# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_p_sq
_database_code_depnum_ccdc_archive 'CCDC 1886813'
loop_
_audit_author_name
_audit_author_address
'Jie Zhang'
;North University of China
China
;
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;
_audit_creation_date             2017-09-16
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H15 N3 Ni O6'
_chemical_formula_sum            'C24 H15 N3 Ni O6'
_chemical_formula_weight         500.10
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 1 2/c 1'
_space_group_name_Hall           '-P 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   11.2448(14)
_cell_length_b                   10.0674(13)
_cell_length_c                   24.394(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.663(2)
_cell_angle_gamma                90
_cell_volume                     2755.9(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1142
_cell_measurement_temperature    293
_cell_measurement_theta_max      20.72
_cell_measurement_theta_min      2.55
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0813 before and 0.0573 after correction. The Ratio of minimum to maximum transmission is 0.8375. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1027
_diffrn_reflns_av_unetI/netI     0.1265
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14763
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.673
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2712
_reflns_number_total             5237
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5237
_refine_ls_number_restraints     177
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0569
_refine_ls_restrained_S_all      0.912
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0599P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1414
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(N3A) \\sim Ueq,
Uanis(C12A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 O5, O6, C13, N3, C14, C15, C9, C12, C11, C11A, N3A, C12A, C13A, O6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, O4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O4(0.5) H4(0.5) O6(0.5) C13(0.5) N3(0.5) H14(0.5) H14A(0.5)
 C12(0.5) C11(0.5) H11(0.5) C11A(0.5) H11A(0.5) N3A(0.5) C12A(0.5) C13A(0.5)
 O6A(0.5) H6A(0.5) O4A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C18(H18), C22(H22), C19(H19), C14(H14), C14(H14A),
 C15(H15), C16(H16), C21(H21), C24(H24), C17(H17), C25(H25), C11(H11),
 C11A(H11A)
5.b Idealised tetrahedral OH refined as rotating group:
 O4(H4), O6A(H6A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.15982(5) 0.73492(5) 0.13304(2) 0.02657(19) Uani 1 1 d . . . . .
O1 O 0.1661(3) -0.1527(3) 0.20870(12) 0.0380(8) Uani 1 1 d . . . . .
O5 O 0.1520(3) 0.2785(3) 0.54825(12) 0.0416(8) Uani 1 1 d . U . . .
O3 O 0.1608(3) 0.5535(3) 0.17120(13) 0.0360(8) Uani 1 1 d . . . . .
O2 O 0.1574(3) -0.0586(3) 0.12741(13) 0.0370(8) Uani 1 1 d . . . . .
O4 O 0.2060(11) 0.4080(13) 0.1069(5) 0.071(4) Uani 0.5 1 d . U P A 1
H4 H 0.189044 0.465772 0.084076 0.106 Uiso 0.5 1 calc GR . P A 1
O6 O 0.2273(9) 0.4745(7) 0.5231(3) 0.071(3) Uani 0.5 1 d . U P B 1
N1 N 0.3453(3) 0.7357(4) 0.13401(16) 0.0380(10) Uani 1 1 d . . . . .
N2 N 0.9756(3) 0.7372(3) 0.13121(15) 0.0322(9) Uani 1 1 d . . . . .
C23 C 0.5952(4) 0.7438(5) 0.1343(2) 0.0410(12) Uani 1 1 d . . . . .
C13 C 0.1842(12) 0.3583(16) 0.5124(7) 0.039(3) Uani 0.5 1 d . U P B 1
C2 C 0.1605(4) 0.0858(4) 0.20477(19) 0.0303(11) Uani 1 1 d . . . . .
N3 N 0.2058(9) 0.3766(9) 0.3602(4) 0.043(2) Uani 0.5 1 d . U P B 1
C3 C 0.1603(4) 0.1950(4) 0.17121(19) 0.0352(12) Uani 1 1 d . . . . .
H3 H 0.160380 0.182495 0.133440 0.042 Uiso 1 1 calc R . . . .
C7 C 0.1594(4) 0.2313(4) 0.28369(18) 0.0343(11) Uani 1 1 d . . . . .
C4 C 0.1601(4) 0.3227(4) 0.19153(19) 0.0342(12) Uani 1 1 d . . . . .
C6 C 0.1593(4) 0.3410(4) 0.24865(18) 0.0333(12) Uani 1 1 d . . . . .
H6 H 0.158739 0.426447 0.263143 0.040 Uiso 1 1 calc R . . . .
C5 C 0.1605(5) 0.4393(5) 0.1539(2) 0.0492(15) Uani 1 1 d . U . . .
C8 C 0.1601(4) 0.1032(4) 0.26129(19) 0.0329(12) Uani 1 1 d . . . . .
H8 H 0.160212 0.029569 0.284306 0.039 Uiso 1 1 calc R . . . .
C1 C 0.1615(4) -0.0500(4) 0.17858(19) 0.0254(11) Uani 1 1 d . . . . .
C18 C 0.9203(5) 0.6991(5) 0.1754(2) 0.0440(13) Uani 1 1 d . . . . .
H18 H 0.966370 0.668567 0.205854 0.053 Uiso 1 1 calc R . . . .
C22 C 0.9061(4) 0.7791(5) 0.0885(2) 0.0463(14) Uani 1 1 d . . . . .
H22 H 0.942005 0.805911 0.057063 0.056 Uiso 1 1 calc R . . . .
C19 C 0.7975(4) 0.7027(5) 0.1782(2) 0.0451(14) Uani 1 1 d . . . . .
H19 H 0.763258 0.676574 0.210194 0.054 Uiso 1 1 calc R . . . .
C20 C 0.7267(4) 0.7450(4) 0.13368(19) 0.0345(11) Uani 1 1 d . . . . .
C14 C 0.1489(5) 0.1876(5) 0.4375(2) 0.0545(16) Uani 1 1 d . U . . .
H14 H 0.127806 0.124563 0.463012 0.065 Uiso 0.5 1 calc R . P C 1
H14A H 0.159480 0.122022 0.464220 0.065 Uiso 0.5 1 calc R . P D 2
C15 C 0.1492(6) 0.1565(5) 0.3822(2) 0.0580(17) Uani 1 1 d . U . . .
H15 H 0.142403 0.068281 0.371181 0.070 Uiso 1 1 calc R . . . .
C9 C 0.1591(4) 0.2531(4) 0.34391(18) 0.0380(12) Uani 1 1 d . U . . .
C12 C 0.1803(11) 0.3132(17) 0.4535(7) 0.029(3) Uani 0.5 1 d . U P B 1
C16 C 0.4128(5) 0.6599(6) 0.1665(2) 0.0690(19) Uani 1 1 d . . . . .
H16 H 0.376004 0.602453 0.189999 0.083 Uiso 1 1 calc R . . . .
C21 C 0.7849(5) 0.7847(5) 0.0885(2) 0.0536(15) Uani 1 1 d . . . . .
H21 H 0.741025 0.815782 0.057514 0.064 Uiso 1 1 calc R . . . .
C24 C 0.5365(6) 0.6606(7) 0.1678(3) 0.083(2) Uani 1 1 d . . . . .
H24 H 0.579853 0.603989 0.191640 0.100 Uiso 1 1 calc R . . . .
C17 C 0.4004(5) 0.8137(6) 0.1015(3) 0.078(2) Uani 1 1 d . . . . .
H17 H 0.354738 0.867757 0.077514 0.094 Uiso 1 1 calc R . . . .
C25 C 0.5225(5) 0.8206(6) 0.1007(3) 0.080(2) Uani 1 1 d . . . . .
H25 H 0.556121 0.879257 0.076614 0.096 Uiso 1 1 calc R . . . .
C11 C 0.2088(11) 0.4026(11) 0.4134(4) 0.048(3) Uani 0.5 1 d . U P B 1
H11 H 0.231911 0.487557 0.424665 0.058 Uiso 0.5 1 calc R . P B 1
C11A C 0.1171(12) 0.4041(11) 0.4114(5) 0.055(3) Uani 0.5 1 d . U P B 2
H11A H 0.100675 0.491092 0.421302 0.066 Uiso 0.5 1 calc R . P B 2
N3A N 0.1233(10) 0.3775(9) 0.3580(4) 0.052(3) Uani 0.5 1 d . U P B 2
C12A C 0.1329(12) 0.3148(18) 0.4514(7) 0.033(3) Uani 0.5 1 d . U P B 2
C13A C 0.1306(12) 0.3530(16) 0.5116(7) 0.044(3) Uani 0.5 1 d . U P B 2
O6A O 0.1011(12) 0.4765(9) 0.5186(4) 0.107(4) Uani 0.5 1 d . U P B 2
H6A H 0.153976 0.514151 0.537366 0.160 Uiso 0.5 1 calc GR . P B 2
O4A O 0.1219(11) 0.4110(13) 0.1028(5) 0.084(5) Uani 0.5 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.162(3) 1_565 ?
Ni1 O5 2.069(3) 4_565 ?
Ni1 O3 2.049(3) . ?
Ni1 O2 2.084(3) 1_565 ?
Ni1 N1 2.085(4) . ?
Ni1 N2 2.070(4) 1_455 ?
Ni1 C1 2.433(4) 1_565 ?
O1 C1 1.268(5) . ?
O5 C13 1.258(15) . ?
O5 C13A 1.179(16) . ?
O3 C5 1.225(5) . ?
O2 C1 1.249(5) . ?
O4 H4 0.8200 . ?
O4 C5 1.321(12) . ?
O6 C13 1.287(16) . ?
N1 C16 1.307(6) . ?
N1 C17 1.300(6) . ?
N2 C18 1.335(5) . ?
N2 C22 1.329(5) . ?
C23 C20 1.480(6) . ?
C23 C24 1.369(7) . ?
C23 C25 1.361(7) . ?
C13 C12 1.50(2) . ?
C2 C3 1.371(6) . ?
C2 C8 1.390(6) . ?
C2 C1 1.509(5) . ?
N3 C9 1.397(10) . ?
N3 C11 1.322(13) . ?
C3 H3 0.9300 . ?
C3 C4 1.378(6) . ?
C7 C6 1.397(6) . ?
C7 C8 1.400(5) . ?
C7 C9 1.486(6) . ?
C4 C6 1.406(6) . ?
C4 C5 1.491(6) . ?
C6 H6 0.9300 . ?
C5 O4A 1.324(12) . ?
C8 H8 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.387(6) . ?
C22 H22 0.9300 . ?
C22 C21 1.364(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.373(6) . ?
C20 C21 1.377(6) . ?
C14 H14 0.9300 . ?
C14 H14A 0.9300 . ?
C14 C15 1.384(6) . ?
C14 C12 1.363(18) . ?
C14 C12A 1.340(18) . ?
C15 H15 0.9300 . ?
C15 C9 1.358(6) . ?
C9 N3A 1.367(10) . ?
C12 C11 1.383(19) . ?
C16 H16 0.9300 . ?
C16 C24 1.390(8) . ?
C21 H21 0.9300 . ?
C24 H24 0.9300 . ?
C17 H17 0.9300 . ?
C17 C25 1.376(7) . ?
C25 H25 0.9300 . ?
C11 H11 0.9300 . ?
C11A H11A 0.9300 . ?
C11A N3A 1.336(14) . ?
C11A C12A 1.33(2) . ?
C12A C13A 1.52(2) . ?
C13A O6A 1.301(17) . ?
O6A H6A 0.8200 . ?

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 C1 31.32(12) 1_565 1_565 ?
O5 Ni1 O1 152.19(12) 4_565 1_565 ?
O5 Ni1 O2 89.98(12) 4_565 1_565 ?
O5 Ni1 N1 89.44(14) 4_565 . ?
O5 Ni1 N2 90.03(14) 4_565 1_455 ?
O5 Ni1 C1 120.87(14) 4_565 1_565 ?
O3 Ni1 O1 94.56(11) . 1_565 ?
O3 Ni1 O5 113.24(12) . 4_565 ?
O3 Ni1 O2 156.73(12) . 1_565 ?
O3 Ni1 N1 91.26(14) . . ?
O3 Ni1 N2 89.77(13) . 1_455 ?
O3 Ni1 C1 125.86(13) . 1_565 ?
O2 Ni1 O1 62.21(11) 1_565 1_565 ?
O2 Ni1 N1 90.35(14) 1_565 . ?
O2 Ni1 C1 30.89(12) 1_565 1_565 ?
N1 Ni1 O1 90.59(14) . 1_565 ?
N1 Ni1 C1 90.75(15) . 1_565 ?
N2 Ni1 O1 89.46(13) 1_455 1_565 ?
N2 Ni1 O2 88.76(13) 1_455 1_565 ?
N2 Ni1 N1 178.97(15) 1_455 . ?
N2 Ni1 C1 88.75(14) 1_455 1_565 ?
C1 O1 Ni1 86.2(3) . 1_545 ?
C13 O5 Ni1 137.8(8) . 4_566 ?
C5 O3 Ni1 132.8(3) . . ?
C1 O2 Ni1 90.2(2) . 1_545 ?
C5 O4 H4 109.5 . . ?
C16 N1 Ni1 123.1(4) . . ?
C17 N1 Ni1 120.7(4) . . ?
C17 N1 C16 116.2(5) . . ?
C18 N2 Ni1 119.8(3) . 1_655 ?
C22 N2 Ni1 123.9(3) . 1_655 ?
C22 N2 C18 116.3(4) . . ?
C24 C23 C20 122.1(5) . . ?
C25 C23 C20 123.5(5) . . ?
C25 C23 C24 114.4(5) . . ?
O5 C13 O6 124.2(14) . . ?
O5 C13 C12 118.6(13) . . ?
O6 C13 C12 117.1(13) . . ?
C3 C2 C8 119.4(4) . . ?
C3 C2 C1 118.3(4) . . ?
C8 C2 C1 122.3(4) . . ?
C11 N3 C9 116.2(8) . . ?
C2 C3 H3 118.9 . . ?
C2 C3 C4 122.2(4) . . ?
C4 C3 H3 118.9 . . ?
C6 C7 C8 119.3(4) . . ?
C6 C7 C9 119.2(4) . . ?
C8 C7 C9 121.5(4) . . ?
C3 C4 C6 118.6(4) . . ?
C3 C4 C5 120.8(4) . . ?
C6 C4 C5 120.5(4) . . ?
C7 C6 C4 120.2(4) . . ?
C7 C6 H6 119.9 . . ?
C4 C6 H6 119.9 . . ?
O3 C5 O4 122.1(7) . . ?
O3 C5 C4 121.7(5) . . ?
O3 C5 O4A 121.4(7) . . ?
O4 C5 C4 111.2(7) . . ?
O4A C5 C4 113.3(7) . . ?
C2 C8 C7 120.2(4) . . ?
C2 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
O1 C1 Ni1 62.5(2) . 1_545 ?
O1 C1 C2 119.6(4) . . ?
O2 C1 Ni1 58.9(2) . 1_545 ?
O2 C1 O1 121.4(4) . . ?
O2 C1 C2 119.0(4) . . ?
C2 C1 Ni1 177.8(3) . 1_545 ?
N2 C18 H18 118.4 . . ?
N2 C18 C19 123.2(5) . . ?
C19 C18 H18 118.4 . . ?
N2 C22 H22 118.3 . . ?
N2 C22 C21 123.4(5) . . ?
C21 C22 H22 118.3 . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.9(5) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 C23 121.3(4) . . ?
C19 C20 C21 116.2(4) . . ?
C21 C20 C23 122.5(4) . . ?
C15 C14 H14 120.9 . . ?
C15 C14 H14A 120.9 . . ?
C12 C14 H14 120.9 . . ?
C12 C14 C15 118.2(8) . . ?
C12A C14 H14A 120.9 . . ?
C12A C14 C15 118.2(9) . . ?
C14 C15 H15 119.5 . . ?
C9 C15 C14 120.9(5) . . ?
C9 C15 H15 119.5 . . ?
N3 C9 C7 112.9(5) . . ?
C15 C9 N3 119.1(6) . . ?
C15 C9 C7 125.5(4) . . ?
C15 C9 N3A 116.4(6) . . ?
N3A C9 C7 113.8(6) . . ?
C14 C12 C13 123.0(14) . . ?
C14 C12 C11 118.0(14) . . ?
C11 C12 C13 119.0(14) . . ?
N1 C16 H16 118.2 . . ?
N1 C16 C24 123.5(5) . . ?
C24 C16 H16 118.2 . . ?
C22 C21 C20 120.9(5) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C23 C24 C16 120.6(5) . . ?
C23 C24 H24 119.7 . . ?
C16 C24 H24 119.7 . . ?
N1 C17 H17 118.2 . . ?
N1 C17 C25 123.7(5) . . ?
C25 C17 H17 118.2 . . ?
C23 C25 C17 121.6(5) . . ?
C23 C25 H25 119.2 . . ?
C17 C25 H25 119.2 . . ?
N3 C11 C12 124.9(12) . . ?
N3 C11 H11 117.5 . . ?
C12 C11 H11 117.5 . . ?
N3A C11A H11A 117.7 . . ?
C12A C11A H11A 117.7 . . ?
C12A C11A N3A 124.6(13) . . ?
C11A N3A C9 117.6(9) . . ?
C14 C12A C13A 119.9(14) . . ?
C11A C12A C14 118.2(15) . . ?
C11A C12A C13A 121.9(15) . . ?
O5 C13A C12A 123.8(15) . . ?
O5 C13A O6A 123.4(15) . . ?
O6A C13A C12A 112.8(14) . . ?
C13A O6A H6A 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 O1 C1 O2 -0.7(4) 1_545 . . . ?
Ni1 O1 C1 C2 179.1(4) 1_545 . . . ?
Ni1 O5 C13 O6 -8(2) 4_566 . . . ?
Ni1 O5 C13 C12 168.0(7) 4_566 . . . ?
Ni1 O5 C13A C12A -177.7(7) 4_566 . . . ?
Ni1 O5 C13A O6A 1(2) 4_566 . . . ?
Ni1 O3 C5 O4 27.7(11) . . . . ?
Ni1 O3 C5 C4 -179.3(3) . . . . ?
Ni1 O3 C5 O4A -21.9(11) . . . . ?
Ni1 O2 C1 O1 0.7(4) 1_545 . . . ?
Ni1 O2 C1 C2 -179.1(4) 1_545 . . . ?
Ni1 N1 C16 C24 -179.4(5) . . . . ?
Ni1 N1 C17 C25 178.9(5) . . . . ?
Ni1 N2 C18 C19 177.4(4) 1_655 . . . ?
Ni1 N2 C22 C21 -177.5(4) 1_655 . . . ?
O5 C13 C12 C14 -3.2(18) . . . . ?
O5 C13 C12 C11 176.2(11) . . . . ?
O6 C13 C12 C14 172.8(11) . . . . ?
O6 C13 C12 C11 -7.7(19) . . . . ?
N1 C16 C24 C23 0.4(11) . . . . ?
N1 C17 C25 C23 0.6(12) . . . . ?
N2 C18 C19 C20 1.1(7) . . . . ?
N2 C22 C21 C20 -0.7(8) . . . . ?
C23 C20 C21 C22 -177.1(5) . . . . ?
C13 C12 C11 N3 -178.1(12) . . . . ?
C2 C3 C4 C6 -0.3(7) . . . . ?
C2 C3 C4 C5 179.7(5) . . . . ?
C3 C2 C8 C7 0.0(7) . . . . ?
C3 C2 C1 O1 177.4(4) . . . . ?
C3 C2 C1 O2 -2.8(6) . . . . ?
C3 C4 C6 C7 0.3(7) . . . . ?
C3 C4 C5 O3 -179.7(5) . . . . ?
C3 C4 C5 O4 -24.1(10) . . . . ?
C3 C4 C5 O4A 21.2(10) . . . . ?
C7 C9 N3A C11A 178.1(9) . . . . ?
C6 C7 C8 C2 -0.1(7) . . . . ?
C6 C7 C9 N3 -24.2(8) . . . . ?
C6 C7 C9 C15 174.2(5) . . . . ?
C6 C7 C9 N3A 18.6(8) . . . . ?
C6 C4 C5 O3 0.3(8) . . . . ?
C6 C4 C5 O4 155.9(8) . . . . ?
C6 C4 C5 O4A -158.7(8) . . . . ?
C5 C4 C6 C7 -179.7(5) . . . . ?
C8 C2 C3 C4 0.2(7) . . . . ?
C8 C2 C1 O1 -2.4(7) . . . . ?
C8 C2 C1 O2 177.4(4) . . . . ?
C8 C7 C6 C4 -0.1(7) . . . . ?
C8 C7 C9 N3 155.7(6) . . . . ?
C8 C7 C9 C15 -6.0(8) . . . . ?
C8 C7 C9 N3A -161.6(7) . . . . ?
C1 C2 C3 C4 -179.6(4) . . . . ?
C1 C2 C8 C7 179.8(4) . . . . ?
C18 N2 C22 C21 0.3(7) . . . . ?
C18 C19 C20 C23 176.9(5) . . . . ?
C18 C19 C20 C21 -1.4(7) . . . . ?
C22 N2 C18 C19 -0.5(7) . . . . ?
C19 C20 C21 C22 1.2(8) . . . . ?
C20 C23 C24 C16 -178.6(6) . . . . ?
C20 C23 C25 C17 178.1(6) . . . . ?
C14 C15 C9 N3 19.9(10) . . . . ?
C14 C15 C9 C7 -179.5(5) . . . . ?
C14 C15 C9 N3A -24.4(10) . . . . ?
C14 C12 C11 N3 1(2) . . . . ?
C14 C12A C13A O5 7(2) . . . . ?
C14 C12A C13A O6A -172.7(12) . . . . ?
C15 C14 C12 C13 -179.5(10) . . . . ?
C15 C14 C12 C11 1.0(15) . . . . ?
C15 C14 C12A C11A 0.6(16) . . . . ?
C15 C14 C12A C13A 179.3(9) . . . . ?
C15 C9 N3A C11A 20.1(14) . . . . ?
C9 N3 C11 C12 6.4(18) . . . . ?
C9 C7 C6 C4 179.7(4) . . . . ?
C9 C7 C8 C2 -179.9(4) . . . . ?
C12 C14 C15 C9 -11.7(11) . . . . ?
C16 N1 C17 C25 -1.0(10) . . . . ?
C24 C23 C20 C19 -24.2(8) . . . . ?
C24 C23 C20 C21 154.0(6) . . . . ?
C24 C23 C25 C17 0.4(10) . . . . ?
C17 N1 C16 C24 0.5(9) . . . . ?
C25 C23 C20 C19 158.2(6) . . . . ?
C25 C23 C20 C21 -23.6(9) . . . . ?
C25 C23 C24 C16 -0.8(10) . . . . ?
C11 N3 C9 C7 -179.7(9) . . . . ?
C11 N3 C9 C15 -16.7(13) . . . . ?
C11A C12A C13A O5 -174.8(13) . . . . ?
C11A C12A C13A O6A 6(2) . . . . ?
N3A C11A C12A C14 -4(2) . . . . ?
N3A C11A C12A C13A 177.0(12) . . . . ?
C12A C14 C15 C9 14.1(11) . . . . ?
C12A C11A N3A C9 -6(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_p
_database_code_depnum_ccdc_archive 'CCDC 1886815'
loop_
_audit_author_name
_audit_author_address
'Jie Zhang'
;North University of China
China
;
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;
_audit_creation_date             2017-09-17
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(C140 H108 Cu6 N28 O24), 2(C3 H7 N O), 6(H2 O)'
_chemical_formula_sum            'C76 H80 Cu3 N16 O20'
_chemical_formula_weight         1728.18
_chemical_melting_point          ?
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'
Cu Cu 0.3201 1.2651 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   14.0116(18)
_cell_length_b                   19.843(3)
_cell_length_c                   15.3662(19)
_cell_angle_alpha                90
_cell_angle_beta                 108.191(3)
_cell_angle_gamma                90
_cell_volume                     4058.8(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3557
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.679
_cell_measurement_theta_min      2.48
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0998 before and 0.0584 after correction. The Ratio of minimum to maximum transmission is 0.8353. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1790
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22948
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.732
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5510
_reflns_number_total             8163
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         8163
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0599
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1072P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1818
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
3. Rigid body (RIGU) restrains
 C22, O7, N4, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Riding coordinates:
 O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B)
4.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C28(H28A,H28B), C33(H33A,H33B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8), C11(H11), C14(H14), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C30(H30),
  C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
4.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Cu1 Cu 0.000000 0.500000 0.000000 0.02411(19) Uani 1 2 d S T P . .
Cu2 Cu 0.57762(4) 0.27016(2) 0.78761(3) 0.02671(17) Uani 1 1 d . . . . .
O1 O 0.0880(2) 0.51618(14) 0.12401(17) 0.0275(6) Uani 1 1 d . . . . .
O2 O 0.1338(2) 0.41019(15) 0.11362(19) 0.0406(8) Uani 1 1 d . . . . .
O3 O 0.3846(2) 0.68487(13) 0.64680(19) 0.0322(7) Uani 1 1 d . . . . .
O4 O 0.5152(2) 0.65948(14) 0.76769(19) 0.0345(7) Uani 1 1 d . . . . .
O5 O 0.5195(2) 0.34253(12) 0.70473(18) 0.0271(6) Uani 1 1 d . . . . .
O6 O 0.6256(2) 0.41113(13) 0.80315(17) 0.0287(6) Uani 1 1 d . . . . .
C3 C 0.2207(3) 0.5295(2) 0.2997(3) 0.0344(10) Uani 1 1 d . . . . .
H3 H 0.189229 0.568046 0.266221 0.041 Uiso 1 1 calc R . . . .
N2 N 0.1061(2) 0.53042(17) -0.0495(2) 0.0284(8) Uani 1 1 d . . . . .
N3 N 0.2470(3) 0.57514(17) -0.0582(2) 0.0281(8) Uani 1 1 d . . . . .
C1 C 0.1375(3) 0.4636(2) 0.1568(3) 0.0289(9) Uani 1 1 d . . . . .
C2 C 0.2047(3) 0.4686(2) 0.2552(3) 0.0270(9) Uani 1 1 d . . . . .
N1 N 0.2768(3) 0.53838(17) 0.3855(2) 0.0354(9) Uani 1 1 d . . . . .
C4 C 0.3217(3) 0.48441(18) 0.4334(3) 0.0243(8) Uani 1 1 d . . . . .
C5 C 0.3094(4) 0.4207(2) 0.3932(3) 0.0420(12) Uani 1 1 d . . . . .
H5 H 0.342162 0.382741 0.427280 0.050 Uiso 1 1 calc R . . . .
C6 C 0.2499(4) 0.4132(2) 0.3044(3) 0.0420(12) Uani 1 1 d . . . . .
H6 H 0.239894 0.369854 0.276849 0.050 Uiso 1 1 calc R . . . .
C7 C 0.3860(3) 0.49675(18) 0.5293(2) 0.0222(8) Uani 1 1 d . . . . .
C8 C 0.3904(3) 0.56116(18) 0.5675(3) 0.0253(8) Uani 1 1 d . . . . .
H8 H 0.351648 0.596493 0.531693 0.030 Uiso 1 1 calc R . . . .
C9 C 0.4487(3) 0.57429(18) 0.6547(3) 0.0245(8) Uani 1 1 d . . . . .
C10 C 0.4510(3) 0.64374(19) 0.6939(3) 0.0261(9) Uani 1 1 d . . . . .
C11 C 0.5073(3) 0.52297(18) 0.7088(3) 0.0230(8) Uani 1 1 d . . . . .
H11 H 0.550211 0.532407 0.768913 0.028 Uiso 1 1 calc R . . . .
C12 C 0.5016(3) 0.45811(17) 0.6730(2) 0.0198(8) Uani 1 1 d . . . . .
C13 C 0.5550(3) 0.40118(18) 0.7328(2) 0.0227(8) Uani 1 1 d . . . . .
C14 C 0.4414(3) 0.44592(17) 0.5837(2) 0.0210(8) Uani 1 1 d . . . . .
H14 H 0.438280 0.401650 0.559399 0.025 Uiso 1 1 calc R . . . .
C15 C 0.1892(3) 0.5639(2) -0.0046(3) 0.0308(9) Uani 1 1 d . . . . .
H15 H 0.205494 0.577973 0.057447 0.037 Uiso 1 1 calc R . . . .
C16 C 0.1987(3) 0.5459(2) -0.1430(3) 0.0319(10) Uani 1 1 d . . . . .
H16 H 0.222305 0.544797 -0.194636 0.038 Uiso 1 1 calc R . . . .
C17 C 0.1127(3) 0.5197(2) -0.1376(3) 0.0305(9) Uani 1 1 d . . . . .
H17 H 0.063724 0.497223 -0.185902 0.037 Uiso 1 1 calc R . . . .
C18 C 0.3480(3) 0.6043(2) -0.0287(3) 0.0322(9) Uani 1 1 d . . . . .
H18A H 0.358338 0.629532 0.029056 0.039 Uiso 1 1 calc R . . . .
H18B H 0.354937 0.636336 -0.075780 0.039 Uiso 1 1 calc R . . . .
C19 C 0.4269(3) 0.5500(2) -0.0142(3) 0.0273(9) Uani 1 1 d . . . . .
C20 C 0.4249(3) 0.4942(2) 0.0397(3) 0.0316(9) Uani 1 1 d . . . . .
H20 H 0.372813 0.489781 0.066743 0.038 Uiso 1 1 calc R . . . .
C21 C 0.5020(3) 0.5549(2) -0.0543(3) 0.0301(9) Uani 1 1 d . . . . .
H21 H 0.503445 0.592386 -0.092248 0.036 Uiso 1 1 calc R . . . .
O7 O 0.8614(5) 0.4277(4) 0.3782(4) 0.140(3) Uani 1 1 d . U . . .
N4 N 0.9775(8) 0.4055(6) 0.5214(8) 0.164(3) Uani 1 1 d . U . . .
C22 C 0.8788(9) 0.4221(6) 0.4600(8) 0.144(4) Uani 1 1 d . U . . .
H22 H 0.825522 0.428761 0.485073 0.173 Uiso 1 1 calc R . . . .
C23 C 1.0000(9) 0.4126(8) 0.6278(8) 0.184(5) Uani 1 1 d . U . . .
H23A H 0.936847 0.410881 0.642446 0.275 Uiso 1 1 calc GR . . . .
H23B H 1.033588 0.455721 0.648295 0.275 Uiso 1 1 calc GR . . . .
H23C H 1.043751 0.375587 0.658985 0.275 Uiso 1 1 calc GR . . . .
C24 C 1.0588(13) 0.3904(9) 0.4702(12) 0.278(9) Uani 1 1 d . U . . .
H24A H 1.060087 0.427880 0.429113 0.416 Uiso 1 1 calc GR . . . .
H24B H 1.040748 0.348732 0.434541 0.416 Uiso 1 1 calc GR . . . .
H24C H 1.125314 0.385250 0.515675 0.416 Uiso 1 1 calc GR . . . .
O8 O 0.3047(3) 0.3222(2) 0.6107(3) 0.0737(12) Uani 1 1 d . . . . .
H8A H 0.279425 0.285602 0.622011 0.111 Uiso 1 1 d R . . . .
H8B H 0.365665 0.324322 0.627781 0.111 Uiso 1 1 d R . . . .
O9 O 0.2538(4) 0.4422(3) 0.6961(4) 0.114(2) Uani 1 1 d . . . . .
H9A H 0.213799 0.472948 0.673590 0.171 Uiso 1 1 d R . . . .
H9B H 0.245179 0.405168 0.666880 0.171 Uiso 1 1 d R . . . .
O10 O 0.2861(3) 0.31607(19) 0.1249(2) 0.0557(10) Uani 1 1 d . . . . .
H10A H 0.239033 0.337684 0.137355 0.084 Uiso 1 1 d R . . . .
H10B H 0.337613 0.341344 0.137245 0.084 Uiso 1 1 d R . . . .
N5 N 0.4897(3) 0.29043(17) 0.8637(2) 0.0308(8) Uani 1 1 d . . . . .
N6 N 0.3627(3) 0.32811(18) 0.9058(3) 0.0350(8) Uani 1 1 d . . . . .
N7 N -0.1747(3) 0.2247(2) 0.7100(3) 0.0516(12) Uani 1 1 d . . . . .
N8 N -0.3141(3) 0.25863(17) 0.7307(3) 0.0350(9) Uani 1 1 d . . . . .
C25 C 0.4141(3) 0.3343(2) 0.8458(3) 0.0317(9) Uani 1 1 d . . . . .
H25 H 0.398616 0.365951 0.796974 0.038 Uiso 1 1 calc R . . . .
C26 C 0.4054(4) 0.2781(2) 0.9660(3) 0.0459(12) Uani 1 1 d . . . . .
H26 H 0.384164 0.262312 1.015354 0.055 Uiso 1 1 calc R . . . .
C27 C 0.4845(4) 0.2554(2) 0.9411(3) 0.0422(12) Uani 1 1 d . . . . .
H27 H 0.529578 0.220875 0.971688 0.051 Uiso 1 1 calc R . . . .
C28 C 0.2679(3) 0.3631(2) 0.8982(3) 0.0405(11) Uani 1 1 d . . . . .
H28A H 0.263433 0.404468 0.861179 0.049 Uiso 1 1 calc R . . . .
H28B H 0.267192 0.376554 0.959995 0.049 Uiso 1 1 calc R . . . .
C29 C 0.1788(4) 0.3190(2) 0.8544(3) 0.0408(11) Uani 1 1 d . . . . .
C30 C 0.0940(4) 0.3227(3) 0.8820(5) 0.0627(16) Uani 1 1 d . . . . .
H30 H 0.092562 0.352572 0.929908 0.075 Uiso 1 1 calc R . . . .
C31 C 0.0109(5) 0.2829(3) 0.8400(5) 0.073(2) Uani 1 1 d . . . . .
H31 H -0.047108 0.286069 0.859325 0.087 Uiso 1 1 calc R . . . .
C32 C 0.0111(4) 0.2391(3) 0.7710(4) 0.0550(15) Uani 1 1 d . . . . .
C33 C -0.0768(4) 0.1904(3) 0.7298(5) 0.0626(17) Uani 1 1 d . . . . .
H33A H -0.070704 0.170858 0.672482 0.075 Uiso 1 1 calc R . . . .
H33B H -0.073466 0.152961 0.773294 0.075 Uiso 1 1 calc R . . . .
C34 C -0.2381(4) 0.2160(2) 0.7579(4) 0.0437(12) Uani 1 1 d . . . . .
H34 H -0.229840 0.183645 0.805254 0.052 Uiso 1 1 calc R . . . .
C35 C -0.2970(4) 0.2957(2) 0.6605(3) 0.0415(11) Uani 1 1 d . . . . .
H35 H -0.339347 0.330552 0.627171 0.050 Uiso 1 1 calc R . . . .
C36 C -0.2129(4) 0.2753(3) 0.6470(4) 0.0541(14) Uani 1 1 d . . . . .
H36 H -0.184396 0.292141 0.602746 0.065 Uiso 1 1 calc R . . . .
C37 C 0.0928(4) 0.2365(3) 0.7408(4) 0.0555(14) Uani 1 1 d . . . . .
H37 H 0.092824 0.207389 0.691650 0.067 Uiso 1 1 calc R . . . .
C38 C 0.1757(4) 0.2763(3) 0.7820(4) 0.0495(13) Uani 1 1 d . . . . .
H38 H 0.232053 0.274332 0.760153 0.059 Uiso 1 1 calc R . . . .


_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
Cu1 O1 1.946(2) 3_565 ?
Cu1 O1 1.946(2) . ?
Cu1 N2 1.965(3) 3_565 ?
Cu1 N2 1.965(3) . ?
Cu2 O3 1.956(3) 2_646 ?
Cu2 O5 1.924(3) . ?
Cu2 N5 1.986(4) . ?
Cu2 N8 1.987(4) 1_655 ?
O1 C1 1.267(5) . ?
O2 C1 1.243(5) . ?
O3 C10 1.279(5) . ?
O4 C10 1.247(5) . ?
O5 C13 1.286(4) . ?
O6 C13 1.232(4) . ?
C3 C2 1.372(6) . ?
C3 N1 1.320(5) . ?
N2 C15 1.330(5) . ?
N2 C17 1.401(5) . ?
N3 C15 1.342(5) . ?
N3 C16 1.393(5) . ?
N3 C18 1.465(5) . ?
C1 C2 1.515(5) . ?
C2 C6 1.371(6) . ?
N1 C4 1.340(5) . ?
C4 C5 1.394(5) . ?
C4 C7 1.488(5) . ?
C5 C6 1.367(6) . ?
C7 C8 1.400(5) . ?
C7 C14 1.383(5) . ?
C8 C9 1.359(5) . ?
C9 C10 1.500(5) . ?
C9 C11 1.406(5) . ?
C11 C12 1.392(5) . ?
C12 C13 1.500(5) . ?
C12 C14 1.389(5) . ?
C16 C17 1.340(6) . ?
C18 C19 1.510(6) . ?
C19 C20 1.387(6) . ?
C19 C21 1.379(6) . ?
C20 C21 1.380(6) 3_665 ?
O7 C22 1.208(11) . ?
N4 C22 1.448(13) . ?
N4 C23 1.572(13) . ?
N4 C24 1.601(17) . ?
N5 C25 1.332(5) . ?
N5 C27 1.400(6) . ?
N6 C25 1.341(5) . ?
N6 C26 1.362(6) . ?
N6 C28 1.470(6) . ?
N7 C33 1.476(6) . ?
N7 C34 1.330(7) . ?
N7 C36 1.382(7) . ?
N8 C34 1.321(6) . ?
N8 C35 1.387(6) . ?
C26 C27 1.357(7) . ?
C28 C29 1.501(7) . ?
C29 C30 1.383(7) . ?
C29 C38 1.389(7) . ?
C30 C31 1.388(8) . ?
C31 C32 1.372(8) . ?
C32 C33 1.539(7) . ?
C32 C37 1.364(8) . ?
C35 C36 1.322(7) . ?
C37 C38 1.384(7) . ?

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 Cu1 O1 180.00(9) 3_565 . ?
O1 Cu1 N2 89.78(12) . 3_565 ?
O1 Cu1 N2 90.22(12) 3_565 3_565 ?
O1 Cu1 N2 90.22(12) . . ?
O1 Cu1 N2 89.78(12) 3_565 . ?
N2 Cu1 N2 180.0 3_565 . ?
O3 Cu2 N5 89.41(13) 2_646 . ?
O3 Cu2 N8 90.36(14) 2_646 1_655 ?
O5 Cu2 O3 167.82(12) . 2_646 ?
O5 Cu2 N5 91.49(13) . . ?
O5 Cu2 N8 91.05(13) . 1_655 ?
N5 Cu2 N8 168.99(15) . 1_655 ?
C1 O1 Cu1 110.7(2) . . ?
C10 O3 Cu2 103.2(2) . 2_656 ?
C13 O5 Cu2 114.5(2) . . ?
N1 C3 C2 124.7(4) . . ?
C15 N2 Cu1 126.7(3) . . ?
C15 N2 C17 105.5(3) . . ?
C17 N2 Cu1 127.8(3) . . ?
C15 N3 C16 107.2(3) . . ?
C15 N3 C18 125.9(3) . . ?
C16 N3 C18 126.4(4) . . ?
O1 C1 C2 115.8(3) . . ?
O2 C1 O1 124.3(4) . . ?
O2 C1 C2 119.9(4) . . ?
C3 C2 C1 120.6(4) . . ?
C6 C2 C3 117.1(4) . . ?
C6 C2 C1 122.3(4) . . ?
C3 N1 C4 118.2(3) . . ?
N1 C4 C5 120.6(4) . . ?
N1 C4 C7 116.6(3) . . ?
C5 C4 C7 122.8(3) . . ?
C6 C5 C4 119.6(4) . . ?
C5 C6 C2 119.7(4) . . ?
C8 C7 C4 120.0(3) . . ?
C14 C7 C4 122.0(3) . . ?
C14 C7 C8 118.0(3) . . ?
C9 C8 C7 121.5(3) . . ?
C8 C9 C10 120.2(3) . . ?
C8 C9 C11 120.3(3) . . ?
C11 C9 C10 119.5(3) . . ?
O3 C10 C9 116.0(3) . . ?
O4 C10 O3 123.0(3) . . ?
O4 C10 C9 120.9(4) . . ?
C12 C11 C9 119.0(3) . . ?
C11 C12 C13 119.8(3) . . ?
C14 C12 C11 119.6(3) . . ?
C14 C12 C13 120.4(3) . . ?
O5 C13 C12 114.2(3) . . ?
O6 C13 O5 124.0(3) . . ?
O6 C13 C12 121.8(3) . . ?
C7 C14 C12 121.5(3) . . ?
N2 C15 N3 111.2(3) . . ?
C17 C16 N3 106.7(4) . . ?
C16 C17 N2 109.4(4) . . ?
N3 C18 C19 110.9(3) . . ?
C20 C19 C18 120.5(4) . . ?
C21 C19 C18 120.6(4) . . ?
C21 C19 C20 118.9(4) . . ?
C21 C20 C19 120.5(4) 3_665 . ?
C19 C21 C20 120.6(4) . 3_665 ?
C22 N4 C23 119.9(11) . . ?
C22 N4 C24 113.8(11) . . ?
C23 N4 C24 125.8(10) . . ?
O7 C22 N4 122.7(12) . . ?
C25 N5 Cu2 127.6(3) . . ?
C25 N5 C27 104.5(4) . . ?
C27 N5 Cu2 127.3(3) . . ?
C25 N6 C26 108.5(4) . . ?
C25 N6 C28 124.6(4) . . ?
C26 N6 C28 126.3(4) . . ?
C34 N7 C33 124.4(5) . . ?
C34 N7 C36 107.6(4) . . ?
C36 N7 C33 127.7(5) . . ?
C34 N8 Cu2 125.8(3) . 1_455 ?
C34 N8 C35 105.5(4) . . ?
C35 N8 Cu2 128.5(3) . 1_455 ?
N5 C25 N6 111.2(4) . . ?
C27 C26 N6 106.0(4) . . ?
C26 C27 N5 109.7(4) . . ?
N6 C28 C29 111.4(4) . . ?
C30 C29 C28 120.4(4) . . ?
C30 C29 C38 117.6(5) . . ?
C38 C29 C28 121.9(4) . . ?
C29 C30 C31 120.2(5) . . ?
C32 C31 C30 121.0(5) . . ?
C31 C32 C33 121.4(5) . . ?
C37 C32 C31 119.5(5) . . ?
C37 C32 C33 119.0(5) . . ?
N7 C33 C32 111.6(4) . . ?
N8 C34 N7 110.7(5) . . ?
C36 C35 N8 109.8(5) . . ?
C35 C36 N7 106.3(5) . . ?
C32 C37 C38 119.7(5) . . ?
C37 C38 C29 121.8(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
Cu1 O1 C1 O2 3.3(5) . . . . ?
Cu1 O1 C1 C2 -176.7(3) . . . . ?
Cu1 N2 C15 N3 178.3(3) . . . . ?
Cu1 N2 C17 C16 -177.3(3) . . . . ?
Cu2 O3 C10 O4 5.7(5) 2_656 . . . ?
Cu2 O3 C10 C9 -173.7(3) 2_656 . . . ?
Cu2 O5 C13 O6 5.3(5) . . . . ?
Cu2 O5 C13 C12 -173.5(2) . . . . ?
Cu2 N5 C25 N6 171.4(3) . . . . ?
Cu2 N5 C27 C26 -170.9(3) . . . . ?
Cu2 N8 C34 N7 -174.9(3) 1_455 . . . ?
Cu2 N8 C35 C36 175.3(3) 1_455 . . . ?
O1 C1 C2 C3 -9.2(6) . . . . ?
O1 C1 C2 C6 169.2(4) . . . . ?
O2 C1 C2 C3 170.7(4) . . . . ?
O2 C1 C2 C6 -10.9(7) . . . . ?
C3 C2 C6 C5 -1.2(7) . . . . ?
C3 N1 C4 C5 0.1(7) . . . . ?
C3 N1 C4 C7 178.7(4) . . . . ?
N3 C16 C17 N2 -1.3(5) . . . . ?
N3 C18 C19 C20 -50.8(5) . . . . ?
N3 C18 C19 C21 129.1(4) . . . . ?
C1 C2 C6 C5 -179.7(4) . . . . ?
C2 C3 N1 C4 0.0(7) . . . . ?
N1 C3 C2 C1 179.0(4) . . . . ?
N1 C3 C2 C6 0.5(7) . . . . ?
N1 C4 C5 C6 -0.9(7) . . . . ?
N1 C4 C7 C8 5.4(6) . . . . ?
N1 C4 C7 C14 -175.7(4) . . . . ?
C4 C5 C6 C2 1.4(8) . . . . ?
C4 C7 C8 C9 -179.6(4) . . . . ?
C4 C7 C14 C12 179.7(4) . . . . ?
C5 C4 C7 C8 -176.1(4) . . . . ?
C5 C4 C7 C14 2.8(6) . . . . ?
C7 C4 C5 C6 -179.3(4) . . . . ?
C7 C8 C9 C10 -179.4(4) . . . . ?
C7 C8 C9 C11 0.5(6) . . . . ?
C8 C7 C14 C12 -1.4(6) . . . . ?
C8 C9 C10 O3 10.7(6) . . . . ?
C8 C9 C10 O4 -168.7(4) . . . . ?
C8 C9 C11 C12 -2.5(6) . . . . ?
C9 C11 C12 C13 -173.7(4) . . . . ?
C9 C11 C12 C14 2.5(6) . . . . ?
C10 C9 C11 C12 177.5(4) . . . . ?
C11 C9 C10 O3 -169.2(4) . . . . ?
C11 C9 C10 O4 11.4(6) . . . . ?
C11 C12 C13 O5 158.0(3) . . . . ?
C11 C12 C13 O6 -20.8(6) . . . . ?
C11 C12 C14 C7 -0.6(6) . . . . ?
C13 C12 C14 C7 175.5(4) . . . . ?
C14 C7 C8 C9 1.4(6) . . . . ?
C14 C12 C13 O5 -18.1(5) . . . . ?
C14 C12 C13 O6 163.1(4) . . . . ?
C15 N2 C17 C16 0.6(5) . . . . ?
C15 N3 C16 C17 1.5(5) . . . . ?
C15 N3 C18 C19 100.3(5) . . . . ?
C16 N3 C15 N2 -1.1(5) . . . . ?
C16 N3 C18 C19 -70.5(5) . . . . ?
C17 N2 C15 N3 0.3(5) . . . . ?
C18 N3 C15 N2 -173.3(4) . . . . ?
C18 N3 C16 C17 173.6(4) . . . . ?
C18 C19 C20 C21 -178.9(4) . . . 3_665 ?
C18 C19 C21 C20 178.9(4) . . . 3_665 ?
C20 C19 C21 C20 -1.2(7) . . . 3_665 ?
C21 C19 C20 C21 1.2(7) . . . 3_665 ?
C23 N4 C22 O7 168.2(12) . . . . ?
C24 N4 C22 O7 -4.1(19) . . . . ?
N6 C26 C27 N5 -1.3(5) . . . . ?
N6 C28 C29 C30 144.9(5) . . . . ?
N6 C28 C29 C38 -38.8(7) . . . . ?
N8 C35 C36 N7 -0.6(6) . . . . ?
C25 N5 C27 C26 1.3(5) . . . . ?
C25 N6 C26 C27 0.9(5) . . . . ?
C25 N6 C28 C29 96.7(5) . . . . ?
C26 N6 C25 N5 -0.1(5) . . . . ?
C26 N6 C28 C29 -73.9(6) . . . . ?
C27 N5 C25 N6 -0.8(5) . . . . ?
C28 N6 C25 N5 -172.0(4) . . . . ?
C28 N6 C26 C27 172.6(4) . . . . ?
C28 C29 C30 C31 178.6(6) . . . . ?
C28 C29 C38 C37 -179.0(5) . . . . ?
C29 C30 C31 C32 0.3(11) . . . . ?
C30 C29 C38 C37 -2.6(8) . . . . ?
C30 C31 C32 C33 174.5(6) . . . . ?
C30 C31 C32 C37 -2.5(10) . . . . ?
C31 C32 C33 N7 46.0(9) . . . . ?
C31 C32 C37 C38 2.1(9) . . . . ?
C32 C37 C38 C29 0.5(9) . . . . ?
C33 N7 C34 N8 173.2(4) . . . . ?
C33 N7 C36 C35 -173.0(5) . . . . ?
C33 C32 C37 C38 -175.0(6) . . . . ?
C34 N7 C33 C32 -107.8(6) . . . . ?
C34 N7 C36 C35 0.9(6) . . . . ?
C34 N8 C35 C36 0.0(5) . . . . ?
C35 N8 C34 N7 0.6(5) . . . . ?
C36 N7 C33 C32 65.2(8) . . . . ?
C36 N7 C34 N8 -1.0(5) . . . . ?
C37 C32 C33 N7 -137.0(6) . . . . ?
C38 C29 C30 C31 2.2(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_p_sq_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1886814'
loop_
_audit_author_name
_audit_author_address
'Jie Zhang'
;North University of China
China
;
_audit_update_record             
;
2018-12-21 deposited with the CCDC.	2019-04-30 downloaded from the CCDC.
;
_audit_creation_date             2017-02-20
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C108 H76 N18 Ni3 O16, 2(C2 H6 O), 3(H2 O)'
_chemical_formula_sum            'C112 H94 N18 Ni3 O21'
_chemical_formula_weight         2204.18
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.107(5)
_cell_length_b                   13.460(8)
_cell_length_c                   23.318(14)
_cell_angle_alpha                92.653(7)
_cell_angle_beta                 95.757(9)
_cell_angle_gamma                109.755(6)
_cell_volume                     2960(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1521
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.547
_cell_measurement_theta_min      2.489
_shelx_estimated_absorpt_T_max   0.973
_shelx_estimated_absorpt_T_min   0.953
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_av_unetI/netI     0.1622
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39771
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_min         2.489
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5811
_reflns_number_total             13512
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         13512
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1601
_refine_ls_R_factor_gt           0.0627
_refine_ls_restrained_S_all      0.908
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0765P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1821
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1W-C1
 1.4 with sigma of 0.01
3. Rigid bond restraints
 O1W, C1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: O5WA(0.25) H5WA(0.25) H5WB(0.25) O5W(0.25) H5WC(0.25) H5WD(0.25)
6.a Riding coordinates:
 O3W(H3WA,H3WB), O1W(H1W), O4W(H4WA,H4WB), O5WA(H5WA,H5WB), O5W(H5WC,H5WD)
6.b Rotating group:
 O2W(H2WA,H2WB)
6.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C1AA(H1AA), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11),
 C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C26(H26),
  C28(H28), C31(H31), C33(H33), C34(H34), C36(H36), C38(H38), C39(H39),
 C40(H40), C41(H41), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C52(H52),
  C53(H53), C54(H54), C55(H55)
6.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C0AA C 0.1663(4) -0.5388(3) 0.05938(19) 0.0386(11) Uani 1 1 d . . . . .
C2 C 0.2392(5) -0.5804(4) 0.0228(2) 0.0517(13) Uani 1 1 d . . . . .
H2 H 0.2407 -0.6488 0.0249 0.062 Uiso 1 1 calc R . . . .
C1AA C 0.3084(6) -0.5156(4) -0.0162(2) 0.0689(16) Uani 1 1 d . . . . .
H1AA H 0.3572 -0.5413 -0.0415 0.083 Uiso 1 1 calc R . . . .
C4 C 0.3085(6) -0.4124(4) -0.0196(2) 0.0729(17) Uani 1 1 d . . . . .
H4 H 0.3578 -0.3715 -0.0468 0.088 Uiso 1 1 calc R . . . .
C5 C 0.2379(6) -0.3692(4) 0.0163(2) 0.0621(15) Uani 1 1 d . . . . .
H5 H 0.2370 -0.3006 0.0138 0.075 Uiso 1 1 calc R . . . .
C6 C 0.1684(5) -0.4344(3) 0.0560(2) 0.0418(11) Uani 1 1 d . . . . .
C7 C 0.0483(4) -0.5107(3) 0.1259(2) 0.0428(12) Uani 1 1 d . . . . .
H7 H -0.0041 -0.5201 0.1571 0.051 Uiso 1 1 calc R . . . .
C8 C 0.0774(5) -0.2981(4) 0.1782(2) 0.0612(15) Uani 1 1 d . . . . .
H8 H 0.0993 -0.3418 0.2045 0.073 Uiso 1 1 calc R . . . .
C9 C 0.0650(5) -0.3244(3) 0.1179(2) 0.0424(11) Uani 1 1 d . . . . .
C10 C 0.0326(5) -0.2610(4) 0.0796(2) 0.0567(14) Uani 1 1 d . . . . .
H10 H 0.0255 -0.2789 0.0401 0.068 Uiso 1 1 calc R . . . .
C11 C 0.0097(5) -0.1692(4) 0.0987(2) 0.0565(14) Uani 1 1 d . . . . .
H11 H -0.0131 -0.1264 0.0721 0.068 Uiso 1 1 calc R . . . .
C12 C 0.0211(5) -0.1422(3) 0.1574(2) 0.0402(11) Uani 1 1 d . . . . .
C13 C 0.0562(6) -0.2061(4) 0.1975(2) 0.0650(15) Uani 1 1 d . . . . .
H13 H 0.0654 -0.1870 0.2370 0.078 Uiso 1 1 calc R . . . .
C14 C 0.0397(4) 0.0439(3) 0.14878(19) 0.0383(11) Uani 1 1 d . . . . .
H14 H 0.0801 0.0491 0.1144 0.046 Uiso 1 1 calc R . . . .
C15 C -0.0534(5) -0.0230(3) 0.2256(2) 0.0413(11) Uani 1 1 d . . . . .
C16 C -0.0444(4) 0.0830(3) 0.22396(19) 0.0365(10) Uani 1 1 d . . . . .
C17 C -0.0882(5) 0.1339(4) 0.2677(2) 0.0511(13) Uani 1 1 d . . . . .
H17 H -0.0819 0.2043 0.2670 0.061 Uiso 1 1 calc R . . . .
C18 C -0.1415(6) 0.0744(4) 0.3124(2) 0.0681(16) Uani 1 1 d . . . . .
H18 H -0.1701 0.1060 0.3428 0.082 Uiso 1 1 calc R . . . .
C19 C -0.1533(6) -0.0325(5) 0.3128(2) 0.0713(17) Uani 1 1 d . . . . .
H19 H -0.1912 -0.0701 0.3432 0.086 Uiso 1 1 calc R . . . .
C20 C -0.1110(6) -0.0832(4) 0.2700(2) 0.0600(14) Uani 1 1 d . . . . .
H20 H -0.1202 -0.1543 0.2704 0.072 Uiso 1 1 calc R . . . .
C21 C 0.3024(4) 0.3181(3) 0.1741(2) 0.0358(10) Uani 1 1 d . . . . .
C22 C 0.4575(4) 0.3467(3) 0.19457(19) 0.0361(10) Uani 1 1 d . . . . .
C23 C 0.5367(4) 0.2995(3) 0.16599(19) 0.0372(11) Uani 1 1 d . . . . .
H23 H 0.4944 0.2507 0.1342 0.045 Uiso 1 1 calc R . . . .
C24 C 0.6809(4) 0.3252(3) 0.18493(19) 0.0363(10) Uani 1 1 d . . . . .
C25 C 0.7663(5) 0.2731(3) 0.1536(2) 0.0383(11) Uani 1 1 d . . . . .
C26 C 0.7450(4) 0.4020(3) 0.2305(2) 0.0427(11) Uani 1 1 d . . . . .
H26 H 0.8412 0.4194 0.2426 0.051 Uiso 1 1 calc R . . . .
C27 C 0.6677(5) 0.4538(3) 0.2586(2) 0.0452(12) Uani 1 1 d . . . . .
C28 C 0.5223(4) 0.4226(3) 0.24072(19) 0.0407(11) Uani 1 1 d . . . . .
H28 H 0.4677 0.4533 0.2601 0.049 Uiso 1 1 calc R . . . .
C29 C 0.7411(5) 0.5412(4) 0.3041(2) 0.0488(12) Uani 1 1 d . . . . .
N30 N 0.8761(4) 0.5560(4) 0.3234(2) 0.0742(14) Uani 1 1 d . . . . .
C31 C 0.9446(6) 0.6354(5) 0.3645(3) 0.0815(19) Uani 1 1 d . . . . .
H31 H 1.0376 0.6439 0.3784 0.098 Uiso 1 1 calc R . . . .
C32 C 0.8868(5) 0.7043(4) 0.3873(2) 0.0535(13) Uani 1 1 d . . . . .
C33 C 0.7499(6) 0.6909(4) 0.3662(2) 0.0701(17) Uani 1 1 d . . . . .
H33 H 0.7062 0.7367 0.3796 0.084 Uiso 1 1 calc R . . . .
C34 C 0.6772(5) 0.6086(4) 0.3245(2) 0.0740(18) Uani 1 1 d . . . . .
H34 H 0.5840 0.5988 0.3102 0.089 Uiso 1 1 calc R . . . .
C35 C 0.9722(6) 0.7927(4) 0.4326(2) 0.0578(14) Uani 1 1 d . . . . .
C36 C 0.8169(5) 0.9754(4) 0.5972(2) 0.0586(14) Uani 1 1 d . . . . .
H36 H 0.8231 1.0452 0.5931 0.070 Uiso 1 1 calc R . . . .
C37 C 0.8435(6) 0.8254(4) 0.5842(2) 0.0641(15) Uani 1 1 d . . . . .
C38 C 0.8815(8) 0.7386(5) 0.5672(3) 0.098(2) Uani 1 1 d . . . . .
H38 H 0.9401 0.7428 0.5384 0.118 Uiso 1 1 calc R . . . .
C39 C 0.8303(10) 0.6477(6) 0.5941(4) 0.137(4) Uani 1 1 d . . . . .
H39 H 0.8536 0.5890 0.5829 0.164 Uiso 1 1 calc R . . . .
C40 C 0.7448(10) 0.6409(6) 0.6374(4) 0.132(3) Uani 1 1 d . . . . .
H40 H 0.7117 0.5777 0.6547 0.159 Uiso 1 1 calc R . . . .
C41 C 0.7067(8) 0.7263(5) 0.6560(3) 0.096(2) Uani 1 1 d . . . . .
H41 H 0.6491 0.7219 0.6852 0.116 Uiso 1 1 calc R . . . .
C42 C 0.7590(6) 0.8174(4) 0.6288(2) 0.0654(15) Uani 1 1 d . . . . .
C43 C 0.6724(5) 0.9532(4) 0.6784(2) 0.0574(14) Uani 1 1 d . . . . .
C44 C 0.6029(6) 1.0216(4) 0.6621(2) 0.0686(16) Uani 1 1 d . . . . .
H44 H 0.5989 1.0397 0.6241 0.082 Uiso 1 1 calc R . . . .
C45 C 0.5396(6) 1.0632(4) 0.7016(3) 0.0719(17) Uani 1 1 d . . . . .
H45 H 0.4945 1.1105 0.6907 0.086 Uiso 1 1 calc R . . . .
C46 C 0.5435(5) 1.0340(4) 0.7585(2) 0.0583(14) Uani 1 1 d . . . . .
C47 C 0.6147(5) 0.9649(4) 0.7749(2) 0.0607(14) Uani 1 1 d . . . . .
H47 H 0.6188 0.9464 0.8128 0.073 Uiso 1 1 calc R . . . .
C48 C 0.6788(5) 0.9244(4) 0.7348(2) 0.0577(14) Uani 1 1 d . . . . .
H48 H 0.7260 0.8783 0.7454 0.069 Uiso 1 1 calc R . . . .
C49 C 0.3911(6) 1.0230(4) 0.8380(2) 0.0637(15) Uani 1 1 d . . . . .
H49 H 0.3626 0.9498 0.8389 0.076 Uiso 1 1 calc R . . . .
C50 C 0.4149(5) 1.1853(4) 0.8568(2) 0.0538(13) Uani 1 1 d . . . . .
C51 C 0.4959(5) 1.1838(4) 0.8121(2) 0.0519(13) Uani 1 1 d . . . . .
C52 C 0.5754(5) 1.2758(4) 0.7896(2) 0.0625(15) Uani 1 1 d . . . . .
H52 H 0.6279 1.2744 0.7592 0.075 Uiso 1 1 calc R . . . .
C53 C 0.5720(6) 1.3703(4) 0.8152(3) 0.0764(17) Uani 1 1 d . . . . .
H53 H 0.6288 1.4341 0.8033 0.092 Uiso 1 1 calc R . . . .
C54 C 0.4877(7) 1.3723(5) 0.8574(3) 0.088(2) Uani 1 1 d . . . . .
H54 H 0.4831 1.4368 0.8713 0.106 Uiso 1 1 calc R . . . .
C55 C 0.4099(6) 1.2811(5) 0.8796(3) 0.0747(17) Uani 1 1 d . . . . .
H55 H 0.3552 1.2833 0.9091 0.090 Uiso 1 1 calc R . . . .
N1 N 0.0897(3) -0.5848(2) 0.10347(16) 0.0378(9) Uani 1 1 d . . . . .
N2 N 0.0889(4) -0.4193(2) 0.09960(17) 0.0443(10) Uani 1 1 d . . . . .
N3 N 0.0023(4) -0.0458(2) 0.17631(16) 0.0399(9) Uani 1 1 d . . . . .
N4 N 0.0145(3) 0.1229(2) 0.17455(15) 0.0353(8) Uani 1 1 d . . . . .
N5 N 0.8768(4) 0.9258(3) 0.56507(17) 0.0588(11) Uani 1 1 d . . . . .
N6 N 0.7446(4) 0.9164(3) 0.63701(18) 0.0580(11) Uani 1 1 d . . . . .
N7 N 0.4810(4) 1.0779(3) 0.80075(18) 0.0568(11) Uani 1 1 d . . . . .
N8 N 0.3498(5) 1.0830(3) 0.87185(19) 0.0665(13) Uani 1 1 d . . . . .
Ni1 Ni 1.0000 1.0000 0.5000 0.0501(3) Uani 1 2 d S T P . .
Ni2 Ni 0.05053(5) 0.26806(4) 0.13848(2) 0.03294(17) Uani 1 1 d . . . . .
O1 O 0.9167(3) 0.8610(2) 0.44656(14) 0.0574(9) Uani 1 1 d . . . . .
O2 O 1.0936(4) 0.7939(3) 0.45328(17) 0.0741(11) Uani 1 1 d . . . . .
O2W O 1.1651(4) 0.9541(3) 0.53690(14) 0.0678(10) Uani 1 1 d . . . . .
H2WA H 1.2605 1.0027 0.5347 0.102 Uiso 1 1 d GR . . . .
H2WB H 1.1683 0.8874 0.5202 0.102 Uiso 1 1 d GR . . . .
O3 O 0.2241(3) 0.3459(2) 0.20555(13) 0.0417(8) Uani 1 1 d . . . . .
O3W O -0.0740(3) 0.1934(2) 0.06109(12) 0.0438(8) Uani 1 1 d . . . . .
H3WA H -0.0909 0.1409 0.0350 0.066 Uiso 1 1 d R . . . .
H3WB H -0.1565 0.1978 0.0605 0.066 Uiso 1 1 d R . . . .
O4 O 0.2509(3) 0.2642(2) 0.12567(13) 0.0403(7) Uani 1 1 d . . . . .
O5 O 0.8947(3) 0.2959(2) 0.17574(12) 0.0362(7) Uani 1 1 d . . . . .
O6 O 0.7088(3) 0.2132(2) 0.10879(15) 0.0556(9) Uani 1 1 d . . . . .
O1W O 0.1833(4) 0.0264(3) -0.03901(18) 0.0807(12) Uani 1 1 d D U . . .
H1W H 0.2157 0.0478 -0.0702 0.121 Uiso 1 1 d R . . . .
O4W O 1.1438(6) 0.5204(4) 0.2743(2) 0.142(2) Uani 1 1 d . . . . .
H4WA H 1.0730 0.5300 0.2873 0.213 Uiso 1 1 d R . . . .
H4WB H 1.1185 0.4584 0.2574 0.213 Uiso 1 1 d R . . . .
O5WA O 1.3910(14) 1.1344(9) 0.5633(6) 0.063(4) Uani 0.25 1 d . . . A 1
H5WA H 1.4661 1.1190 0.5651 0.094 Uiso 0.25 1 d R . . A 1
H5WB H 1.3876 1.1455 0.5999 0.094 Uiso 0.25 1 d R . . A 1
O5W O 1.4487(13) 1.0380(15) 0.5248(8) 0.113(7) Uani 0.25 1 d . . . B 2
H5WC H 1.4902 1.0942 0.5447 0.170 Uiso 0.25 1 d R . . B 2
H5WD H 1.4845 1.0455 0.4932 0.170 Uiso 0.25 1 d R . . B 2
C1 C 0.2754(12) 0.0863(9) 0.0123(4) 0.203(5) Uani 1 1 d D U . . .
H1A H 0.2166 0.1069 0.0374 0.244 Uiso 1 1 calc R . . . .
H1B H 0.3398 0.1509 0.0000 0.244 Uiso 1 1 calc R . . . .
C3 C 0.3612(17) 0.0367(13) 0.0474(6) 0.300(8) Uani 1 1 d . U . . .
H3A H 0.3193 -0.0389 0.0408 0.450 Uiso 1 1 calc GR . . . .
H3B H 0.3647 0.0576 0.0876 0.450 Uiso 1 1 calc GR . . . .
H3C H 0.4555 0.0592 0.0368 0.450 Uiso 1 1 calc GR . . . .


_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
C0AA C2 1.395(5) . ?
C0AA C6 1.403(5) . ?
C0AA N1 1.391(5) . ?
C2 H2 0.9300 . ?
C2 C1AA 1.365(6) . ?
C1AA H1AA 0.9300 . ?
C1AA C4 1.395(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.379(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.383(6) . ?
C6 N2 1.405(5) . ?
C7 H7 0.9300 . ?
C7 N1 1.312(4) . ?
C7 N2 1.356(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.416(7) . ?
C8 C13 1.389(6) . ?
C9 C10 1.356(6) . ?
C9 N2 1.433(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.392(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.384(6) . ?
C12 C13 1.398(6) . ?
C12 N3 1.430(5) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 N3 1.351(5) . ?
C14 N4 1.309(4) . ?
C15 C16 1.402(5) . ?
C15 C20 1.395(6) . ?
C15 N3 1.395(5) . ?
C16 C17 1.391(6) . ?
C16 N4 1.396(5) . ?
C17 H17 0.9300 . ?
C17 C18 1.383(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.404(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.364(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.503(6) . ?
C21 Ni2 2.447(4) . ?
C21 O3 1.262(4) . ?
C21 O4 1.275(5) . ?
C22 C23 1.379(5) . ?
C22 C28 1.391(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.398(5) . ?
C24 C25 1.504(5) . ?
C24 C26 1.388(6) . ?
C25 O5 1.275(5) . ?
C25 O6 1.249(5) . ?
C26 H26 0.9300 . ?
C26 C27 1.397(5) . ?
C27 C28 1.397(6) . ?
C27 C29 1.483(6) . ?
C28 H28 0.9300 . ?
C29 N30 1.337(6) . ?
C29 C34 1.373(6) . ?
N30 C31 1.346(6) . ?
C31 H31 0.9300 . ?
C31 C32 1.366(6) . ?
C32 C33 1.370(7) . ?
C32 C35 1.512(7) . ?
C33 H33 0.9300 . ?
C33 C34 1.385(7) . ?
C34 H34 0.9300 . ?
C35 O1 1.274(5) . ?
C35 O2 1.267(6) . ?
C36 H36 0.9300 . ?
C36 N5 1.300(5) . ?
C36 N6 1.357(6) . ?
C37 C38 1.401(7) . ?
C37 C42 1.396(7) . ?
C37 N5 1.385(6) . ?
C38 H38 0.9300 . ?
C38 C39 1.366(8) . ?
C39 H39 0.9300 . ?
C39 C40 1.381(9) . ?
C40 H40 0.9300 . ?
C40 C41 1.395(8) . ?
C41 H41 0.9300 . ?
C41 C42 1.373(7) . ?
C42 N6 1.396(6) . ?
C43 C44 1.379(7) . ?
C43 C48 1.389(7) . ?
C43 N6 1.431(6) . ?
C44 H44 0.9300 . ?
C44 C45 1.374(7) . ?
C45 H45 0.9300 . ?
C45 C46 1.401(7) . ?
C46 C47 1.399(7) . ?
C46 N7 1.429(6) . ?
C47 H47 0.9300 . ?
C47 C48 1.381(6) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
C49 N7 1.375(6) . ?
C49 N8 1.297(6) . ?
C50 C51 1.392(6) . ?
C50 C55 1.391(7) . ?
C50 N8 1.390(6) . ?
C51 C52 1.388(6) . ?
C51 N7 1.392(6) . ?
C52 H52 0.9300 . ?
C52 C53 1.393(7) . ?
C53 H53 0.9300 . ?
C53 C54 1.370(8) . ?
C54 H54 0.9300 . ?
C54 C55 1.371(8) . ?
C55 H55 0.9300 . ?
N1 Ni2 2.105(3) 1_545 ?
N4 Ni2 2.095(3) . ?
N5 Ni1 2.128(4) . ?
Ni1 N5 2.128(4) 2_776 ?
Ni1 O1 2.067(3) 2_776 ?
Ni1 O1 2.067(3) . ?
Ni1 O2W 2.090(4) 2_776 ?
Ni1 O2W 2.089(4) . ?
Ni2 N1 2.105(3) 1_565 ?
Ni2 O3 2.163(3) . ?
Ni2 O3W 2.091(3) . ?
Ni2 O4 2.094(3) . ?
Ni2 O5 2.005(3) 1_455 ?
O2W H2WA 0.9733 . ?
O2W H2WB 0.9732 . ?
O3W H3WA 0.8696 . ?
O3W H3WB 0.8539 . ?
O5 Ni2 2.005(3) 1_655 ?
O1W H1W 0.8500 . ?
O1W C1 1.458(8) . ?
O4W H4WA 0.8501 . ?
O4W H4WB 0.8504 . ?
O5WA H5WA 0.8499 . ?
O5WA H5WB 0.8643 . ?
O5W H5WC 0.8220 . ?
O5W H5WD 0.8499 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C3 1.472(14) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C0AA C6 120.3(4) . . ?
N1 C0AA C2 129.5(4) . . ?
N1 C0AA C6 110.1(3) . . ?
C0AA C2 H2 121.6 . . ?
C1AA C2 C0AA 116.7(4) . . ?
C1AA C2 H2 121.6 . . ?
C2 C1AA H1AA 118.8 . . ?
C2 C1AA C4 122.4(5) . . ?
C4 C1AA H1AA 118.8 . . ?
C1AA C4 H4 119.0 . . ?
C5 C4 C1AA 122.0(5) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 H5 122.2 . . ?
C4 C5 C6 115.6(4) . . ?
C6 C5 H5 122.2 . . ?
C0AA C6 N2 104.6(4) . . ?
C5 C6 C0AA 122.8(4) . . ?
C5 C6 N2 132.6(4) . . ?
N1 C7 H7 123.0 . . ?
N1 C7 N2 113.9(4) . . ?
N2 C7 H7 123.0 . . ?
C9 C8 H8 120.5 . . ?
C13 C8 H8 120.5 . . ?
C13 C8 C9 119.0(5) . . ?
C8 C9 N2 117.5(4) . . ?
C10 C9 C8 120.6(4) . . ?
C10 C9 N2 121.9(4) . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.6(5) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.7(5) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 120.4(4) . . ?
C11 C12 N3 119.0(4) . . ?
C13 C12 N3 120.6(4) . . ?
C8 C13 C12 119.7(5) . . ?
C8 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
N3 C14 H14 122.8 . . ?
N4 C14 H14 122.8 . . ?
N4 C14 N3 114.4(4) . . ?
C20 C15 C16 121.6(4) . . ?
N3 C15 C16 105.3(4) . . ?
N3 C15 C20 133.1(4) . . ?
C17 C16 C15 121.3(4) . . ?
C17 C16 N4 129.2(4) . . ?
N4 C16 C15 109.4(3) . . ?
C16 C17 H17 121.7 . . ?
C18 C17 C16 116.7(4) . . ?
C18 C17 H17 121.7 . . ?
C17 C18 H18 119.3 . . ?
C17 C18 C19 121.5(5) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 H19 118.8 . . ?
C20 C19 C18 122.3(5) . . ?
C20 C19 H19 118.8 . . ?
C15 C20 H20 121.7 . . ?
C19 C20 C15 116.6(5) . . ?
C19 C20 H20 121.7 . . ?
C22 C21 Ni2 178.3(3) . . ?
O3 C21 C22 119.7(4) . . ?
O3 C21 Ni2 62.0(2) . . ?
O3 C21 O4 120.8(4) . . ?
O4 C21 C22 119.5(3) . . ?
O4 C21 Ni2 58.83(19) . . ?
C23 C22 C21 119.4(4) . . ?
C23 C22 C28 119.9(4) . . ?
C28 C22 C21 120.6(3) . . ?
C22 C23 H23 120.1 . . ?
C22 C23 C24 119.8(4) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 C25 119.4(4) . . ?
C26 C24 C23 119.8(4) . . ?
C26 C24 C25 120.7(4) . . ?
O5 C25 C24 115.4(4) . . ?
O6 C25 C24 119.0(4) . . ?
O6 C25 O5 125.6(4) . . ?
C24 C26 H26 119.4 . . ?
C24 C26 C27 121.2(4) . . ?
C27 C26 H26 119.4 . . ?
C26 C27 C28 117.8(4) . . ?
C26 C27 C29 119.9(4) . . ?
C28 C27 C29 122.3(4) . . ?
C22 C28 C27 121.4(4) . . ?
C22 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
N30 C29 C27 117.7(4) . . ?
N30 C29 C34 120.1(4) . . ?
C34 C29 C27 122.2(4) . . ?
C29 N30 C31 118.4(4) . . ?
N30 C31 H31 117.8 . . ?
N30 C31 C32 124.5(5) . . ?
C32 C31 H31 117.8 . . ?
C31 C32 C33 117.0(5) . . ?
C31 C32 C35 121.1(5) . . ?
C33 C32 C35 121.9(4) . . ?
C32 C33 H33 120.4 . . ?
C32 C33 C34 119.2(4) . . ?
C34 C33 H33 120.4 . . ?
C29 C34 C33 120.8(5) . . ?
C29 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
O1 C35 C32 117.1(5) . . ?
O2 C35 C32 117.7(4) . . ?
O2 C35 O1 125.1(5) . . ?
N5 C36 H36 123.0 . . ?
N5 C36 N6 114.1(5) . . ?
N6 C36 H36 123.0 . . ?
C42 C37 C38 119.4(5) . . ?
N5 C37 C38 131.4(5) . . ?
N5 C37 C42 109.2(4) . . ?
C37 C38 H38 120.9 . . ?
C39 C38 C37 118.2(6) . . ?
C39 C38 H38 120.9 . . ?
C38 C39 H39 119.3 . . ?
C38 C39 C40 121.5(6) . . ?
C40 C39 H39 119.3 . . ?
C39 C40 H40 119.1 . . ?
C39 C40 C41 121.9(6) . . ?
C41 C40 H40 119.1 . . ?
C40 C41 H41 121.9 . . ?
C42 C41 C40 116.2(6) . . ?
C42 C41 H41 121.9 . . ?
C41 C42 C37 122.9(5) . . ?
C41 C42 N6 131.4(5) . . ?
N6 C42 C37 105.7(5) . . ?
C44 C43 C48 120.8(5) . . ?
C44 C43 N6 118.9(5) . . ?
C48 C43 N6 120.2(5) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 C43 120.4(5) . . ?
C45 C44 H44 119.8 . . ?
C44 C45 H45 120.3 . . ?
C44 C45 C46 119.5(5) . . ?
C46 C45 H45 120.3 . . ?
C45 C46 N7 120.6(5) . . ?
C47 C46 C45 119.9(5) . . ?
C47 C46 N7 119.4(5) . . ?
C46 C47 H47 120.1 . . ?
C48 C47 C46 119.8(5) . . ?
C48 C47 H47 120.1 . . ?
C43 C48 H48 120.2 . . ?
C47 C48 C43 119.5(5) . . ?
C47 C48 H48 120.2 . . ?
N7 C49 H49 123.2 . . ?
N8 C49 H49 123.2 . . ?
N8 C49 N7 113.6(5) . . ?
C55 C50 C51 119.9(5) . . ?
N8 C50 C51 110.0(4) . . ?
N8 C50 C55 130.1(5) . . ?
C50 C51 N7 105.3(4) . . ?
C52 C51 C50 122.2(5) . . ?
C52 C51 N7 132.4(4) . . ?
C51 C52 H52 122.0 . . ?
C51 C52 C53 116.0(5) . . ?
C53 C52 H52 122.0 . . ?
C52 C53 H53 118.9 . . ?
C54 C53 C52 122.1(5) . . ?
C54 C53 H53 118.9 . . ?
C53 C54 H54 119.3 . . ?
C53 C54 C55 121.3(6) . . ?
C55 C54 H54 119.3 . . ?
C50 C55 H55 120.9 . . ?
C54 C55 C50 118.2(5) . . ?
C54 C55 H55 120.9 . . ?
C0AA N1 Ni2 132.9(2) . 1_545 ?
C7 N1 C0AA 104.9(3) . . ?
C7 N1 Ni2 122.0(3) . 1_545 ?
C6 N2 C9 128.3(4) . . ?
C7 N2 C6 106.5(3) . . ?
C7 N2 C9 125.0(4) . . ?
C14 N3 C12 125.0(3) . . ?
C14 N3 C15 106.2(3) . . ?
C15 N3 C12 128.8(4) . . ?
C14 N4 C16 104.7(3) . . ?
C14 N4 Ni2 122.2(3) . . ?
C16 N4 Ni2 133.0(2) . . ?
C36 N5 C37 105.4(4) . . ?
C36 N5 Ni1 122.2(4) . . ?
C37 N5 Ni1 132.4(3) . . ?
C36 N6 C42 105.5(4) . . ?
C36 N6 C43 125.1(4) . . ?
C42 N6 C43 129.4(4) . . ?
C49 N7 C46 126.6(4) . . ?
C49 N7 C51 105.8(4) . . ?
C51 N7 C46 127.5(4) . . ?
C49 N8 C50 105.2(4) . . ?
N5 Ni1 N5 180.0 . 2_776 ?
O1 Ni1 N5 90.01(14) 2_776 . ?
O1 Ni1 N5 90.01(14) . 2_776 ?
O1 Ni1 N5 89.99(14) 2_776 2_776 ?
O1 Ni1 N5 89.99(14) . . ?
O1 Ni1 O1 180.0 2_776 . ?
O1 Ni1 O2W 91.60(14) 2_776 2_776 ?
O1 Ni1 O2W 88.40(14) 2_776 . ?
O1 Ni1 O2W 91.60(14) . . ?
O1 Ni1 O2W 88.40(14) . 2_776 ?
O2W Ni1 N5 88.90(15) 2_776 2_776 ?
O2W Ni1 N5 88.90(15) . . ?
O2W Ni1 N5 91.10(15) 2_776 . ?
O2W Ni1 N5 91.10(16) . 2_776 ?
O2W Ni1 O2W 180.0 . 2_776 ?
N1 Ni2 C21 90.07(13) 1_565 . ?
N1 Ni2 O3 88.05(13) 1_565 . ?
N4 Ni2 C21 89.07(13) . . ?
N4 Ni2 N1 178.97(14) . 1_565 ?
N4 Ni2 O3 90.92(12) . . ?
O3 Ni2 C21 31.00(11) . . ?
O3W Ni2 C21 134.23(12) . . ?
O3W Ni2 N1 89.26(13) . 1_565 ?
O3W Ni2 N4 91.75(13) . . ?
O3W Ni2 O3 164.93(10) . . ?
O3W Ni2 O4 102.96(11) . . ?
O4 Ni2 C21 31.39(11) . . ?
O4 Ni2 N1 92.65(12) . 1_565 ?
O4 Ni2 N4 86.91(12) . . ?
O4 Ni2 O3 62.39(11) . . ?
O5 Ni2 C21 129.65(13) 1_455 . ?
O5 Ni2 N1 87.49(12) 1_455 1_565 ?
O5 Ni2 N4 92.62(12) 1_455 . ?
O5 Ni2 O3 98.65(11) 1_455 . ?
O5 Ni2 O3W 96.04(12) 1_455 . ?
O5 Ni2 O4 161.01(12) 1_455 . ?
C35 O1 Ni1 130.4(3) . . ?
Ni1 O2W H2WA 116.0 . . ?
Ni1 O2W H2WB 115.4 . . ?
H2WA O2W H2WB 102.4 . . ?
C21 O3 Ni2 87.0(3) . . ?
Ni2 O3W H3WA 143.9 . . ?
Ni2 O3W H3WB 109.9 . . ?
H3WA O3W H3WB 100.6 . . ?
C21 O4 Ni2 89.8(2) . . ?
C25 O5 Ni2 126.8(3) . 1_655 ?
C1 O1W H1W 112.4 . . ?
H4WA O4W H4WB 109.5 . . ?
H5WA O5WA H5WB 99.2 . . ?
H5WC O5W H5WD 105.2 . . ?
O1W C1 H1A 107.5 . . ?
O1W C1 H1B 107.5 . . ?
O1W C1 C3 119.2(11) . . ?
H1A C1 H1B 107.0 . . ?
C3 C1 H1A 107.5 . . ?
C3 C1 H1B 107.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C0AA C2 C1AA C4 0.6(8) . . . . ?
C0AA C6 N2 C7 1.1(5) . . . . ?
C0AA C6 N2 C9 175.3(4) . . . . ?
C2 C0AA C6 C5 1.7(7) . . . . ?
C2 C0AA C6 N2 -178.3(4) . . . . ?
C2 C0AA N1 C7 177.2(5) . . . . ?
C2 C0AA N1 Ni2 2.3(7) . . . 1_545 ?
C2 C1AA C4 C5 -0.4(9) . . . . ?
C1AA C4 C5 C6 0.7(9) . . . . ?
C4 C5 C6 C0AA -1.4(8) . . . . ?
C4 C5 C6 N2 178.6(5) . . . . ?
C5 C6 N2 C7 -178.9(5) . . . . ?
C5 C6 N2 C9 -4.7(9) . . . . ?
C6 C0AA C2 C1AA -1.3(7) . . . . ?
C6 C0AA N1 C7 -0.4(5) . . . . ?
C6 C0AA N1 Ni2 -175.3(3) . . . 1_545 ?
C8 C9 C10 C11 -0.5(8) . . . . ?
C8 C9 N2 C6 -135.6(5) . . . . ?
C8 C9 N2 C7 37.7(6) . . . . ?
C9 C8 C13 C12 1.0(8) . . . . ?
C9 C10 C11 C12 0.4(8) . . . . ?
C10 C9 N2 C6 44.0(7) . . . . ?
C10 C9 N2 C7 -142.8(5) . . . . ?
C10 C11 C12 C13 0.4(7) . . . . ?
C10 C11 C12 N3 177.8(4) . . . . ?
C11 C12 C13 C8 -1.1(8) . . . . ?
C11 C12 N3 C14 -33.3(6) . . . . ?
C11 C12 N3 C15 148.2(5) . . . . ?
C13 C8 C9 C10 -0.2(8) . . . . ?
C13 C8 C9 N2 179.4(4) . . . . ?
C13 C12 N3 C14 144.1(5) . . . . ?
C13 C12 N3 C15 -34.4(7) . . . . ?
C15 C16 C17 C18 -0.4(7) . . . . ?
C15 C16 N4 C14 -0.4(5) . . . . ?
C15 C16 N4 Ni2 175.5(3) . . . . ?
C16 C15 C20 C19 -2.4(7) . . . . ?
C16 C15 N3 C12 178.6(4) . . . . ?
C16 C15 N3 C14 -0.1(5) . . . . ?
C16 C17 C18 C19 -1.2(8) . . . . ?
C17 C16 N4 C14 178.4(5) . . . . ?
C17 C16 N4 Ni2 -5.7(7) . . . . ?
C17 C18 C19 C20 1.1(9) . . . . ?
C18 C19 C20 C15 0.7(8) . . . . ?
C20 C15 C16 C17 2.3(7) . . . . ?
C20 C15 C16 N4 -178.7(4) . . . . ?
C20 C15 N3 C12 -2.5(8) . . . . ?
C20 C15 N3 C14 178.8(5) . . . . ?
C21 C22 C23 C24 -179.7(4) . . . . ?
C21 C22 C28 C27 -177.0(4) . . . . ?
C22 C21 O3 Ni2 -179.6(3) . . . . ?
C22 C21 O4 Ni2 179.7(3) . . . . ?
C22 C23 C24 C25 179.8(4) . . . . ?
C22 C23 C24 C26 -3.2(6) . . . . ?
C23 C22 C28 C27 0.9(7) . . . . ?
C23 C24 C25 O5 -175.8(4) . . . . ?
C23 C24 C25 O6 4.8(6) . . . . ?
C23 C24 C26 C27 0.7(7) . . . . ?
C24 C25 O5 Ni2 -166.1(3) . . . 1_655 ?
C24 C26 C27 C28 2.5(7) . . . . ?
C24 C26 C27 C29 -175.3(4) . . . . ?
C25 C24 C26 C27 177.6(4) . . . . ?
C26 C24 C25 O5 7.4(6) . . . . ?
C26 C24 C25 O6 -172.1(4) . . . . ?
C26 C27 C28 C22 -3.4(7) . . . . ?
C26 C27 C29 N30 -10.8(7) . . . . ?
C26 C27 C29 C34 166.4(5) . . . . ?
C27 C29 N30 C31 179.7(5) . . . . ?
C27 C29 C34 C33 -178.6(5) . . . . ?
C28 C22 C23 C24 2.4(6) . . . . ?
C28 C27 C29 N30 171.5(5) . . . . ?
C28 C27 C29 C34 -11.3(8) . . . . ?
C29 C27 C28 C22 174.4(4) . . . . ?
C29 N30 C31 C32 -1.6(10) . . . . ?
N30 C29 C34 C33 -1.5(9) . . . . ?
N30 C31 C32 C33 -0.3(10) . . . . ?
N30 C31 C32 C35 -178.8(6) . . . . ?
C31 C32 C33 C34 1.4(9) . . . . ?
C31 C32 C35 O1 171.8(5) . . . . ?
C31 C32 C35 O2 -7.4(8) . . . . ?
C32 C33 C34 C29 -0.5(9) . . . . ?
C32 C35 O1 Ni1 -173.9(3) . . . . ?
C33 C32 C35 O1 -6.6(8) . . . . ?
C33 C32 C35 O2 174.2(5) . . . . ?
C34 C29 N30 C31 2.5(8) . . . . ?
C35 C32 C33 C34 179.8(5) . . . . ?
C37 C38 C39 C40 -0.8(13) . . . . ?
C37 C42 N6 C36 1.2(6) . . . . ?
C37 C42 N6 C43 -177.9(5) . . . . ?
C38 C37 C42 C41 -2.2(10) . . . . ?
C38 C37 C42 N6 177.7(6) . . . . ?
C38 C37 N5 C36 -178.0(7) . . . . ?
C38 C37 N5 Ni1 0.8(10) . . . . ?
C38 C39 C40 C41 -0.2(15) . . . . ?
C39 C40 C41 C42 0.0(13) . . . . ?
C40 C41 C42 C37 1.2(11) . . . . ?
C40 C41 C42 N6 -178.7(7) . . . . ?
C41 C42 N6 C36 -178.9(7) . . . . ?
C41 C42 N6 C43 1.9(11) . . . . ?
C42 C37 C38 C39 1.9(11) . . . . ?
C42 C37 N5 C36 0.8(6) . . . . ?
C42 C37 N5 Ni1 179.6(4) . . . . ?
C43 C44 C45 C46 -1.3(9) . . . . ?
C44 C43 C48 C47 0.1(8) . . . . ?
C44 C43 N6 C36 37.2(8) . . . . ?
C44 C43 N6 C42 -143.9(6) . . . . ?
C44 C45 C46 C47 1.6(9) . . . . ?
C44 C45 C46 N7 178.7(5) . . . . ?
C45 C46 C47 C48 -1.1(8) . . . . ?
C45 C46 N7 C49 132.0(6) . . . . ?
C45 C46 N7 C51 -46.7(8) . . . . ?
C46 C47 C48 C43 0.3(8) . . . . ?
C47 C46 N7 C49 -51.0(8) . . . . ?
C47 C46 N7 C51 130.3(6) . . . . ?
C48 C43 C44 C45 0.5(9) . . . . ?
C48 C43 N6 C36 -139.5(5) . . . . ?
C48 C43 N6 C42 39.4(8) . . . . ?
C50 C51 C52 C53 1.4(8) . . . . ?
C50 C51 N7 C46 -180.0(5) . . . . ?
C50 C51 N7 C49 1.1(6) . . . . ?
C51 C50 C55 C54 -0.9(9) . . . . ?
C51 C50 N8 C49 0.5(6) . . . . ?
C51 C52 C53 C54 -4.4(9) . . . . ?
C52 C51 N7 C46 -3.1(9) . . . . ?
C52 C51 N7 C49 178.0(6) . . . . ?
C52 C53 C54 C55 4.9(10) . . . . ?
C53 C54 C55 C50 -2.1(10) . . . . ?
C55 C50 C51 C52 1.2(8) . . . . ?
C55 C50 C51 N7 178.5(5) . . . . ?
C55 C50 N8 C49 -178.9(6) . . . . ?
N1 C0AA C2 C1AA -178.7(5) . . . . ?
N1 C0AA C6 C5 179.6(4) . . . . ?
N1 C0AA C6 N2 -0.4(5) . . . . ?
N1 C7 N2 C6 -1.5(5) . . . . ?
N1 C7 N2 C9 -176.0(4) . . . . ?
N2 C7 N1 C0AA 1.2(5) . . . . ?
N2 C7 N1 Ni2 176.8(3) . . . 1_545 ?
N2 C9 C10 C11 179.9(4) . . . . ?
N3 C12 C13 C8 -178.5(4) . . . . ?
N3 C14 N4 C16 0.4(5) . . . . ?
N3 C14 N4 Ni2 -176.1(3) . . . . ?
N3 C15 C16 C17 -178.6(4) . . . . ?
N3 C15 C16 N4 0.4(5) . . . . ?
N3 C15 C20 C19 178.8(5) . . . . ?
N4 C14 N3 C12 -178.9(4) . . . . ?
N4 C14 N3 C15 -0.2(5) . . . . ?
N4 C16 C17 C18 -179.1(5) . . . . ?
N5 C36 N6 C42 -0.8(6) . . . . ?
N5 C36 N6 C43 178.4(5) . . . . ?
N5 C37 C38 C39 -179.4(7) . . . . ?
N5 C37 C42 C41 178.9(6) . . . . ?
N5 C37 C42 N6 -1.3(6) . . . . ?
N6 C36 N5 C37 0.0(6) . . . . ?
N6 C36 N5 Ni1 -178.9(3) . . . . ?
N6 C43 C44 C45 -176.2(5) . . . . ?
N6 C43 C48 C47 176.7(5) . . . . ?
N7 C46 C47 C48 -178.2(5) . . . . ?
N7 C49 N8 C50 0.2(6) . . . . ?
N7 C51 C52 C53 -175.1(6) . . . . ?
N8 C49 N7 C46 -179.8(5) . . . . ?
N8 C49 N7 C51 -0.9(6) . . . . ?
N8 C50 C51 C52 -178.3(5) . . . . ?
N8 C50 C51 N7 -1.1(6) . . . . ?
N8 C50 C55 C54 178.5(6) . . . . ?
O2 C35 O1 Ni1 5.2(8) . . . . ?
O3 C21 C22 C23 167.5(4) . . . . ?
O3 C21 C22 C28 -14.6(6) . . . . ?
O3 C21 O4 Ni2 1.1(4) . . . . ?
O4 C21 C22 C23 -11.1(6) . . . . ?
O4 C21 C22 C28 166.8(4) . . . . ?
O4 C21 O3 Ni2 -1.1(4) . . . . ?
O6 C25 O5 Ni2 13.3(6) . . . 1_655 ?

_shelx_SHELXL_version_number     2014/7

_olex2_submission_special_instructions 'No special instructions were received'
