# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2021

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

data_mdemad190918
_database_code_depnum_ccdc_archive 'CCDC 2089518'
loop_
_audit_author_name
_audit_author_address
'Lydia KARMAZIN'
;Federation de Recherche de Chimie
France
;
_audit_update_record             
;
2021-06-11 deposited with the CCDC.	2021-10-29 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         'C12 H11 N4 O4, C H4 O, Br'
_chemical_formula_sum            'C13 H15 Br N4 O5'
_chemical_formula_weight         387.20

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'
Br Br -0.2901 2.4595 '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                   8.3771(5)
_cell_length_b                   18.9639(14)
_cell_length_c                   10.5829(7)
_cell_angle_alpha                90
_cell_angle_beta                 115.046(5)
_cell_angle_gamma                90
_cell_volume                     1523.14(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4605
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.25

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_F_000             784
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    2.731
_shelx_estimated_absorpt_T_min   0.685
_shelx_estimated_absorpt_T_max   0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6114
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  triumph
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33353
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_av_R_equivalents  0.1479
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.148
_diffrn_reflns_theta_max         29.052
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4065
_reflns_number_gt                2550
_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0416P)²+1.4453P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4065
_refine_ls_number_parameters     223
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1191
_refine_ls_wR_factor_gt          0.1006
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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 1.1536(5) 0.5556(2) 0.4215(4) 0.0260(9) Uani 1 1 d . . . . .
C2 C 1.1234(5) 0.6203(2) 0.4627(4) 0.0256(9) Uani 1 1 d . . . . .
H2 H 1.2197 0.6502 0.5153 0.031 Uiso 1 1 calc R U . . .
C3 C 0.9505(5) 0.6429(2) 0.4277(4) 0.0228(8) Uani 1 1 d . . . . .
C4 C 0.8075(5) 0.5972(2) 0.3475(4) 0.0230(8) Uani 1 1 d . . . . .
C5 C 0.8384(5) 0.5309(2) 0.3025(4) 0.0254(8) Uani 1 1 d . . . . .
H5 H 0.7426 0.5010 0.2483 0.031 Uiso 1 1 calc R U . . .
C6 C 1.0087(5) 0.5100(2) 0.3378(4) 0.0240(8) Uani 1 1 d . . . . .
C7 C 0.7584(5) 0.7263(2) 0.4380(4) 0.0225(8) Uani 1 1 d . . . . .
C8 C 0.5611(5) 0.8139(2) 0.4595(4) 0.0265(9) Uani 1 1 d . . . . .
C9 C 0.4321(5) 0.7067(2) 0.3217(4) 0.0251(8) Uani 1 1 d . . . . .
C10 C 0.6144(5) 0.6842(2) 0.3576(4) 0.0220(8) Uani 1 1 d . . . . .
C11 C 0.8780(5) 0.8371(2) 0.5589(5) 0.0343(10) Uani 1 1 d . . . . .
H11A H 0.9632 0.8134 0.6426 0.051 Uiso 1 1 calc R U . . .
H11B H 0.8369 0.8805 0.5857 0.051 Uiso 1 1 calc R U . . .
H11C H 0.9343 0.8486 0.4970 0.051 Uiso 1 1 calc R U . . .
C12 C 0.2431(6) 0.7985(2) 0.3450(5) 0.0373(11) Uani 1 1 d . . . . .
H12A H 0.1552 0.7717 0.2678 0.056 Uiso 1 1 calc R U . . .
H12B H 0.2372 0.8483 0.3185 0.056 Uiso 1 1 calc R U . . .
H12C H 0.2191 0.7941 0.4276 0.056 Uiso 1 1 calc R U . . .
C13 C 0.2506(6) 0.5274(3) 0.0705(5) 0.0446(12) Uani 1 1 d . . . . .
H13A H 0.1570 0.5273 0.1029 0.067 Uiso 1 1 calc R U . . .
H13B H 0.2307 0.4889 0.0038 0.067 Uiso 1 1 calc R U . . .
H13C H 0.2498 0.5725 0.0251 0.067 Uiso 1 1 calc R U . . .
N1 N 0.9241(4) 0.70755(17) 0.4715(3) 0.0248(7) Uani 1 1 d . . . . .
N2 N 0.6428(4) 0.62098(17) 0.3161(3) 0.0216(7) Uani 1 1 d . . . . .
N3 N 0.7278(4) 0.79027(17) 0.4861(3) 0.0241(7) Uani 1 1 d . . . . .
N4 N 0.4193(4) 0.77097(18) 0.3766(3) 0.0252(7) Uani 1 1 d . . . . .
O1 O 1.3148(4) 0.52789(16) 0.4531(3) 0.0307(7) Uani 1 1 d . . . . .
O2 O 1.0382(4) 0.44661(16) 0.2963(3) 0.0324(7) Uani 1 1 d . . . . .
O3 O 0.5359(4) 0.86905(17) 0.5064(3) 0.0363(7) Uani 1 1 d . . . . .
O4 O 0.3051(4) 0.67128(17) 0.2475(3) 0.0369(7) Uani 1 1 d . . . . .
O5 O 0.4171(4) 0.51797(16) 0.1867(3) 0.0341(7) Uani 1 1 d . . . . .
Br1 Br 0.60359(5) 0.63524(2) 0.66112(4) 0.02742(13) Uani 1 1 d . . . . .
H5A H 0.4327 0.4751 0.2453 0.050 Uiso 1 1 d . . . . .
H1 H 1.394(7) 0.561(3) 0.500(5) 0.049(16) Uiso 1 1 d . . . . .
H2A H 1.138(7) 0.440(3) 0.312(5) 0.043(15) Uiso 1 1 d . . . . .
H2N H 0.550(7) 0.593(3) 0.260(5) 0.044(14) 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
C1 O1 1.353(5) . ?
C1 C2 1.361(6) . ?
C1 C6 1.449(6) . ?
C2 C3 1.402(5) . ?
C2 H2 0.9500 . ?
C3 N1 1.360(5) . ?
C3 C4 1.431(5) . ?
C4 N2 1.352(5) . ?
C4 C5 1.407(5) . ?
C5 C6 1.372(5) . ?
C5 H5 0.9500 . ?
C6 O2 1.338(5) . ?
C7 N1 1.327(5) . ?
C7 N3 1.381(5) . ?
C7 C10 1.396(5) . ?
C8 O3 1.215(5) . ?
C8 N3 1.377(5) . ?
C8 N4 1.400(5) . ?
C9 O4 1.222(5) . ?
C9 N4 1.374(5) . ?
C9 C10 1.472(5) . ?
C10 N2 1.332(5) . ?
C11 N3 1.464(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N4 1.465(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O5 1.427(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N2 H2N 0.93(5) . ?
O1 H1 0.90(5) . ?
O2 H2A 0.80(5) . ?
O5 H5A 0.9972 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 125.0(4) . . ?
O1 C1 C6 114.1(4) . . ?
C2 C1 C6 120.9(4) . . ?
C1 C2 C3 120.2(4) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
N1 C3 C2 119.0(3) . . ?
N1 C3 C4 122.2(3) . . ?
C2 C3 C4 118.9(4) . . ?
N2 C4 C5 122.0(4) . . ?
N2 C4 C3 117.0(3) . . ?
C5 C4 C3 121.0(4) . . ?
C6 C5 C4 119.0(4) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
O2 C6 C5 119.1(4) . . ?
O2 C6 C1 120.9(4) . . ?
C5 C6 C1 120.0(4) . . ?
N1 C7 N3 118.3(4) . . ?
N1 C7 C10 123.1(4) . . ?
N3 C7 C10 118.7(4) . . ?
O3 C8 N3 122.2(4) . . ?
O3 C8 N4 120.6(4) . . ?
N3 C8 N4 117.2(3) . . ?
O4 C9 N4 123.8(4) . . ?
O4 C9 C10 122.2(4) . . ?
N4 C9 C10 114.0(3) . . ?
N2 C10 C7 119.1(4) . . ?
N2 C10 C9 119.1(4) . . ?
C7 C10 C9 121.7(4) . . ?
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 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C13 H13A 109.5 . . ?
O5 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O5 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C7 N1 C3 116.9(3) . . ?
C10 N2 C4 121.7(3) . . ?
C10 N2 H2N 121(3) . . ?
C4 N2 H2N 117(3) . . ?
C8 N3 C7 122.7(3) . . ?
C8 N3 C11 118.8(3) . . ?
C7 N3 C11 118.3(3) . . ?
C9 N4 C8 125.7(3) . . ?
C9 N4 C12 118.1(3) . . ?
C8 N4 C12 116.2(3) . . ?
C1 O1 H1 107(3) . . ?
C6 O2 H2A 114(4) . . ?
C13 O5 H5A 117.5 . . ?

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
O1 C1 C2 C3 -177.9(4) . . . . ?
C6 C1 C2 C3 1.8(6) . . . . ?
C1 C2 C3 N1 179.3(4) . . . . ?
C1 C2 C3 C4 -0.5(6) . . . . ?
N1 C3 C4 N2 0.2(5) . . . . ?
C2 C3 C4 N2 180.0(3) . . . . ?
N1 C3 C4 C5 179.4(4) . . . . ?
C2 C3 C4 C5 -0.8(6) . . . . ?
N2 C4 C5 C6 179.9(4) . . . . ?
C3 C4 C5 C6 0.7(6) . . . . ?
C4 C5 C6 O2 179.3(4) . . . . ?
C4 C5 C6 C1 0.6(6) . . . . ?
O1 C1 C6 O2 -0.8(5) . . . . ?
C2 C1 C6 O2 179.4(4) . . . . ?
O1 C1 C6 C5 177.8(4) . . . . ?
C2 C1 C6 C5 -1.9(6) . . . . ?
N1 C7 C10 N2 2.5(6) . . . . ?
N3 C7 C10 N2 -176.9(3) . . . . ?
N1 C7 C10 C9 -179.7(4) . . . . ?
N3 C7 C10 C9 0.9(6) . . . . ?
O4 C9 C10 N2 -4.7(6) . . . . ?
N4 C9 C10 N2 176.5(3) . . . . ?
O4 C9 C10 C7 177.4(4) . . . . ?
N4 C9 C10 C7 -1.3(5) . . . . ?
N3 C7 N1 C3 177.2(3) . . . . ?
C10 C7 N1 C3 -2.2(6) . . . . ?
C2 C3 N1 C7 -178.9(4) . . . . ?
C4 C3 N1 C7 0.9(5) . . . . ?
C7 C10 N2 C4 -1.3(6) . . . . ?
C9 C10 N2 C4 -179.2(3) . . . . ?
C5 C4 N2 C10 -179.1(4) . . . . ?
C3 C4 N2 C10 0.1(5) . . . . ?
O3 C8 N3 C7 177.3(4) . . . . ?
N4 C8 N3 C7 -1.8(6) . . . . ?
O3 C8 N3 C11 -7.6(6) . . . . ?
N4 C8 N3 C11 173.2(4) . . . . ?
N1 C7 N3 C8 -178.7(4) . . . . ?
C10 C7 N3 C8 0.8(6) . . . . ?
N1 C7 N3 C11 6.3(5) . . . . ?
C10 C7 N3 C11 -174.3(4) . . . . ?
O4 C9 N4 C8 -178.6(4) . . . . ?
C10 C9 N4 C8 0.2(6) . . . . ?
O4 C9 N4 C12 0.3(6) . . . . ?
C10 C9 N4 C12 179.1(4) . . . . ?
O3 C8 N4 C9 -177.8(4) . . . . ?
N3 C8 N4 C9 1.3(6) . . . . ?
O3 C8 N4 C12 3.3(6) . . . . ?
N3 C8 N4 C12 -177.6(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A Br1 1.00 2.39 3.362(3) 165.0 3_666
O1 H1 Br1 0.90(5) 2.33(6) 3.215(3) 168(4) 1_655
O2 H2A Br1 0.80(5) 2.50(5) 3.236(3) 155(5) 3_766
N2 H2N O5 0.93(5) 1.76(5) 2.660(4) 162(5) .

_refine_diff_density_max         0.962
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.112

####################################################################### 
# 
# 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_mdemad190722
_database_code_depnum_ccdc_archive 'CCDC 2089519'
loop_
_audit_author_name
_audit_author_address
'Lydia KARMAZIN'
;Federation de Recherche de Chimie
France
;
_audit_update_record             
;
2021-06-11 deposited with the CCDC.	2021-10-29 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         'C54 H66 N18 Ni3 O18, 2(C3 H7 N O), 2(H2 O)'
_chemical_formula_sum            'C60 H84 N20 Ni3 O22'
_chemical_formula_weight         1613.60

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                   15.3127(7)
_cell_length_b                   15.8385(8)
_cell_length_c                   16.6042(7)
_cell_angle_alpha                105.2160(10)
_cell_angle_beta                 97.156(2)
_cell_angle_gamma                111.045(2)
_cell_volume                     3518.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9113
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.67

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_F_000             1688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.885
_shelx_estimated_absorpt_T_min   0.879
_shelx_estimated_absorpt_T_max   0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7169
_exptl_absorpt_correction_T_max  0.7405
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            251128
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_av_R_equivalents  0.1117
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.979
_diffrn_reflns_theta_max         27.915
_diffrn_reflns_theta_full        25.242
_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             16804
_reflns_number_gt                12300
_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0576P)²+6.5447P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16804
_refine_ls_number_parameters     976
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1366
_refine_ls_wR_factor_gt          0.1174
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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 0.5575(2) 0.3575(2) 0.23453(18) 0.0210(6) Uani 1 1 d . . . . .
C2 C 0.4593(2) 0.3142(2) 0.21010(18) 0.0210(6) Uani 1 1 d . . . . .
H2 H 0.4232 0.3523 0.2167 0.025 Uiso 1 1 calc R U . . .
C3 C 0.4107(2) 0.2140(2) 0.17529(17) 0.0186(5) Uani 1 1 d . . . . .
C4 C 0.4662(2) 0.1552(2) 0.16613(18) 0.0197(6) Uani 1 1 d . . . . .
C5 C 0.5668(2) 0.1998(2) 0.19144(19) 0.0220(6) Uani 1 1 d . . . . .
H5 H 0.6029 0.1616 0.1853 0.026 Uiso 1 1 calc R U . . .
C6 C 0.6153(2) 0.2994(2) 0.22559(18) 0.0196(6) Uani 1 1 d . . . . .
C7 C 0.2712(2) 0.0758(2) 0.11822(18) 0.0193(6) Uani 1 1 d . . . . .
C8 C 0.1674(2) 0.0326(2) 0.09453(18) 0.0199(6) Uani 1 1 d . . . . .
C9 C 0.1753(2) -0.1237(2) 0.0575(2) 0.0267(7) Uani 1 1 d . . . . .
C10 C 0.3247(2) 0.0208(2) 0.10944(18) 0.0208(6) Uani 1 1 d . . . . .
C11 C 0.0183(2) -0.1144(2) 0.0425(2) 0.0257(6) Uani 1 1 d . . . . .
H11A H -0.0032 -0.1295 0.0922 0.039 Uiso 1 1 calc R U . . .
H11B H -0.0027 -0.1739 -0.0061 0.039 Uiso 1 1 calc R U . . .
H11C H -0.0097 -0.0726 0.0266 0.039 Uiso 1 1 calc R U . . .
C12 C 0.3268(3) -0.1399(3) 0.0618(3) 0.0395(9) Uani 1 1 d . . . . .
H12A H 0.3294 -0.1660 0.1090 0.059 Uiso 1 1 calc R U . . .
H12B H 0.3926 -0.1022 0.0596 0.059 Uiso 1 1 calc R U . . .
H12C H 0.2938 -0.1927 0.0072 0.059 Uiso 1 1 calc R U . . .
C13 C 0.2463(2) 0.4209(2) 0.19657(18) 0.0201(6) Uani 1 1 d . . . . .
C14 C 0.2929(2) 0.5185(2) 0.2219(2) 0.0223(6) Uani 1 1 d . . . . .
H14 H 0.3612 0.5483 0.2421 0.027 Uiso 1 1 calc R U . . .
C15 C 0.2411(2) 0.5753(2) 0.21834(18) 0.0196(6) Uani 1 1 d . . . . .
C16 C 0.1365(2) 0.5301(2) 0.18475(19) 0.0206(6) Uani 1 1 d . . . . .
C17 C 0.0892(2) 0.4302(2) 0.15696(19) 0.0222(6) Uani 1 1 d . . . . .
H17 H 0.0214 0.4003 0.1336 0.027 Uiso 1 1 calc R U . . .
C18 C 0.1406(2) 0.3732(2) 0.16308(19) 0.0209(6) Uani 1 1 d . . . . .
C19 C 0.2343(2) 0.7227(2) 0.24208(18) 0.0202(6) Uani 1 1 d . . . . .
C20 C 0.2857(2) 0.8250(2) 0.27252(19) 0.0217(6) Uani 1 1 d . . . . .
C21 C 0.1308(2) 0.8358(2) 0.2370(2) 0.0249(6) Uani 1 1 d . . . . .
C22 C 0.1347(2) 0.6787(2) 0.20925(19) 0.0216(6) Uani 1 1 d . . . . .
C23 C 0.2817(3) 0.9819(2) 0.2991(2) 0.0298(7) Uani 1 1 d . . . . .
H23A H 0.3050 1.0050 0.3619 0.045 Uiso 1 1 calc R U . . .
H23B H 0.2370 1.0096 0.2832 0.045 Uiso 1 1 calc R U . . .
H23C H 0.3364 1.0012 0.2731 0.045 Uiso 1 1 calc R U . . .
C24 C -0.0179(2) 0.6937(3) 0.1670(2) 0.0320(7) Uani 1 1 d . . . . .
H24A H -0.0483 0.7349 0.1940 0.048 Uiso 1 1 calc R U . . .
H24B H -0.0477 0.6307 0.1737 0.048 Uiso 1 1 calc R U . . .
H24C H -0.0269 0.6862 0.1057 0.048 Uiso 1 1 calc R U . . .
C25 C 0.5847(2) 0.7073(2) 0.31553(19) 0.0222(6) Uani 1 1 d . . . . .
C26 C 0.6375(2) 0.6535(2) 0.3152(2) 0.0241(6) Uani 1 1 d . . . . .
H26 H 0.6052 0.5858 0.2997 0.029 Uiso 1 1 calc R U . . .
C27 C 0.7385(2) 0.6968(2) 0.33747(18) 0.0206(6) Uani 1 1 d . . . . .
C28 C 0.7890(2) 0.8008(2) 0.36341(18) 0.0216(6) Uani 1 1 d . . . . .
C29 C 0.7345(2) 0.8553(2) 0.36489(18) 0.0219(6) Uani 1 1 d . . . . .
H29 H 0.7668 0.9231 0.3817 0.026 Uiso 1 1 calc R U . . .
C30 C 0.6337(2) 0.8127(2) 0.34229(18) 0.0204(6) Uani 1 1 d . . . . .
C31 C 0.8860(2) 0.6885(2) 0.35990(19) 0.0221(6) Uani 1 1 d . . . . .
C32 C 0.9385(2) 0.6290(2) 0.35740(19) 0.0223(6) Uani 1 1 d . . . . .
C33 C 1.0864(2) 0.7764(2) 0.4175(2) 0.0263(6) Uani 1 1 d . . . . .
C34 C 0.9329(2) 0.7874(2) 0.38638(19) 0.0238(6) Uani 1 1 d . . . . .
C35 C 1.0933(2) 0.6187(3) 0.3890(2) 0.0289(7) Uani 1 1 d . . . . .
H35A H 1.0913 0.6004 0.4409 0.043 Uiso 1 1 calc R U . . .
H35B H 1.1603 0.6565 0.3901 0.043 Uiso 1 1 calc R U . . .
H35C H 1.0659 0.5608 0.3380 0.043 Uiso 1 1 calc R U . . .
C36 C 1.0829(3) 0.9341(2) 0.4446(3) 0.0378(8) Uani 1 1 d . . . . .
H36A H 1.0680 0.9593 0.4992 0.057 Uiso 1 1 calc R U . . .
H36B H 1.0611 0.9598 0.4024 0.057 Uiso 1 1 calc R U . . .
H36C H 1.1527 0.9532 0.4537 0.057 Uiso 1 1 calc R U . . .
C37 C 0.7936(2) 0.4552(2) 0.12825(19) 0.0240(6) Uani 1 1 d . . . . .
H37 H 0.8197 0.4185 0.1521 0.029 Uiso 1 1 calc R U . . .
C38 C 0.8488(3) 0.4033(3) 0.0015(2) 0.0376(8) Uani 1 1 d . . . . .
H38A H 0.9062 0.4491 -0.0079 0.056 Uiso 1 1 calc R U . . .
H38B H 0.8048 0.3595 -0.0541 0.056 Uiso 1 1 calc R U . . .
H38C H 0.8679 0.3664 0.0337 0.056 Uiso 1 1 calc R U . . .
C39 C 0.7644(4) 0.5104(4) 0.0096(3) 0.0489(11) Uani 1 1 d . . . . .
H39A H 0.7413 0.5488 0.0508 0.073 Uiso 1 1 calc R U . . .
H39B H 0.7112 0.4670 -0.0407 0.073 Uiso 1 1 calc R U . . .
H39C H 0.8163 0.5530 -0.0086 0.073 Uiso 1 1 calc R U . . .
C40 C 0.6848(3) 0.4925(2) 0.4567(2) 0.0286(7) Uani 1 1 d . . . . .
H40 H 0.6233 0.4761 0.4217 0.034 Uiso 1 1 calc R U . . .
C41 C 0.6094(3) 0.4865(3) 0.5778(2) 0.0406(9) Uani 1 1 d . . . . .
H41A H 0.5524 0.4751 0.5352 0.061 Uiso 1 1 calc R U . . .
H41B H 0.6212 0.5412 0.6286 0.061 Uiso 1 1 calc R U . . .
H41C H 0.5983 0.4294 0.5946 0.061 Uiso 1 1 calc R U . . .
C42 C 0.7858(3) 0.5348(3) 0.5975(2) 0.0414(9) Uani 1 1 d . . . . .
H42A H 0.7836 0.4832 0.6204 0.062 Uiso 1 1 calc R U . . .
H42B H 0.8004 0.5935 0.6451 0.062 Uiso 1 1 calc R U . . .
H42C H 0.8359 0.5462 0.5653 0.062 Uiso 1 1 calc R U . . .
C43 C 0.2821(3) 0.2873(3) 0.0106(2) 0.0282(7) Uani 1 1 d . . . . .
H43 H 0.3278 0.3392 0.0586 0.034 Uiso 1 1 calc R U . . .
C44 C 0.2269(3) 0.2088(4) -0.1429(3) 0.0537(12) Uani 1 1 d . . . . .
H44A H 0.1734 0.1667 -0.1259 0.081 Uiso 1 1 calc R U . . .
H44B H 0.2599 0.1718 -0.1722 0.081 Uiso 1 1 calc R U . . .
H44C H 0.2018 0.2363 -0.1819 0.081 Uiso 1 1 calc R U . . .
C45 C 0.3748(3) 0.3601(3) -0.0815(3) 0.0462(10) Uani 1 1 d . . . . .
H45A H 0.4147 0.4081 -0.0259 0.069 Uiso 1 1 calc R U . . .
H45B H 0.3496 0.3909 -0.1169 0.069 Uiso 1 1 calc R U . . .
H45C H 0.4140 0.3314 -0.1111 0.069 Uiso 1 1 calc R U . . .
C46 C 0.2722(3) 0.2413(2) 0.3247(2) 0.0289(7) Uani 1 1 d . . . . .
H46 H 0.3301 0.2738 0.3099 0.035 Uiso 1 1 calc R U . . .
C47 C 0.1956(3) 0.1803(5) 0.4267(3) 0.0760(19) Uani 1 1 d . . . . .
H47A H 0.1742 0.2282 0.4574 0.114 Uiso 1 1 calc R U . . .
H47B H 0.2105 0.1471 0.4651 0.114 Uiso 1 1 calc R U . . .
H47C H 0.1442 0.1337 0.3762 0.114 Uiso 1 1 calc R U . . .
C48 C 0.3731(3) 0.2587(4) 0.4577(3) 0.0572(13) Uani 1 1 d . . . . .
H48A H 0.4247 0.2846 0.4300 0.086 Uiso 1 1 calc R U . . .
H48B H 0.3783 0.2043 0.4723 0.086 Uiso 1 1 calc R U . . .
H48C H 0.3792 0.3087 0.5103 0.086 Uiso 1 1 calc R U . . .
C49 C 0.5094(2) 0.8194(2) 0.1550(2) 0.0253(6) Uani 1 1 d . . . . .
H49 H 0.5504 0.8766 0.2007 0.030 Uiso 1 1 calc R U . . .
C50 C 0.4611(3) 0.7256(3) 0.0024(2) 0.0379(8) Uani 1 1 d . . . . .
H50A H 0.4227 0.6753 0.0233 0.057 Uiso 1 1 calc R U . . .
H50B H 0.5014 0.7029 -0.0310 0.057 Uiso 1 1 calc R U . . .
H50C H 0.4180 0.7412 -0.0340 0.057 Uiso 1 1 calc R U . . .
C51 C 0.5924(3) 0.8901(3) 0.0580(3) 0.0433(9) Uani 1 1 d . . . . .
H51A H 0.6311 0.9415 0.1122 0.065 Uiso 1 1 calc R U . . .
H51B H 0.5585 0.9146 0.0223 0.065 Uiso 1 1 calc R U . . .
H51C H 0.6348 0.8675 0.0274 0.065 Uiso 1 1 calc R U . . .
C52 C 0.4363(2) 0.8365(2) 0.4830(2) 0.0247(6) Uani 1 1 d . . . . .
H52 H 0.4689 0.8980 0.4785 0.030 Uiso 1 1 calc R U . . .
C53 C 0.3670(4) 0.7389(3) 0.5664(3) 0.0553(13) Uani 1 1 d . . . . .
H53A H 0.3477 0.6886 0.5104 0.083 Uiso 1 1 calc R U . . .
H53B H 0.3095 0.7381 0.5869 0.083 Uiso 1 1 calc R U . . .
H53C H 0.4090 0.7273 0.6078 0.083 Uiso 1 1 calc R U . . .
C54 C 0.4454(3) 0.9161(3) 0.6327(2) 0.0379(8) Uani 1 1 d . . . . .
H54A H 0.4838 0.9733 0.6199 0.057 Uiso 1 1 calc R U . . .
H54B H 0.4835 0.9107 0.6815 0.057 Uiso 1 1 calc R U . . .
H54C H 0.3870 0.9215 0.6471 0.057 Uiso 1 1 calc R U . . .
C55 C 0.0045(3) 0.7397(3) 0.6354(3) 0.0541(11) Uani 1 1 d . . . . .
H55 H -0.0400 0.7476 0.6686 0.065 Uiso 1 1 calc R U . . .
C56 C 0.1435(5) 0.7016(5) 0.6242(4) 0.086(2) Uani 1 1 d . . . . .
H56A H 0.1298 0.6334 0.6000 0.129 Uiso 1 1 calc R U . . .
H56B H 0.2069 0.7351 0.6651 0.129 Uiso 1 1 calc R U . . .
H56C H 0.1436 0.7290 0.5777 0.129 Uiso 1 1 calc R U . . .
C57 C 0.0779(4) 0.6982(4) 0.7508(4) 0.0638(14) Uani 1 1 d . . . . .
H57A H 0.1399 0.7454 0.7896 0.096 Uiso 1 1 calc R U . . .
H57B H 0.0738 0.6334 0.7438 0.096 Uiso 1 1 calc R U . . .
H57C H 0.0252 0.7065 0.7750 0.096 Uiso 1 1 calc R U . . .
C58 C 0.1899(3) 0.9432(3) 0.7388(3) 0.0540(11) Uani 1 1 d . . . . .
H58 H 0.1820 0.9450 0.6817 0.065 Uiso 1 1 calc R U . . .
C59 C 0.0414(4) 0.9673(4) 0.7408(3) 0.0622(13) Uani 1 1 d . . . . .
H59A H 0.0424 0.9612 0.6807 0.093 Uiso 1 1 calc R U . . .
H59B H 0.0453 1.0311 0.7712 0.093 Uiso 1 1 calc R U . . .
H59C H -0.0186 0.9183 0.7431 0.093 Uiso 1 1 calc R U . . .
C60 C 0.1293(4) 0.9519(4) 0.8684(3) 0.0638(13) Uani 1 1 d . . . . .
H60A H 0.1817 0.9336 0.8850 0.096 Uiso 1 1 calc R U . . .
H60B H 0.0682 0.9050 0.8712 0.096 Uiso 1 1 calc R U . . .
H60C H 0.1420 1.0155 0.9078 0.096 Uiso 1 1 calc R U . . .
N1 N 0.31408(18) 0.17229(17) 0.15121(15) 0.0188(5) Uani 1 1 d . . . . .
N2 N 0.42026(18) 0.05748(18) 0.13295(16) 0.0212(5) Uani 1 1 d . . . . .
N3 N 0.12425(18) -0.06523(18) 0.06480(16) 0.0220(5) Uani 1 1 d . . . . .
N4 N 0.27422(19) -0.07851(19) 0.07602(18) 0.0264(6) Uani 1 1 d . . . . .
N5 N 0.28771(18) 0.67117(18) 0.24591(15) 0.0202(5) Uani 1 1 d . . . . .
N6 N 0.08496(18) 0.58402(18) 0.18055(16) 0.0218(5) Uani 1 1 d . . . . .
N7 N 0.2313(2) 0.87673(19) 0.26802(17) 0.0243(5) Uani 1 1 d . . . . .
N8 N 0.08519(19) 0.73728(19) 0.20825(18) 0.0249(5) Uani 1 1 d . . . . .
N9 N 0.78936(18) 0.64277(18) 0.33532(16) 0.0212(5) Uani 1 1 d . . . . .
N10 N 0.88691(19) 0.84467(19) 0.38776(17) 0.0240(5) Uani 1 1 d . . . . .
N11 N 1.03692(18) 0.67600(19) 0.38575(17) 0.0243(5) Uani 1 1 d . . . . .
N12 N 1.03365(19) 0.82930(19) 0.41271(17) 0.0259(6) Uani 1 1 d . . . . .
N13 N 0.8006(2) 0.4547(2) 0.05002(17) 0.0258(6) Uani 1 1 d . . . . .
N14 N 0.6930(2) 0.5073(2) 0.54067(17) 0.0291(6) Uani 1 1 d . . . . .
N15 N 0.2940(2) 0.2850(2) -0.06746(19) 0.0349(7) Uani 1 1 d . . . . .
N16 N 0.2806(2) 0.2270(2) 0.39953(18) 0.0336(7) Uani 1 1 d . . . . .
N17 N 0.5227(2) 0.8114(2) 0.07592(17) 0.0287(6) Uani 1 1 d . . . . .
N18 N 0.4185(2) 0.83138(19) 0.55787(17) 0.0265(6) Uani 1 1 d . . . . .
N19 N 0.0705(3) 0.7120(3) 0.6680(2) 0.0521(9) Uani 1 1 d . . . . .
N20 N 0.1232(3) 0.9545(3) 0.7817(2) 0.0466(8) Uani 1 1 d . . . . .
O1 O 0.60522(16) 0.44989(15) 0.26536(15) 0.0272(5) Uani 1 1 d . . . . .
O2 O 0.70808(15) 0.34642(16) 0.25015(14) 0.0247(5) Uani 1 1 d . . . . .
O3 O 0.11892(15) 0.08152(15) 0.10141(13) 0.0220(4) Uani 1 1 d . . . . .
O4 O 0.13275(18) -0.21031(16) 0.03540(18) 0.0363(6) Uani 1 1 d . . . . .
O5 O 0.29028(15) 0.36545(15) 0.20233(14) 0.0249(5) Uani 1 1 d . . . . .
O6 O 0.10164(15) 0.28131(15) 0.14298(14) 0.0230(4) Uani 1 1 d . . . . .
O7 O 0.37495(16) 0.86552(15) 0.30035(14) 0.0243(4) Uani 1 1 d . . . . .
O8 O 0.08651(18) 0.88583(17) 0.23565(16) 0.0320(5) Uani 1 1 d . . . . .
O9 O 0.49115(16) 0.66981(16) 0.29424(16) 0.0288(5) Uani 1 1 d . . . . .
O10 O 0.57906(15) 0.85952(15) 0.34436(13) 0.0227(4) Uani 1 1 d . . . . .
O11 O 0.89810(15) 0.53988(16) 0.33045(14) 0.0246(5) Uani 1 1 d . . . . .
O12 O 1.17410(17) 0.81296(18) 0.44543(17) 0.0355(6) Uani 1 1 d . . . . .
O13 O 0.75539(17) 0.49988(16) 0.17297(14) 0.0266(5) Uani 1 1 d . . . . .
O14 O 0.75224(17) 0.49887(17) 0.42203(14) 0.0303(5) Uani 1 1 d . . . . .
O15 O 0.21416(16) 0.22524(16) 0.02446(14) 0.0257(5) Uani 1 1 d . . . . .
O16 O 0.19568(16) 0.21590(17) 0.27244(13) 0.0272(5) Uani 1 1 d . . . . .
O17 O 0.44656(16) 0.75640(16) 0.17197(14) 0.0269(5) Uani 1 1 d . . . . .
O18 O 0.41250(18) 0.76486(16) 0.41831(14) 0.0289(5) Uani 1 1 d . . . . .
O19 O -0.0040(3) 0.7558(3) 0.5674(2) 0.0670(10) Uani 1 1 d . . . . .
O20 O 0.2604(3) 0.9308(3) 0.7690(3) 0.0761(11) Uani 1 1 d . . . . .
O21 O 0.6547(2) 1.0053(2) 0.50407(17) 0.0351(6) Uani 1 1 d . . . . .
O22 O 0.5205(3) 0.5045(3) 0.8660(2) 0.0623(9) Uani 1 1 d . . . . .
Ni1 Ni 0.74696(3) 0.49289(3) 0.29496(2) 0.02067(9) Uani 1 1 d . . . . .
Ni2 Ni 0.20567(3) 0.22791(3) 0.15005(2) 0.01835(9) Uani 1 1 d . . . . .
Ni3 Ni 0.43498(3) 0.76451(3) 0.29785(2) 0.01963(9) Uani 1 1 d . . . . .
H3W H 0.4811 0.5204 0.8380 0.050 Uiso 1 1 d . . . . .
H4W H 0.5179 0.4523 0.8308 0.050 Uiso 1 1 d . . . . .
H1W H 0.637(4) 0.970(4) 0.449(3) 0.059(15) Uiso 1 1 d . . . . .
H2W H 0.708(4) 1.057(4) 0.506(3) 0.072(17) 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
C1 O1 1.297(4) . ?
C1 C2 1.363(4) . ?
C1 C6 1.482(4) . ?
C2 C3 1.403(4) . ?
C2 H2 0.9500 . ?
C3 N1 1.341(4) . ?
C3 C4 1.464(4) . ?
C4 N2 1.366(4) . ?
C4 C5 1.397(4) . ?
C5 C6 1.396(4) . ?
C5 H5 0.9500 . ?
C6 O2 1.295(4) . ?
C7 N1 1.348(4) . ?
C7 C10 1.387(4) . ?
C7 C8 1.439(4) . ?
C8 O3 1.246(4) . ?
C8 N3 1.366(4) . ?
C9 O4 1.215(4) . ?
C9 N4 1.376(4) . ?
C9 N3 1.402(4) . ?
C10 N2 1.326(4) . ?
C10 N4 1.393(4) . ?
C11 N3 1.472(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N4 1.463(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O5 1.299(4) . ?
C13 C14 1.367(4) . ?
C13 C18 1.475(4) . ?
C14 C15 1.404(4) . ?
C14 H14 0.9500 . ?
C15 N5 1.342(4) . ?
C15 C16 1.460(4) . ?
C16 N6 1.363(4) . ?
C16 C17 1.397(4) . ?
C17 C18 1.408(4) . ?
C17 H17 0.9500 . ?
C18 O6 1.288(4) . ?
C19 N5 1.354(4) . ?
C19 C22 1.393(4) . ?
C19 C20 1.434(4) . ?
C20 O7 1.245(4) . ?
C20 N7 1.369(4) . ?
C21 O8 1.216(4) . ?
C21 N8 1.377(4) . ?
C21 N7 1.401(4) . ?
C22 N6 1.331(4) . ?
C22 N8 1.395(4) . ?
C23 N7 1.470(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N8 1.462(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 O9 1.297(4) . ?
C25 C26 1.369(4) . ?
C25 C30 1.474(4) . ?
C26 C27 1.400(4) . ?
C26 H26 0.9500 . ?
C27 N9 1.345(4) . ?
C27 C28 1.459(4) . ?
C28 N10 1.360(4) . ?
C28 C29 1.397(4) . ?
C29 C30 1.398(4) . ?
C29 H29 0.9500 . ?
C30 O10 1.300(4) . ?
C31 N9 1.344(4) . ?
C31 C34 1.384(4) . ?
C31 C32 1.438(4) . ?
C32 O11 1.244(4) . ?
C32 N11 1.371(4) . ?
C33 O12 1.225(4) . ?
C33 N12 1.365(4) . ?
C33 N11 1.406(4) . ?
C34 N10 1.331(4) . ?
C34 N12 1.398(4) . ?
C35 N11 1.466(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 N12 1.464(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 O13 1.235(4) . ?
C37 N13 1.315(4) . ?
C37 H37 0.9500 . ?
C38 N13 1.446(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 N13 1.451(4) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 O14 1.230(4) . ?
C40 N14 1.333(4) . ?
C40 H40 0.9500 . ?
C41 N14 1.459(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 N14 1.450(5) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 O15 1.243(4) . ?
C43 N15 1.325(4) . ?
C43 H43 0.9500 . ?
C44 N15 1.441(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 N15 1.470(5) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 O16 1.230(4) . ?
C46 N16 1.319(4) . ?
C46 H46 0.9500 . ?
C47 N16 1.441(5) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 N16 1.444(5) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 O17 1.236(4) . ?
C49 N17 1.334(4) . ?
C49 H49 0.9500 . ?
C50 N17 1.466(5) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 N17 1.449(5) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 O18 1.241(4) . ?
C52 N18 1.322(4) . ?
C52 H52 0.9500 . ?
C53 N18 1.448(5) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 N18 1.454(4) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 O19 1.222(6) . ?
C55 N19 1.347(6) . ?
C55 H55 0.9500 . ?
C56 N19 1.442(6) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 N19 1.445(6) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 O20 1.234(6) . ?
C58 N20 1.352(6) . ?
C58 H58 0.9500 . ?
C59 N20 1.454(6) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 N20 1.443(6) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
N1 Ni2 2.141(2) . ?
N5 Ni3 2.114(3) . ?
N9 Ni1 2.111(3) . ?
O1 Ni1 1.978(2) . ?
O2 Ni1 2.069(2) . ?
O3 Ni2 2.081(2) . ?
O5 Ni2 1.969(2) . ?
O6 Ni2 2.059(2) . ?
O7 Ni3 2.106(2) . ?
O9 Ni3 1.971(2) . ?
O10 Ni3 2.076(2) . ?
O11 Ni1 2.110(2) . ?
O13 Ni1 2.075(2) . ?
O14 Ni1 2.077(2) . ?
O15 Ni2 2.096(2) . ?
O16 Ni2 2.109(2) . ?
O17 Ni3 2.094(2) . ?
O18 Ni3 2.070(2) . ?
O21 H1W 0.88(5) . ?
O21 H2W 0.91(6) . ?
O22 H3W 0.8627 . ?
O22 H4W 0.8627 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 122.9(3) . . ?
O1 C1 C6 116.6(3) . . ?
C2 C1 C6 120.5(3) . . ?
C1 C2 C3 120.9(3) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
N1 C3 C2 120.3(3) . . ?
N1 C3 C4 120.1(3) . . ?
C2 C3 C4 119.6(3) . . ?
N2 C4 C5 120.2(3) . . ?
N2 C4 C3 120.5(3) . . ?
C5 C4 C3 119.4(3) . . ?
C6 C5 C4 121.1(3) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
O2 C6 C5 125.1(3) . . ?
O2 C6 C1 116.4(3) . . ?
C5 C6 C1 118.5(3) . . ?
N1 C7 C10 121.5(3) . . ?
N1 C7 C8 116.7(3) . . ?
C10 C7 C8 121.7(3) . . ?
O3 C8 N3 121.3(3) . . ?
O3 C8 C7 122.1(3) . . ?
N3 C8 C7 116.5(3) . . ?
O4 C9 N4 122.3(3) . . ?
O4 C9 N3 120.6(3) . . ?
N4 C9 N3 117.1(3) . . ?
N2 C10 C7 123.7(3) . . ?
N2 C10 N4 118.8(3) . . ?
C7 C10 N4 117.5(3) . . ?
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 . . ?
N4 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O5 C13 C14 123.1(3) . . ?
O5 C13 C18 116.4(3) . . ?
C14 C13 C18 120.5(3) . . ?
C13 C14 C15 120.7(3) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
N5 C15 C14 119.9(3) . . ?
N5 C15 C16 120.0(3) . . ?
C14 C15 C16 120.1(3) . . ?
N6 C16 C17 120.0(3) . . ?
N6 C16 C15 121.0(3) . . ?
C17 C16 C15 119.1(3) . . ?
C16 C17 C18 121.0(3) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
O6 C18 C17 124.6(3) . . ?
O6 C18 C13 116.7(3) . . ?
C17 C18 C13 118.7(3) . . ?
N5 C19 C22 121.8(3) . . ?
N5 C19 C20 116.6(3) . . ?
C22 C19 C20 121.6(3) . . ?
O7 C20 N7 121.2(3) . . ?
O7 C20 C19 122.4(3) . . ?
N7 C20 C19 116.3(3) . . ?
O8 C21 N8 121.9(3) . . ?
O8 C21 N7 121.0(3) . . ?
N8 C21 N7 117.1(3) . . ?
N6 C22 C19 123.0(3) . . ?
N6 C22 N8 118.9(3) . . ?
C19 C22 N8 118.0(3) . . ?
N7 C23 H23A 109.5 . . ?
N7 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N7 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N8 C24 H24A 109.5 . . ?
N8 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N8 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O9 C25 C26 122.8(3) . . ?
O9 C25 C30 117.0(3) . . ?
C26 C25 C30 120.2(3) . . ?
C25 C26 C27 121.0(3) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
N9 C27 C26 120.3(3) . . ?
N9 C27 C28 119.7(3) . . ?
C26 C27 C28 120.0(3) . . ?
N10 C28 C29 120.2(3) . . ?
N10 C28 C27 121.1(3) . . ?
C29 C28 C27 118.6(3) . . ?
C28 C29 C30 121.7(3) . . ?
C28 C29 H29 119.1 . . ?
C30 C29 H29 119.1 . . ?
O10 C30 C29 124.6(3) . . ?
O10 C30 C25 117.0(3) . . ?
C29 C30 C25 118.4(3) . . ?
N9 C31 C34 122.1(3) . . ?
N9 C31 C32 116.3(3) . . ?
C34 C31 C32 121.5(3) . . ?
O11 C32 N11 121.1(3) . . ?
O11 C32 C31 122.7(3) . . ?
N11 C32 C31 116.2(3) . . ?
O12 C33 N12 122.7(3) . . ?
O12 C33 N11 119.7(3) . . ?
N12 C33 N11 117.6(3) . . ?
N10 C34 C31 123.3(3) . . ?
N10 C34 N12 118.4(3) . . ?
C31 C34 N12 118.4(3) . . ?
N11 C35 H35A 109.5 . . ?
N11 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N11 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N12 C36 H36A 109.5 . . ?
N12 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N12 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O13 C37 N13 124.7(3) . . ?
O13 C37 H37 117.7 . . ?
N13 C37 H37 117.7 . . ?
N13 C38 H38A 109.5 . . ?
N13 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N13 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N13 C39 H39A 109.5 . . ?
N13 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N13 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O14 C40 N14 123.9(3) . . ?
O14 C40 H40 118.1 . . ?
N14 C40 H40 118.1 . . ?
N14 C41 H41A 109.5 . . ?
N14 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N14 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N14 C42 H42A 109.5 . . ?
N14 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N14 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O15 C43 N15 123.4(3) . . ?
O15 C43 H43 118.3 . . ?
N15 C43 H43 118.3 . . ?
N15 C44 H44A 109.5 . . ?
N15 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N15 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N15 C45 H45A 109.5 . . ?
N15 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N15 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O16 C46 N16 125.3(3) . . ?
O16 C46 H46 117.3 . . ?
N16 C46 H46 117.3 . . ?
N16 C47 H47A 109.5 . . ?
N16 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N16 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N16 C48 H48A 109.5 . . ?
N16 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N16 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O17 C49 N17 123.5(3) . . ?
O17 C49 H49 118.3 . . ?
N17 C49 H49 118.3 . . ?
N17 C50 H50A 109.5 . . ?
N17 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
N17 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N17 C51 H51A 109.5 . . ?
N17 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N17 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O18 C52 N18 123.2(3) . . ?
O18 C52 H52 118.4 . . ?
N18 C52 H52 118.4 . . ?
N18 C53 H53A 109.5 . . ?
N18 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
N18 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N18 C54 H54A 109.5 . . ?
N18 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
N18 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O19 C55 N19 126.7(5) . . ?
O19 C55 H55 116.7 . . ?
N19 C55 H55 116.7 . . ?
N19 C56 H56A 109.5 . . ?
N19 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
N19 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N19 C57 H57A 109.5 . . ?
N19 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
N19 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O20 C58 N20 124.3(5) . . ?
O20 C58 H58 117.8 . . ?
N20 C58 H58 117.8 . . ?
N20 C59 H59A 109.5 . . ?
N20 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
N20 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N20 C60 H60A 109.5 . . ?
N20 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
N20 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C3 N1 C7 117.8(2) . . ?
C3 N1 Ni2 133.0(2) . . ?
C7 N1 Ni2 109.15(19) . . ?
C10 N2 C4 116.4(3) . . ?
C8 N3 C9 123.7(3) . . ?
C8 N3 C11 119.6(2) . . ?
C9 N3 C11 116.6(2) . . ?
C9 N4 C10 123.1(3) . . ?
C9 N4 C12 116.9(3) . . ?
C10 N4 C12 119.9(3) . . ?
C15 N5 C19 117.7(3) . . ?
C15 N5 Ni3 132.5(2) . . ?
C19 N5 Ni3 109.87(19) . . ?
C22 N6 C16 116.6(3) . . ?
C20 N7 C21 124.2(3) . . ?
C20 N7 C23 117.7(3) . . ?
C21 N7 C23 118.1(3) . . ?
C21 N8 C22 122.8(3) . . ?
C21 N8 C24 117.5(3) . . ?
C22 N8 C24 119.4(3) . . ?
C31 N9 C27 117.5(3) . . ?
C31 N9 Ni1 110.3(2) . . ?
C27 N9 Ni1 132.1(2) . . ?
C34 N10 C28 116.2(3) . . ?
C32 N11 C33 123.6(3) . . ?
C32 N11 C35 118.3(3) . . ?
C33 N11 C35 118.0(3) . . ?
C33 N12 C34 122.3(3) . . ?
C33 N12 C36 119.1(3) . . ?
C34 N12 C36 118.3(3) . . ?
C37 N13 C38 122.3(3) . . ?
C37 N13 C39 121.2(3) . . ?
C38 N13 C39 116.4(3) . . ?
C40 N14 C42 120.4(3) . . ?
C40 N14 C41 122.3(3) . . ?
C42 N14 C41 117.0(3) . . ?
C43 N15 C44 121.1(3) . . ?
C43 N15 C45 122.0(3) . . ?
C44 N15 C45 116.9(3) . . ?
C46 N16 C47 120.1(3) . . ?
C46 N16 C48 122.3(3) . . ?
C47 N16 C48 117.6(3) . . ?
C49 N17 C51 121.5(3) . . ?
C49 N17 C50 120.9(3) . . ?
C51 N17 C50 117.4(3) . . ?
C52 N18 C53 119.8(3) . . ?
C52 N18 C54 122.5(3) . . ?
C53 N18 C54 117.6(3) . . ?
C55 N19 C56 121.1(4) . . ?
C55 N19 C57 123.1(4) . . ?
C56 N19 C57 115.7(4) . . ?
C58 N20 C60 121.4(4) . . ?
C58 N20 C59 120.8(4) . . ?
C60 N20 C59 117.8(4) . . ?
C1 O1 Ni1 114.19(19) . . ?
C6 O2 Ni1 111.39(18) . . ?
C8 O3 Ni2 112.02(19) . . ?
C13 O5 Ni2 113.45(19) . . ?
C18 O6 Ni2 110.74(19) . . ?
C20 O7 Ni3 111.02(19) . . ?
C25 O9 Ni3 113.74(19) . . ?
C30 O10 Ni3 110.17(18) . . ?
C32 O11 Ni1 110.70(19) . . ?
C37 O13 Ni1 120.9(2) . . ?
C40 O14 Ni1 125.1(2) . . ?
C43 O15 Ni2 121.3(2) . . ?
C46 O16 Ni2 116.5(2) . . ?
C49 O17 Ni3 122.9(2) . . ?
C52 O18 Ni3 126.5(2) . . ?
H1W O21 H2W 102(4) . . ?
H3W O22 H4W 105.4 . . ?
O1 Ni1 O2 81.37(9) . . ?
O1 Ni1 O13 91.81(10) . . ?
O2 Ni1 O13 90.61(9) . . ?
O1 Ni1 O14 93.05(10) . . ?
O2 Ni1 O14 93.78(9) . . ?
O13 Ni1 O14 173.89(10) . . ?
O1 Ni1 O11 178.29(9) . . ?
O2 Ni1 O11 99.14(8) . . ?
O13 Ni1 O11 89.82(9) . . ?
O14 Ni1 O11 85.29(9) . . ?
O1 Ni1 N9 99.64(9) . . ?
O2 Ni1 N9 177.19(9) . . ?
O13 Ni1 N9 86.74(9) . . ?
O14 Ni1 N9 88.80(9) . . ?
O11 Ni1 N9 79.92(9) . . ?
O5 Ni2 O6 81.56(9) . . ?
O5 Ni2 O3 176.71(9) . . ?
O6 Ni2 O3 100.01(8) . . ?
O5 Ni2 O15 94.05(9) . . ?
O6 Ni2 O15 90.16(9) . . ?
O3 Ni2 O15 88.85(9) . . ?
O5 Ni2 O16 90.97(9) . . ?
O6 Ni2 O16 93.62(9) . . ?
O3 Ni2 O16 86.05(9) . . ?
O15 Ni2 O16 174.11(9) . . ?
O5 Ni2 N1 98.64(9) . . ?
O6 Ni2 N1 177.24(9) . . ?
O3 Ni2 N1 79.93(9) . . ?
O15 Ni2 N1 87.08(9) . . ?
O16 Ni2 N1 89.13(9) . . ?
O9 Ni3 O18 90.57(10) . . ?
O9 Ni3 O10 81.87(9) . . ?
O18 Ni3 O10 94.44(9) . . ?
O9 Ni3 O17 89.92(10) . . ?
O18 Ni3 O17 175.54(9) . . ?
O10 Ni3 O17 90.01(9) . . ?
O9 Ni3 O7 179.40(9) . . ?
O18 Ni3 O7 90.02(9) . . ?
O10 Ni3 O7 98.19(8) . . ?
O17 Ni3 O7 89.49(9) . . ?
O9 Ni3 N5 99.89(9) . . ?
O18 Ni3 N5 87.81(9) . . ?
O10 Ni3 N5 177.14(9) . . ?
O17 Ni3 N5 87.74(9) . . ?
O7 Ni3 N5 80.03(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
O1 C1 C2 C3 178.6(3) . . . . ?
C6 C1 C2 C3 -0.6(4) . . . . ?
C1 C2 C3 N1 -179.8(3) . . . . ?
C1 C2 C3 C4 0.8(4) . . . . ?
N1 C3 C4 N2 0.1(4) . . . . ?
C2 C3 C4 N2 179.5(3) . . . . ?
N1 C3 C4 C5 179.9(3) . . . . ?
C2 C3 C4 C5 -0.7(4) . . . . ?
N2 C4 C5 C6 -179.9(3) . . . . ?
C3 C4 C5 C6 0.3(4) . . . . ?
C4 C5 C6 O2 -179.6(3) . . . . ?
C4 C5 C6 C1 0.0(4) . . . . ?
O1 C1 C6 O2 0.6(4) . . . . ?
C2 C1 C6 O2 179.8(3) . . . . ?
O1 C1 C6 C5 -179.0(3) . . . . ?
C2 C1 C6 C5 0.2(4) . . . . ?
N1 C7 C8 O3 2.2(4) . . . . ?
C10 C7 C8 O3 -179.3(3) . . . . ?
N1 C7 C8 N3 -177.1(2) . . . . ?
C10 C7 C8 N3 1.4(4) . . . . ?
N1 C7 C10 N2 0.7(5) . . . . ?
C8 C7 C10 N2 -177.8(3) . . . . ?
N1 C7 C10 N4 179.0(3) . . . . ?
C8 C7 C10 N4 0.5(4) . . . . ?
O5 C13 C14 C15 -176.7(3) . . . . ?
C18 C13 C14 C15 1.5(4) . . . . ?
C13 C14 C15 N5 178.0(3) . . . . ?
C13 C14 C15 C16 -2.0(4) . . . . ?
N5 C15 C16 N6 0.2(4) . . . . ?
C14 C15 C16 N6 -179.8(3) . . . . ?
N5 C15 C16 C17 -179.5(3) . . . . ?
C14 C15 C16 C17 0.4(4) . . . . ?
N6 C16 C17 C18 -178.1(3) . . . . ?
C15 C16 C17 C18 1.7(4) . . . . ?
C16 C17 C18 O6 176.3(3) . . . . ?
C16 C17 C18 C13 -2.2(4) . . . . ?
O5 C13 C18 O6 0.3(4) . . . . ?
C14 C13 C18 O6 -178.0(3) . . . . ?
O5 C13 C18 C17 178.9(3) . . . . ?
C14 C13 C18 C17 0.6(4) . . . . ?
N5 C19 C20 O7 0.8(4) . . . . ?
C22 C19 C20 O7 -178.4(3) . . . . ?
N5 C19 C20 N7 179.7(2) . . . . ?
C22 C19 C20 N7 0.4(4) . . . . ?
N5 C19 C22 N6 0.8(4) . . . . ?
C20 C19 C22 N6 -180.0(3) . . . . ?
N5 C19 C22 N8 179.5(3) . . . . ?
C20 C19 C22 N8 -1.3(4) . . . . ?
O9 C25 C26 C27 179.1(3) . . . . ?
C30 C25 C26 C27 -2.1(4) . . . . ?
C25 C26 C27 N9 -178.8(3) . . . . ?
C25 C26 C27 C28 1.5(4) . . . . ?
N9 C27 C28 N10 -1.7(4) . . . . ?
C26 C27 C28 N10 178.0(3) . . . . ?
N9 C27 C28 C29 179.8(3) . . . . ?
C26 C27 C28 C29 -0.4(4) . . . . ?
N10 C28 C29 C30 -178.4(3) . . . . ?
C27 C28 C29 C30 0.0(4) . . . . ?
C28 C29 C30 O10 178.3(3) . . . . ?
C28 C29 C30 C25 -0.6(4) . . . . ?
O9 C25 C30 O10 1.6(4) . . . . ?
C26 C25 C30 O10 -177.3(3) . . . . ?
O9 C25 C30 C29 -179.4(3) . . . . ?
C26 C25 C30 C29 1.7(4) . . . . ?
N9 C31 C32 O11 3.2(4) . . . . ?
C34 C31 C32 O11 -176.9(3) . . . . ?
N9 C31 C32 N11 -177.5(3) . . . . ?
C34 C31 C32 N11 2.4(4) . . . . ?
N9 C31 C34 N10 -1.6(5) . . . . ?
C32 C31 C34 N10 178.5(3) . . . . ?
N9 C31 C34 N12 178.6(3) . . . . ?
C32 C31 C34 N12 -1.3(4) . . . . ?
C2 C3 N1 C7 -179.9(3) . . . . ?
C4 C3 N1 C7 -0.5(4) . . . . ?
C2 C3 N1 Ni2 2.2(4) . . . . ?
C4 C3 N1 Ni2 -178.45(19) . . . . ?
C10 C7 N1 C3 0.2(4) . . . . ?
C8 C7 N1 C3 178.8(2) . . . . ?
C10 C7 N1 Ni2 178.6(2) . . . . ?
C8 C7 N1 Ni2 -2.9(3) . . . . ?
C7 C10 N2 C4 -1.1(4) . . . . ?
N4 C10 N2 C4 -179.3(3) . . . . ?
C5 C4 N2 C10 -179.1(3) . . . . ?
C3 C4 N2 C10 0.7(4) . . . . ?
O3 C8 N3 C9 -178.6(3) . . . . ?
C7 C8 N3 C9 0.7(4) . . . . ?
O3 C8 N3 C11 -1.7(4) . . . . ?
C7 C8 N3 C11 177.6(3) . . . . ?
O4 C9 N3 C8 175.6(3) . . . . ?
N4 C9 N3 C8 -4.6(5) . . . . ?
O4 C9 N3 C11 -1.5(5) . . . . ?
N4 C9 N3 C11 178.4(3) . . . . ?
O4 C9 N4 C10 -173.5(3) . . . . ?
N3 C9 N4 C10 6.7(5) . . . . ?
O4 C9 N4 C12 4.5(5) . . . . ?
N3 C9 N4 C12 -175.3(3) . . . . ?
N2 C10 N4 C9 173.7(3) . . . . ?
C7 C10 N4 C9 -4.7(4) . . . . ?
N2 C10 N4 C12 -4.3(4) . . . . ?
C7 C10 N4 C12 177.3(3) . . . . ?
C14 C15 N5 C19 -179.3(3) . . . . ?
C16 C15 N5 C19 0.7(4) . . . . ?
C14 C15 N5 Ni3 0.2(4) . . . . ?
C16 C15 N5 Ni3 -179.8(2) . . . . ?
C22 C19 N5 C15 -1.3(4) . . . . ?
C20 C19 N5 C15 179.5(3) . . . . ?
C22 C19 N5 Ni3 179.2(2) . . . . ?
C20 C19 N5 Ni3 -0.1(3) . . . . ?
C19 C22 N6 C16 0.1(4) . . . . ?
N8 C22 N6 C16 -178.5(3) . . . . ?
C17 C16 N6 C22 179.1(3) . . . . ?
C15 C16 N6 C22 -0.7(4) . . . . ?
O7 C20 N7 C21 179.6(3) . . . . ?
C19 C20 N7 C21 0.7(4) . . . . ?
O7 C20 N7 C23 -1.5(4) . . . . ?
C19 C20 N7 C23 179.7(3) . . . . ?
O8 C21 N7 C20 179.1(3) . . . . ?
N8 C21 N7 C20 -1.0(4) . . . . ?
O8 C21 N7 C23 0.1(4) . . . . ?
N8 C21 N7 C23 -179.9(3) . . . . ?
O8 C21 N8 C22 -180.0(3) . . . . ?
N7 C21 N8 C22 0.1(4) . . . . ?
O8 C21 N8 C24 6.6(4) . . . . ?
N7 C21 N8 C24 -173.4(3) . . . . ?
N6 C22 N8 C21 179.8(3) . . . . ?
C19 C22 N8 C21 1.0(4) . . . . ?
N6 C22 N8 C24 -6.9(4) . . . . ?
C19 C22 N8 C24 174.3(3) . . . . ?
C34 C31 N9 C27 -0.2(4) . . . . ?
C32 C31 N9 C27 179.7(3) . . . . ?
C34 C31 N9 Ni1 177.6(2) . . . . ?
C32 C31 N9 Ni1 -2.5(3) . . . . ?
C26 C27 N9 C31 -178.0(3) . . . . ?
C28 C27 N9 C31 1.8(4) . . . . ?
C26 C27 N9 Ni1 4.7(4) . . . . ?
C28 C27 N9 Ni1 -175.5(2) . . . . ?
C31 C34 N10 C28 1.6(4) . . . . ?
N12 C34 N10 C28 -178.6(3) . . . . ?
C29 C28 N10 C34 178.4(3) . . . . ?
C27 C28 N10 C34 0.0(4) . . . . ?
O11 C32 N11 C33 -179.5(3) . . . . ?
C31 C32 N11 C33 1.2(4) . . . . ?
O11 C32 N11 C35 -4.0(4) . . . . ?
C31 C32 N11 C35 176.7(3) . . . . ?
O12 C33 N11 C32 176.5(3) . . . . ?
N12 C33 N11 C32 -5.8(4) . . . . ?
O12 C33 N11 C35 1.0(4) . . . . ?
N12 C33 N11 C35 178.8(3) . . . . ?
O12 C33 N12 C34 -175.4(3) . . . . ?
N11 C33 N12 C34 6.9(4) . . . . ?
O12 C33 N12 C36 -2.0(5) . . . . ?
N11 C33 N12 C36 -179.6(3) . . . . ?
N10 C34 N12 C33 176.6(3) . . . . ?
C31 C34 N12 C33 -3.6(4) . . . . ?
N10 C34 N12 C36 3.1(4) . . . . ?
C31 C34 N12 C36 -177.1(3) . . . . ?
O13 C37 N13 C38 178.1(3) . . . . ?
O13 C37 N13 C39 1.3(5) . . . . ?
O14 C40 N14 C42 1.5(5) . . . . ?
O14 C40 N14 C41 -171.5(3) . . . . ?
O15 C43 N15 C44 0.5(5) . . . . ?
O15 C43 N15 C45 179.5(3) . . . . ?
O16 C46 N16 C47 -1.5(6) . . . . ?
O16 C46 N16 C48 179.9(4) . . . . ?
O17 C49 N17 C51 175.2(3) . . . . ?
O17 C49 N17 C50 0.8(5) . . . . ?
O18 C52 N18 C53 -1.3(5) . . . . ?
O18 C52 N18 C54 -178.9(3) . . . . ?
O19 C55 N19 C56 2.4(8) . . . . ?
O19 C55 N19 C57 177.4(5) . . . . ?
O20 C58 N20 C60 -0.6(8) . . . . ?
O20 C58 N20 C59 -179.0(5) . . . . ?
C2 C1 O1 Ni1 -179.8(2) . . . . ?
C6 C1 O1 Ni1 -0.5(3) . . . . ?
C5 C6 O2 Ni1 179.3(2) . . . . ?
C1 C6 O2 Ni1 -0.3(3) . . . . ?
N3 C8 O3 Ni2 179.2(2) . . . . ?
C7 C8 O3 Ni2 -0.1(3) . . . . ?
C14 C13 O5 Ni2 -174.2(2) . . . . ?
C18 C13 O5 Ni2 7.6(3) . . . . ?
C17 C18 O6 Ni2 173.9(2) . . . . ?
C13 C18 O6 Ni2 -7.5(3) . . . . ?
N7 C20 O7 Ni3 -179.9(2) . . . . ?
C19 C20 O7 Ni3 -1.1(3) . . . . ?
C26 C25 O9 Ni3 -178.5(2) . . . . ?
C30 C25 O9 Ni3 2.6(3) . . . . ?
C29 C30 O10 Ni3 176.5(2) . . . . ?
C25 C30 O10 Ni3 -4.6(3) . . . . ?
N11 C32 O11 Ni1 178.8(2) . . . . ?
C31 C32 O11 Ni1 -1.9(4) . . . . ?
N13 C37 O13 Ni1 179.0(2) . . . . ?
N14 C40 O14 Ni1 -172.1(2) . . . . ?
N15 C43 O15 Ni2 175.2(2) . . . . ?
N16 C46 O16 Ni2 -170.1(3) . . . . ?
N17 C49 O17 Ni3 174.0(2) . . . . ?
N18 C52 O18 Ni3 179.1(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O22 H3W O1 0.86 2.28 3.124(4) 164.7 2_666
O22 H4W O9 0.86 2.39 3.225(4) 164.2 2_666
O21 H1W O10 0.88(5) 1.95(5) 2.794(3) 161(5) .
O21 H2W O12 0.91(6) 2.06(6) 2.937(4) 161(5) 2_776

_refine_diff_density_max         2.668
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.092

