# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1564005'
_audit_update_record             
;
2017-07-24 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H28 N4 Ni O10 S'
_chemical_formula_weight         647.29

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'
S S 0.1246 0.1234 '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           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

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

_cell_length_a                   11.3241(14)
_cell_length_b                   5.9908(7)
_cell_length_c                   19.470(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.203(2)
_cell_angle_gamma                90
_cell_volume                     1307.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2008
_cell_measurement_theta_min      1.967
_cell_measurement_theta_max      28.439

_exptl_crystal_description       block
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   0.878
_exptl_transmission_factor_max   0.908
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.891
_shelx_estimated_absorpt_T_min   0.878
_shelx_estimated_absorpt_T_max   0.908
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9260
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.967
_diffrn_reflns_theta_max         28.439
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3272
_reflns_number_gt                2522
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0472P)²+0.7332P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3272
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1003
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.5000 0.5000 0.01878(12) Uani 1 2 d S . P . .
S1 S 0.2500 0.69478(13) 0.2500 0.0266(2) Uani 1 2 d S T P . .
O1 O -0.19355(16) 0.2508(4) 0.11484(10) 0.0417(5) Uani 1 1 d . . . . .
O1W O -0.16514(14) 0.6341(3) 0.51087(8) 0.0258(4) Uani 1 1 d . . . . .
H1WA H -0.1681 0.7532 0.5275 0.031 Uiso 1 1 d R U . . .
H1WB H -0.2006 0.5479 0.5455 0.031 Uiso 1 1 d R U . . .
N1 N -0.03175(17) 0.5498(3) 0.39071(9) 0.0223(4) Uani 1 1 d . . . . .
C1 C -0.0076(2) 0.3832(4) 0.34915(12) 0.0263(5) Uani 1 1 d . . . . .
H1A H 0.0209 0.2496 0.3695 0.032 Uiso 1 1 calc R U . . .
O2W O 0.08989(14) 0.7950(3) 0.52385(8) 0.0255(4) Uani 1 1 d . . . . .
H2WA H 0.1574 0.8201 0.5478 0.031 Uiso 1 1 d R U . . .
H2WB H 0.0864 0.8700 0.4866 0.031 Uiso 1 1 d R U . . .
O2 O 0.18083(16) 0.9601(3) 0.41952(8) 0.0298(4) Uani 1 1 d . . . . .
N2 N -0.0280(2) 0.4608(3) 0.12818(10) 0.0296(5) Uani 1 1 d . . . . .
H2B H 0.0458 0.4712 0.1226 0.036 Uiso 1 1 calc R U . . .
C2 C -0.0750(2) 0.7382(4) 0.35989(12) 0.0261(5) Uani 1 1 d . . . . .
H2A H -0.0941 0.8553 0.3876 0.031 Uiso 1 1 calc R U . . .
C3 C -0.0228(2) 0.3991(4) 0.27752(12) 0.0271(5) Uani 1 1 d . . . . .
H3A H -0.0048 0.2783 0.2508 0.032 Uiso 1 1 calc R U . . .
O3 O 0.26962(16) 0.6330(3) 0.40348(9) 0.0338(4) Uani 1 1 d . . . . .
C4 C -0.0926(2) 0.7668(4) 0.28871(12) 0.0278(5) Uani 1 1 d . . . . .
H4A H -0.1230 0.9008 0.2695 0.033 Uiso 1 1 calc R U . . .
C5 C -0.0649(2) 0.5953(4) 0.24605(11) 0.0234(5) Uani 1 1 d . . . . .
C6 C -0.0798(3) 0.6304(4) 0.16827(12) 0.0337(6) Uani 1 1 d . . . . .
H6A H -0.1645 0.6398 0.1513 0.040 Uiso 1 1 calc R U . . .
H6B H -0.0447 0.7733 0.1593 0.040 Uiso 1 1 calc R U . . .
C7 C -0.0934(2) 0.2878(4) 0.09962(12) 0.0262(5) Uani 1 1 d . . . . .
C8 C -0.0416(2) 0.1430(4) 0.04854(11) 0.0232(5) Uani 1 1 d . . . . .
C9 C -0.0586(2) -0.1983(4) -0.01865(12) 0.0276(5) Uani 1 1 d . . . . .
H9A H -0.0985 -0.3313 -0.0308 0.033 Uiso 1 1 calc R U . . .
C10 C -0.0996(2) -0.0575(4) 0.02897(12) 0.0258(5) Uani 1 1 d . . . . .
H10A H -0.1671 -0.0970 0.0483 0.031 Uiso 1 1 calc R U . . .
C11 C 0.2434(2) 0.8934(4) 0.31230(12) 0.0233(5) Uani 1 1 d . . . . .
C12 C 0.2454(2) 1.1041(4) 0.28557(12) 0.0292(5) Uani 1 1 d . . . . .
H12A H 0.2412 1.2332 0.3116 0.035 Uiso 1 1 calc R U . . .
C13 C 0.2313(2) 0.8234(4) 0.38445(12) 0.0234(5) 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
Ni1 O2W 2.0592(16) 3_566 ?
Ni1 O2W 2.0593(16) . ?
Ni1 O1W 2.0737(15) . ?
Ni1 O1W 2.0737(15) 3_566 ?
Ni1 N1 2.1277(18) 3_566 ?
Ni1 N1 2.1278(18) . ?
S1 C11 1.709(2) 2 ?
S1 C11 1.709(2) . ?
O1 C7 1.233(3) . ?
N1 C1 1.338(3) . ?
N1 C2 1.338(3) . ?
C1 C3 1.384(3) . ?
O2 C13 1.255(3) . ?
N2 C7 1.347(3) . ?
N2 C6 1.455(3) . ?
C2 C4 1.382(3) . ?
C3 C5 1.379(3) . ?
O3 C13 1.257(3) . ?
C4 C5 1.385(3) . ?
C5 C6 1.514(3) . ?
C7 C8 1.501(3) . ?
C8 C9 1.387(3) 3 ?
C8 C10 1.395(3) . ?
C9 C10 1.382(3) . ?
C9 C8 1.387(3) 3 ?
C11 C12 1.367(3) . ?
C11 C13 1.491(3) . ?
C12 C12 1.404(5) 2 ?

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
O2W Ni1 O2W 180.0 3_566 . ?
O2W Ni1 O1W 86.07(6) 3_566 . ?
O2W Ni1 O1W 93.93(6) . . ?
O2W Ni1 O1W 93.93(6) 3_566 3_566 ?
O2W Ni1 O1W 86.07(6) . 3_566 ?
O1W Ni1 O1W 180.0 . 3_566 ?
O2W Ni1 N1 96.47(7) 3_566 3_566 ?
O2W Ni1 N1 83.53(7) . 3_566 ?
O1W Ni1 N1 88.76(7) . 3_566 ?
O1W Ni1 N1 91.24(7) 3_566 3_566 ?
O2W Ni1 N1 83.53(7) 3_566 . ?
O2W Ni1 N1 96.47(7) . . ?
O1W Ni1 N1 91.24(7) . . ?
O1W Ni1 N1 88.76(7) 3_566 . ?
N1 Ni1 N1 180.00(10) 3_566 . ?
C11 S1 C11 91.69(16) 2 . ?
C1 N1 C2 116.84(19) . . ?
C1 N1 Ni1 118.72(15) . . ?
C2 N1 Ni1 124.44(15) . . ?
N1 C1 C3 123.5(2) . . ?
C7 N2 C6 121.3(2) . . ?
N1 C2 C4 123.1(2) . . ?
C5 C3 C1 119.5(2) . . ?
C2 C4 C5 119.8(2) . . ?
C3 C5 C4 117.4(2) . . ?
C3 C5 C6 123.0(2) . . ?
C4 C5 C6 119.6(2) . . ?
N2 C6 C5 116.3(2) . . ?
O1 C7 N2 120.6(2) . . ?
O1 C7 C8 121.0(2) . . ?
N2 C7 C8 118.4(2) . . ?
C9 C8 C10 118.2(2) 3 . ?
C9 C8 C7 124.1(2) 3 . ?
C10 C8 C7 117.7(2) . . ?
C10 C9 C8 120.6(2) . 3 ?
C9 C10 C8 121.2(2) . . ?
C12 C11 C13 128.9(2) . . ?
C12 C11 S1 111.60(17) . . ?
C13 C11 S1 119.46(17) . . ?
C11 C12 C12 112.54(13) . 2 ?
O2 C13 O3 126.6(2) . . ?
O2 C13 C11 116.0(2) . . ?
O3 C13 C11 117.3(2) . . ?

_refine_diff_density_max         0.453
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.072

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1564006'
_audit_update_record             
;
2017-07-24 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H62 N8 Ni2 O21'
_chemical_formula_weight         1300.55

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

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

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

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

_cell_length_a                   13.6891(9)
_cell_length_b                   14.2539(9)
_cell_length_c                   16.5959(10)
_cell_angle_alpha                86.6470(10)
_cell_angle_beta                 87.3560(10)
_cell_angle_gamma                64.8310(10)
_cell_volume                     2925.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4219
_cell_measurement_theta_min      1.229
_cell_measurement_theta_max      28.349

_exptl_crystal_description       block
_exptl_crystal_colour            cyan
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_F_000             1356
_exptl_transmission_factor_min   0.874
_exptl_transmission_factor_max   0.989
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    0.729
_shelx_estimated_absorpt_T_min   0.874
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS-
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21915
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.229
_diffrn_reflns_theta_max         28.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14490
_reflns_number_gt                9192
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0859P)²+1.5743P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14490
_refine_ls_number_parameters     784
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0569
_refine_ls_wR_factor_ref         0.1732
_refine_ls_wR_factor_gt          0.1460
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.11916(3) 0.26704(3) -0.12592(2) 0.02651(11) Uani 1 1 d . . . . .
O1 O 0.06802(17) 0.23113(18) -0.22919(13) 0.0346(5) Uani 1 1 d . . . . .
O1W O 0.2782(2) 0.1793(2) -0.16378(16) 0.0517(7) Uani 1 1 d . . . . .
H1WA H 0.3186 0.1856 -0.1291 0.062 Uiso 1 1 d R U . . .
H1WB H 0.3105 0.1730 -0.2095 0.062 Uiso 1 1 d R U . . .
N1 N 0.1226(2) 0.4005(2) -0.18698(17) 0.0337(6) Uani 1 1 d . . . . .
C1 C -0.0241(3) 0.2612(3) -0.25739(19) 0.0332(7) Uani 1 1 d . . . . .
Ni2 Ni -0.37126(3) 0.23017(3) -0.62242(2) 0.02548(11) Uani 1 1 d . . . . .
C2 C -0.0312(2) 0.2190(2) -0.33666(18) 0.0291(7) Uani 1 1 d . . . . .
O2W O -0.03807(18) 0.36104(18) -0.09067(14) 0.0383(6) Uani 1 1 d . . . . .
H2WA H -0.0791 0.3752 -0.1309 0.046 Uiso 1 1 d R U . . .
H2WB H -0.0677 0.4097 -0.0580 0.046 Uiso 1 1 d R U . . .
N2 N 0.0048(2) 0.7621(2) -0.3057(2) 0.0451(8) Uani 1 1 d . . . . .
H2A H -0.0507 0.7571 -0.3235 0.054 Uiso 1 1 calc R U . . .
O2 O -0.1096(2) 0.3244(3) -0.22486(17) 0.0686(10) Uani 1 1 d . . . . .
O3 O -0.24390(17) 0.21446(18) -0.55436(13) 0.0325(5) Uani 1 1 d . . . . .
O3W O -0.26252(18) 0.1433(2) -0.70918(14) 0.0441(6) Uani 1 1 d . . . . .
H3WA H -0.2790 0.1585 -0.7586 0.053 Uiso 1 1 d R U . . .
H3WB H -0.1989 0.0953 -0.7077 0.053 Uiso 1 1 d R U . . .
C3 C 0.0604(3) 0.1432(3) -0.3720(2) 0.0401(8) Uani 1 1 d . . . . .
H3A H 0.1261 0.1184 -0.3461 0.048 Uiso 1 1 calc R U . . .
N3 N -0.4713(3) 1.2524(2) -0.2341(2) 0.0533(9) Uani 1 1 d . . . . .
H3B H -0.4178 1.2690 -0.2342 0.064 Uiso 1 1 calc R U . . .
O4W O -0.48612(17) 0.31241(17) -0.53327(13) 0.0324(5) Uani 1 1 d . . . . .
H4WA H -0.4720 0.3223 -0.4860 0.039 Uiso 1 1 d R U . . .
H4WB H -0.5474 0.3603 -0.5454 0.039 Uiso 1 1 d R U . . .
O4 O -0.32547(18) 0.31758(19) -0.45252(14) 0.0398(6) Uani 1 1 d . . . . .
N4 N -0.6202(2) 1.6269(2) -0.32473(16) 0.0324(6) Uani 1 1 d . . . . .
C4 C 0.0548(3) 0.1044(3) -0.4451(2) 0.0468(9) Uani 1 1 d . . . . .
H4A H 0.1166 0.0543 -0.4685 0.056 Uiso 1 1 calc R U . . .
O5W O -0.3534(2) 0.5088(2) -0.39999(17) 0.0545(7) Uani 1 1 d . . . . .
H5WA H -0.2917 0.4659 -0.4166 0.065 Uiso 1 1 d R U . . .
H5WB H -0.3971 0.4814 -0.4033 0.065 Uiso 1 1 d R U . . .
O5 O -0.50120(18) 0.25272(19) -0.68955(13) 0.0373(6) Uani 1 1 d . . . . .
N5 N 0.1231(2) 0.1287(2) -0.06925(16) 0.0303(6) Uani 1 1 d . . . . .
C5 C -0.0437(3) 0.1405(3) -0.4837(2) 0.0371(8) Uani 1 1 d . . . . .
H5A H -0.0478 0.1143 -0.5328 0.045 Uiso 1 1 calc R U . . .
N6 N 0.2664(2) -0.2468(2) 0.0271(2) 0.0428(7) Uani 1 1 d . . . . .
H6A H 0.3222 -0.2350 0.0331 0.051 Uiso 1 1 calc R U . . .
C6 C -0.1354(2) 0.2157(2) -0.44867(17) 0.0255(6) Uani 1 1 d . . . . .
O6 O -0.42567(19) 0.1767(2) -0.80381(16) 0.0530(7) Uani 1 1 d . . . . .
O6W O -0.3305(3) 0.3971(4) -0.2273(2) 0.131(2) Uani 1 1 d . . . . .
H6WA H -0.2711 0.3877 -0.2067 0.158 Uiso 1 1 d R U . . .
H6WB H -0.3512 0.4522 -0.2571 0.158 Uiso 1 1 d R U . . .
C7 C -0.1292(2) 0.2548(2) -0.37543(17) 0.0263(6) Uani 1 1 d . . . . .
H7A H -0.1908 0.3052 -0.3521 0.032 Uiso 1 1 calc R U . . .
O7 O -0.83110(17) 0.30086(18) -1.02131(13) 0.0340(5) Uani 1 1 d . . . . .
N7 N -0.3649(2) 0.0903(2) -0.56771(16) 0.0308(6) Uani 1 1 d . . . . .
O7W O -0.4251(2) 0.1675(2) -0.05193(19) 0.0667(9) Uani 1 1 d . . . . .
H7WA H -0.4042 0.1568 -0.1010 0.080 Uiso 1 1 d R U . . .
H7WB H -0.4922 0.2080 -0.0517 0.080 Uiso 1 1 d R U . . .
O8 O -0.6546(2) 0.2446(3) -1.04256(16) 0.0630(9) Uani 1 1 d . . . . .
N8 N -0.2688(2) -0.2847(2) -0.4694(2) 0.0445(8) Uani 1 1 d . . . . .
H8A H -0.2817 -0.3274 -0.4969 0.053 Uiso 1 1 calc R U . . .
C8 C -0.2429(2) 0.2520(2) -0.48868(18) 0.0263(6) Uani 1 1 d . . . . .
O8W O -0.4100(4) 0.0206(4) 0.1055(5) 0.234(5) Uani 1 1 d . . . . .
H8WA H -0.4319 0.0602 0.1455 0.281 Uiso 1 1 d R U . . .
H8WB H -0.3464 -0.0248 0.1162 0.281 Uiso 1 1 d R U . . .
O9 O 0.0635(2) 0.8645(3) -0.2438(2) 0.0704(9) Uani 1 1 d . . . . .
C9 C -0.5055(3) 0.2313(3) -0.76111(19) 0.0316(7) Uani 1 1 d . . . . .
O9W O -0.3967(10) -0.0247(12) -0.0230(10) 0.497(10) Uani 1 1 d . U . . .
H9WA H -0.3800 0.0101 -0.0569 0.596 Uiso 1 1 d R U . . .
H9WB H -0.3865 -0.0816 -0.0357 0.596 Uiso 1 1 d R U . . .
C10 C -0.6155(2) 0.2788(2) -0.79824(18) 0.0284(7) Uani 1 1 d . . . . .
O10 O -0.5257(3) 1.1295(3) -0.2570(3) 0.0890(12) Uani 1 1 d . . . . .
O11 O 0.2059(2) -0.3619(2) -0.01055(18) 0.0540(7) Uani 1 1 d . . . . .
C11 C -0.7046(3) 0.3458(3) -0.7559(2) 0.0402(8) Uani 1 1 d . . . . .
H11A H -0.6973 0.3604 -0.7033 0.048 Uiso 1 1 calc R U . . .
O12 O -0.1480(2) -0.2461(2) -0.41220(19) 0.0582(8) Uani 1 1 d . . . . .
C12 C -0.8049(3) 0.3914(3) -0.7910(2) 0.0476(10) Uani 1 1 d . . . . .
H12A H -0.8647 0.4361 -0.7620 0.057 Uiso 1 1 calc R U . . .
C13 C -0.8154(3) 0.3700(3) -0.8697(2) 0.0396(8) Uani 1 1 d . . . . .
H13A H -0.8826 0.4007 -0.8934 0.048 Uiso 1 1 calc R U . . .
C14 C -0.7271(2) 0.3036(2) -0.91307(18) 0.0278(7) Uani 1 1 d . . . . .
C15 C -0.6264(2) 0.2579(2) -0.87710(17) 0.0275(6) Uani 1 1 d . . . . .
H15A H -0.5665 0.2132 -0.9061 0.033 Uiso 1 1 calc R U . . .
C16 C -0.7380(3) 0.2805(3) -0.99849(19) 0.0323(7) Uani 1 1 d . . . . .
C17 C 0.1309(3) 0.4060(3) -0.2673(2) 0.0406(8) Uani 1 1 d . . . . .
H17A H 0.1399 0.3483 -0.2956 0.049 Uiso 1 1 calc R U . . .
C18 C 0.1118(3) 0.4835(3) -0.1480(2) 0.0415(8) Uani 1 1 d . . . . .
H18A H 0.1063 0.4812 -0.0920 0.050 Uiso 1 1 calc R U . . .
C19 C 0.1267(3) 0.4933(3) -0.3104(2) 0.0426(9) Uani 1 1 d . . . . .
H19A H 0.1320 0.4940 -0.3665 0.051 Uiso 1 1 calc R U . . .
C20 C 0.1084(3) 0.5734(3) -0.1875(2) 0.0446(9) Uani 1 1 d . . . . .
H20A H 0.1017 0.6295 -0.1581 0.053 Uiso 1 1 calc R U . . .
C21 C 0.1148(3) 0.5789(3) -0.2704(2) 0.0371(8) Uani 1 1 d . . . . .
C22 C 0.1088(3) 0.6764(3) -0.3160(3) 0.0501(10) Uani 1 1 d . . . . .
H22A H 0.1642 0.6947 -0.2970 0.060 Uiso 1 1 calc R U . . .
H22B H 0.1230 0.6630 -0.3730 0.060 Uiso 1 1 calc R U . . .
C23 C -0.0101(3) 0.8482(3) -0.2702(2) 0.0426(9) Uani 1 1 d . . . . .
C24 C -0.1253(3) 0.9274(3) -0.2643(2) 0.0409(8) Uani 1 1 d . . . . .
C25 C -0.2089(3) 0.9012(3) -0.2390(2) 0.0463(9) Uani 1 1 d . . . . .
H25A H -0.1942 0.8321 -0.2263 0.056 Uiso 1 1 calc R U . . .
C26 C -0.1494(3) 1.0313(3) -0.2826(3) 0.0523(10) Uani 1 1 d . . . . .
H26A H -0.0943 1.0504 -0.2992 0.063 Uiso 1 1 calc R U . . .
C27 C -0.3123(4) 0.9754(3) -0.2324(2) 0.0500(10) Uani 1 1 d . . . . .
H27A H -0.3673 0.9566 -0.2149 0.060 Uiso 1 1 calc R U . . .
C28 C -0.2530(3) 1.1055(3) -0.2765(3) 0.0550(11) Uani 1 1 d . . . . .
H28A H -0.2681 1.1747 -0.2890 0.066 Uiso 1 1 calc R U . . .
C29 C -0.3360(3) 1.0781(3) -0.2515(2) 0.0468(9) Uani 1 1 d . . . . .
C30 C -0.4529(4) 1.1564(3) -0.2477(3) 0.0520(10) Uani 1 1 d . . . . .
C31 C -0.5798(3) 1.3314(3) -0.2187(3) 0.0595(12) Uani 1 1 d . . . . .
H31A H -0.5936 1.3368 -0.1609 0.071 Uiso 1 1 calc R U . . .
H31B H -0.6318 1.3112 -0.2412 0.071 Uiso 1 1 calc R U . . .
C32 C -0.5937(3) 1.4345(3) -0.2554(2) 0.0418(9) Uani 1 1 d . . . . .
C33 C -0.5962(3) 1.4522(3) -0.3381(2) 0.0441(9) Uani 1 1 d . . . . .
H33A H -0.5887 1.3997 -0.3720 0.053 Uiso 1 1 calc R U . . .
C34 C -0.6059(3) 1.5151(3) -0.2087(2) 0.0472(10) Uani 1 1 d . . . . .
H34A H -0.6062 1.5066 -0.1527 0.057 Uiso 1 1 calc R U . . .
C35 C -0.6100(3) 1.5479(3) -0.3697(2) 0.0382(8) Uani 1 1 d . . . . .
H35A H -0.6124 1.5587 -0.4255 0.046 Uiso 1 1 calc R U . . .
C36 C -0.6176(3) 1.6089(3) -0.2447(2) 0.0415(8) Uani 1 1 d . . . . .
H36A H -0.6241 1.6619 -0.2119 0.050 Uiso 1 1 calc R U . . .
C37 C 0.1198(3) 0.1142(3) 0.0105(2) 0.0415(8) Uani 1 1 d . . . . .
H37A H 0.1094 0.1693 0.0425 0.050 Uiso 1 1 calc R U . . .
C38 C 0.1385(3) 0.0475(3) -0.1129(2) 0.0457(9) Uani 1 1 d . . . . .
H38A H 0.1412 0.0553 -0.1689 0.055 Uiso 1 1 calc R U . . .
C39 C 0.1506(4) -0.0474(3) -0.0792(2) 0.0518(10) Uani 1 1 d . . . . .
H39A H 0.1609 -0.1015 -0.1122 0.062 Uiso 1 1 calc R U . . .
C40 C 0.1308(3) 0.0219(3) 0.0480(2) 0.0474(9) Uani 1 1 d . . . . .
H40A H 0.1270 0.0161 0.1041 0.057 Uiso 1 1 calc R U . . .
C41 C 0.1476(3) -0.0618(3) 0.0033(2) 0.0357(8) Uani 1 1 d . . . . .
C42 C 0.1595(3) -0.1640(3) 0.0419(3) 0.0512(11) Uani 1 1 d . . . . .
H42A H 0.1465 -0.1568 0.0997 0.061 Uiso 1 1 calc R U . . .
H42B H 0.1055 -0.1827 0.0210 0.061 Uiso 1 1 calc R U . . .
C43 C 0.2807(3) -0.3402(3) 0.0047(2) 0.0368(8) Uani 1 1 d . . . . .
C44 C 0.3949(3) -0.4209(3) 0.0022(2) 0.0352(7) Uani 1 1 d . . . . .
C45 C 0.4819(3) -0.3993(3) -0.0226(2) 0.0433(9) Uani 1 1 d . . . . .
H45A H 0.4701 -0.3316 -0.0382 0.052 Uiso 1 1 calc R U . . .
C46 C 0.5855(3) -0.4769(3) -0.0242(2) 0.0394(8) Uani 1 1 d . . . . .
H46A H 0.6429 -0.4609 -0.0402 0.047 Uiso 1 1 calc R U . . .
C47 C -0.3676(3) 0.0147(3) -0.6098(2) 0.0403(8) Uani 1 1 d . . . . .
H47A H -0.3723 0.0234 -0.6657 0.048 Uiso 1 1 calc R U . . .
C48 C -0.3564(3) 0.0749(3) -0.4878(2) 0.0384(8) Uani 1 1 d . . . . .
H48A H -0.3530 0.1264 -0.4577 0.046 Uiso 1 1 calc R U . . .
C49 C -0.3637(3) -0.0767(3) -0.5728(3) 0.0470(9) Uani 1 1 d . . . . .
H49A H -0.3661 -0.1277 -0.6041 0.056 Uiso 1 1 calc R U . . .
C50 C -0.3526(3) -0.0145(3) -0.4479(2) 0.0429(9) Uani 1 1 d . . . . .
H50A H -0.3475 -0.0218 -0.3920 0.051 Uiso 1 1 calc R U . . .
C51 C -0.3563(3) -0.0925(3) -0.4908(2) 0.0385(8) Uani 1 1 d . . . . .
C52 C -0.3581(3) -0.1873(3) -0.4454(3) 0.0536(11) Uani 1 1 d . . . . .
H52A H -0.3544 -0.1802 -0.3880 0.064 Uiso 1 1 calc R U . . .
H52B H -0.4260 -0.1905 -0.4549 0.064 Uiso 1 1 calc R U . . .
C53 C -0.1688(3) -0.3072(3) -0.4492(2) 0.0358(8) Uani 1 1 d . . . . .
C54 C -0.0829(3) -0.4081(3) -0.4757(2) 0.0338(7) Uani 1 1 d . . . . .
C55 C 0.0099(3) -0.4079(3) -0.5126(2) 0.0398(8) Uani 1 1 d . . . . .
H55A H 0.0162 -0.3457 -0.5210 0.048 Uiso 1 1 calc R U . . .
C56 C 0.0925(3) -0.4983(3) -0.5368(2) 0.0401(8) Uani 1 1 d . . . . .
H56A H 0.1545 -0.4974 -0.5614 0.048 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O7 2.049(2) 1_656 ?
Ni1 O1 2.051(2) . ?
Ni1 O2W 2.072(2) . ?
Ni1 O1W 2.086(2) . ?
Ni1 N5 2.115(3) . ?
Ni1 N1 2.120(3) . ?
O1 C1 1.251(4) . ?
N1 C18 1.331(4) . ?
N1 C17 1.334(4) . ?
C1 O2 1.254(4) . ?
C1 C2 1.502(4) . ?
Ni2 O5 2.040(2) . ?
Ni2 O3 2.046(2) . ?
Ni2 O3W 2.065(2) . ?
Ni2 N7 2.110(3) . ?
Ni2 O4W 2.111(2) . ?
Ni2 N4 2.128(3) 2_474 ?
C2 C7 1.390(4) . ?
C2 C3 1.392(5) . ?
N2 C23 1.325(5) . ?
N2 C22 1.439(5) . ?
O3 C8 1.245(4) . ?
C3 C4 1.381(5) . ?
N3 C30 1.313(5) . ?
N3 C31 1.454(5) . ?
O4 C8 1.271(4) . ?
N4 C36 1.337(4) . ?
N4 C35 1.342(4) . ?
N4 Ni2 2.128(3) 2_474 ?
C4 C5 1.394(5) . ?
O5 C9 1.253(4) . ?
N5 C37 1.329(4) . ?
N5 C38 1.338(4) . ?
C5 C6 1.387(4) . ?
N6 C43 1.335(4) . ?
N6 C42 1.459(4) . ?
C6 C7 1.387(4) . ?
C6 C8 1.509(4) . ?
O6 C9 1.253(4) . ?
O7 C16 1.253(4) . ?
O7 Ni1 2.048(2) 1_454 ?
N7 C47 1.333(4) . ?
N7 C48 1.334(4) . ?
O8 C16 1.253(4) . ?
N8 C53 1.322(4) . ?
N8 C52 1.468(4) . ?
O9 C23 1.229(4) . ?
C9 C10 1.509(4) . ?
C10 C11 1.379(5) . ?
C10 C15 1.388(4) . ?
O10 C30 1.230(5) . ?
O11 C43 1.229(4) . ?
C11 C12 1.384(5) . ?
O12 C53 1.227(4) . ?
C12 C13 1.386(5) . ?
C13 C14 1.379(5) . ?
C14 C15 1.395(4) . ?
C14 C16 1.502(4) . ?
C17 C19 1.380(5) . ?
C18 C20 1.388(5) . ?
C19 C21 1.370(5) . ?
C20 C21 1.374(5) . ?
C21 C22 1.516(5) . ?
C23 C24 1.502(5) . ?
C24 C25 1.388(5) . ?
C24 C26 1.392(5) . ?
C25 C27 1.364(6) . ?
C26 C28 1.366(6) . ?
C27 C29 1.379(5) . ?
C28 C29 1.390(5) . ?
C29 C30 1.513(6) . ?
C31 C32 1.495(5) . ?
C32 C34 1.371(6) . ?
C32 C33 1.379(5) . ?
C33 C35 1.371(5) . ?
C34 C36 1.379(5) . ?
C37 C40 1.373(5) . ?
C38 C39 1.378(5) . ?
C39 C41 1.373(5) . ?
C40 C41 1.372(5) . ?
C41 C42 1.502(5) . ?
C43 C44 1.497(5) . ?
C44 C45 1.391(5) . ?
C44 C46 1.393(5) 2_645 ?
C45 C46 1.379(5) . ?
C46 C44 1.393(5) 2_645 ?
C47 C49 1.388(5) . ?
C48 C50 1.383(5) . ?
C49 C51 1.368(5) . ?
C50 C51 1.374(5) . ?
C51 C52 1.517(5) . ?
C53 C54 1.494(5) . ?
C54 C55 1.385(5) . ?
C54 C56 1.399(5) 2_544 ?
C55 C56 1.371(5) . ?
C56 C54 1.399(5) 2_544 ?

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
O7 Ni1 O1 178.71(9) 1_656 . ?
O7 Ni1 O2W 88.09(9) 1_656 . ?
O1 Ni1 O2W 91.52(9) . . ?
O7 Ni1 O1W 91.56(10) 1_656 . ?
O1 Ni1 O1W 88.89(10) . . ?
O2W Ni1 O1W 177.02(10) . . ?
O7 Ni1 N5 89.74(10) 1_656 . ?
O1 Ni1 N5 89.08(10) . . ?
O2W Ni1 N5 95.99(10) . . ?
O1W Ni1 N5 86.97(11) . . ?
O7 Ni1 N1 91.50(10) 1_656 . ?
O1 Ni1 N1 89.71(10) . . ?
O2W Ni1 N1 87.03(10) . . ?
O1W Ni1 N1 90.03(11) . . ?
N5 Ni1 N1 176.78(11) . . ?
C1 O1 Ni1 131.4(2) . . ?
C18 N1 C17 117.2(3) . . ?
C18 N1 Ni1 122.2(2) . . ?
C17 N1 Ni1 120.5(2) . . ?
O1 C1 O2 124.8(3) . . ?
O1 C1 C2 116.8(3) . . ?
O2 C1 C2 118.4(3) . . ?
O5 Ni2 O3 177.47(9) . . ?
O5 Ni2 O3W 92.80(9) . . ?
O3 Ni2 O3W 88.84(9) . . ?
O5 Ni2 N7 92.93(10) . . ?
O3 Ni2 N7 89.04(9) . . ?
O3W Ni2 N7 88.14(11) . . ?
O5 Ni2 O4W 85.55(9) . . ?
O3 Ni2 O4W 92.90(9) . . ?
O3W Ni2 O4W 176.65(9) . . ?
N7 Ni2 O4W 89.03(9) . . ?
O5 Ni2 N4 87.20(10) . 2_474 ?
O3 Ni2 N4 90.79(10) . 2_474 ?
O3W Ni2 N4 93.16(11) . 2_474 ?
N7 Ni2 N4 178.69(10) . 2_474 ?
O4W Ni2 N4 89.68(10) . 2_474 ?
C7 C2 C3 119.3(3) . . ?
C7 C2 C1 120.5(3) . . ?
C3 C2 C1 120.3(3) . . ?
C23 N2 C22 123.5(3) . . ?
C8 O3 Ni2 130.1(2) . . ?
C4 C3 C2 120.6(3) . . ?
C30 N3 C31 121.7(4) . . ?
C36 N4 C35 116.4(3) . . ?
C36 N4 Ni2 121.5(2) . 2_474 ?
C35 N4 Ni2 122.0(2) . 2_474 ?
C3 C4 C5 119.9(3) . . ?
C9 O5 Ni2 130.2(2) . . ?
C37 N5 C38 116.4(3) . . ?
C37 N5 Ni1 122.8(2) . . ?
C38 N5 Ni1 120.5(2) . . ?
C6 C5 C4 119.8(3) . . ?
C43 N6 C42 122.3(3) . . ?
C7 C6 C5 120.1(3) . . ?
C7 C6 C8 120.0(3) . . ?
C5 C6 C8 119.9(3) . . ?
C6 C7 C2 120.4(3) . . ?
C16 O7 Ni1 130.3(2) . 1_454 ?
C47 N7 C48 117.6(3) . . ?
C47 N7 Ni2 122.8(2) . . ?
C48 N7 Ni2 119.6(2) . . ?
C53 N8 C52 120.4(3) . . ?
O3 C8 O4 125.1(3) . . ?
O3 C8 C6 117.3(3) . . ?
O4 C8 C6 117.6(3) . . ?
O6 C9 O5 125.0(3) . . ?
O6 C9 C10 118.6(3) . . ?
O5 C9 C10 116.4(3) . . ?
C11 C10 C15 119.5(3) . . ?
C11 C10 C9 120.9(3) . . ?
C15 C10 C9 119.5(3) . . ?
C10 C11 C12 120.7(3) . . ?
C11 C12 C13 119.5(3) . . ?
C14 C13 C12 120.6(3) . . ?
C13 C14 C15 119.4(3) . . ?
C13 C14 C16 120.8(3) . . ?
C15 C14 C16 119.8(3) . . ?
C10 C15 C14 120.2(3) . . ?
O7 C16 O8 124.4(3) . . ?
O7 C16 C14 117.2(3) . . ?
O8 C16 C14 118.4(3) . . ?
N1 C17 C19 123.0(3) . . ?
N1 C18 C20 122.8(4) . . ?
C21 C19 C17 119.8(3) . . ?
C21 C20 C18 119.5(4) . . ?
C19 C21 C20 117.7(3) . . ?
C19 C21 C22 121.0(4) . . ?
C20 C21 C22 121.3(4) . . ?
N2 C22 C21 111.7(3) . . ?
O9 C23 N2 123.8(4) . . ?
O9 C23 C24 121.0(4) . . ?
N2 C23 C24 115.1(3) . . ?
C25 C24 C26 118.5(4) . . ?
C25 C24 C23 122.4(3) . . ?
C26 C24 C23 119.1(3) . . ?
C27 C25 C24 120.8(3) . . ?
C28 C26 C24 120.7(4) . . ?
C25 C27 C29 120.5(4) . . ?
C26 C28 C29 120.3(4) . . ?
C27 C29 C28 119.2(4) . . ?
C27 C29 C30 118.3(4) . . ?
C28 C29 C30 122.4(3) . . ?
O10 C30 N3 122.8(4) . . ?
O10 C30 C29 120.4(4) . . ?
N3 C30 C29 116.8(4) . . ?
N3 C31 C32 111.1(3) . . ?
C34 C32 C33 117.6(3) . . ?
C34 C32 C31 121.6(4) . . ?
C33 C32 C31 120.8(4) . . ?
C35 C33 C32 119.3(4) . . ?
C32 C34 C36 119.9(3) . . ?
N4 C35 C33 123.7(3) . . ?
N4 C36 C34 123.0(4) . . ?
N5 C37 C40 123.2(3) . . ?
N5 C38 C39 123.3(4) . . ?
C41 C39 C38 119.9(4) . . ?
C41 C40 C37 120.4(3) . . ?
C40 C41 C39 116.8(3) . . ?
C40 C41 C42 122.0(3) . . ?
C39 C41 C42 121.2(4) . . ?
N6 C42 C41 112.3(3) . . ?
O11 C43 N6 123.4(3) . . ?
O11 C43 C44 120.7(3) . . ?
N6 C43 C44 115.9(3) . . ?
C45 C44 C46 118.6(3) . 2_645 ?
C45 C44 C43 123.3(3) . . ?
C46 C44 C43 118.1(3) 2_645 . ?
C46 C45 C44 120.8(3) . . ?
C45 C46 C44 120.6(3) . 2_645 ?
N7 C47 C49 122.1(3) . . ?
N7 C48 C50 122.7(3) . . ?
C51 C49 C47 120.6(3) . . ?
C51 C50 C48 120.1(4) . . ?
C49 C51 C50 117.0(3) . . ?
C49 C51 C52 123.8(4) . . ?
C50 C51 C52 119.1(4) . . ?
N8 C52 C51 113.1(3) . . ?
O12 C53 N8 121.0(3) . . ?
O12 C53 C54 122.0(3) . . ?
N8 C53 C54 117.0(3) . . ?
C55 C54 C56 119.5(3) . 2_544 ?
C55 C54 C53 118.2(3) . . ?
C56 C54 C53 122.3(3) 2_544 . ?
C56 C55 C54 120.9(3) . . ?
C55 C56 C54 119.6(3) . 2_544 ?

_refine_diff_density_max         1.218
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.083

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1564007'
_audit_update_record             
;
2017-07-24 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H58 N8 Ni2 O17'
_chemical_formula_weight         1256.54

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

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

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

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

_cell_length_a                   12.3335(6)
_cell_length_b                   14.1746(7)
_cell_length_c                   17.1395(8)
_cell_angle_alpha                103.9720(10)
_cell_angle_beta                 95.2220(10)
_cell_angle_gamma                91.7380(10)
_cell_volume                     2891.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8085
_cell_measurement_theta_min      1.231
_cell_measurement_theta_max      28.216

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            Cyan
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_F_000             1308
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.730
_shelx_estimated_absorpt_T_min   0.898
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21348
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.231
_diffrn_reflns_theta_max         28.216
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14163
_reflns_number_gt                9256
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0974P)²+2.5546P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14163
_refine_ls_number_parameters     766
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1777
_refine_ls_wR_factor_gt          0.1556
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.53993(2) -0.37646(2) -0.58713(2) 0.02268(10) Uani 1 1 d . . . . .
O1 O 0.50842(15) -0.33885(14) -0.69323(10) 0.0287(4) Uani 1 1 d . . . . .
O1W O 0.38464(15) -0.42662(15) -0.57711(11) 0.0324(4) Uani 1 1 d . . . . .
H1WA H 0.3480 -0.4695 -0.5619 0.039 Uiso 1 1 d R U . . .
H1WB H 0.3406 -0.3992 -0.6046 0.039 Uiso 1 1 d R U . . .
N1 N 0.50069(18) -0.23897(16) -0.51749(13) 0.0277(5) Uani 1 1 d . . . . .
C1 C 0.4181(2) -0.3580(2) -0.73674(15) 0.0305(6) Uani 1 1 d . . . . .
Ni2 Ni 0.03641(3) -0.37357(2) -1.08479(2) 0.02393(10) Uani 1 1 d . . . . .
O2W O -0.11870(16) -0.42529(15) -1.07716(11) 0.0340(4) Uani 1 1 d . . . . .
H2WA H -0.1458 -0.4722 -1.0610 0.041 Uiso 1 1 d R U . . .
H2WB H -0.1711 -0.3927 -1.0902 0.041 Uiso 1 1 d R U . . .
N2 N 0.57968(19) -0.51504(17) -0.65361(13) 0.0287(5) Uani 1 1 d . . . . .
C2 C 0.4191(2) -0.36006(19) -0.82515(14) 0.0262(5) Uani 1 1 d . . . . .
O2 O 0.33010(18) -0.3765(2) -0.71268(13) 0.0539(7) Uani 1 1 d . . . . .
O3 O 0.20660(15) -0.33286(14) -1.06339(10) 0.0291(4) Uani 1 1 d . . . . .
C3 C 0.3203(2) -0.36629(19) -0.87230(14) 0.0253(5) Uani 1 1 d . . . . .
H3A H 0.2551 -0.3697 -0.8495 0.030 Uiso 1 1 calc R U . . .
N3 N -0.00334(19) -0.23770(17) -1.01138(13) 0.0300(5) Uani 1 1 d . . . . .
O3W O 0.1786(3) 0.0824(3) -0.7900(2) 0.0907(10) Uani 1 1 d . . . . .
H3WA H 0.2393 0.1107 -0.7927 0.109 Uiso 1 1 d R U . . .
H3WB H 0.1913 0.0386 -0.7645 0.109 Uiso 1 1 d R U . . .
O4 O 0.12817(14) -0.40659(13) -0.98323(10) 0.0266(4) Uani 1 1 d . . . . .
C4 C 0.3192(2) -0.36747(18) -0.95377(14) 0.0237(5) Uani 1 1 d . . . . .
N4 N 0.07893(19) -0.51063(17) -1.15291(13) 0.0304(5) Uani 1 1 d . . . . .
O4W O 0.3422(4) -0.7823(3) -0.7680(3) 0.149(2) Uani 1 1 d . . . . .
H4WA H 0.3185 -0.7267 -0.7686 0.179 Uiso 1 1 d R U . . .
H4WB H 0.4104 -0.7717 -0.7490 0.179 Uiso 1 1 d R U . . .
N5 N 0.1681(2) -0.80321(17) -1.36839(14) 0.0358(5) Uani 1 1 d . . . . .
H5B H 0.2087 -0.7975 -1.4054 0.043 Uiso 1 1 calc R U . . .
O5 O 1.00402(16) -0.33145(14) -0.18884(11) 0.0314(4) Uani 1 1 d . . . . .
C5 C 0.4164(2) -0.36615(19) -0.98856(15) 0.0268(5) Uani 1 1 d . . . . .
H5A H 0.4147 -0.3673 -1.0431 0.032 Uiso 1 1 calc R U . . .
O5W O 0.8008(3) 0.0777(4) -0.2880(3) 0.1439(19) Uani 1 1 d . . . . .
H5WA H 0.7376 0.0694 -0.3142 0.173 Uiso 1 1 d R U . . .
H5WB H 0.8366 0.1201 -0.3039 0.173 Uiso 1 1 d R U . . .
C6 C 0.5169(2) -0.3632(2) -0.94296(16) 0.0297(6) Uani 1 1 d . . . . .
N6 N -0.0533(2) 0.06299(18) -0.78345(16) 0.0409(6) Uani 1 1 d . . . . .
H6A H 0.0130 0.0863 -0.7711 0.049 Uiso 1 1 calc R U . . .
O6 O 0.82441(19) -0.3622(2) -0.20831(13) 0.0527(6) Uani 1 1 d . . . . .
C7 C 0.5158(2) -0.3583(2) -0.86074(16) 0.0299(6) Uani 1 1 d . . . . .
H7A H 0.5817 -0.3538 -0.8288 0.036 Uiso 1 1 calc R U . . .
N7 N 0.4158(2) 0.05058(18) -0.29382(16) 0.0410(6) Uani 1 1 d . . . . .
H7B H 0.3646 0.0330 -0.2686 0.049 Uiso 1 1 calc R U . . .
O7 O 0.58448(19) 0.11733(18) -0.28569(14) 0.0518(6) Uani 1 1 d . . . . .
C8 C 0.6211(3) -0.3647(3) -0.9824(2) 0.0467(8) Uani 1 1 d . . . . .
H8A H 0.6820 -0.3623 -0.9427 0.070 Uiso 1 1 calc R U . . .
H8B H 0.6211 -0.4234 -1.0244 0.070 Uiso 1 1 calc R U . . .
H8C H 0.6267 -0.3093 -1.0051 0.070 Uiso 1 1 calc R U . . .
N8 N 0.6710(3) -0.80924(19) -0.86976(15) 0.0437(6) Uani 1 1 d . . . . .
H8D H 0.7191 -0.7968 -0.8997 0.052 Uiso 1 1 calc R U . . .
O8 O -0.20667(19) 0.01755(18) -0.73910(14) 0.0497(6) Uani 1 1 d . . . . .
O9 O 0.5007(3) -0.8683(2) -0.86477(17) 0.0706(9) Uani 1 1 d . . . . .
C9 C 0.2131(2) -0.36947(18) -1.00283(13) 0.0226(5) Uani 1 1 d . . . . .
O10 O 0.0066(2) -0.85274(19) -1.33667(14) 0.0527(6) Uani 1 1 d . . . . .
C10 C 0.0838(3) -0.5895(2) -1.12398(18) 0.0387(7) Uani 1 1 d . . . . .
H10A H 0.0578 -0.5868 -1.0743 0.046 Uiso 1 1 calc R U . . .
O11 O 0.71060(15) -0.33480(14) -0.56496(10) 0.0278(4) Uani 1 1 d . . . . .
C11 C 0.1255(3) -0.6751(2) -1.16388(19) 0.0408(7) Uani 1 1 d . . . . .
H11A H 0.1289 -0.7277 -1.1402 0.049 Uiso 1 1 calc R U . . .
O12 O 0.63074(14) -0.40616(13) -0.48374(10) 0.0258(4) Uani 1 1 d . . . . .
C12 C 0.1620(2) -0.6830(2) -1.23872(16) 0.0325(6) Uani 1 1 d . . . . .
C13 C 0.1558(4) -0.6022(3) -1.26901(19) 0.0565(10) Uani 1 1 d . . . . .
H13A H 0.1791 -0.6038 -1.3194 0.068 Uiso 1 1 calc R U . . .
C14 C 0.1152(4) -0.5187(3) -1.22539(19) 0.0564(10) Uani 1 1 d . . . . .
H14A H 0.1128 -0.4649 -1.2474 0.068 Uiso 1 1 calc R U . . .
C15 C 0.2112(3) -0.7736(2) -1.28404(18) 0.0395(7) Uani 1 1 d . . . . .
H15A H 0.2896 -0.7620 -1.2806 0.047 Uiso 1 1 calc R U . . .
H15B H 0.1970 -0.8262 -1.2585 0.047 Uiso 1 1 calc R U . . .
C16 C 0.0645(3) -0.8397(2) -1.38864(18) 0.0362(6) Uani 1 1 d . . . . .
C18 C 0.0242(3) -0.8650(2) -1.47661(18) 0.0365(6) Uani 1 1 d . . . . .
C19 C -0.0874(3) -0.8718(3) -1.4980(2) 0.0486(8) Uani 1 1 d . . . . .
H19A H -0.1346 -0.8593 -1.4579 0.058 Uiso 1 1 calc R U . . .
C20 C -0.1290(3) -0.8968(3) -1.5775(2) 0.0476(8) Uani 1 1 d . . . . .
H20A H -0.2042 -0.9012 -1.5905 0.057 Uiso 1 1 calc R U . . .
C22 C -0.0823(3) -0.1876(2) -1.03817(19) 0.0454(8) Uani 1 1 d . . . . .
H22A H -0.1176 -0.2129 -1.0897 0.055 Uiso 1 1 calc R U . . .
C23 C -0.1143(3) -0.0999(3) -0.9931(2) 0.0481(8) Uani 1 1 d . . . . .
H23A H -0.1693 -0.0674 -1.0147 0.058 Uiso 1 1 calc R U . . .
C24 C -0.0641(2) -0.0606(2) -0.91587(17) 0.0337(6) Uani 1 1 d . . . . .
C25 C 0.0161(3) -0.1126(2) -0.88780(18) 0.0438(8) Uani 1 1 d . . . . .
H25A H 0.0514 -0.0896 -0.8360 0.053 Uiso 1 1 calc R U . . .
C26 C 0.4354(2) -0.0605(2) -0.42756(17) 0.0325(6) Uani 1 1 d . . . . .
C27 C -0.0967(3) 0.0370(2) -0.86778(19) 0.0428(7) Uani 1 1 d . . . . .
H27A H -0.0725 0.0871 -0.8931 0.051 Uiso 1 1 calc R U . . .
H27B H -0.1756 0.0363 -0.8707 0.051 Uiso 1 1 calc R U . . .
C28 C -0.1120(2) 0.0522(2) -0.72434(18) 0.0363(6) Uani 1 1 d . . . . .
C29 C -0.0612(2) 0.0846(2) -0.63863(19) 0.0356(6) Uani 1 1 d . . . . .
C30 C 0.0507(3) 0.0932(3) -0.6178(2) 0.0471(8) Uani 1 1 d . . . . .
H30A H 0.0978 0.0821 -0.6581 0.056 Uiso 1 1 calc R U . . .
C31 C 0.0923(3) 0.1180(2) -0.5377(2) 0.0459(8) Uani 1 1 d . . . . .
H31A H 0.1674 0.1233 -0.5246 0.055 Uiso 1 1 calc R U . . .
C34 C 0.4194(2) -0.1927(2) -0.54626(17) 0.0350(6) Uani 1 1 d . . . . .
H34A H 0.3840 -0.2211 -0.5972 0.042 Uiso 1 1 calc R U . . .
C35 C 0.3854(2) -0.1043(2) -0.50375(18) 0.0367(6) Uani 1 1 d . . . . .
H35A H 0.3290 -0.0744 -0.5265 0.044 Uiso 1 1 calc R U . . .
C36 C 0.0443(3) -0.1995(2) -0.93671(18) 0.0412(7) Uani 1 1 d . . . . .
H36A H 0.0995 -0.2330 -0.9164 0.049 Uiso 1 1 calc R U . . .
C37 C 0.5193(3) -0.1082(2) -0.39776(19) 0.0447(8) Uani 1 1 d . . . . .
H37A H 0.5552 -0.0817 -0.3467 0.054 Uiso 1 1 calc R U . . .
C38 C 0.5501(3) -0.1958(2) -0.44401(18) 0.0411(7) Uani 1 1 d . . . . .
H38A H 0.6078 -0.2260 -0.4231 0.049 Uiso 1 1 calc R U . . .
C39 C 0.3987(3) 0.0362(2) -0.38033(19) 0.0388(7) Uani 1 1 d . . . . .
H39A H 0.4378 0.0885 -0.3954 0.047 Uiso 1 1 calc R U . . .
H39B H 0.3217 0.0404 -0.3957 0.047 Uiso 1 1 calc R U . . .
C40 C 0.5101(3) 0.0908(2) -0.25172(19) 0.0384(7) Uani 1 1 d . . . . .
C41 C 0.5213(3) 0.1012(2) -0.16262(19) 0.0389(7) Uani 1 1 d . . . . .
C42 C 0.6266(3) 0.1102(2) -0.12416(19) 0.0439(7) Uani 1 1 d . . . . .
H42A H 0.6858 0.1076 -0.1544 0.053 Uiso 1 1 calc R U . . .
C43 C 0.6439(3) 0.1231(2) -0.04189(19) 0.0450(8) Uani 1 1 d . . . . .
H43A H 0.7148 0.1281 -0.0170 0.054 Uiso 1 1 calc R U . . .
C44 C 0.5569(3) 0.1286(2) 0.00441(19) 0.0406(7) Uani 1 1 d . . . . .
C45 C 0.4518(3) 0.1167(2) -0.0337(2) 0.0480(8) Uani 1 1 d . . . . .
H45A H 0.3929 0.1183 -0.0033 0.058 Uiso 1 1 calc R U . . .
C46 C 0.4338(3) 0.1024(2) -0.1169(2) 0.0462(8) Uani 1 1 d . . . . .
H46A H 0.3630 0.0935 -0.1421 0.055 Uiso 1 1 calc R U . . .
C48 C 0.7155(2) -0.36919(18) -0.50317(13) 0.0223(5) Uani 1 1 d . . . . .
C49 C 0.8209(2) -0.36471(18) -0.45216(14) 0.0230(5) Uani 1 1 d . . . . .
C50 C 0.9195(2) -0.36559(19) -0.48574(15) 0.0276(5) Uani 1 1 d . . . . .
H50A H 0.9194 -0.3689 -0.5406 0.033 Uiso 1 1 calc R U . . .
C51 C 1.0182(2) -0.3617(2) -0.43864(17) 0.0303(6) Uani 1 1 d . . . . .
C52 C 1.1242(3) -0.3684(3) -0.4761(2) 0.0471(8) Uani 1 1 d . . . . .
H52A H 1.1835 -0.3644 -0.4349 0.071 Uiso 1 1 calc R U . . .
H52B H 1.1241 -0.4292 -0.5157 0.071 Uiso 1 1 calc R U . . .
H52C H 1.1326 -0.3157 -0.5017 0.071 Uiso 1 1 calc R U . . .
C53 C 1.0151(2) -0.3521(2) -0.35581(16) 0.0315(6) Uani 1 1 d . . . . .
H53A H 1.0804 -0.3459 -0.3228 0.038 Uiso 1 1 calc R U . . .
C54 C 0.9170(2) -0.3516(2) -0.32110(15) 0.0282(5) Uani 1 1 d . . . . .
C55 C 0.8193(2) -0.35931(19) -0.37009(14) 0.0261(5) Uani 1 1 d . . . . .
H55A H 0.7532 -0.3608 -0.3482 0.031 Uiso 1 1 calc R U . . .
C56 C 0.9138(2) -0.3483(2) -0.23245(15) 0.0320(6) Uani 1 1 d . . . . .
C57 C 0.5808(3) -0.5931(2) -0.62374(17) 0.0380(7) Uani 1 1 d . . . . .
H57A H 0.5563 -0.5881 -0.5732 0.046 Uiso 1 1 calc R U . . .
C58 C 0.6164(3) -0.6816(2) -0.66379(19) 0.0420(7) Uani 1 1 d . . . . .
H58A H 0.6164 -0.7339 -0.6398 0.050 Uiso 1 1 calc R U . . .
C59 C 0.6520(3) -0.6924(2) -0.73923(16) 0.0371(7) Uani 1 1 d . . . . .
C60 C 0.6521(4) -0.6111(3) -0.76993(19) 0.0609(11) Uani 1 1 d . . . . .
H60A H 0.6768 -0.6141 -0.8201 0.073 Uiso 1 1 calc R U . . .
C61 C 0.6156(4) -0.5256(3) -0.72639(19) 0.0568(11) Uani 1 1 d . . . . .
H61A H 0.6158 -0.4720 -0.7488 0.068 Uiso 1 1 calc R U . . .
C62 C 0.6967(4) -0.7864(3) -0.78292(19) 0.0527(9) Uani 1 1 d . . . . .
H62A H 0.7753 -0.7823 -0.7707 0.063 Uiso 1 1 calc R U . . .
H62B H 0.6678 -0.8392 -0.7626 0.063 Uiso 1 1 calc R U . . .
C63 C 0.5729(3) -0.8496(2) -0.90405(19) 0.0441(8) 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
Ni1 O1 2.0234(17) . ?
Ni1 O1W 2.0590(19) . ?
Ni1 N2 2.116(2) . ?
Ni1 N1 2.120(2) . ?
Ni1 O11 2.1435(18) . ?
Ni1 O12 2.1446(17) . ?
Ni1 C48 2.474(2) . ?
O1 C1 1.266(3) . ?
N1 C34 1.336(3) . ?
N1 C38 1.341(3) . ?
C1 O2 1.239(4) . ?
C1 C2 1.510(3) . ?
Ni2 O5 2.0236(18) 1_454 ?
Ni2 O2W 2.054(2) . ?
Ni2 N4 2.119(2) . ?
Ni2 N3 2.129(2) . ?
Ni2 O3 2.1349(19) . ?
Ni2 O4 2.1440(17) . ?
Ni2 C9 2.474(2) . ?
N2 C57 1.327(4) . ?
N2 C61 1.337(4) . ?
C2 C3 1.388(3) . ?
C2 C7 1.390(4) . ?
O3 C9 1.265(3) . ?
C3 C4 1.391(3) . ?
N3 C22 1.334(4) . ?
N3 C36 1.336(4) . ?
O4 C9 1.266(3) . ?
C4 C5 1.389(4) . ?
C4 C9 1.485(3) . ?
N4 C10 1.328(4) . ?
N4 C14 1.338(4) . ?
N5 C16 1.347(4) . ?
N5 C15 1.450(4) . ?
O5 C56 1.265(3) . ?
O5 Ni2 2.0237(18) 1_656 ?
C5 C6 1.398(4) . ?
C6 C7 1.396(4) . ?
C6 C8 1.503(4) . ?
N6 C28 1.332(4) . ?
N6 C27 1.450(4) . ?
O6 C56 1.239(4) . ?
N7 C40 1.344(4) . ?
N7 C39 1.442(4) . ?
O7 C40 1.226(4) . ?
N8 C63 1.342(5) . ?
N8 C62 1.448(4) . ?
O8 C28 1.233(4) . ?
O9 C63 1.225(4) . ?
O10 C16 1.234(4) . ?
C10 C11 1.381(4) . ?
O11 C48 1.266(3) . ?
C11 C12 1.378(4) . ?
O12 C48 1.262(3) . ?
C12 C13 1.368(4) . ?
C12 C15 1.508(4) . ?
C13 C14 1.374(4) . ?
C16 C18 1.497(4) . ?
C18 C31 1.382(4) 1_544 ?
C18 C19 1.386(5) . ?
C19 C20 1.368(5) . ?
C20 C29 1.381(4) 1_544 ?
C22 C23 1.386(4) . ?
C23 C24 1.386(4) . ?
C24 C25 1.371(4) . ?
C24 C27 1.516(4) . ?
C25 C36 1.386(4) . ?
C26 C37 1.379(4) . ?
C26 C35 1.382(4) . ?
C26 C39 1.519(4) . ?
C28 C29 1.500(4) . ?
C29 C20 1.381(4) 1_566 ?
C29 C30 1.388(4) . ?
C30 C31 1.378(5) . ?
C31 C18 1.383(4) 1_566 ?
C34 C35 1.387(4) . ?
C37 C38 1.386(4) . ?
C40 C41 1.491(4) . ?
C41 C42 1.389(5) . ?
C41 C46 1.388(4) . ?
C42 C43 1.373(4) . ?
C43 C44 1.384(4) . ?
C44 C45 1.384(5) . ?
C44 C63 1.517(4) 1_566 ?
C45 C46 1.387(5) . ?
C48 C49 1.490(3) . ?
C49 C50 1.391(4) . ?
C49 C55 1.392(3) . ?
C50 C51 1.390(4) . ?
C51 C53 1.397(4) . ?
C51 C52 1.504(4) . ?
C53 C54 1.396(4) . ?
C54 C55 1.390(3) . ?
C54 C56 1.513(3) . ?
C57 C58 1.382(4) . ?
C58 C59 1.378(4) . ?
C59 C60 1.378(4) . ?
C59 C62 1.510(4) . ?
C60 C61 1.373(4) . ?
C63 C44 1.517(4) 1_544 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1W 97.86(8) . . ?
O1 Ni1 N2 88.28(8) . . ?
O1W Ni1 N2 92.13(9) . . ?
O1 Ni1 N1 93.32(8) . . ?
O1W Ni1 N1 87.52(8) . . ?
N2 Ni1 N1 178.39(8) . . ?
O1 Ni1 O11 98.61(7) . . ?
O1W Ni1 O11 163.53(7) . . ?
N2 Ni1 O11 88.74(8) . . ?
N1 Ni1 O11 91.15(8) . . ?
O1 Ni1 O12 159.71(8) . . ?
O1W Ni1 O12 102.14(7) . . ?
N2 Ni1 O12 87.58(8) . . ?
N1 Ni1 O12 90.96(8) . . ?
O11 Ni1 O12 61.45(6) . . ?
O1 Ni1 C48 129.26(8) . . ?
O1W Ni1 C48 132.82(8) . . ?
N2 Ni1 C48 87.61(8) . . ?
N1 Ni1 C48 91.47(8) . . ?
O11 Ni1 C48 30.77(7) . . ?
O12 Ni1 C48 30.68(7) . . ?
C1 O1 Ni1 123.81(17) . . ?
C34 N1 C38 116.8(2) . . ?
C34 N1 Ni1 119.02(18) . . ?
C38 N1 Ni1 124.11(19) . . ?
O2 C1 O1 125.2(2) . . ?
O2 C1 C2 117.9(2) . . ?
O1 C1 C2 117.0(2) . . ?
O5 Ni2 O2W 97.21(8) 1_454 . ?
O5 Ni2 N4 89.28(8) 1_454 . ?
O2W Ni2 N4 92.47(9) . . ?
O5 Ni2 N3 93.35(8) 1_454 . ?
O2W Ni2 N3 87.67(9) . . ?
N4 Ni2 N3 177.33(8) . . ?
O5 Ni2 O3 98.38(7) 1_454 . ?
O2W Ni2 O3 164.42(7) . . ?
N4 Ni2 O3 87.38(8) . . ?
N3 Ni2 O3 91.76(8) . . ?
O5 Ni2 O4 159.62(8) 1_454 . ?
O2W Ni2 O4 102.91(7) . . ?
N4 Ni2 O4 86.64(8) . . ?
N3 Ni2 O4 90.73(8) . . ?
O3 Ni2 O4 61.52(7) . . ?
O5 Ni2 C9 129.02(8) 1_454 . ?
O2W Ni2 C9 133.67(8) . . ?
N4 Ni2 C9 86.10(8) . . ?
N3 Ni2 C9 91.88(8) . . ?
O3 Ni2 C9 30.76(7) . . ?
O4 Ni2 C9 30.77(7) . . ?
C57 N2 C61 116.3(2) . . ?
C57 N2 Ni1 123.07(18) . . ?
C61 N2 Ni1 120.3(2) . . ?
C3 C2 C7 119.4(2) . . ?
C3 C2 C1 118.7(2) . . ?
C7 C2 C1 121.9(2) . . ?
C9 O3 Ni2 89.60(15) . . ?
C2 C3 C4 119.7(2) . . ?
C22 N3 C36 116.4(3) . . ?
C22 N3 Ni2 120.06(19) . . ?
C36 N3 Ni2 123.5(2) . . ?
C9 O4 Ni2 89.17(14) . . ?
C5 C4 C3 120.2(2) . . ?
C5 C4 C9 120.5(2) . . ?
C3 C4 C9 119.3(2) . . ?
C10 N4 C14 116.0(3) . . ?
C10 N4 Ni2 123.29(18) . . ?
C14 N4 Ni2 120.2(2) . . ?
C16 N5 C15 119.9(3) . . ?
C56 O5 Ni2 124.49(18) . 1_656 ?
C4 C5 C6 121.1(2) . . ?
C5 C6 C7 117.4(2) . . ?
C5 C6 C8 120.3(2) . . ?
C7 C6 C8 122.3(3) . . ?
C28 N6 C27 122.6(3) . . ?
C2 C7 C6 122.1(2) . . ?
C40 N7 C39 121.4(3) . . ?
C63 N8 C62 120.8(3) . . ?
O3 C9 O4 119.7(2) . . ?
O3 C9 C4 120.4(2) . . ?
O4 C9 C4 119.9(2) . . ?
O3 C9 Ni2 59.64(13) . . ?
O4 C9 Ni2 60.06(12) . . ?
C4 C9 Ni2 179.8(2) . . ?
N4 C10 C11 123.4(3) . . ?
C48 O11 Ni1 89.19(15) . . ?
C12 C11 C10 120.1(3) . . ?
C48 O12 Ni1 89.23(13) . . ?
C13 C12 C11 116.5(3) . . ?
C13 C12 C15 121.0(3) . . ?
C11 C12 C15 122.5(3) . . ?
C12 C13 C14 120.3(3) . . ?
N4 C14 C13 123.6(3) . . ?
N5 C15 C12 112.7(2) . . ?
O10 C16 N5 121.0(3) . . ?
O10 C16 C18 122.0(3) . . ?
N5 C16 C18 116.9(3) . . ?
C31 C18 C19 118.2(3) 1_544 . ?
C31 C18 C16 123.5(3) 1_544 . ?
C19 C18 C16 118.3(3) . . ?
C20 C19 C18 120.9(3) . . ?
C19 C20 C29 121.1(3) . 1_544 ?
N3 C22 C23 123.3(3) . . ?
C22 C23 C24 119.8(3) . . ?
C25 C24 C23 116.9(3) . . ?
C25 C24 C27 123.3(3) . . ?
C23 C24 C27 119.7(3) . . ?
C24 C25 C36 119.9(3) . . ?
C37 C26 C35 117.0(3) . . ?
C37 C26 C39 122.5(3) . . ?
C35 C26 C39 120.5(3) . . ?
N6 C27 C24 114.9(3) . . ?
O8 C28 N6 121.1(3) . . ?
O8 C28 C29 120.2(3) . . ?
N6 C28 C29 118.7(3) . . ?
C20 C29 C30 118.5(3) 1_566 . ?
C20 C29 C28 118.5(3) 1_566 . ?
C30 C29 C28 123.0(3) . . ?
C31 C30 C29 120.3(3) . . ?
C30 C31 C18 121.1(3) . 1_566 ?
N1 C34 C35 123.1(3) . . ?
C26 C35 C34 120.0(3) . . ?
N3 C36 C25 123.6(3) . . ?
C26 C37 C38 120.0(3) . . ?
N1 C38 C37 123.1(3) . . ?
N7 C39 C26 114.1(3) . . ?
O7 C40 N7 120.9(3) . . ?
O7 C40 C41 121.3(3) . . ?
N7 C40 C41 117.7(3) . . ?
C42 C41 C46 118.9(3) . . ?
C42 C41 C40 116.9(3) . . ?
C46 C41 C40 124.1(3) . . ?
C43 C42 C41 120.6(3) . . ?
C42 C43 C44 120.7(3) . . ?
C45 C44 C43 119.1(3) . . ?
C45 C44 C63 118.7(3) . 1_566 ?
C43 C44 C63 122.1(3) . 1_566 ?
C44 C45 C46 120.4(3) . . ?
C45 C46 C41 120.2(3) . . ?
O12 C48 O11 120.1(2) . . ?
O12 C48 C49 119.6(2) . . ?
O11 C48 C49 120.2(2) . . ?
O12 C48 Ni1 60.09(12) . . ?
O11 C48 Ni1 60.04(12) . . ?
C49 C48 Ni1 179.66(17) . . ?
C50 C49 C55 120.4(2) . . ?
C50 C49 C48 120.7(2) . . ?
C55 C49 C48 118.9(2) . . ?
C51 C50 C49 121.1(2) . . ?
C50 C51 C53 117.7(2) . . ?
C50 C51 C52 120.8(3) . . ?
C53 C51 C52 121.5(3) . . ?
C54 C53 C51 122.0(2) . . ?
C55 C54 C53 119.1(2) . . ?
C55 C54 C56 119.0(2) . . ?
C53 C54 C56 121.8(2) . . ?
C54 C55 C49 119.6(2) . . ?
O6 C56 O5 125.3(2) . . ?
O6 C56 C54 118.2(2) . . ?
O5 C56 C54 116.6(2) . . ?
N2 C57 C58 123.4(3) . . ?
C59 C58 C57 120.0(3) . . ?
C60 C59 C58 116.6(3) . . ?
C60 C59 C62 121.8(3) . . ?
C58 C59 C62 121.4(3) . . ?
C61 C60 C59 119.9(3) . . ?
N2 C61 C60 123.7(3) . . ?
N8 C62 C59 113.7(3) . . ?
O9 C63 N8 122.8(3) . . ?
O9 C63 C44 121.6(4) . 1_544 ?
N8 C63 C44 115.6(3) . 1_544 ?

_refine_diff_density_max         1.707
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.081

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1564008'
_audit_update_record             
;
2017-07-24 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H76 N12 Ni3 O26'
_chemical_formula_weight         1773.63

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

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

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

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

_cell_length_a                   10.1922(6)
_cell_length_b                   10.6522(6)
_cell_length_c                   17.2595(10)
_cell_angle_alpha                84.5830(10)
_cell_angle_beta                 87.6350(10)
_cell_angle_gamma                80.7770(10)
_cell_volume                     1840.72(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3641
_cell_measurement_theta_min      1.945
_cell_measurement_theta_max      28.288

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_F_000             920
_exptl_transmission_factor_min   0.882
_exptl_transmission_factor_max   0.912
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.855
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13664
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.945
_diffrn_reflns_theta_max         28.288
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9058
_reflns_number_gt                6696
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0535P)²+1.1926P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9058
_refine_ls_number_parameters     538
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 1.0000 0.5000 0.01834(11) Uani 1 2 d S . P . .
O1 O -0.03588(17) 0.81675(16) 0.51350(11) 0.0233(4) Uani 1 1 d . . . . .
O1W O -0.20256(18) 1.06704(18) 0.52004(12) 0.0300(4) Uani 1 1 d . . . . .
H1WA H -0.2715 1.0311 0.5227 0.036 Uiso 1 1 d R U . . .
H1WB H -0.2121 1.1209 0.5540 0.036 Uiso 1 1 d R U . . .
N1 N 0.0235(2) 0.9862(2) 0.62287(13) 0.0224(4) Uani 1 1 d . . . . .
C1 C 0.1198(3) 1.0385(3) 0.65180(16) 0.0292(6) Uani 1 1 d . . . . .
H1A H 0.1779 1.0750 0.6169 0.035 Uiso 1 1 calc R U . . .
Ni2 Ni 0.44774(3) 0.29986(3) 0.64911(2) 0.02072(9) Uani 1 1 d . . . . .
O2 O -0.25484(17) 0.81850(17) 0.53357(11) 0.0271(4) Uani 1 1 d . . . . .
N2 N 0.1933(2) 0.9858(2) 0.89723(13) 0.0293(5) Uani 1 1 d . . . . .
H2A H 0.2551 0.9373 0.8740 0.035 Uiso 1 1 calc R U . . .
O2W O 0.45128(19) 0.2929(2) 0.53142(12) 0.0373(5) Uani 1 1 d . . . . .
H2WA H 0.4064 0.2843 0.4924 0.045 Uiso 1 1 d R U . . .
H2WB H 0.4831 0.3620 0.5223 0.045 Uiso 1 1 d R U . . .
C2 C 0.1380(3) 1.0413(3) 0.73032(17) 0.0328(6) Uani 1 1 d . . . . .
H2B H 0.2083 1.0768 0.7470 0.039 Uiso 1 1 calc R U . . .
O3W O 0.3300(2) 0.6937(3) 0.55120(16) 0.0602(7) Uani 1 1 d . . . . .
H3WA H 0.3345 0.6226 0.5785 0.072 Uiso 1 1 d R U . . .
H3WB H 0.2787 0.7490 0.5753 0.072 Uiso 1 1 d R U . . .
O3 O -0.39095(16) 0.38947(17) 0.63783(11) 0.0259(4) Uani 1 1 d . . . . .
C3 C 0.0518(3) 0.9914(2) 0.78419(16) 0.0247(5) Uani 1 1 d . . . . .
N3 N 0.4258(2) 0.3195(2) 0.76947(14) 0.0270(5) Uani 1 1 d . . . . .
O4 O -0.2312(2) 0.22014(19) 0.64477(15) 0.0449(6) Uani 1 1 d . . . . .
N4 N 0.2473(2) 0.3402(3) 1.04820(15) 0.0359(6) Uani 1 1 d . . . . .
H4A H 0.2120 0.2772 1.0356 0.043 Uiso 1 1 calc R U . . .
C4 C -0.0477(3) 0.9363(3) 0.75459(17) 0.0316(6) Uani 1 1 d . . . . .
H4B H -0.1076 0.9000 0.7883 0.038 Uiso 1 1 calc R U . . .
O4W O -0.1181(8) 1.2607(6) 0.8225(4) 0.270(5) Uani 1 1 d . . . . .
H4WA H -0.1394 1.2576 0.7758 0.324 Uiso 1 1 d R U . . .
H4WB H -0.1316 1.3388 0.8321 0.324 Uiso 1 1 d R U . . .
O5 O 0.29180(16) 0.47606(18) 0.63104(12) 0.0283(4) Uani 1 1 d . . . . .
N5 N -0.4022(2) 0.3398(2) 1.25618(14) 0.0324(6) Uani 1 1 d . . . . .
H5A H -0.3652 0.3854 1.2846 0.039 Uiso 1 1 calc R U . . .
C5 C -0.0581(3) 0.9353(3) 0.67517(16) 0.0309(6) Uani 1 1 d . . . . .
H5B H -0.1254 0.8972 0.6570 0.037 Uiso 1 1 calc R U . . .
O6 O 0.24464(16) 0.28196(17) 0.64147(11) 0.0253(4) Uani 1 1 d . . . . .
N6 N 0.5095(2) 0.1011(2) 0.66572(14) 0.0264(5) Uani 1 1 d . . . . .
C6 C 0.0583(3) 0.9995(3) 0.87032(16) 0.0317(6) Uani 1 1 d . . . . .
H6A H 0.0101 1.0813 0.8833 0.038 Uiso 1 1 calc R U . . .
H6B H 0.0145 0.9332 0.8976 0.038 Uiso 1 1 calc R U . . .
O7 O 0.14412(19) 1.1202(2) 0.99235(12) 0.0356(5) Uani 1 1 d . . . . .
C7 C 0.2250(3) 1.0457(3) 0.95671(16) 0.0260(6) Uani 1 1 d . . . . .
O8 O 0.2253(3) 0.5080(3) 1.12038(18) 0.0651(8) Uani 1 1 d . . . . .
C8 C 0.3678(3) 1.0193(3) 0.97826(16) 0.0268(6) Uani 1 1 d . . . . .
O9 O -0.3900(2) 0.2312(2) 1.15037(12) 0.0380(5) Uani 1 1 d . . . . .
C9 C 0.4693(3) 1.0099(3) 0.92201(17) 0.0353(7) Uani 1 1 d . . . . .
H9A H 0.4491 1.0163 0.8696 0.042 Uiso 1 1 calc R U . . .
C10 C 0.6010(3) 0.9909(3) 0.94398(17) 0.0341(7) Uani 1 1 d . . . . .
H10A H 0.6688 0.9849 0.9061 0.041 Uiso 1 1 calc R U . . .
C11 C -0.1359(2) 0.7643(2) 0.53562(14) 0.0185(5) Uani 1 1 d . . . . .
C12 C -0.1042(2) 0.6274(2) 0.56944(14) 0.0178(5) Uani 1 1 d . . . . .
C13 C 0.0281(2) 0.5775(2) 0.58457(14) 0.0200(5) Uani 1 1 d . . . . .
H13A H 0.0931 0.6294 0.5745 0.024 Uiso 1 1 calc R U . . .
C14 C 0.0642(2) 0.4518(2) 0.61447(14) 0.0188(5) Uani 1 1 d . . . . .
C15 C 0.2082(2) 0.4006(2) 0.62959(15) 0.0216(5) Uani 1 1 d . . . . .
C16 C -0.0334(2) 0.3742(2) 0.62953(15) 0.0203(5) Uani 1 1 d . . . . .
H16A H -0.0094 0.2891 0.6482 0.024 Uiso 1 1 calc R U . . .
C17 C -0.1667(2) 0.4232(2) 0.61687(14) 0.0184(5) Uani 1 1 d . . . . .
C18 C -0.2014(2) 0.5497(2) 0.58679(14) 0.0181(5) Uani 1 1 d . . . . .
H18A H -0.2902 0.5827 0.5782 0.022 Uiso 1 1 calc R U . . .
C19 C -0.2704(2) 0.3368(2) 0.63451(15) 0.0217(5) Uani 1 1 d . . . . .
C20 C 0.5267(3) 0.3337(3) 0.81304(18) 0.0347(7) Uani 1 1 d . . . . .
H20A H 0.6096 0.3363 0.7888 0.042 Uiso 1 1 calc R U . . .
C21 C 0.5144(3) 0.3449(3) 0.89232(18) 0.0347(7) Uani 1 1 d . . . . .
H21A H 0.5884 0.3518 0.9204 0.042 Uiso 1 1 calc R U . . .
C22 C 0.3912(3) 0.3457(3) 0.92972(17) 0.0286(6) Uani 1 1 d . . . . .
C23 C 0.2858(3) 0.3347(3) 0.88404(17) 0.0311(6) Uani 1 1 d . . . . .
H23A H 0.2007 0.3375 0.9061 0.037 Uiso 1 1 calc R U . . .
C24 C 0.3069(3) 0.3198(3) 0.80618(17) 0.0298(6) Uani 1 1 d . . . . .
H24A H 0.2351 0.3093 0.7773 0.036 Uiso 1 1 calc R U . . .
C25 C 0.3780(3) 0.3566(4) 1.01598(18) 0.0402(8) Uani 1 1 d . . . . .
H25A H 0.4442 0.2927 1.0420 0.048 Uiso 1 1 calc R U . . .
H25B H 0.3961 0.4399 1.0266 0.048 Uiso 1 1 calc R U . . .
C26 C 0.1801(3) 0.4194(3) 1.09661(18) 0.0368(7) Uani 1 1 d . . . . .
C27 C 0.0436(3) 0.3925(3) 1.12089(18) 0.0336(7) Uani 1 1 d . . . . .
C28 C 0.0003(3) 0.4011(3) 1.19797(18) 0.0370(7) Uani 1 1 d . . . . .
H28A H 0.0548 0.4262 1.2336 0.044 Uiso 1 1 calc R U . . .
C29 C -0.1236(3) 0.3726(3) 1.22185(17) 0.0333(7) Uani 1 1 d . . . . .
H29A H -0.1512 0.3774 1.2737 0.040 Uiso 1 1 calc R U . . .
C30 C -0.2074(3) 0.3368(3) 1.16918(16) 0.0261(6) Uani 1 1 d . . . . .
C31 C -0.1650(3) 0.3319(3) 1.09153(17) 0.0321(6) Uani 1 1 d . . . . .
H31A H -0.2214 0.3110 1.0554 0.039 Uiso 1 1 calc R U . . .
C32 C -0.0402(3) 0.3578(3) 1.06742(17) 0.0335(7) Uani 1 1 d . . . . .
H32A H -0.0123 0.3522 1.0157 0.040 Uiso 1 1 calc R U . . .
C33 C -0.3399(3) 0.2992(3) 1.19117(17) 0.0281(6) Uani 1 1 d . . . . .
C34 C -0.5326(3) 0.3068(3) 1.27886(19) 0.0363(7) Uani 1 1 d . . . . .
H34A H -0.5928 0.3343 1.2363 0.044 Uiso 1 1 calc R U . . .
H34B H -0.5675 0.3526 1.3232 0.044 Uiso 1 1 calc R U . . .
C35 C 0.4479(3) 0.0285(3) 0.62342(19) 0.0355(7) Uani 1 1 d . . . . .
H35A H 0.3980 0.0686 0.5816 0.043 Uiso 1 1 calc R U . . .
C36 C 0.4550(3) -0.1007(3) 0.63874(19) 0.0383(7) Uani 1 1 d . . . . .
H36A H 0.4100 -0.1457 0.6078 0.046 Uiso 1 1 calc R U . . .
C37 C 0.5286(3) -0.1646(3) 0.70001(17) 0.0293(6) Uani 1 1 d . . . . .
C38 C 0.5975(3) -0.0919(3) 0.74076(18) 0.0332(7) Uani 1 1 d . . . . .
H38A H 0.6520 -0.1309 0.7809 0.040 Uiso 1 1 calc R U . . .
C39 C 0.5860(3) 0.0385(3) 0.72220(17) 0.0307(6) Uani 1 1 d . . . . .
H39A H 0.6340 0.0848 0.7505 0.037 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0334(17) . ?
Ni1 O1 2.0334(17) 2_576 ?
Ni1 O1W 2.0993(18) . ?
Ni1 O1W 2.0993(18) 2_576 ?
Ni1 N1 2.133(2) . ?
Ni1 N1 2.133(2) 2_576 ?
O1 C11 1.268(3) . ?
N1 C5 1.338(3) . ?
N1 C1 1.338(3) . ?
C1 C2 1.379(4) . ?
Ni2 O3 2.0232(17) 1_655 ?
Ni2 O2W 2.038(2) . ?
Ni2 N6 2.106(2) . ?
Ni2 N3 2.107(2) . ?
Ni2 O6 2.1196(17) . ?
Ni2 O5 2.2629(18) . ?
O2 C11 1.257(3) . ?
N2 C7 1.335(3) . ?
N2 C6 1.451(3) . ?
C2 C3 1.381(4) . ?
O3 C19 1.268(3) . ?
O3 Ni2 2.0232(17) 1_455 ?
C3 C4 1.387(4) . ?
C3 C6 1.502(4) . ?
N3 C20 1.335(4) . ?
N3 C24 1.344(3) . ?
O4 C19 1.241(3) . ?
N4 C26 1.334(4) . ?
N4 C25 1.452(4) . ?
C4 C5 1.380(4) . ?
O5 C15 1.264(3) . ?
N5 C33 1.340(4) . ?
N5 C34 1.457(4) . ?
O6 C15 1.258(3) . ?
N6 C39 1.333(3) . ?
N6 C35 1.351(4) . ?
O7 C7 1.236(3) . ?
C7 C8 1.493(4) . ?
O8 C26 1.224(4) . ?
C8 C10 1.382(4) 2_677 ?
C8 C9 1.387(4) . ?
O9 C33 1.235(3) . ?
C9 C10 1.388(4) . ?
C10 C8 1.382(4) 2_677 ?
C11 C12 1.509(3) . ?
C12 C13 1.393(3) . ?
C12 C18 1.395(3) . ?
C13 C14 1.387(3) . ?
C14 C16 1.394(3) . ?
C14 C15 1.506(3) . ?
C16 C17 1.393(3) . ?
C17 C18 1.392(3) . ?
C17 C19 1.514(3) . ?
C20 C21 1.384(4) . ?
C21 C22 1.387(4) . ?
C22 C23 1.385(4) . ?
C22 C25 1.503(4) . ?
C23 C24 1.372(4) . ?
C26 C27 1.500(4) . ?
C27 C28 1.391(4) . ?
C27 C32 1.396(4) . ?
C28 C29 1.383(4) . ?
C29 C30 1.390(4) . ?
C30 C31 1.394(4) . ?
C30 C33 1.494(4) . ?
C31 C32 1.383(4) . ?
C34 C37 1.519(4) 2_557 ?
C35 C36 1.367(4) . ?
C36 C37 1.382(4) . ?
C37 C38 1.380(4) . ?
C37 C34 1.519(4) 2_557 ?
C38 C39 1.383(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.0 . 2_576 ?
O1 Ni1 O1W 90.37(7) . . ?
O1 Ni1 O1W 89.63(7) 2_576 . ?
O1 Ni1 O1W 89.63(7) . 2_576 ?
O1 Ni1 O1W 90.37(7) 2_576 2_576 ?
O1W Ni1 O1W 180.0 . 2_576 ?
O1 Ni1 N1 87.31(8) . . ?
O1 Ni1 N1 92.69(8) 2_576 . ?
O1W Ni1 N1 87.81(8) . . ?
O1W Ni1 N1 92.19(8) 2_576 . ?
O1 Ni1 N1 92.69(8) . 2_576 ?
O1 Ni1 N1 87.31(8) 2_576 2_576 ?
O1W Ni1 N1 92.19(8) . 2_576 ?
O1W Ni1 N1 87.81(8) 2_576 2_576 ?
N1 Ni1 N1 180.0 . 2_576 ?
C11 O1 Ni1 134.46(16) . . ?
C5 N1 C1 116.0(2) . . ?
C5 N1 Ni1 124.32(18) . . ?
C1 N1 Ni1 119.50(18) . . ?
N1 C1 C2 123.8(3) . . ?
O3 Ni2 O2W 89.30(8) 1_655 . ?
O3 Ni2 N6 109.54(8) 1_655 . ?
O2W Ni2 N6 90.94(9) . . ?
O3 Ni2 N3 93.03(8) 1_655 . ?
O2W Ni2 N3 174.26(9) . . ?
N6 Ni2 N3 93.22(9) . . ?
O3 Ni2 O6 156.32(7) 1_655 . ?
O2W Ni2 O6 84.13(8) . . ?
N6 Ni2 O6 93.34(8) . . ?
N3 Ni2 O6 91.67(8) . . ?
O3 Ni2 O5 97.28(7) 1_655 . ?
O2W Ni2 O5 86.99(8) . . ?
N6 Ni2 O5 153.08(8) . . ?
N3 Ni2 O5 87.51(8) . . ?
O6 Ni2 O5 59.74(7) . . ?
C7 N2 C6 122.5(2) . . ?
C1 C2 C3 120.1(3) . . ?
C19 O3 Ni2 126.55(17) . 1_455 ?
C2 C3 C4 116.4(3) . . ?
C2 C3 C6 123.4(2) . . ?
C4 C3 C6 120.2(2) . . ?
C20 N3 C24 116.5(2) . . ?
C20 N3 Ni2 122.69(19) . . ?
C24 N3 Ni2 120.81(19) . . ?
C26 N4 C25 122.4(3) . . ?
C5 C4 C3 120.1(3) . . ?
C15 O5 Ni2 86.66(15) . . ?
C33 N5 C34 120.2(3) . . ?
N1 C5 C4 123.6(3) . . ?
C15 O6 Ni2 93.33(15) . . ?
C39 N6 C35 116.0(2) . . ?
C39 N6 Ni2 126.6(2) . . ?
C35 N6 Ni2 116.43(19) . . ?
N2 C6 C3 113.1(2) . . ?
O7 C7 N2 123.6(3) . . ?
O7 C7 C8 120.5(3) . . ?
N2 C7 C8 115.9(2) . . ?
C10 C8 C9 119.5(3) 2_677 . ?
C10 C8 C7 118.9(2) 2_677 . ?
C9 C8 C7 121.5(3) . . ?
C8 C9 C10 120.0(3) . . ?
C8 C10 C9 120.5(3) 2_677 . ?
O2 C11 O1 125.2(2) . . ?
O2 C11 C12 119.5(2) . . ?
O1 C11 C12 115.2(2) . . ?
C13 C12 C18 119.0(2) . . ?
C13 C12 C11 118.1(2) . . ?
C18 C12 C11 122.9(2) . . ?
C14 C13 C12 121.0(2) . . ?
C13 C14 C16 119.4(2) . . ?
C13 C14 C15 119.7(2) . . ?
C16 C14 C15 120.9(2) . . ?
O6 C15 O5 120.1(2) . . ?
O6 C15 C14 119.5(2) . . ?
O5 C15 C14 120.4(2) . . ?
C17 C16 C14 120.4(2) . . ?
C18 C17 C16 119.5(2) . . ?
C18 C17 C19 121.4(2) . . ?
C16 C17 C19 119.1(2) . . ?
C17 C18 C12 120.7(2) . . ?
O4 C19 O3 125.0(2) . . ?
O4 C19 C17 117.7(2) . . ?
O3 C19 C17 117.3(2) . . ?
N3 C20 C21 123.4(3) . . ?
C20 C21 C22 119.7(3) . . ?
C23 C22 C21 116.8(3) . . ?
C23 C22 C25 123.4(3) . . ?
C21 C22 C25 119.8(3) . . ?
C24 C23 C22 120.0(3) . . ?
N3 C24 C23 123.5(3) . . ?
N4 C25 C22 113.3(2) . . ?
O8 C26 N4 123.1(3) . . ?
O8 C26 C27 121.5(3) . . ?
N4 C26 C27 115.3(3) . . ?
C28 C27 C32 119.5(3) . . ?
C28 C27 C26 119.5(3) . . ?
C32 C27 C26 121.0(3) . . ?
C29 C28 C27 120.2(3) . . ?
C28 C29 C30 120.7(3) . . ?
C29 C30 C31 118.8(3) . . ?
C29 C30 C33 123.8(3) . . ?
C31 C30 C33 117.4(3) . . ?
C32 C31 C30 120.9(3) . . ?
C31 C32 C27 119.8(3) . . ?
O9 C33 N5 120.9(3) . . ?
O9 C33 C30 120.4(3) . . ?
N5 C33 C30 118.6(3) . . ?
N5 C34 C37 112.7(2) . 2_557 ?
N6 C35 C36 123.6(3) . . ?
C35 C36 C37 120.3(3) . . ?
C38 C37 C36 116.3(3) . . ?
C38 C37 C34 122.1(3) . 2_557 ?
C36 C37 C34 121.6(3) . 2_557 ?
C37 C38 C39 120.4(3) . . ?
N6 C39 C38 123.3(3) . . ?

_refine_diff_density_max         0.571
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.075

