d . . . . .
H21A H 0.7120 -0.1671 0.8704 0.056 Uiso 1 1 calc R U . . .
H21B H 0.7671 -0.1900 0.8977 0.056 Uiso 1 1 calc R U . . .
H21C H 0.7259 -0.1503 0.7712 0.056 Uiso 1 1 calc R U . . .
C22 C 0.76261(14) 0.0592(5) 1.0022(3) 0.0290(10) Uani 1 1 d . . . . .
H22A H 0.7368 0.0258 1.0181 0.044 Uiso 1 1 calc R U . . .
H22B H 0.7695 0.1678 1.0213 0.044 Uiso 1 1 calc R U . . .
H22C H 0.7920 -0.0011 1.0479 0.044 Uiso 1 1 calc R U . . .
N1 N 0.41585(12) 0.1991(4) 0.9000(3) 0.0201(7) Uani 1 1 d . . . . .
N2 N 0.49406(12) 0.1415(4) 0.8483(3) 0.0197(7) Uani 1 1 d . . . . .
N3 N 0.50621(10) 0.4660(4) 0.9118(3) 0.0168(7) Uani 1 1 d . . . . .
N4 N 0.67144(11) 0.3502(4) 0.8469(3) 0.0181(7) Uani 1 1 d . . . . .
N5 N 0.73710(11) 0.3200(3) 0.7531(3) 0.0170(7) Uani 1 1 d . . . . .
N6 N 0.74641(11) 0.0362(4) 0.8777(3) 0.0220(7) Uani 1 1 d . . . . .
O1 O 0.44416(9) 0.3818(3) 0.6472(2) 0.0210(6) Uani 1 1 d . . . . .
O2 O 0.38684(9) 0.2197(3) 0.6358(2) 0.0238(6) Uani 1 1 d . . . . .
O1W O 0.32783(10) -0.0553(4) 0.5520(2) 0.0287(7) Uani 1 1 d D . . . .
O3 O 0.39713(9) 0.5038(3) 0.7943(2) 0.0221(6) Uani 1 1 d . . . . .
O4 O 0.36312(10) 0.7376(3) 0.7351(2) 0.0282(7) Uani 1 1 d . . . . .
O5 O 0.63520(10) 0.0329(3) 0.7825(2) 0.0241(6) Uani 1 1 d . . . . .
O6 O 0.57828(10) -0.1561(3) 0.7318(3) 0.0303(7) Uani 1 1 d . . . . .
O7 O 0.62792(10) 0.2340(4) 0.5810(2) 0.0265(6) Uani 1 1 d . . . . .
O8 O 0.67699(10) 0.0322(3) 0.6107(2) 0.0258(6) Uani 1 1 d . . . . .
Ni1 Ni 0.44165(2) 0.32708(5) 0.80198(3) 0.01547(13) Uani 1 1 d . . . . .
Ni2 Ni 0.68310(2) 0.16384(5) 0.75498(3) 0.01635(14) Uani 1 1 d . . . . .
H1 H 0.353(2) 0.027(6) 0.581(6) 0.13(3) Uiso 1 1 d D . . . .
H2 H 0.341(2) -0.126(6) 0.619(4) 0.076(19) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.251(5) . ?
C1 O1 1.255(5) . ?
C1 H2A 0.9300 . ?
C2 O4 1.235(5) . ?
C2 O3 1.253(5) . ?
C2 H2N 0.9300 . ?
C3 N1 1.487(5) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N1 1.478(5) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N1 1.480(5) . ?
C5 C6 1.509(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N2 1.486(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N2 1.483(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 N2 1.476(5) . ?
C8 C9 1.510(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N3 1.479(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N3 1.486(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N3 1.478(5) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 O7 1.257(5) . ?
C12 O8 1.261(5) . ?
C12 H12 0.9300 . ?
C13 O6 1.221(5) . ?
C13 O5 1.253(5) . ?
C13 H13 0.9300 . ?
C14 N4 1.486(5) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 N4 1.478(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 N4 1.474(5) . ?
C16 C17 1.520(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N5 1.477(5) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 N5 1.477(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N6 1.475(5) . ?
C19 C20 1.512(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N5 1.493(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N6 1.481(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 N6 1.479(5) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
N1 Ni1 2.121(3) . ?
N2 Ni1 2.133(3) . ?
N3 Ni1 2.162(3) . ?
N4 Ni2 2.137(3) . ?
N5 Ni2 2.144(3) . ?
N6 Ni2 2.135(3) . ?
O1 Ni1 2.131(3) . ?
O2 Ni1 2.216(3) . ?
O1W H1 0.98(3) . ?
O1W H2 0.98(3) . ?
O3 Ni1 2.012(3) . ?
O5 Ni2 2.022(3) . ?
O7 Ni2 2.176(3) . ?
O8 Ni2 2.140(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
O2 C1 O1 122.2(4) . . ?
O2 C1 H2A 118.9 . . ?
O1 C1 H2A 118.9 . . ?
O4 C2 O3 126.2(4) . . ?
O4 C2 H2N 116.9 . . ?
O3 C2 H2N 116.9 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 109.4(3) . . ?
N1 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
N1 C5 H5B 109.8 . . ?
C6 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
N2 C6 C5 109.7(3) . . ?
N2 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 111.6(3) . . ?
N2 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
N2 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
N3 C9 C8 110.4(3) . . ?
N3 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N3 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O7 C12 O8 122.0(4) . . ?
O7 C12 H12 119.0 . . ?
O8 C12 H12 119.0 . . ?
O6 C13 O5 129.4(4) . . ?
O6 C13 H13 115.3 . . ?
O5 C13 H13 115.3 . . ?
N4 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N4 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 C17 111.3(3) . . ?
N4 C16 H16A 109.4 . . ?
C17 C16 H16A 109.4 . . ?
N4 C16 H16B 109.4 . . ?
C17 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
N5 C17 C16 110.7(3) . . ?
N5 C17 H17A 109.5 . . ?
C16 C17 H17A 109.5 . . ?
N5 C17 H17B 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
N5 C18 H18A 109.5 . . ?
N5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N6 C19 C20 110.3(3) . . ?
N6 C19 H19A 109.6 . . ?
C20 C19 H19A 109.6 . . ?
N6 C19 H19B 109.6 . . ?
C20 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
N5 C20 C19 109.0(3) . . ?
N5 C20 H20A 109.9 . . ?
C19 C20 H20A 109.9 . . ?
N5 C20 H20B 109.9 . . ?
C19 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
N6 C21 H21A 109.5 . . ?
N6 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N6 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N6 C22 H22A 109.5 . . ?
N6 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N6 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C4 N1 C5 110.4(3) . . ?
C4 N1 C3 108.1(3) . . ?
C5 N1 C3 109.3(3) . . ?
C4 N1 Ni1 114.1(2) . . ?
C5 N1 Ni1 105.0(2) . . ?
C3 N1 Ni1 109.9(2) . . ?
C8 N2 C7 109.0(3) . . ?
C8 N2 C6 111.9(3) . . ?
C7 N2 C6 109.0(3) . . ?
C8 N2 Ni1 105.1(2) . . ?
C7 N2 Ni1 115.8(2) . . ?
C6 N2 Ni1 105.9(2) . . ?
C11 N3 C9 109.8(3) . . ?
C11 N3 C10 107.0(3) . . ?
C9 N3 C10 109.5(3) . . ?
C11 N3 Ni1 116.2(2) . . ?
C9 N3 Ni1 106.0(2) . . ?
C10 N3 Ni1 108.2(2) . . ?
C16 N4 C15 109.7(3) . . ?
C16 N4 C14 109.9(3) . . ?
C15 N4 C14 106.9(3) . . ?
C16 N4 Ni2 107.5(2) . . ?
C15 N4 Ni2 117.4(2) . . ?
C14 N4 Ni2 105.2(2) . . ?
C17 N5 C18 108.6(3) . . ?
C17 N5 C20 110.7(3) . . ?
C18 N5 C20 108.2(3) . . ?
C17 N5 Ni2 106.4(2) . . ?
C18 N5 Ni2 116.9(2) . . ?
C20 N5 Ni2 106.1(2) . . ?
C19 N6 C22 110.3(3) . . ?
C19 N6 C21 109.3(3) . . ?
C22 N6 C21 107.9(3) . . ?
C19 N6 Ni2 102.6(2) . . ?
C22 N6 Ni2 117.8(2) . . ?
C21 N6 Ni2 108.7(3) . . ?
C1 O1 Ni1 90.5(2) . . ?
C1 O2 Ni1 86.8(2) . . ?
H1 O1W H2 101(4) . . ?
C2 O3 Ni1 127.7(3) . . ?
C13 O5 Ni2 127.0(3) . . ?
C12 O7 Ni2 87.6(2) . . ?
C12 O8 Ni2 89.1(2) . . ?
O3 Ni1 N1 88.34(11) . . ?
O3 Ni1 O1 97.31(10) . . ?
N1 Ni1 O1 153.53(11) . . ?
O3 Ni1 N2 167.92(11) . . ?
N1 Ni1 N2 84.04(12) . . ?
O1 Ni1 N2 93.66(11) . . ?
O3 Ni1 N3 90.22(11) . . ?
N1 Ni1 N3 111.79(12) . . ?
O1 Ni1 N3 94.10(11) . . ?
N2 Ni1 N3 83.96(11) . . ?
O3 Ni1 O2 95.07(11) . . ?
N1 Ni1 O2 93.28(11) . . ?
O1 Ni1 O2 60.55(10) . . ?
N2 Ni1 O2 94.71(11) . . ?
N3 Ni1 O2 154.54(11) . . ?
O5 Ni2 N6 93.33(11) . . ?
O5 Ni2 N4 88.49(11) . . ?
N6 Ni2 N4 107.17(12) . . ?
O5 Ni2 O8 96.37(10) . . ?
N6 Ni2 O8 93.37(11) . . ?
N4 Ni2 O8 158.61(11) . . ?
O5 Ni2 N5 170.46(11) . . ?
N6 Ni2 N5 84.21(11) . . ?
N4 Ni2 N5 83.45(12) . . ?
O8 Ni2 N5 92.99(11) . . ?
O5 Ni2 O7 94.42(11) . . ?
N6 Ni2 O7 154.23(12) . . ?
N4 Ni2 O7 97.58(11) . . ?
O8 Ni2 O7 61.35(11) . . ?
N5 Ni2 O7 91.71(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C5 C6 N2 -58.2(4) . . . . ?
N2 C8 C9 N3 -55.6(4) . . . . ?
N4 C16 C17 N5 -52.4(4) . . . . ?
N6 C19 C20 N5 -59.8(4) . . . . ?
C6 C5 N1 C4 -78.4(4) . . . . ?
C6 C5 N1 C3 162.9(3) . . . . ?
C6 C5 N1 Ni1 45.0(3) . . . . ?
C9 C8 N2 C7 167.0(3) . . . . ?
C9 C8 N2 C6 -72.3(4) . . . . ?
C9 C8 N2 Ni1 42.2(3) . . . . ?
C5 C6 N2 C8 152.3(3) . . . . ?
C5 C6 N2 C7 -87.0(4) . . . . ?
C5 C6 N2 Ni1 38.3(3) . . . . ?
C8 C9 N3 C11 163.0(3) . . . . ?
C8 C9 N3 C10 -79.8(4) . . . . ?
C8 C9 N3 Ni1 36.7(3) . . . . ?
C17 C16 N4 C15 163.8(3) . . . . ?
C17 C16 N4 C14 -78.8(4) . . . . ?
C17 C16 N4 Ni2 35.1(3) . . . . ?
C16 C17 N5 C18 166.8(3) . . . . ?
C16 C17 N5 C20 -74.6(4) . . . . ?
C16 C17 N5 Ni2 40.2(3) . . . . ?
C19 C20 N5 C17 149.9(3) . . . . ?
C19 C20 N5 C18 -91.2(3) . . . . ?
C19 C20 N5 Ni2 34.9(3) . . . . ?
C20 C19 N6 C22 -76.6(4) . . . . ?
C20 C19 N6 C21 164.9(3) . . . . ?
C20 C19 N6 Ni2 49.6(3) . . . . ?
O2 C1 O1 Ni1 0.5(4) . . . . ?
O1 C1 O2 Ni1 -0.5(4) . . . . ?
O4 C2 O3 Ni1 -165.8(3) . . . . ?
O6 C13 O5 Ni2 -177.9(4) . . . . ?
O8 C12 O7 Ni2 0.2(4) . . . . ?
O7 C12 O8 Ni2 -0.2(4) . . . . ?

_refine_diff_density_max         0.273
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.043

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1519505'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H38 N4 Ni2 O9'
_chemical_formula_sum            'C16 H38 N4 Ni2 O9'
_chemical_formula_weight         547.92

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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   27.1365(6)
_cell_length_b                   13.9455(2)
_cell_length_c                   27.7677(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.481(2)
_cell_angle_gamma                90
_cell_volume                     9966.3(4)
_cell_oxdiff_measurement_reflns_used 18153
_cell_oxdiff_twin_number         2
loop_
_cell_oxdiff_twin_id
_cell_oxdiff_twin_matrix_11
_cell_oxdiff_twin_matrix_12
_cell_oxdiff_twin_matrix_13
_cell_oxdiff_twin_matrix_21
_cell_oxdiff_twin_matrix_22
_cell_oxdiff_twin_matrix_23
_cell_oxdiff_twin_matrix_31
_cell_oxdiff_twin_matrix_32
_cell_oxdiff_twin_matrix_33
1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000
2 -0.0324 0.0001 0.9669 0.0002 -0.9999 0.0004 1.0335 0.0007 0.0330

_cell_formula_units_Z            16
_cell_measurement_temperature    293
_cell_measurement_reflns_used    18153
_cell_measurement_theta_min      3.7530
_cell_measurement_theta_max      67.0990

_exptl_crystal_description       block
_exptl_crystal_colour            green

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_F_000             4640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_exptl_absorpt_coefficient_mu    2.314
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.63744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'oxford gemini s'
_diffrn_measurement_method       'ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            77514
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.605
_diffrn_reflns_theta_max         66.999
_diffrn_reflns_theta_full        67.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_oxdiff_twin_integration_method simultaneous
loop_
_diffrn_oxdiff_twin_id
_diffrn_oxdiff_twin_ratio
_diffrn_oxdiff_twin_reflns_isolated
_diffrn_oxdiff_twin_reflns_overlapped
1 0.6734 32401 12785
2 0.3266 32328 12785


_reflns_number_total             16923
_reflns_number_gt                13084
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'

_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0785P)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         16923
_refine_ls_number_parameters     580
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1081
_refine_ls_wR_factor_gt          0.1049
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_restrained_S_all      0.966
_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 -0.08050(10) -0.36475(18) 0.22237(11) 0.0481(7) Uani 1 1 d . . . . .
H1A H -0.0537 -0.4095 0.2307 0.058 Uiso 1 1 calc R U . . .
C2 C -0.09700(9) -0.10737(17) 0.18064(10) 0.0407(6) Uani 1 1 d . U . . .
H2A H -0.0785 -0.0546 0.1750 0.049 Uiso 1 1 calc R U . . .
C3 C -0.25129(11) -0.1325(2) 0.09866(12) 0.0584(8) Uani 1 1 d . U . . .
H3A H -0.2725 -0.0944 0.0729 0.070 Uiso 1 1 calc R U . . .
C4 C -0.20101(12) -0.3520(2) 0.28586(13) 0.0591(8) Uani 1 1 d . . . . .
H4A H -0.2095 -0.3916 0.3090 0.071 Uiso 1 1 calc R U . . .
C5 C -0.26841(11) -0.3848(2) 0.10664(13) 0.0649(8) Uani 1 1 d . . . . .
H5A H -0.2704 -0.3705 0.1398 0.097 Uiso 1 1 calc R U . . .
H5B H -0.2889 -0.4407 0.0935 0.097 Uiso 1 1 calc R U . . .
H5C H -0.2815 -0.3315 0.0844 0.097 Uiso 1 1 calc R U . . .
C6 C -0.19496(12) -0.48510(19) 0.14438(12) 0.0629(8) Uani 1 1 d . . . . .
H6A H -0.1966 -0.4696 0.1775 0.094 Uiso 1 1 calc R U . . .
H6B H -0.1597 -0.4992 0.1466 0.094 Uiso 1 1 calc R U . . .
H6C H -0.2164 -0.5400 0.1313 0.094 Uiso 1 1 calc R U . . .
C7 C -0.21132(11) -0.4253(2) 0.05893(11) 0.0593(8) Uani 1 1 d . . . . .
H7A H -0.2346 -0.3830 0.0344 0.071 Uiso 1 1 calc R U . . .
H7B H -0.2228 -0.4908 0.0501 0.071 Uiso 1 1 calc R U . . .
C8 C -0.15720(12) -0.4137(2) 0.05650(11) 0.0561(7) Uani 1 1 d . . . . .
H8A H -0.1340 -0.4572 0.0804 0.067 Uiso 1 1 calc R U . . .
H8B H -0.1566 -0.4300 0.0227 0.067 Uiso 1 1 calc R U . . .
C9 C -0.16049(13) -0.2519(2) 0.02405(11) 0.0606(8) Uani 1 1 d . . . . .
H9A H -0.1483 -0.1875 0.0325 0.091 Uiso 1 1 calc R U . . .
H9B H -0.1977 -0.2529 0.0142 0.091 Uiso 1 1 calc R U . . .
H9C H -0.1495 -0.2746 -0.0035 0.091 Uiso 1 1 calc R U . . .
C10 C -0.08151(11) -0.3114(3) 0.08110(13) 0.0721(10) Uani 1 1 d . . . . .
H10A H -0.0696 -0.2467 0.0889 0.108 Uiso 1 1 calc R U . . .
H10B H -0.0720 -0.3338 0.0525 0.108 Uiso 1 1 calc R U . . .
H10C H -0.0658 -0.3517 0.1099 0.108 Uiso 1 1 calc R U . . .
C11 C -0.01882(10) -0.1585(3) 0.32602(12) 0.0658(9) Uani 1 1 d . . . . .
H11A H -0.0207 -0.1140 0.2991 0.099 Uiso 1 1 calc R U . . .
H11B H -0.0083 -0.2202 0.3174 0.099 Uiso 1 1 calc R U . . .
H11C H 0.0061 -0.1361 0.3569 0.099 Uiso 1 1 calc R U . . .
C12 C -0.06596(14) -0.2351(3) 0.37468(12) 0.0742(10) Uani 1 1 d . . . . .
H12A H -0.0561 -0.2968 0.3654 0.111 Uiso 1 1 calc R U . . .
H12B H -0.0988 -0.2402 0.3808 0.111 Uiso 1 1 calc R U . . .
H12C H -0.0400 -0.2130 0.4049 0.111 Uiso 1 1 calc R U . . .
C13 C -0.08565(12) -0.0705(2) 0.34562(13) 0.0687(9) Uani 1 1 d . . . . .
H13A H -0.0743 -0.0227 0.3261 0.082 Uiso 1 1 calc R U . . .
H13B H -0.0684 -0.0575 0.3813 0.082 Uiso 1 1 calc R U . . .
C14 C -0.14265(12) -0.0624(2) 0.33466(12) 0.0707(10) Uani 1 1 d . . . . .
H14A H -0.1511 0.0017 0.3430 0.085 Uiso 1 1 calc R U . . .
H14B H -0.1538 -0.1074 0.3557 0.085 Uiso 1 1 calc R U . . .
C15 C -0.17009(12) 0.00172(19) 0.24877(13) 0.0664(9) Uani 1 1 d . . . . .
H15A H -0.1884 -0.0126 0.2138 0.100 Uiso 1 1 calc R U . . .
H15B H -0.1348 0.0183 0.2523 0.100 Uiso 1 1 calc R U . . .
H15C H -0.1866 0.0546 0.2596 0.100 Uiso 1 1 calc R U . . .
C16 C -0.22581(11) -0.1024(2) 0.27475(13) 0.0651(8) Uani 1 1 d . . . . .
H16A H -0.2279 -0.1572 0.2949 0.098 Uiso 1 1 calc R U . . .
H16B H -0.2446 -0.1150 0.2398 0.098 Uiso 1 1 calc R U . . .
H16C H -0.2406 -0.0477 0.2861 0.098 Uiso 1 1 calc R U . . .
C17 C -0.01391(12) 0.13469(18) 0.17277(10) 0.0511(7) Uani 1 1 d . . . . .
H19 H -0.0086 0.0917 0.1996 0.061 Uiso 1 1 calc R U . . .
C18 C -0.05927(11) 0.38878(18) 0.14755(10) 0.0464(6) Uani 1 1 d . . . . .
H18 H -0.0691 0.4418 0.1627 0.056 Uiso 1 1 calc R U . . .
C19 C 0.07439(17) 0.1548(2) 0.06986(17) 0.0781(10) Uani 1 1 d . . . . .
H20 H 0.1018 0.1192 0.0659 0.094 Uiso 1 1 calc R U . . .
C20 C -0.12301(17) 0.3520(2) -0.00701(13) 0.0797(12) Uani 1 1 d . . . . .
H17 H -0.1480 0.3858 -0.0320 0.096 Uiso 1 1 calc R U . . .
C21 C 0.14330(14) 0.2688(3) 0.20865(16) 0.0888(12) Uani 1 1 d . . . . .
H27A H 0.1545 0.2621 0.1793 0.133 Uiso 1 1 calc R U . . .
H27B H 0.1324 0.2076 0.2174 0.133 Uiso 1 1 calc R U . . .
H27C H 0.1715 0.2927 0.2366 0.133 Uiso 1 1 calc R U . . .
C22 C 0.08406(14) 0.3457(3) 0.24284(12) 0.0848(12) Uani 1 1 d . . . . .
H28A H 0.0741 0.2840 0.2520 0.127 Uiso 1 1 calc R U . . .
H28B H 0.0552 0.3890 0.2363 0.127 Uiso 1 1 calc R U . . .
H28C H 0.1127 0.3701 0.2702 0.127 Uiso 1 1 calc R U . . .
C23 C 0.11421(17) 0.4327(3) 0.18500(14) 0.0965(14) Uani 1 1 d . . . . .
H29A H 0.0925 0.4797 0.1944 0.116 Uiso 1 1 calc R U . . .
H29B H 0.1499 0.4451 0.2054 0.116 Uiso 1 1 calc R U . . .
C24 C 0.10949(14) 0.4459(3) 0.13214(15) 0.0956(14) Uani 1 1 d . . . . .
H30A H 0.1360 0.4078 0.1245 0.115 Uiso 1 1 calc R U . . .
H30B H 0.1162 0.5127 0.1267 0.115 Uiso 1 1 calc R U . . .
C25 C 0.02219(13) 0.5003(2) 0.08836(14) 0.0723(9) Uani 1 1 d . . . . .
H32A H -0.0107 0.4815 0.0649 0.108 Uiso 1 1 calc R U . . .
H32B H 0.0358 0.5536 0.0747 0.108 Uiso 1 1 calc R U . . .
H32C H 0.0177 0.5185 0.1200 0.108 Uiso 1 1 calc R U . . .
C26 C 0.06530(17) 0.3977(3) 0.04691(14) 0.0864(12) Uani 1 1 d . . . . .
H31A H 0.0890 0.3451 0.0506 0.130 Uiso 1 1 calc R U . . .
H31B H 0.0789 0.4531 0.0349 0.130 Uiso 1 1 calc R U . . .
H31C H 0.0323 0.3808 0.0230 0.130 Uiso 1 1 calc R U . . .
C27 C -0.21020(15) 0.2482(3) 0.0748(2) 0.1123(18) Uani 1 1 d D . . . .
H27D H -0.2423 0.2237 0.0775 0.168 Uiso 1 1 calc R U . . .
H27E H -0.2145 0.2638 0.0400 0.168 Uiso 1 1 calc R U . . .
H27F H -0.2005 0.3048 0.0953 0.168 Uiso 1 1 calc R U . . .
C28 C -0.16570(17) 0.1564(4) 0.14461(17) 0.124(2) Uani 1 1 d D . . . .
H22A H -0.1568 0.2142 0.1642 0.185 Uiso 1 1 calc R U . . .
H22B H -0.1391 0.1092 0.1580 0.185 Uiso 1 1 calc R U . . .
H22C H -0.1983 0.1325 0.1463 0.185 Uiso 1 1 calc R U . . .
C29 C -0.1755(3) 0.0735(5) 0.0746(4) 0.075(3) Uani 0.561(14) 1 d D . P A 1
H29C H -0.1517 0.0335 0.1002 0.090 Uiso 0.561(14) 1 calc R U P A 1
H29D H -0.2106 0.0514 0.0700 0.090 Uiso 0.561(14) 1 calc R U P A 1
C30 C -0.1638(4) 0.0649(9) 0.0256(4) 0.083(4) Uani 0.561(14) 1 d D . P A 1
H30C H -0.1716 0.0004 0.0122 0.100 Uiso 0.561(14) 1 calc R U P A 1
H30D H -0.1851 0.1095 0.0009 0.100 Uiso 0.561(14) 1 calc R U P A 1
C29' C -0.1955(3) 0.1117(7) 0.0477(4) 0.065(3) Uani 0.439(14) 1 d D . P A 2
H29E H -0.2253 0.0796 0.0526 0.078 Uiso 0.439(14) 1 calc R U P A 2
H29F H -0.2073 0.1489 0.0166 0.078 Uiso 0.439(14) 1 calc R U P A 2
C30' C -0.1560(5) 0.0401(9) 0.0445(6) 0.067(4) Uani 0.439(14) 1 d D . P A 2
H30E H -0.1719 -0.0048 0.0173 0.081 Uiso 0.439(14) 1 calc R U P A 2
H30F H -0.1444 0.0042 0.0760 0.081 Uiso 0.439(14) 1 calc R U P A 2
C31 C -0.1085(2) 0.1040(3) -0.01726(13) 0.1063(16) Uani 1 1 d D . . . .
H26A H -0.0746 0.1257 -0.0162 0.159 Uiso 1 1 calc R U . . .
H26B H -0.1338 0.1522 -0.0328 0.159 Uiso 1 1 calc R U . . .
H26C H -0.1167 0.0458 -0.0367 0.159 Uiso 1 1 calc R U . . .
C32 C -0.07061(14) 0.0094(2) 0.05562(13) 0.0749(10) Uani 1 1 d D . . . .
H25A H -0.0368 0.0309 0.0562 0.112 Uiso 1 1 calc R U . . .
H25B H -0.0800 -0.0468 0.0347 0.112 Uiso 1 1 calc R U . . .
H25C H -0.0700 -0.0058 0.0895 0.112 Uiso 1 1 calc R U . . .
N1 N -0.21359(8) -0.40306(15) 0.11015(8) 0.0469(5) Uani 1 1 d . . . . .
N2 N -0.13892(8) -0.31438(16) 0.06860(8) 0.0457(5) Uani 1 1 d . . . . .
N3 N -0.07054(8) -0.16647(15) 0.33315(8) 0.0459(5) Uani 1 1 d . . . . .
N4 N -0.17082(8) -0.08263(15) 0.28020(8) 0.0469(5) Uani 1 1 d . . . . .
N5 N 0.09952(9) 0.33649(17) 0.19729(9) 0.0538(6) Uani 1 1 d . . . . .
N6 N 0.05863(9) 0.41939(15) 0.09672(9) 0.0495(6) Uani 1 1 d . . . . .
N7 N -0.17008(9) 0.17656(18) 0.09228(10) 0.0603(7) Uani 1 1 d D . . . .
N8 N -0.10908(10) 0.08588(16) 0.03481(9) 0.0570(6) Uani 1 1 d D . . . .
O1 O -0.10447(7) -0.35761(14) 0.17630(7) 0.0525(5) Uani 1 1 d . . . . .
O2 O -0.08664(7) -0.32200(13) 0.25870(7) 0.0536(5) Uani 1 1 d . . . . .
O3 O -0.12077(7) -0.15358(13) 0.14192(7) 0.0516(5) Uani 1 1 d . U . . .
O4 O -0.09421(6) -0.12089(12) 0.22534(7) 0.0453(4) Uani 1 1 d . U . . .
O5 O -0.22503(7) -0.19342(14) 0.08508(7) 0.0530(5) Uani 1 1 d . U . . .
O6 O -0.25317(9) -0.11572(17) 0.14159(9) 0.0772(7) Uani 1 1 d . U . . .
O7 O -0.16622(8) -0.29117(13) 0.30416(7) 0.0557(5) Uani 1 1 d . . . . .
O8 O -0.22548(9) -0.36565(17) 0.24057(9) 0.0748(7) Uani 1 1 d . . . . .
O9 O -0.18835(6) -0.24082(11) 0.19495(6) 0.0382(4) Uani 1 1 d . . . . .
H1 H -0.2079 -0.2948 0.2015 0.046 Uiso 1 1 calc R U . . .
H2 H -0.2121 -0.1870 0.1854 0.046 Uiso 1 1 calc R U . . .
O10 O 0.02511(8) 0.17817(14) 0.17152(8) 0.0620(6) Uani 1 1 d . . . . .
O11 O -0.05924(7) 0.13932(14) 0.14384(7) 0.0549(5) Uani 1 1 d . . . . .
O12 O -0.01196(7) 0.37831(13) 0.15723(7) 0.0505(5) Uani 1 1 d . . . . .
O13 O -0.09583(7) 0.33943(14) 0.12073(8) 0.0586(5) Uani 1 1 d . . . . .
O14 O 0.08576(8) 0.21140(14) 0.10622(9) 0.0655(6) Uani 1 1 d . . . . .
O15 O 0.03177(12) 0.1396(2) 0.03849(12) 0.1014(10) Uani 1 1 d . . . . .
O16 O -0.07808(11) 0.3735(2) -0.00190(10) 0.0991(10) Uani 1 1 d . . . . .
O17 O -0.14009(8) 0.29152(14) 0.01643(8) 0.0662(6) Uani 1 1 d . . . . .
O18 O -0.02717(7) 0.25515(11) 0.06742(6) 0.0449(4) Uani 1 1 d . . . . .
H3 H -0.0347 0.3083 0.0437 0.054 Uiso 1 1 calc R U . . .
H4 H -0.0162 0.2016 0.0510 0.054 Uiso 1 1 calc R U . . .
Ni1 Ni -0.16421(2) -0.27567(3) 0.13237(2) 0.03809(12) Uani 1 1 d . . . . .
Ni2 Ni -0.13003(2) -0.20548(3) 0.26389(2) 0.03584(12) Uani 1 1 d . . . . .
Ni3 Ni 0.03602(2) 0.29521(3) 0.13165(2) 0.03996(12) Uani 1 1 d . . . . .
Ni4 Ni -0.09705(2) 0.21586(3) 0.08082(2) 0.04337(13) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.228(3) . ?
C1 O1 1.242(3) . ?
C1 H1A 0.9300 . ?
C2 O4 1.234(3) . ?
C2 O3 1.244(3) . ?
C2 H2A 0.9300 . ?
C3 O6 1.232(4) . ?
C3 O5 1.241(4) . ?
C3 H3A 0.9300 . ?
C4 O8 1.236(4) . ?
C4 O7 1.251(3) . ?
C4 H4A 0.9300 . ?
C5 N1 1.482(4) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 N1 1.471(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 N1 1.476(4) . ?
C7 C8 1.500(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.474(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.474(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 N2 1.485(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N3 1.483(4) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N3 1.473(4) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N3 1.473(4) . ?
C13 C14 1.483(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 N4 1.489(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N4 1.469(4) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 N4 1.477(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O10 1.230(3) . ?
C17 O11 1.239(3) . ?
C17 H19 0.9300 . ?
C18 O12 1.234(3) . ?
C18 O13 1.242(3) . ?
C18 H18 0.9300 . ?
C19 O15 1.226(4) . ?
C19 O14 1.241(4) . ?
C19 H20 0.9300 . ?
C20 O16 1.219(5) . ?
C20 O17 1.242(4) . ?
C20 H17 0.9300 . ?
C21 N5 1.471(4) . ?
C21 H27A 0.9600 . ?
C21 H27B 0.9600 . ?
C21 H27C 0.9600 . ?
C22 N5 1.459(4) . ?
C22 H28A 0.9600 . ?
C22 H28B 0.9600 . ?
C22 H28C 0.9600 . ?
C23 C24 1.444(5) . ?
C23 N5 1.471(4) . ?
C23 H29A 0.9700 . ?
C23 H29B 0.9700 . ?
C24 N6 1.466(4) . ?
C24 H30A 0.9700 . ?
C24 H30B 0.9700 . ?
C25 N6 1.469(4) . ?
C25 H32A 0.9600 . ?
C25 H32B 0.9600 . ?
C25 H32C 0.9600 . ?
C26 N6 1.482(4) . ?
C26 H31A 0.9600 . ?
C26 H31B 0.9600 . ?
C26 H31C 0.9600 . ?
C27 N7 1.444(4) . ?
C27 H27D 0.9600 . ?
C27 H27E 0.9600 . ?
C27 H27F 0.9600 . ?
C28 N7 1.447(5) . ?
C28 H22A 0.9600 . ?
C28 H22B 0.9600 . ?
C28 H22C 0.9600 . ?
C29 C30 1.497(15) . ?
C29 N7 1.511(8) . ?
C29 H29C 0.9700 . ?
C29 H29D 0.9700 . ?
C30 N8 1.454(12) . ?
C30 H30C 0.9700 . ?
C30 H30D 0.9700 . ?
C29' C30' 1.490(16) . ?
C29' N7 1.512(8) . ?
C29' H29E 0.9700 . ?
C29' H29F 0.9700 . ?
C30' N8 1.521(14) . ?
C30' H30E 0.9700 . ?
C30' H30F 0.9700 . ?
C31 N8 1.473(4) . ?
C31 H26A 0.9600 . ?
C31 H26B 0.9600 . ?
C31 H26C 0.9600 . ?
C32 N8 1.477(4) . ?
C32 H25A 0.9600 . ?
C32 H25B 0.9600 . ?
C32 H25C 0.9600 . ?
N1 Ni1 2.193(2) . ?
N2 Ni1 2.160(2) . ?
N3 Ni2 2.1522(19) . ?
N4 Ni2 2.164(2) . ?
N5 Ni3 2.152(2) . ?
N6 Ni3 2.166(2) . ?
N7 Ni4 2.175(3) . ?
N8 Ni4 2.182(2) . ?
O1 Ni1 2.0415(17) . ?
O2 Ni2 2.0385(18) . ?
O3 Ni1 2.0398(17) . ?
O4 Ni2 2.0353(18) . ?
O5 Ni1 2.0953(17) . ?
O7 Ni2 2.083(2) . ?
O9 Ni1 2.0993(18) . ?
O9 Ni2 2.1194(15) . ?
O9 H1 0.9700 . ?
O9 H2 0.9700 . ?
O10 Ni3 2.0458(19) . ?
O11 Ni4 2.0287(18) . ?
O12 Ni3 2.0319(19) . ?
O13 Ni4 2.0433(19) . ?
O14 Ni3 2.071(2) . ?
O17 Ni4 2.0857(19) . ?
O18 Ni4 2.1170(19) . ?
O18 Ni3 2.1200(16) . ?
O18 H3 0.9700 . ?
O18 H4 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 130.1(2) . . ?
O2 C1 H1A 114.9 . . ?
O1 C1 H1A 114.9 . . ?
O4 C2 O3 129.8(2) . . ?
O4 C2 H2A 115.1 . . ?
O3 C2 H2A 115.1 . . ?
O6 C3 O5 128.9(3) . . ?
O6 C3 H3A 115.5 . . ?
O5 C3 H3A 115.5 . . ?
O8 C4 O7 127.6(3) . . ?
O8 C4 H4A 116.2 . . ?
O7 C4 H4A 116.2 . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 C8 111.2(2) . . ?
N1 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N1 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N2 C8 C7 110.8(2) . . ?
N2 C8 H8A 109.5 . . ?
C7 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 H11A 109.5 . . ?
N3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 C14 111.8(2) . . ?
N3 C13 H13A 109.3 . . ?
C14 C13 H13A 109.3 . . ?
N3 C13 H13B 109.3 . . ?
C14 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 N4 111.1(3) . . ?
C13 C14 H14A 109.4 . . ?
N4 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
N4 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 H16A 109.5 . . ?
N4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O10 C17 O11 130.0(2) . . ?
O10 C17 H19 115.0 . . ?
O11 C17 H19 115.0 . . ?
O12 C18 O13 130.0(3) . . ?
O12 C18 H18 115.0 . . ?
O13 C18 H18 115.0 . . ?
O15 C19 O14 128.6(3) . . ?
O15 C19 H20 115.7 . . ?
O14 C19 H20 115.7 . . ?
O16 C20 O17 129.1(3) . . ?
O16 C20 H17 115.4 . . ?
O17 C20 H17 115.4 . . ?
N5 C21 H27A 109.5 . . ?
N5 C21 H27B 109.5 . . ?
H27A C21 H27B 109.5 . . ?
N5 C21 H27C 109.5 . . ?
H27A C21 H27C 109.5 . . ?
H27B C21 H27C 109.5 . . ?
N5 C22 H28A 109.5 . . ?
N5 C22 H28B 109.5 . . ?
H28A C22 H28B 109.5 . . ?
N5 C22 H28C 109.5 . . ?
H28A C22 H28C 109.5 . . ?
H28B C22 H28C 109.5 . . ?
C24 C23 N5 114.1(3) . . ?
C24 C23 H29A 108.7 . . ?
N5 C23 H29A 108.7 . . ?
C24 C23 H29B 108.7 . . ?
N5 C23 H29B 108.7 . . ?
H29A C23 H29B 107.6 . . ?
C23 C24 N6 114.3(3) . . ?
C23 C24 H30A 108.7 . . ?
N6 C24 H30A 108.7 . . ?
C23 C24 H30B 108.7 . . ?
N6 C24 H30B 108.7 . . ?
H30A C24 H30B 107.6 . . ?
N6 C25 H32A 109.5 . . ?
N6 C25 H32B 109.5 . . ?
H32A C25 H32B 109.5 . . ?
N6 C25 H32C 109.5 . . ?
H32A C25 H32C 109.5 . . ?
H32B C25 H32C 109.5 . . ?
N6 C26 H31A 109.5 . . ?
N6 C26 H31B 109.5 . . ?
H31A C26 H31B 109.5 . . ?
N6 C26 H31C 109.5 . . ?
H31A C26 H31C 109.5 . . ?
H31B C26 H31C 109.5 . . ?
N7 C27 H27D 109.5 . . ?
N7 C27 H27E 109.5 . . ?
H27D C27 H27E 109.5 . . ?
N7 C27 H27F 109.5 . . ?
H27D C27 H27F 109.5 . . ?
H27E C27 H27F 109.5 . . ?
N7 C28 H22A 109.5 . . ?
N7 C28 H22B 109.5 . . ?
H22A C28 H22B 109.5 . . ?
N7 C28 H22C 109.5 . . ?
H22A C28 H22C 109.5 . . ?
H22B C28 H22C 109.5 . . ?
C30 C29 N7 110.2(8) . . ?
C30 C29 H29C 109.6 . . ?
N7 C29 H29C 109.6 . . ?
C30 C29 H29D 109.6 . . ?
N7 C29 H29D 109.6 . . ?
H29C C29 H29D 108.1 . . ?
N8 C30 C29 108.9(8) . . ?
N8 C30 H30C 109.9 . . ?
C29 C30 H30C 109.9 . . ?
N8 C30 H30D 109.9 . . ?
C29 C30 H30D 109.9 . . ?
H30C C30 H30D 108.3 . . ?
C30' C29' N7 107.4(9) . . ?
C30' C29' H29E 110.2 . . ?
N7 C29' H29E 110.2 . . ?
C30' C29' H29F 110.2 . . ?
N7 C29' H29F 110.2 . . ?
H29E C29' H29F 108.5 . . ?
C29' C30' N8 112.8(9) . . ?
C29' C30' H30E 109.0 . . ?
N8 C30' H30E 109.0 . . ?
C29' C30' H30F 109.0 . . ?
N8 C30' H30F 109.0 . . ?
H30E C30' H30F 107.8 . . ?
N8 C31 H26A 109.5 . . ?
N8 C31 H26B 109.5 . . ?
H26A C31 H26B 109.5 . . ?
N8 C31 H26C 109.5 . . ?
H26A C31 H26C 109.5 . . ?
H26B C31 H26C 109.5 . . ?
N8 C32 H25A 109.5 . . ?
N8 C32 H25B 109.5 . . ?
H25A C32 H25B 109.5 . . ?
N8 C32 H25C 109.5 . . ?
H25A C32 H25C 109.5 . . ?
H25B C32 H25C 109.5 . . ?
C6 N1 C7 110.4(2) . . ?
C6 N1 C5 108.0(2) . . ?
C7 N1 C5 108.7(2) . . ?
C6 N1 Ni1 113.21(16) . . ?
C7 N1 Ni1 103.49(16) . . ?
C5 N1 Ni1 113.00(17) . . ?
C8 N2 C9 110.4(2) . . ?
C8 N2 C10 109.4(2) . . ?
C9 N2 C10 106.7(3) . . ?
C8 N2 Ni1 104.50(18) . . ?
C9 N2 Ni1 113.29(18) . . ?
C10 N2 Ni1 112.55(17) . . ?
C13 N3 C12 111.5(3) . . ?
C13 N3 C11 108.0(2) . . ?
C12 N3 C11 107.8(2) . . ?
C13 N3 Ni2 104.71(15) . . ?
C12 N3 Ni2 112.87(17) . . ?
C11 N3 Ni2 111.93(17) . . ?
C15 N4 C16 107.0(2) . . ?
C15 N4 C14 110.6(2) . . ?
C16 N4 C14 108.4(2) . . ?
C15 N4 Ni2 113.93(18) . . ?
C16 N4 Ni2 113.47(17) . . ?
C14 N4 Ni2 103.32(15) . . ?
C22 N5 C23 107.1(3) . . ?
C22 N5 C21 107.8(3) . . ?
C23 N5 C21 112.0(3) . . ?
C22 N5 Ni3 112.63(19) . . ?
C23 N5 Ni3 104.51(18) . . ?
C21 N5 Ni3 112.7(2) . . ?
C24 N6 C25 110.8(3) . . ?
C24 N6 C26 108.1(3) . . ?
C25 N6 C26 106.5(3) . . ?
C24 N6 Ni3 103.97(18) . . ?
C25 N6 Ni3 114.36(18) . . ?
C26 N6 Ni3 112.97(18) . . ?
C27 N7 C28 106.5(4) . . ?
C27 N7 C29 124.4(4) . . ?
C28 N7 C29 96.3(5) . . ?
C27 N7 C29' 92.2(5) . . ?
C28 N7 C29' 125.3(5) . . ?
C27 N7 Ni4 113.7(2) . . ?
C28 N7 Ni4 114.0(2) . . ?
C29 N7 Ni4 101.0(3) . . ?
C29' N7 Ni4 103.4(4) . . ?
C30 N8 C31 101.0(5) . . ?
C30 N8 C32 118.6(5) . . ?
C31 N8 C32 106.4(3) . . ?
C31 N8 C30' 121.0(6) . . ?
C32 N8 C30' 98.9(5) . . ?
C30 N8 Ni4 103.0(5) . . ?
C31 N8 Ni4 112.74(18) . . ?
C32 N8 Ni4 114.53(17) . . ?
C30' N8 Ni4 102.9(6) . . ?
C1 O1 Ni1 135.88(17) . . ?
C1 O2 Ni2 132.62(17) . . ?
C2 O3 Ni1 131.65(17) . . ?
C2 O4 Ni2 136.92(16) . . ?
C3 O5 Ni1 126.73(19) . . ?
C4 O7 Ni2 126.5(2) . . ?
Ni1 O9 Ni2 117.51(8) . . ?
Ni1 O9 H1 107.9 . . ?
Ni2 O9 H1 107.9 . . ?
Ni1 O9 H2 107.9 . . ?
Ni2 O9 H2 107.9 . . ?
H1 O9 H2 107.2 . . ?
C17 O10 Ni3 133.01(18) . . ?
C17 O11 Ni4 135.50(18) . . ?
C18 O12 Ni3 136.80(17) . . ?
C18 O13 Ni4 131.67(18) . . ?
C19 O14 Ni3 128.0(2) . . ?
C20 O17 Ni4 126.3(2) . . ?
Ni4 O18 Ni3 116.81(8) . . ?
Ni4 O18 H3 108.1 . . ?
Ni3 O18 H3 108.1 . . ?
Ni4 O18 H4 108.1 . . ?
Ni3 O18 H4 108.1 . . ?
H3 O18 H4 107.3 . . ?
O3 Ni1 O1 94.18(8) . . ?
O3 Ni1 O5 86.13(8) . . ?
O1 Ni1 O5 178.06(8) . . ?
O3 Ni1 O9 91.05(7) . . ?
O1 Ni1 O9 91.83(7) . . ?
O5 Ni1 O9 90.08(7) . . ?
O3 Ni1 N2 89.68(8) . . ?
O1 Ni1 N2 87.23(8) . . ?
O5 Ni1 N2 90.86(8) . . ?
O9 Ni1 N2 178.85(8) . . ?
O3 Ni1 N1 171.60(8) . . ?
O1 Ni1 N1 90.76(8) . . ?
O5 Ni1 N1 88.71(8) . . ?
O9 Ni1 N1 95.58(8) . . ?
N2 Ni1 N1 83.77(9) . . ?
O4 Ni2 O2 92.40(8) . . ?
O4 Ni2 O7 179.31(8) . . ?
O2 Ni2 O7 87.81(9) . . ?
O4 Ni2 O9 90.23(7) . . ?
O2 Ni2 O9 91.91(7) . . ?
O7 Ni2 O9 90.42(7) . . ?
O4 Ni2 N3 88.59(8) . . ?
O2 Ni2 N3 88.75(8) . . ?
O7 Ni2 N3 90.75(8) . . ?
O9 Ni2 N3 178.67(8) . . ?
O4 Ni2 N4 90.71(8) . . ?
O2 Ni2 N4 172.36(8) . . ?
O7 Ni2 N4 88.99(9) . . ?
O9 Ni2 N4 95.05(7) . . ?
N3 Ni2 N4 84.35(8) . . ?
O12 Ni3 O10 92.70(9) . . ?
O12 Ni3 O14 179.25(8) . . ?
O10 Ni3 O14 87.48(9) . . ?
O12 Ni3 O18 90.42(7) . . ?
O10 Ni3 O18 91.59(7) . . ?
O14 Ni3 O18 90.30(8) . . ?
O12 Ni3 N5 88.92(8) . . ?
O10 Ni3 N5 88.25(8) . . ?
O14 Ni3 N5 90.36(9) . . ?
O18 Ni3 N5 179.30(9) . . ?
O12 Ni3 N6 90.25(9) . . ?
O10 Ni3 N6 171.95(8) . . ?
O14 Ni3 N6 89.48(9) . . ?
O18 Ni3 N6 95.88(7) . . ?
N5 Ni3 N6 84.32(9) . . ?
O11 Ni4 O13 93.40(8) . . ?
O11 Ni4 O17 176.59(9) . . ?
O13 Ni4 O17 86.94(9) . . ?
O11 Ni4 O18 92.95(7) . . ?
O13 Ni4 O18 90.89(7) . . ?
O17 Ni4 O18 90.44(8) . . ?
O11 Ni4 N7 88.65(9) . . ?
O13 Ni4 N7 89.55(9) . . ?
O17 Ni4 N7 87.95(9) . . ?
O18 Ni4 N7 178.31(8) . . ?
O11 Ni4 N8 90.51(8) . . ?
O13 Ni4 N8 172.71(8) . . ?
O17 Ni4 N8 88.80(8) . . ?
O18 Ni4 N8 95.06(8) . . ?
N7 Ni4 N8 84.39(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C7 C8 N2 -60.3(3) . . . . ?
N3 C13 C14 N4 -58.5(4) . . . . ?
N5 C23 C24 N6 52.2(5) . . . . ?
N7 C29 C30 N8 66.9(12) . . . . ?
N7 C29' C30' N8 -62.0(15) . . . . ?
C8 C7 N1 C6 -79.9(3) . . . . ?
C8 C7 N1 C5 161.9(2) . . . . ?
C8 C7 N1 Ni1 41.5(3) . . . . ?
C7 C8 N2 C9 -79.7(3) . . . . ?
C7 C8 N2 C10 163.1(2) . . . . ?
C7 C8 N2 Ni1 42.4(2) . . . . ?
C14 C13 N3 C12 -83.2(3) . . . . ?
C14 C13 N3 C11 158.6(3) . . . . ?
C14 C13 N3 Ni2 39.2(3) . . . . ?
C13 C14 N4 C15 -79.8(3) . . . . ?
C13 C14 N4 C16 163.1(3) . . . . ?
C13 C14 N4 Ni2 42.5(3) . . . . ?
C24 C23 N5 C22 -155.3(4) . . . . ?
C24 C23 N5 C21 86.7(4) . . . . ?
C24 C23 N5 Ni3 -35.6(4) . . . . ?
C23 C24 N6 C25 86.7(4) . . . . ?
C23 C24 N6 C26 -156.9(4) . . . . ?
C23 C24 N6 Ni3 -36.7(4) . . . . ?
C30 C29 N7 C27 83.4(8) . . . . ?
C30 C29 N7 C28 -161.6(7) . . . . ?
C30 C29 N7 C29' 52.1(9) . . . . ?
C30 C29 N7 Ni4 -45.6(8) . . . . ?
C30' C29' N7 C27 163.3(9) . . . . ?
C30' C29' N7 C28 -84.5(10) . . . . ?
C30' C29' N7 C29 -42.1(9) . . . . ?
C30' C29' N7 Ni4 48.4(10) . . . . ?
C29 C30 N8 C31 -163.0(8) . . . . ?
C29 C30 N8 C32 81.4(10) . . . . ?
C29 C30 N8 C30' 46(2) . . . . ?
C29 C30 N8 Ni4 -46.3(10) . . . . ?
C29' C30' N8 C30 -54.4(19) . . . . ?
C29' C30' N8 C31 -88.3(12) . . . . ?
C29' C30' N8 C32 156.5(11) . . . . ?
C29' C30' N8 Ni4 38.6(13) . . . . ?
O2 C1 O1 Ni1 1.6(5) . . . . ?
O1 C1 O2 Ni2 -10.7(5) . . . . ?
O4 C2 O3 Ni1 -2.6(4) . . . . ?
O3 C2 O4 Ni2 -10.3(5) . . . . ?
O6 C3 O5 Ni1 -11.2(5) . . . . ?
O8 C4 O7 Ni2 -9.8(5) . . . . ?
O11 C17 O10 Ni3 13.0(5) . . . . ?
O10 C17 O11 Ni4 -0.9(5) . . . . ?
O13 C18 O12 Ni3 10.5(5) . . . . ?
O12 C18 O13 Ni4 1.8(5) . . . . ?
O15 C19 O14 Ni3 5.3(6) . . . . ?
O16 C20 O17 Ni4 8.8(6) . . . . ?

_refine_diff_density_max         0.282
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.075

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT412_shelx               
;
PROBLEM: Short Intra XH3 .. XHn     H27E   ..  H29F    ..       1.76 Ang.  
RESPONSE: Hydrogen atom H29F belongs to a pmdta ligand, of which
the carbon atoms C29 and C30 could be refined reliable as being disordered.
Hydrogen atom H27E belongs to the same pmdta ligand. Most likely,
the choosen model of disorder reflects the real situation not precisely
and therefore this alert is generated. Trials to apply other models
of disorder gave, however, not reliable results.
;
# end Validation Reply Form
