# 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 2018

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

data_111
_database_code_depnum_ccdc_archive 'CCDC 1845008'
_audit_update_record             
;
2018-05-24 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_audit_creation_date             2017-11-05
_chemical_formula_sum            'C23 H19 N3 Ni O6'
_chemical_formula_weight         492.120
_refine_ls_R_factor_all          0.041
_cell_length_a                   6.7959(6)
_cell_length_b                   13.2063(13)
_cell_length_c                   21.361(2)
_cell_angle_alpha                90.000
_cell_angle_beta                 91.545(4)
_cell_angle_gamma                90.000
_cell_volume                     1916.4(3)
_cell_formula_units_Z            4
_symmetry_int_tables_number      14
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  -P_2yn

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,1/2+y,1/2-z
3 -x,-y,-z
4 1/2+x,1/2-y,1/2+z

loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_radius_bond
Ni ? 1.200
O ? 1.200
H ? 1.200
N ? 1.200
C ? 1.200


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_attached_hydrogens
_atom_site_calc_flag
_atom_site_thermal_displace_type
_atom_site_u_iso_or_equiv
Ni1 Ni 0.3501(0) 0.352() 0.2321(0) 1.000 4 e ? d Uani 0.01593(10)
O1 O 0.5387(2) 0.6973(1) -0.1468(1) 1.000 4 e ? d Uani 0.0236(4)
O3 O -0.4654(2) 0.6172(1) 0.1802(1) 1.000 4 e ? d Uani 0.0271(4)
O2 O 0.2426(2) 0.7627(1) -0.1725(1) 1.000 4 e ? d Uani 0.0250(4)
O6 O 0.5592(2) 0.2649(1) 0.2785(1) 1.000 4 e ? d Uani 0.0243(4)
H6A H 0.6301 0.3018 0.3041 1.000 4 e ? d Uiso 0.03600
H6B H 0.6371 0.2369 0.2519 1.000 4 e ? d Uiso 0.03600
O4 O -0.4408(2) 0.4702(1) 0.2324(1) 1.000 4 e ? d Uani 0.0264(4)
O5 O 0.1445(2) 0.2319(1) 0.2313(1) 1.000 4 e ? d Uani 0.0257(4)
H5A H 0.0378 0.2492 0.2110 1.000 4 e ? d Uiso 0.03900
H5B H 0.1145 0.2163 0.2692 1.000 4 e ? d Uiso 0.03900
N7 N 0.1420(3) 0.4402(1) 0.1840(1) 1.000 4 e ? d Uani 0.0167(4)
N8 N 0.2680(3) 0.4055(2) 0.3192(1) 1.000 4 e ? d Uani 0.0189(4)
N1 N 0.2348(3) 0.6112(2) 0.6269(1) 1.000 4 e ? d Uani 0.0321(5)
C1 C 0.3605(3) 0.7182(2) -0.1359(1) 1.000 4 e ? d Uani 0.0169(5)
C19 C 0.2389(3) 0.5285(2) 0.5052(1) 1.000 4 e ? d Uani 0.0204(5)
C8 C 0.0794(3) 0.5569(2) 0.0988(1) 1.000 4 e ? d Uani 0.0164(5)
C2 C 0.2875(3) 0.6839(2) -0.0731(1) 1.000 4 e ? d Uani 0.0157(5)
C5 C 0.1517(3) 0.6049(2) 0.0406(1) 1.000 4 e ? d Uani 0.0168(5)
C12 C 0.1966(3) 0.4881(2) 0.1322(1) 1.000 4 e ? d Uani 0.0177(5)
H12 H 0.3213 0.4745 0.1174 1.000 4 e ? calc Uiso 0.02100
C10 C -0.1705(3) 0.5234(2) 0.1740(1) 1.000 4 e ? d Uani 0.0159(5)
C16 C 0.2430(3) 0.4858(2) 0.4409(1) 1.000 4 e ? d Uani 0.0187(5)
C9 C -0.1064(3) 0.5744(2) 0.1220(1) 1.000 4 e ? d Uani 0.0193(5)
H9 H -0.1891 0.6212 0.1021 1.000 4 e ? calc Uiso 0.02300
C11 C -0.0410(3) 0.4568(2) 0.2039(1) 1.000 4 e ? d Uani 0.0171(5)
H11 H -0.0826 0.4223 0.2390 1.000 4 e ? calc Uiso 0.02000
C13 C -0.3768(3) 0.5389(2) 0.1976(1) 1.000 4 e ? d Uani 0.0176(5)
C3 C 0.0887(3) 0.6858(2) -0.0598(1) 1.000 4 e ? d Uani 0.0193(5)
H3 H -0.0008 0.7145 -0.0883 1.000 4 e ? calc Uiso 0.02300
C14 C 0.2431(3) 0.5048(2) 0.3291(1) 1.000 4 e ? d Uani 0.0224(5)
H14 H 0.2351 0.5475 0.2945 1.000 4 e ? calc Uiso 0.02700
C18 C 0.2749(4) 0.3461(2) 0.3699(1) 1.000 4 e ? d Uani 0.0230(5)
H18 H 0.2872 0.2766 0.3642 1.000 4 e ? calc Uiso 0.02800
C23 C 0.2750(4) 0.4704(2) 0.5582(1) 1.000 4 e ? d Uani 0.0276(6)
H23 H 0.3007 0.4016 0.5541 1.000 4 e ? calc Uiso 0.03300
C6 C 0.3518(3) 0.6078(2) 0.0283(1) 1.000 4 e ? d Uani 0.0207(5)
H6 H 0.4425 0.5845 0.0584 1.000 4 e ? calc Uiso 0.02500
C15 C 0.2287(4) 0.5468(2) 0.3876(1) 1.000 4 e ? d Uani 0.0238(5)
H15 H 0.2093 0.6162 0.3918 1.000 4 e ? calc Uiso 0.02900
C4 C 0.0225(3) 0.6453(2) -0.0044(1) 1.000 4 e ? d Uani 0.0202(5)
H4 H -0.1118 0.6452 0.0030 1.000 4 e ? calc Uiso 0.02400
C17 C 0.2648(4) 0.3825(2) 0.4300(1) 1.000 4 e ? d Uani 0.0244(6)
H17 H 0.2725 0.3378 0.4636 1.000 4 e ? calc Uiso 0.02900
C7 C 0.4176(3) 0.6449(2) -0.0278(1) 1.000 4 e ? d Uani 0.0210(5)
H7 H 0.5516 0.6437 -0.0356 1.000 4 e ? calc Uiso 0.02500
C20 C 0.1953(4) 0.6296(2) 0.5156(1) 1.000 4 e ? d Uani 0.0296(6)
H20 H 0.1674 0.6724 0.4819 1.000 4 e ? calc Uiso 0.03600
C22 C 0.2732(4) 0.5137(2) 0.6172(1) 1.000 4 e ? d Uani 0.0292(6)
H22 H 0.3002 0.4727 0.6517 1.000 4 e ? calc Uiso 0.03500
C21 C 0.1933(4) 0.6665(2) 0.5759(1) 1.000 4 e ? d Uani 0.0334(6)
H21 H 0.1610 0.7343 0.5815 1.000 4 e ? calc Uiso 0.04000



loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O6 . . 2.0615(16) no
Ni1 N8 . . 2.0814(19) no
Ni1 N7 . . 2.0815(19) no
Ni1 O1 . 3_665 2.0949(16) no
Ni1 O4 . 1_655 2.1107(17) no
Ni1 O5 . . 2.1136(17) no
O1 C1 . . 1.269(3) no
O1 Ni1 . 3_665 2.0950(16) no
O3 C13 . . 1.248(3) no
O2 C1 . . 1.251(3) no
O4 C13 . . 1.259(3) no
O4 Ni1 . 1_455 2.1107(17) no
N7 C12 . . 1.337(3) no
N7 C11 . . 1.342(3) no
N8 C18 . . 1.336(3) no
N8 C14 . . 1.340(3) no
N1 C22 . . 1.330(4) no
N1 C21 . . 1.336(4) no
C1 C2 . . 1.513(3) no
C19 C23 . . 1.383(3) no
C19 C20 . . 1.387(3) no
C19 C16 . . 1.487(3) no
C8 C9 . . 1.388(3) no
C8 C12 . . 1.392(3) no
C8 C5 . . 1.490(3) no
C2 C3 . . 1.389(3) no
C2 C7 . . 1.391(3) no
C5 C4 . . 1.391(3) no
C5 C6 . . 1.393(3) no
C10 C9 . . 1.380(3) no
C10 C11 . . 1.387(3) no
C10 C13 . . 1.516(3) no
C16 C17 . . 1.393(3) no
C16 C15 . . 1.396(3) no
C3 C4 . . 1.385(3) no
C14 C15 . . 1.375(3) no
C18 C17 . . 1.375(3) no
C23 C22 . . 1.385(3) no
C6 C7 . . 1.381(3) no
C20 C21 . . 1.377(4) no

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O6 Ni1 N8 . . . 87.55(7) no
O6 Ni1 N7 . . . 179.11(7) no
N8 Ni1 N7 . . . 93.19(7) no
O6 Ni1 O1 . . 3_665 89.16(6) no
N8 Ni1 O1 . . 3_665 174.31(7) no
N7 Ni1 O1 . . 3_665 90.07(7) no
O6 Ni1 O4 . . 1_655 87.45(7) no
N8 Ni1 O4 . . 1_655 86.69(7) no
N7 Ni1 O4 . . 1_655 92.08(7) no
O1 Ni1 O4 3_665 . 1_655 88.52(7) no
O6 Ni1 O5 . . . 91.86(7) no
N8 Ni1 O5 . . . 93.96(7) no
N7 Ni1 O5 . . . 88.60(7) no
O1 Ni1 O5 3_665 . . 90.79(7) no
O4 Ni1 O5 1_655 . . 179.03(7) no
C1 O1 Ni1 . . 3_665 126.47(15) no
C13 O4 Ni1 . . 1_455 140.74(16) no
C12 N7 C11 . . . 117.64(19) no
C12 N7 Ni1 . . . 118.24(15) no
C11 N7 Ni1 . . . 124.00(15) no
C18 N8 C14 . . . 116.7(2) no
C18 N8 Ni1 . . . 121.36(16) no
C14 N8 Ni1 . . . 120.72(16) no
C22 N1 C21 . . . 116.0(2) no
O2 C1 O1 . . . 125.9(2) no
O2 C1 C2 . . . 118.4(2) no
O1 C1 C2 . . . 115.7(2) no
C23 C19 C20 . . . 116.0(2) no
C23 C19 C16 . . . 122.5(2) no
C20 C19 C16 . . . 121.5(2) no
C9 C8 C12 . . . 116.1(2) no
C9 C8 C5 . . . 123.4(2) no
C12 C8 C5 . . . 120.5(2) no
C3 C2 C7 . . . 117.9(2) no
C3 C2 C1 . . . 121.4(2) no
C7 C2 C1 . . . 120.7(2) no
C4 C5 C6 . . . 117.4(2) no
C4 C5 C8 . . . 121.6(2) no
C6 C5 C8 . . . 121.0(2) no
N7 C12 C8 . . . 124.4(2) no
C9 C10 C11 . . . 118.0(2) no
C9 C10 C13 . . . 121.1(2) no
C11 C10 C13 . . . 121.0(2) no
C17 C16 C15 . . . 115.8(2) no
C17 C16 C19 . . . 122.1(2) no
C15 C16 C19 . . . 122.1(2) no
C10 C9 C8 . . . 121.1(2) no
N7 C11 C10 . . . 122.8(2) no
O3 C13 O4 . . . 127.0(2) no
O3 C13 C10 . . . 117.2(2) no
O4 C13 C10 . . . 115.8(2) no
C4 C3 C2 . . . 120.5(2) no
N8 C14 C15 . . . 123.4(2) no
N8 C18 C17 . . . 123.4(2) no
C19 C23 C22 . . . 120.6(2) no
C7 C6 C5 . . . 120.9(2) no
C14 C15 C16 . . . 120.3(2) no
C3 C4 C5 . . . 121.7(2) no
C18 C17 C16 . . . 120.4(2) no
C6 C7 C2 . . . 121.4(2) no
C21 C20 C19 . . . 119.8(3) no
N1 C22 C23 . . . 123.3(3) no
N1 C21 C20 . . . 124.2(3) no

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O6 Ni1 N7 C12 . . . . -8.(5) no
N8 Ni1 N7 C12 . . . . 136.83(17) no
O1 Ni1 N7 C12 3_665 . . . -38.50(17) no
O4 Ni1 N7 C12 1_655 . . . 50.03(17) no
O5 Ni1 N7 C12 . . . . -129.28(17) no
O6 Ni1 N7 C11 . . . . 176.(100) no
N8 Ni1 N7 C11 . . . . -39.20(18) no
O1 Ni1 N7 C11 3_665 . . . 145.48(18) no
O4 Ni1 N7 C11 1_655 . . . -126.00(18) no
O5 Ni1 N7 C11 . . . . 54.69(18) no
O6 Ni1 N8 C18 . . . . -34.45(18) no
N7 Ni1 N8 C18 . . . . 146.06(18) no
O1 Ni1 N8 C18 3_665 . . . -89.2(8) no
O4 Ni1 N8 C18 1_655 . . . -122.04(18) no
O5 Ni1 N8 C18 . . . . 57.25(18) no
O6 Ni1 N8 C14 . . . . 132.57(18) no
N7 Ni1 N8 C14 . . . . -46.93(18) no
O1 Ni1 N8 C14 3_665 . . . 77.9(8) no
O4 Ni1 N8 C14 1_655 . . . 44.98(18) no
O5 Ni1 N8 C14 . . . . -135.74(18) no
Ni1 O1 C1 O2 3_665 . . . -38.9(3) no
Ni1 O1 C1 C2 3_665 . . . 140.04(16) no
O2 C1 C2 C3 . . . . 10.6(3) no
O1 C1 C2 C3 . . . . -168.5(2) no
O2 C1 C2 C7 . . . . -172.5(2) no
O1 C1 C2 C7 . . . . 8.5(3) no
C9 C8 C5 C4 . . . . -19.9(3) no
C12 C8 C5 C4 . . . . 158.0(2) no
C9 C8 C5 C6 . . . . 162.3(2) no
C12 C8 C5 C6 . . . . -19.9(3) no
C11 N7 C12 C8 . . . . 2.7(3) no
Ni1 N7 C12 C8 . . . . -173.60(18) no
C9 C8 C12 N7 . . . . -0.7(3) no
C5 C8 C12 N7 . . . . -178.7(2) no
C23 C19 C16 C17 . . . . 6.4(4) no
C20 C19 C16 C17 . . . . -172.7(2) no
C23 C19 C16 C15 . . . . -172.6(2) no
C20 C19 C16 C15 . . . . 8.4(3) no
C11 C10 C9 C8 . . . . 2.3(3) no
C13 C10 C9 C8 . . . . -177.2(2) no
C12 C8 C9 C10 . . . . -1.9(3) no
C5 C8 C9 C10 . . . . 176.1(2) no
C12 N7 C11 C10 . . . . -2.2(3) no
Ni1 N7 C11 C10 . . . . 173.84(17) no
C9 C10 C11 N7 . . . . -0.2(3) no
C13 C10 C11 N7 . . . . 179.3(2) no
Ni1 O4 C13 O3 1_455 . . . 69.9(4) no
Ni1 O4 C13 C10 1_455 . . . -109.5(2) no
C9 C10 C13 O3 . . . . -19.4(3) no
C11 C10 C13 O3 . . . . 161.2(2) no
C9 C10 C13 O4 . . . . 160.1(2) no
C11 C10 C13 O4 . . . . -19.4(3) no
C7 C2 C3 C4 . . . . -3.1(3) no
C1 C2 C3 C4 . . . . 173.9(2) no
C18 N8 C14 C15 . . . . 1.3(3) no
Ni1 N8 C14 C15 . . . . -166.30(18) no
C14 N8 C18 C17 . . . . -2.4(3) no
Ni1 N8 C18 C17 . . . . 165.16(19) no
C20 C19 C23 C22 . . . . -2.1(4) no
C16 C19 C23 C22 . . . . 178.8(2) no
C4 C5 C6 C7 . . . . -3.2(4) no
C8 C5 C6 C7 . . . . 174.7(2) no
N8 C14 C15 C16 . . . . 1.0(4) no
C17 C16 C15 C14 . . . . -2.3(3) no
C19 C16 C15 C14 . . . . 176.7(2) no
C2 C3 C4 C5 . . . . 2.3(4) no
C6 C5 C4 C3 . . . . 0.9(3) no
C8 C5 C4 C3 . . . . -177.0(2) no
N8 C18 C17 C16 . . . . 1.1(4) no
C15 C16 C17 C18 . . . . 1.3(4) no
C19 C16 C17 C18 . . . . -177.7(2) no
C5 C6 C7 C2 . . . . 2.4(4) no
C3 C2 C7 C6 . . . . 0.8(3) no
C1 C2 C7 C6 . . . . -176.2(2) no
C23 C19 C20 C21 . . . . 1.1(4) no
C16 C19 C20 C21 . . . . -179.8(2) no
C21 N1 C22 C23 . . . . 1.2(4) no
C19 C23 C22 N1 . . . . 1.0(4) no
C22 N1 C21 C20 . . . . -2.4(4) no
C19 C20 C21 N1 . . . . 1.3(4) no
####################################################################### 
# 
# 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_111_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1845010'
_audit_update_record             
;
2018-05-24 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H44 N4 Ni4 O24'
_chemical_formula_weight         1343.75

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.3518(4)
_cell_length_b                   16.1904(10)
_cell_length_c                   25.4391(15)
_cell_angle_alpha                107.083(2)
_cell_angle_beta                 95.543(2)
_cell_angle_gamma                92.724(2)
_cell_volume                     2481.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5418
_cell_measurement_theta_min      2.351
_cell_measurement_theta_max      27.695

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    1.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5978
_exptl_absorpt_correction_T_max  0.8442
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            76011
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         25.01
_reflns_number_total             8755
_reflns_number_gt                6514
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1535P)²+18.9924P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8755
_refine_ls_number_parameters     765
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0815
_refine_ls_wR_factor_ref         0.2560
_refine_ls_wR_factor_gt          0.2239
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.95114(16) 0.85990(7) 0.03508(4) 0.0159(3) Uani 1 1 d . . .
Ni2 Ni 0.94585(16) 0.65215(7) -0.02099(4) 0.0166(3) Uani 1 1 d . . .
Ni3 Ni 2.48711(16) 1.17991(7) 0.53246(4) 0.0162(3) Uani 1 1 d . . .
Ni4 Ni 2.51967(16) 1.32886(7) 0.47046(4) 0.0162(3) Uani 1 1 d . . .
O15 O 2.3221(8) 1.2169(4) 0.4672(2) 0.0171(12) Uani 1 1 d . . .
O5 O 0.1221(9) 0.7526(4) 0.0426(2) 0.0179(13) Uani 1 1 d . . .
O13 O 1.1325(9) 0.9472(4) 0.0998(2) 0.0254(14) Uani 1 1 d . . .
O7 O 1.0995(10) 0.9296(4) 0.4412(2) 0.0241(14) Uani 1 1 d . . .
O9 O -0.3149(9) 0.2904(4) -0.4652(2) 0.0192(13) Uani 1 1 d . . .
O3 O 0.7726(9) 0.7580(4) -0.0278(2) 0.0212(13) Uani 1 1 d . . .
O8 O 1.3371(9) 0.8427(4) 0.4021(2) 0.0223(14) Uani 1 1 d . . .
O16 O 2.3068(10) 1.0915(4) 0.3982(3) 0.0301(16) Uani 1 1 d . . .
O1 O 1.1289(10) 0.8693(4) -0.0263(2) 0.0256(14) Uani 1 1 d . . .
H1A H 1.1955 0.9214 -0.0189 0.038 Uiso 1 1 d R . .
H1B H 1.0473 0.8600 -0.0580 0.038 Uiso 1 1 d R . .
O21 O 2.3551(10) 1.4015(4) 0.5311(3) 0.0270(15) Uani 1 1 d . . .
H21A H 2.3427 1.4528 0.5277 0.040 Uiso 1 1 d R . .
H21B H 2.4224 1.4071 0.5634 0.040 Uiso 1 1 d R . .
O2 O -0.3562(10) 0.6476(4) -0.4045(2) 0.0257(14) Uani 1 1 d . . .
O4 O 0.7860(10) 0.8062(4) -0.1016(3) 0.0286(15) Uani 1 1 d . . .
O6 O 0.1180(11) 0.6949(5) 0.1126(3) 0.0343(17) Uani 1 1 d . . .
O11 O 0.4920(10) 0.5139(5) -0.0538(3) 0.0304(16) Uani 1 1 d . . .
O10 O -0.0923(10) 0.5668(4) -0.4345(2) 0.0269(15) Uani 1 1 d . . .
O14 O 1.4025(9) 0.9970(4) 0.0642(2) 0.0230(14) Uani 1 1 d . . .
O12 O 0.7779(10) 0.5608(4) -0.0842(3) 0.0298(15) Uani 1 1 d . . .
O23 O 2.6527(10) 1.1069(4) 0.4721(3) 0.0283(15) Uani 1 1 d . . .
H23A H 2.7631 1.1372 0.4696 0.042 Uiso 1 1 d R . .
H23B H 2.5752 1.0911 0.4409 0.042 Uiso 1 1 d R . .
O17 O 0.7585(10) 0.6379(4) 0.0382(3) 0.0288(15) Uani 1 1 d . . .
H17A H 0.8357 0.6401 0.0689 0.043 Uiso 1 1 d R . .
H17B H 0.6840 0.5880 0.0265 0.043 Uiso 1 1 d R . .
O18 O -0.3130(10) 0.4105(4) -0.3920(3) 0.0291(15) Uani 1 1 d . . .
O19 O 0.7592(10) 0.9519(4) 0.0202(3) 0.0273(15) Uani 1 1 d . . .
H19A H 0.6501 0.9555 0.0386 0.041 Uiso 1 1 d R . .
H19B H 0.7132 0.9382 -0.0149 0.041 Uiso 1 1 d R . .
O20 O 2.7374(10) 1.4330(4) 0.4826(2) 0.0256(14) Uani 1 1 d . . .
H20A H 2.6793 1.4733 0.4721 0.038 Uiso 1 1 d R . .
H20B H 2.8411 1.4168 0.4636 0.038 Uiso 1 1 d R . .
O22 O 2.2782(10) 1.0734(4) 0.5199(2) 0.0270(15) Uani 1 1 d . . .
H22A H 2.2297 1.0519 0.4850 0.040 Uiso 1 1 d R . .
H22B H 2.1707 1.0875 0.5386 0.040 Uiso 1 1 d R . .
O1A O 1.1481(10) 0.5656(4) -0.0028(3) 0.0301(15) Uani 1 1 d . . .
H1AA H 1.2058 0.5852 0.0311 0.045 Uiso 1 1 d R . .
H1AB H 1.2471 0.5583 -0.0243 0.045 Uiso 1 1 d R . .
N3 N 1.7069(10) 1.2541(5) 0.4136(3) 0.0174(15) Uani 1 1 d . . .
N2 N 0.7507(10) 0.8435(4) 0.0929(3) 0.0159(15) Uani 1 1 d . . .
N1 N 0.1437(10) 0.6677(5) -0.0797(3) 0.0176(15) Uani 1 1 d . . .
N4 N 0.2994(11) 0.2536(4) -0.4099(3) 0.0176(15) Uani 1 1 d . . .
C24 C 1.1370(15) 0.8198(6) 0.2964(4) 0.028(2) Uani 1 1 d . . .
H24 H 1.2689 0.7981 0.2997 0.034 Uiso 1 1 calc R . .
C22 C 0.8527(15) 0.8955(7) 0.3377(4) 0.032(2) Uani 1 1 d . . .
H22 H 0.7946 0.9271 0.3689 0.038 Uiso 1 1 calc R . .
C12 C 0.0688(13) 0.6585(5) -0.1318(3) 0.0194(18) Uani 1 1 d . . .
H12 H -0.0722 0.6377 -0.1433 0.023 Uiso 1 1 calc R . .
C39 C 1.3114(13) 0.9884(6) 0.1038(3) 0.0181(18) Uani 1 1 d . . .
C6 C 0.2073(14) 0.6235(6) -0.2722(4) 0.026(2) Uani 1 1 d . . .
H6 H 0.3443 0.6084 -0.2650 0.031 Uiso 1 1 calc R . .
C15 C 0.4222(12) 0.7842(5) 0.1114(3) 0.0156(17) Uani 1 1 d . . .
C27 C 2.2348(12) 1.1604(6) 0.4219(3) 0.0176(18) Uani 1 1 d . . .
C51 C 0.3736(13) 0.2948(5) -0.3570(3) 0.0183(18) Uani 1 1 d . . .
H51 H 0.5089 0.2846 -0.3441 0.022 Uiso 1 1 calc R . .
C7 C 0.1148(14) 0.6068(7) -0.3263(4) 0.030(2) Uani 1 1 d . . .
H7 H 0.1898 0.5791 -0.3553 0.036 Uiso 1 1 calc R . .
C8 C 0.1888(14) 0.6780(6) -0.1705(3) 0.022(2) Uani 1 1 d . . .
C29 C 1.9067(13) 1.2416(6) 0.4303(3) 0.0193(18) Uani 1 1 d . . .
H29 H 1.9691 1.2757 0.4650 0.023 Uiso 1 1 calc R . .
C34 C 1.4212(15) 1.0674(7) 0.2605(4) 0.032(2) Uani 1 1 d . . .
H34 H 1.3503 1.0679 0.2909 0.039 Uiso 1 1 calc R . .
C21 C 0.7401(14) 0.8797(7) 0.2861(4) 0.029(2) Uani 1 1 d . . .
H21 H 0.6043 0.8982 0.2832 0.035 Uiso 1 1 calc R . .
C37 C 1.6317(15) 1.0629(7) 0.1701(4) 0.030(2) Uani 1 1 d . . .
H37 H 1.7045 1.0603 0.1397 0.036 Uiso 1 1 calc R . .
C38 C 1.7327(15) 1.1004(7) 0.2223(4) 0.031(2) Uani 1 1 d . . .
H38 H 1.8723 1.1237 0.2269 0.038 Uiso 1 1 calc R . .
C28 C 2.0248(13) 1.1801(5) 0.3981(4) 0.0196(18) Uani 1 1 d . . .
C42 C 0.2992(14) 0.4448(6) -0.1652(4) 0.027(2) Uani 1 1 d . . .
H42 H 0.2103 0.4506 -0.1376 0.032 Uiso 1 1 calc R . .
C50 C 0.1015(13) 0.2670(6) -0.4276(3) 0.0192(18) Uani 1 1 d U . .
H50 H 0.0439 0.2357 -0.4634 0.023 Uiso 1 1 calc R . .
C43 C 0.2187(13) 0.4060(6) -0.2202(4) 0.026(2) Uani 1 1 d . . .
H43 H 0.0752 0.3876 -0.2292 0.031 Uiso 1 1 calc R . .
C49 C -0.0205(13) 0.3254(5) -0.3950(3) 0.0165(17) Uani 1 1 d . . .
C11 C 0.3476(13) 0.6970(5) -0.0639(3) 0.0165(17) Uani 1 1 d . . .
H11 H 0.4055 0.6999 -0.0283 0.020 Uiso 1 1 calc R . .
C4 C -0.1074(15) 0.6876(7) -0.2395(4) 0.034(2) Uani 1 1 d . . .
H4 H -0.1830 0.7145 -0.2104 0.041 Uiso 1 1 calc R . .
C45 C 0.5645(16) 0.4229(7) -0.2473(4) 0.039(3) Uani 1 1 d . . .
H45 H 0.6553 0.4147 -0.2747 0.047 Uiso 1 1 calc R . .
C1 C -0.1834(13) 0.6146(6) -0.3968(3) 0.0190(19) Uani 1 1 d . . .
C3 C -0.1959(14) 0.6719(7) -0.2945(4) 0.031(2) Uani 1 1 d . . .
H3 H -0.3300 0.6896 -0.3017 0.037 Uiso 1 1 calc R . .
C36 C 1.4209(14) 1.0282(6) 0.1615(4) 0.0206(19) Uani 1 1 d . . .
C5 C 0.0940(13) 0.6627(6) -0.2289(4) 0.024(2) Uani 1 1 d . . .
C26 C 1.1705(13) 0.8813(5) 0.3996(3) 0.0182(18) Uani 1 1 d . . .
C33 C 1.6291(13) 1.1042(6) 0.2689(4) 0.024(2) Uani 1 1 d . . .
C13 C 0.6959(13) 0.7658(6) -0.0749(4) 0.0208(19) Uani 1 1 d . . .
C46 C 0.6436(14) 0.4630(7) -0.1924(4) 0.033(2) Uani 1 1 d . . .
H46 H 0.7866 0.4821 -0.1833 0.040 Uiso 1 1 calc R . .
C19 C 0.5109(13) 0.7896(6) 0.1641(4) 0.023(2) Uani 1 1 d . . .
H19 H 0.4323 0.7700 0.1877 0.028 Uiso 1 1 calc R . .
C47 C 0.2600(13) 0.3517(5) -0.3207(3) 0.0182(18) Uani 1 1 d . . .
C35 C 1.3183(15) 1.0299(6) 0.2075(4) 0.030(2) Uani 1 1 d . . .
H35 H 1.1794 1.0057 0.2028 0.036 Uiso 1 1 calc R . .
C23 C 1.0495(13) 0.8653(5) 0.3436(3) 0.0173(18) Uani 1 1 d . . .
C16 C 0.5456(13) 0.8133(5) 0.0768(3) 0.0184(18) Uani 1 1 d . . .
H16 H 0.4847 0.8118 0.0418 0.022 Uiso 1 1 calc R . .
C9 C 0.3960(13) 0.7138(6) -0.1514(3) 0.023(2) Uani 1 1 d . . .
H9 H 0.4796 0.7312 -0.1749 0.027 Uiso 1 1 calc R . .
C20 C 0.8262(13) 0.8365(6) 0.2387(3) 0.0210(19) Uani 1 1 d . . .
C31 C 1.7325(14) 1.1481(6) 0.3253(3) 0.0196(18) Uani 1 1 d . . .
C17 C 0.8316(12) 0.8484(5) 0.1442(3) 0.0136(17) Uani 1 1 d U . .
H17 H 0.9728 0.8692 0.1554 0.016 Uiso 1 1 calc R . .
C48 C 0.0639(13) 0.3695(6) -0.3408(4) 0.0217(19) Uani 1 1 d . . .
H48 H -0.0119 0.4108 -0.3184 0.026 Uiso 1 1 calc R . .
C30 C 1.6230(14) 1.2092(6) 0.3620(3) 0.0221(19) Uani 1 1 d . . .
H30 H 1.4862 1.2190 0.3499 0.026 Uiso 1 1 calc R . .
C2 C -0.0880(13) 0.6306(6) -0.3383(3) 0.0189(18) Uani 1 1 d . . .
C32 C 1.9333(13) 1.1320(6) 0.3446(3) 0.0222(19) Uani 1 1 d . . .
H32 H 2.0071 1.0898 0.3222 0.027 Uiso 1 1 calc R . .
C44 C 0.3487(14) 0.3944(6) -0.2619(4) 0.0225(19) Uani 1 1 d . . .
C40 C 0.5988(13) 0.5197(5) -0.0914(3) 0.0191(19) Uani 1 1 d . . .
C18 C 0.7178(13) 0.8244(6) 0.1815(3) 0.0187(18) Uani 1 1 d . . .
C10 C 0.4762(13) 0.7231(5) -0.0978(3) 0.0181(18) Uani 1 1 d . . .
C41 C 0.5114(14) 0.4749(6) -0.1512(3) 0.0218(19) Uani 1 1 d . . .
C52 C -0.2327(13) 0.3453(6) -0.4177(3) 0.0173(18) Uani 1 1 d . . .
C25 C 1.0268(14) 0.8070(7) 0.2445(4) 0.030(2) Uani 1 1 d . . .
H25 H 1.0879 0.7782 0.2131 0.036 Uiso 1 1 calc R . .
C14 C 0.2021(13) 0.7410(6) 0.0888(3) 0.0182(18) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O13 2.036(6) . ?
Ni1 O1 2.050(6) . ?
Ni1 O19 2.065(6) . ?
Ni1 N2 2.100(7) . ?
Ni1 O3 2.118(6) . ?
Ni1 O5 2.137(6) 1_655 ?
Ni2 O12 2.009(6) . ?
Ni2 O17 2.064(6) . ?
Ni2 O1A 2.066(6) . ?
Ni2 N1 2.104(7) 1_655 ?
Ni2 O5 2.109(5) 1_655 ?
Ni2 O3 2.120(6) . ?
Ni3 O8 2.046(6) 2_976 ?
Ni3 O22 2.053(6) . ?
Ni3 O23 2.055(6) . ?
Ni3 N4 2.107(7) 1_766 ?
Ni3 O9 2.120(6) 1_866 ?
Ni3 O15 2.127(6) . ?
Ni4 O2 2.029(6) 2_775 ?
Ni4 O21 2.055(6) . ?
Ni4 O20 2.059(6) . ?
Ni4 N3 2.101(7) 1_655 ?
Ni4 O9 2.121(6) 1_866 ?
Ni4 O15 2.130(6) . ?
O15 C27 1.297(10) . ?
O5 C14 1.304(10) . ?
O5 Ni2 2.109(5) 1_455 ?
O5 Ni1 2.137(6) 1_455 ?
O13 C39 1.269(10) . ?
O7 C26 1.253(10) . ?
O9 C52 1.313(10) . ?
O9 Ni3 2.120(6) 1_244 ?
O9 Ni4 2.121(6) 1_244 ?
O3 C13 1.292(10) . ?
O8 C26 1.260(10) . ?
O8 Ni3 2.046(6) 2_976 ?
O16 C27 1.234(11) . ?
O1 H1A 0.8847 . ?
O1 H1B 0.8832 . ?
O21 H21A 0.8655 . ?
O21 H21B 0.8652 . ?
O2 C1 1.266(10) . ?
O2 Ni4 2.029(6) 2_775 ?
O4 C13 1.232(11) . ?
O6 C14 1.223(11) . ?
O11 C40 1.247(11) . ?
O10 C1 1.252(11) . ?
O14 C39 1.246(10) . ?
O12 C40 1.260(10) . ?
O23 H23A 0.8556 . ?
O23 H23B 0.8557 . ?
O17 H17A 0.8724 . ?
O17 H17B 0.8720 . ?
O18 C52 1.230(11) . ?
O19 H19A 0.8694 . ?
O19 H19B 0.8702 . ?
O20 H20A 0.8607 . ?
O20 H20B 0.8603 . ?
O22 H22A 0.8715 . ?
O22 H22B 0.8705 . ?
O1A H1AA 0.8627 . ?
O1A H1AB 0.8624 . ?
N3 C29 1.343(11) . ?
N3 C30 1.343(11) . ?
N3 Ni4 2.101(7) 1_455 ?
N2 C17 1.335(10) . ?
N2 C16 1.350(11) . ?
N1 C12 1.326(10) . ?
N1 C11 1.339(10) . ?
N1 Ni2 2.104(7) 1_455 ?
N4 C51 1.340(11) . ?
N4 C50 1.344(11) . ?
N4 Ni3 2.107(7) 1_344 ?
C24 C25 1.386(12) . ?
C24 C23 1.392(13) . ?
C24 H24 0.9300 . ?
C22 C23 1.375(12) . ?
C22 C21 1.379(13) . ?
C22 H22 0.9300 . ?
C12 C8 1.397(12) . ?
C12 H12 0.9300 . ?
C39 C36 1.502(12) . ?
C6 C5 1.386(13) . ?
C6 C7 1.387(12) . ?
C6 H6 0.9300 . ?
C15 C19 1.381(12) . ?
C15 C16 1.396(12) . ?
C15 C14 1.513(11) . ?
C27 C28 1.499(11) . ?
C51 C47 1.384(12) . ?
C51 H51 0.9300 . ?
C7 C2 1.393(12) . ?
C7 H7 0.9300 . ?
C8 C9 1.394(12) . ?
C8 C5 1.493(12) . ?
C29 C28 1.391(12) . ?
C29 H29 0.9300 . ?
C34 C35 1.388(13) . ?
C34 C33 1.394(13) . ?
C34 H34 0.9300 . ?
C21 C20 1.382(13) . ?
C21 H21 0.9300 . ?
C37 C38 1.369(13) . ?
C37 C36 1.398(12) . ?
C37 H37 0.9300 . ?
C38 C33 1.396(13) . ?
C38 H38 0.9300 . ?
C28 C32 1.407(12) . ?
C42 C41 1.387(12) . ?
C42 C43 1.389(12) . ?
C42 H42 0.9300 . ?
C50 C49 1.385(12) . ?
C50 H50 0.9300 . ?
C43 C44 1.380(13) . ?
C43 H43 0.9300 . ?
C49 C48 1.392(12) . ?
C49 C52 1.501(11) . ?
C11 C10 1.380(12) . ?
C11 H11 0.9300 . ?
C4 C5 1.385(13) . ?
C4 C3 1.401(13) . ?
C4 H4 0.9300 . ?
C45 C46 1.388(13) . ?
C45 C44 1.404(13) . ?
C45 H45 0.9300 . ?
C1 C2 1.496(11) . ?
C3 C2 1.383(13) . ?
C3 H3 0.9300 . ?
C36 C35 1.388(13) . ?
C26 C23 1.499(12) . ?
C33 C31 1.474(11) . ?
C13 C10 1.510(12) . ?
C46 C41 1.381(13) . ?
C46 H46 0.9300 . ?
C19 C18 1.382(12) . ?
C19 H19 0.9300 . ?
C47 C48 1.376(12) . ?
C47 C44 1.493(12) . ?
C35 H35 0.9300 . ?
C16 H16 0.9300 . ?
C9 C10 1.371(12) . ?
C9 H9 0.9300 . ?
C20 C25 1.392(13) . ?
C20 C18 1.502(11) . ?
C31 C32 1.385(12) . ?
C31 C30 1.407(12) . ?
C17 C18 1.377(11) . ?
C17 H17 0.9300 . ?
C48 H48 0.9300 . ?
C30 H30 0.9300 . ?
C32 H32 0.9300 . ?
C40 C41 1.516(11) . ?
C25 H25 0.9300 . ?

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
O13 Ni1 O1 97.8(2) . . ?
O13 Ni1 O19 93.4(3) . . ?
O1 Ni1 O19 90.9(3) . . ?
O13 Ni1 N2 86.9(2) . . ?
O1 Ni1 N2 175.3(3) . . ?
O19 Ni1 N2 88.3(3) . . ?
O13 Ni1 O3 173.4(2) . . ?
O1 Ni1 O3 85.0(2) . . ?
O19 Ni1 O3 92.6(2) . . ?
N2 Ni1 O3 90.4(2) . . ?
O13 Ni1 O5 94.0(2) . 1_655 ?
O1 Ni1 O5 88.9(2) . 1_655 ?
O19 Ni1 O5 172.6(2) . 1_655 ?
N2 Ni1 O5 91.2(2) . 1_655 ?
O3 Ni1 O5 80.0(2) . 1_655 ?
O12 Ni2 O17 95.4(3) . . ?
O12 Ni2 O1A 93.3(3) . . ?
O17 Ni2 O1A 90.7(3) . . ?
O12 Ni2 N1 85.9(3) . 1_655 ?
O17 Ni2 N1 178.5(3) . 1_655 ?
O1A Ni2 N1 88.5(3) . 1_655 ?
O12 Ni2 O5 176.9(3) . 1_655 ?
O17 Ni2 O5 86.7(2) . 1_655 ?
O1A Ni2 O5 89.0(2) . 1_655 ?
N1 Ni2 O5 92.0(2) 1_655 1_655 ?
O12 Ni2 O3 97.1(3) . . ?
O17 Ni2 O3 88.6(2) . . ?
O1A Ni2 O3 169.6(2) . . ?
N1 Ni2 O3 92.0(2) 1_655 . ?
O5 Ni2 O3 80.6(2) 1_655 . ?
O8 Ni3 O22 93.5(3) 2_976 . ?
O8 Ni3 O23 96.2(2) 2_976 . ?
O22 Ni3 O23 88.8(3) . . ?
O8 Ni3 N4 87.4(2) 2_976 1_766 ?
O22 Ni3 N4 89.5(3) . 1_766 ?
O23 Ni3 N4 176.1(3) . 1_766 ?
O8 Ni3 O9 94.0(2) 2_976 1_866 ?
O22 Ni3 O9 172.3(2) . 1_866 ?
O23 Ni3 O9 88.6(2) . 1_866 ?
N4 Ni3 O9 92.7(3) 1_766 1_866 ?
O8 Ni3 O15 173.8(2) 2_976 . ?
O22 Ni3 O15 92.5(2) . . ?
O23 Ni3 O15 85.3(2) . . ?
N4 Ni3 O15 91.2(2) 1_766 . ?
O9 Ni3 O15 80.0(2) 1_866 . ?
O2 Ni4 O21 98.1(2) 2_775 . ?
O2 Ni4 O20 92.8(3) 2_775 . ?
O21 Ni4 O20 90.3(3) . . ?
O2 Ni4 N3 86.4(3) 2_775 1_655 ?
O21 Ni4 N3 175.3(3) . 1_655 ?
O20 Ni4 N3 88.3(3) . 1_655 ?
O2 Ni4 O9 174.1(2) 2_775 1_866 ?
O21 Ni4 O9 85.7(2) . 1_866 ?
O20 Ni4 O9 91.8(2) . 1_866 ?
N3 Ni4 O9 89.9(2) 1_655 1_866 ?
O2 Ni4 O15 95.4(2) 2_775 . ?
O21 Ni4 O15 89.2(2) . . ?
O20 Ni4 O15 171.8(2) . . ?
N3 Ni4 O15 91.4(3) 1_655 . ?
O9 Ni4 O15 79.9(2) 1_866 . ?
C27 O15 Ni3 122.1(5) . . ?
C27 O15 Ni4 124.6(5) . . ?
Ni3 O15 Ni4 99.7(2) . . ?
C14 O5 Ni2 122.0(5) . 1_455 ?
C14 O5 Ni1 125.9(5) . 1_455 ?
Ni2 O5 Ni1 99.5(2) 1_455 1_455 ?
C39 O13 Ni1 132.6(5) . . ?
C52 O9 Ni3 120.7(5) . 1_244 ?
C52 O9 Ni4 123.4(5) . 1_244 ?
Ni3 O9 Ni4 100.3(2) 1_244 1_244 ?
C13 O3 Ni1 123.3(6) . . ?
C13 O3 Ni2 122.6(5) . . ?
Ni1 O3 Ni2 99.8(2) . . ?
C26 O8 Ni3 131.4(5) . 2_976 ?
Ni1 O1 H1A 112.2 . . ?
Ni1 O1 H1B 110.6 . . ?
H1A O1 H1B 106.7 . . ?
Ni4 O21 H21A 110.6 . . ?
Ni4 O21 H21B 109.7 . . ?
H21A O21 H21B 108.3 . . ?
C1 O2 Ni4 134.6(6) . 2_775 ?
C40 O12 Ni2 134.9(6) . . ?
Ni3 O23 H23A 109.2 . . ?
Ni3 O23 H23B 110.1 . . ?
H23A O23 H23B 109.1 . . ?
Ni2 O17 H17A 111.2 . . ?
Ni2 O17 H17B 110.3 . . ?
H17A O17 H17B 107.9 . . ?
Ni1 O19 H19A 110.8 . . ?
Ni1 O19 H19B 110.2 . . ?
H19A O19 H19B 108.2 . . ?
Ni4 O20 H20A 110.3 . . ?
Ni4 O20 H20B 109.6 . . ?
H20A O20 H20B 108.7 . . ?
Ni3 O22 H22A 110.9 . . ?
Ni3 O22 H22B 110.3 . . ?
H22A O22 H22B 108.0 . . ?
Ni2 O1A H1AA 110.3 . . ?
Ni2 O1A H1AB 109.6 . . ?
H1AA O1A H1AB 108.7 . . ?
C29 N3 C30 118.3(7) . . ?
C29 N3 Ni4 120.1(5) . 1_455 ?
C30 N3 Ni4 121.1(5) . 1_455 ?
C17 N2 C16 117.8(7) . . ?
C17 N2 Ni1 120.3(5) . . ?
C16 N2 Ni1 120.9(6) . . ?
C12 N1 C11 117.3(7) . . ?
C12 N1 Ni2 122.1(6) . 1_455 ?
C11 N1 Ni2 120.2(5) . 1_455 ?
C51 N4 C50 117.5(7) . . ?
C51 N4 Ni3 123.2(5) . 1_344 ?
C50 N4 Ni3 118.9(6) . 1_344 ?
C25 C24 C23 119.8(8) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C23 C22 C21 120.9(9) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
N1 C12 C8 124.1(8) . . ?
N1 C12 H12 118.0 . . ?
C8 C12 H12 118.0 . . ?
O14 C39 O13 125.5(8) . . ?
O14 C39 C36 118.4(7) . . ?
O13 C39 C36 116.1(7) . . ?
C5 C6 C7 119.5(8) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C19 C15 C16 118.8(7) . . ?
C19 C15 C14 121.5(7) . . ?
C16 C15 C14 119.5(7) . . ?
O16 C27 O15 125.6(8) . . ?
O16 C27 C28 118.1(8) . . ?
O15 C27 C28 116.3(7) . . ?
N4 C51 C47 123.6(7) . . ?
N4 C51 H51 118.2 . . ?
C47 C51 H51 118.2 . . ?
C6 C7 C2 121.5(8) . . ?
C6 C7 H7 119.3 . . ?
C2 C7 H7 119.3 . . ?
C9 C8 C12 116.8(8) . . ?
C9 C8 C5 122.6(8) . . ?
C12 C8 C5 120.6(8) . . ?
N3 C29 C28 123.0(8) . . ?
N3 C29 H29 118.5 . . ?
C28 C29 H29 118.5 . . ?
C35 C34 C33 120.9(9) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C22 C21 C20 120.9(8) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C38 C37 C36 121.2(9) . . ?
C38 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?
C37 C38 C33 120.9(9) . . ?
C37 C38 H38 119.5 . . ?
C33 C38 H38 119.5 . . ?
C29 C28 C32 118.1(8) . . ?
C29 C28 C27 120.5(8) . . ?
C32 C28 C27 121.1(8) . . ?
C41 C42 C43 120.4(8) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
N4 C50 C49 122.8(7) . . ?
N4 C50 H50 118.6 . . ?
C49 C50 H50 118.6 . . ?
C44 C43 C42 120.9(8) . . ?
C44 C43 H43 119.6 . . ?
C42 C43 H43 119.6 . . ?
C50 C49 C48 118.1(7) . . ?
C50 C49 C52 121.5(7) . . ?
C48 C49 C52 120.3(7) . . ?
N1 C11 C10 123.2(8) . . ?
N1 C11 H11 118.4 . . ?
C10 C11 H11 118.4 . . ?
C5 C4 C3 119.2(9) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C46 C45 C44 120.5(9) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
O10 C1 O2 124.7(8) . . ?
O10 C1 C2 117.9(7) . . ?
O2 C1 C2 117.3(8) . . ?
C2 C3 C4 121.3(9) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C35 C36 C37 118.2(8) . . ?
C35 C36 C39 121.3(8) . . ?
C37 C36 C39 120.5(8) . . ?
C4 C5 C6 120.3(8) . . ?
C4 C5 C8 119.7(8) . . ?
C6 C5 C8 120.0(8) . . ?
O7 C26 O8 123.7(8) . . ?
O7 C26 C23 119.2(7) . . ?
O8 C26 C23 117.1(7) . . ?
C34 C33 C38 118.1(8) . . ?
C34 C33 C31 120.4(8) . . ?
C38 C33 C31 121.5(8) . . ?
O4 C13 O3 125.2(8) . . ?
O4 C13 C10 118.2(8) . . ?
O3 C13 C10 116.6(7) . . ?
C41 C46 C45 120.5(9) . . ?
C41 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C15 C19 C18 119.3(8) . . ?
C15 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C48 C47 C51 117.9(8) . . ?
C48 C47 C44 120.8(8) . . ?
C51 C47 C44 121.3(7) . . ?
C34 C35 C36 120.6(9) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C22 C23 C24 119.1(8) . . ?
C22 C23 C26 121.0(8) . . ?
C24 C23 C26 120.0(7) . . ?
N2 C16 C15 121.9(8) . . ?
N2 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C10 C9 C8 119.6(8) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C21 C20 C25 118.2(8) . . ?
C21 C20 C18 122.9(8) . . ?
C25 C20 C18 118.9(8) . . ?
C32 C31 C30 117.8(8) . . ?
C32 C31 C33 123.3(8) . . ?
C30 C31 C33 118.9(8) . . ?
N2 C17 C18 123.8(7) . . ?
N2 C17 H17 118.1 . . ?
C18 C17 H17 118.1 . . ?
C47 C48 C49 119.7(8) . . ?
C47 C48 H48 120.1 . . ?
C49 C48 H48 120.1 . . ?
N3 C30 C31 123.0(8) . . ?
N3 C30 H30 118.5 . . ?
C31 C30 H30 118.5 . . ?
C3 C2 C7 118.1(8) . . ?
C3 C2 C1 120.9(8) . . ?
C7 C2 C1 120.9(8) . . ?
C31 C32 C28 119.6(8) . . ?
C31 C32 H32 120.2 . . ?
C28 C32 H32 120.2 . . ?
C43 C44 C45 118.4(8) . . ?
C43 C44 C47 120.2(8) . . ?
C45 C44 C47 121.4(8) . . ?
O11 C40 O12 125.3(8) . . ?
O11 C40 C41 119.2(8) . . ?
O12 C40 C41 115.4(8) . . ?
C17 C18 C19 118.3(7) . . ?
C17 C18 C20 118.2(7) . . ?
C19 C18 C20 123.6(8) . . ?
C9 C10 C11 118.7(8) . . ?
C9 C10 C13 121.0(8) . . ?
C11 C10 C13 120.2(8) . . ?
C46 C41 C42 119.2(8) . . ?
C46 C41 C40 120.1(8) . . ?
C42 C41 C40 120.7(7) . . ?
O18 C52 O9 125.6(8) . . ?
O18 C52 C49 119.0(7) . . ?
O9 C52 C49 115.4(7) . . ?
C24 C25 C20 121.1(8) . . ?
C24 C25 H25 119.5 . . ?
C20 C25 H25 119.5 . . ?
O6 C14 O5 125.0(8) . . ?
O6 C14 C15 119.3(7) . . ?
O5 C14 C15 115.6(7) . . ?

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
O8 Ni3 O15 C27 156.6(19) 2_976 . . . ?
O22 Ni3 O15 C27 -36.7(6) . . . . ?
O23 Ni3 O15 C27 51.9(6) . . . . ?
N4 Ni3 O15 C27 -126.2(6) 1_766 . . . ?
O9 Ni3 O15 C27 141.3(6) 1_866 . . . ?
O8 Ni3 O15 Ni4 15(2) 2_976 . . . ?
O22 Ni3 O15 Ni4 -178.6(2) . . . . ?
O23 Ni3 O15 Ni4 -90.1(3) . . . . ?
N4 Ni3 O15 Ni4 91.8(3) 1_766 . . . ?
O9 Ni3 O15 Ni4 -0.7(2) 1_866 . . . ?
O2 Ni4 O15 C27 36.2(6) 2_775 . . . ?
O21 Ni4 O15 C27 134.3(6) . . . . ?
O20 Ni4 O15 C27 -138.7(15) . . . . ?
N3 Ni4 O15 C27 -50.3(6) 1_655 . . . ?
O9 Ni4 O15 C27 -140.0(6) 1_866 . . . ?
O2 Ni4 O15 Ni3 176.9(2) 2_775 . . . ?
O21 Ni4 O15 Ni3 -85.0(2) . . . . ?
O20 Ni4 O15 Ni3 2.0(17) . . . . ?
N3 Ni4 O15 Ni3 90.3(3) 1_655 . . . ?
O9 Ni4 O15 Ni3 0.7(2) 1_866 . . . ?
O1 Ni1 O13 C39 -7.1(8) . . . . ?
O19 Ni1 O13 C39 -98.5(8) . . . . ?
N2 Ni1 O13 C39 173.3(8) . . . . ?
O3 Ni1 O13 C39 107(2) . . . . ?
O5 Ni1 O13 C39 82.3(8) 1_655 . . . ?
O13 Ni1 O3 C13 -166.6(18) . . . . ?
O1 Ni1 O3 C13 -51.3(6) . . . . ?
O19 Ni1 O3 C13 39.4(6) . . . . ?
N2 Ni1 O3 C13 127.7(6) . . . . ?
O5 Ni1 O3 C13 -141.1(6) 1_655 . . . ?
O13 Ni1 O3 Ni2 -26(2) . . . . ?
O1 Ni1 O3 Ni2 88.9(3) . . . . ?
O19 Ni1 O3 Ni2 179.6(2) . . . . ?
N2 Ni1 O3 Ni2 -92.1(3) . . . . ?
O5 Ni1 O3 Ni2 -0.9(2) 1_655 . . . ?
O12 Ni2 O3 C13 -36.3(6) . . . . ?
O17 Ni2 O3 C13 -131.6(6) . . . . ?
O1A Ni2 O3 C13 142.1(13) . . . . ?
N1 Ni2 O3 C13 49.8(6) 1_655 . . . ?
O5 Ni2 O3 C13 141.5(6) 1_655 . . . ?
O12 Ni2 O3 Ni1 -176.9(3) . . . . ?
O17 Ni2 O3 Ni1 87.8(3) . . . . ?
O1A Ni2 O3 Ni1 1.6(15) . . . . ?
N1 Ni2 O3 Ni1 -90.8(3) 1_655 . . . ?
O5 Ni2 O3 Ni1 0.9(2) 1_655 . . . ?
O17 Ni2 O12 C40 13.2(9) . . . . ?
O1A Ni2 O12 C40 104.3(9) . . . . ?
N1 Ni2 O12 C40 -167.5(9) 1_655 . . . ?
O5 Ni2 O12 C40 -120(4) 1_655 . . . ?
O3 Ni2 O12 C40 -76.0(9) . . . . ?
O13 Ni1 N2 C17 -34.6(6) . . . . ?
O1 Ni1 N2 C17 151(3) . . . . ?
O19 Ni1 N2 C17 -128.0(6) . . . . ?
O3 Ni1 N2 C17 139.4(6) . . . . ?
O5 Ni1 N2 C17 59.4(6) 1_655 . . . ?
O13 Ni1 N2 C16 157.0(6) . . . . ?
O1 Ni1 N2 C16 -17(3) . . . . ?
O19 Ni1 N2 C16 63.6(6) . . . . ?
O3 Ni1 N2 C16 -29.0(6) . . . . ?
O5 Ni1 N2 C16 -109.0(6) 1_655 . . . ?
C11 N1 C12 C8 -0.6(13) . . . . ?
Ni2 N1 C12 C8 172.1(7) 1_455 . . . ?
Ni1 O13 C39 O14 15.4(14) . . . . ?
Ni1 O13 C39 C36 -163.6(6) . . . . ?
Ni3 O15 C27 O16 -36.4(11) . . . . ?
Ni4 O15 C27 O16 96.0(9) . . . . ?
Ni3 O15 C27 C28 141.1(6) . . . . ?
Ni4 O15 C27 C28 -86.4(8) . . . . ?
C50 N4 C51 C47 -1.9(13) . . . . ?
Ni3 N4 C51 C47 171.9(7) 1_344 . . . ?
C5 C6 C7 C2 1.7(16) . . . . ?
N1 C12 C8 C9 -3.6(14) . . . . ?
N1 C12 C8 C5 177.8(8) . . . . ?
C30 N3 C29 C28 -4.7(13) . . . . ?
Ni4 N3 C29 C28 167.2(7) 1_455 . . . ?
C23 C22 C21 C20 -3.1(16) . . . . ?
C36 C37 C38 C33 0.9(16) . . . . ?
N3 C29 C28 C32 3.2(13) . . . . ?
N3 C29 C28 C27 -171.3(8) . . . . ?
O16 C27 C28 C29 160.9(8) . . . . ?
O15 C27 C28 C29 -16.9(12) . . . . ?
O16 C27 C28 C32 -13.5(13) . . . . ?
O15 C27 C28 C32 168.7(8) . . . . ?
C51 N4 C50 C49 4.6(13) . . . . ?
Ni3 N4 C50 C49 -169.4(7) 1_344 . . . ?
C41 C42 C43 C44 1.8(15) . . . . ?
N4 C50 C49 C48 -2.5(13) . . . . ?
N4 C50 C49 C52 174.0(8) . . . . ?
C12 N1 C11 C10 4.6(12) . . . . ?
Ni2 N1 C11 C10 -168.3(6) 1_455 . . . ?
Ni4 O2 C1 O10 -19.5(14) 2_775 . . . ?
Ni4 O2 C1 C2 163.7(6) 2_775 . . . ?
C5 C4 C3 C2 1.2(16) . . . . ?
C38 C37 C36 C35 -2.3(15) . . . . ?
C38 C37 C36 C39 179.1(9) . . . . ?
O14 C39 C36 C35 172.3(9) . . . . ?
O13 C39 C36 C35 -8.7(13) . . . . ?
O14 C39 C36 C37 -9.1(13) . . . . ?
O13 C39 C36 C37 169.9(9) . . . . ?
C3 C4 C5 C6 0.6(16) . . . . ?
C3 C4 C5 C8 -179.2(9) . . . . ?
C7 C6 C5 C4 -2.1(15) . . . . ?
C7 C6 C5 C8 177.8(9) . . . . ?
C9 C8 C5 C4 -133.6(10) . . . . ?
C12 C8 C5 C4 45.0(14) . . . . ?
C9 C8 C5 C6 46.6(14) . . . . ?
C12 C8 C5 C6 -134.9(10) . . . . ?
Ni3 O8 C26 O7 14.6(13) 2_976 . . . ?
Ni3 O8 C26 C23 -163.5(6) 2_976 . . . ?
C35 C34 C33 C38 -1.6(16) . . . . ?
C35 C34 C33 C31 176.6(9) . . . . ?
C37 C38 C33 C34 1.1(16) . . . . ?
C37 C38 C33 C31 -177.1(9) . . . . ?
Ni1 O3 C13 O4 38.4(12) . . . . ?
Ni2 O3 C13 O4 -93.1(10) . . . . ?
Ni1 O3 C13 C10 -140.1(6) . . . . ?
Ni2 O3 C13 C10 88.4(8) . . . . ?
C44 C45 C46 C41 0.6(17) . . . . ?
C16 C15 C19 C18 0.7(13) . . . . ?
C14 C15 C19 C18 175.6(8) . . . . ?
N4 C51 C47 C48 -2.9(13) . . . . ?
N4 C51 C47 C44 178.7(8) . . . . ?
C33 C34 C35 C36 0.2(16) . . . . ?
C37 C36 C35 C34 1.8(15) . . . . ?
C39 C36 C35 C34 -179.6(9) . . . . ?
C21 C22 C23 C24 1.5(15) . . . . ?
C21 C22 C23 C26 -179.0(9) . . . . ?
C25 C24 C23 C22 1.1(15) . . . . ?
C25 C24 C23 C26 -178.5(9) . . . . ?
O7 C26 C23 C22 -6.6(13) . . . . ?
O8 C26 C23 C22 171.5(9) . . . . ?
O7 C26 C23 C24 172.9(8) . . . . ?
O8 C26 C23 C24 -8.9(12) . . . . ?
C17 N2 C16 C15 -2.8(12) . . . . ?
Ni1 N2 C16 C15 165.9(6) . . . . ?
C19 C15 C16 N2 2.4(12) . . . . ?
C14 C15 C16 N2 -172.5(7) . . . . ?
C12 C8 C9 C10 3.9(13) . . . . ?
C5 C8 C9 C10 -177.5(8) . . . . ?
C22 C21 C20 C25 2.1(15) . . . . ?
C22 C21 C20 C18 -174.6(9) . . . . ?
C34 C33 C31 C32 131.3(10) . . . . ?
C38 C33 C31 C32 -50.5(14) . . . . ?
C34 C33 C31 C30 -48.5(13) . . . . ?
C38 C33 C31 C30 129.7(10) . . . . ?
C16 N2 C17 C18 0.0(12) . . . . ?
Ni1 N2 C17 C18 -168.7(7) . . . . ?
C51 C47 C48 C49 5.0(13) . . . . ?
C44 C47 C48 C49 -176.6(8) . . . . ?
C50 C49 C48 C47 -2.5(13) . . . . ?
C52 C49 C48 C47 -179.0(8) . . . . ?
C29 N3 C30 C31 2.0(13) . . . . ?
Ni4 N3 C30 C31 -169.9(7) 1_455 . . . ?
C32 C31 C30 N3 2.2(14) . . . . ?
C33 C31 C30 N3 -178.0(8) . . . . ?
C4 C3 C2 C7 -1.6(15) . . . . ?
C4 C3 C2 C1 -179.6(9) . . . . ?
C6 C7 C2 C3 0.2(15) . . . . ?
C6 C7 C2 C1 178.2(9) . . . . ?
O10 C1 C2 C3 -170.4(9) . . . . ?
O2 C1 C2 C3 6.6(13) . . . . ?
O10 C1 C2 C7 11.7(13) . . . . ?
O2 C1 C2 C7 -171.3(9) . . . . ?
C30 C31 C32 C28 -3.6(13) . . . . ?
C33 C31 C32 C28 176.6(9) . . . . ?
C29 C28 C32 C31 1.1(13) . . . . ?
C27 C28 C32 C31 175.6(8) . . . . ?
C42 C43 C44 C45 -0.1(15) . . . . ?
C42 C43 C44 C47 179.3(9) . . . . ?
C46 C45 C44 C43 -1.1(16) . . . . ?
C46 C45 C44 C47 179.5(10) . . . . ?
C48 C47 C44 C43 40.3(13) . . . . ?
C51 C47 C44 C43 -141.3(9) . . . . ?
C48 C47 C44 C45 -140.3(10) . . . . ?
C51 C47 C44 C45 38.1(14) . . . . ?
Ni2 O12 C40 O11 -16.4(15) . . . . ?
Ni2 O12 C40 C41 163.4(6) . . . . ?
N2 C17 C18 C19 3.1(13) . . . . ?
N2 C17 C18 C20 -177.6(8) . . . . ?
C15 C19 C18 C17 -3.3(13) . . . . ?
C15 C19 C18 C20 177.4(8) . . . . ?
C21 C20 C18 C17 128.2(10) . . . . ?
C25 C20 C18 C17 -48.5(12) . . . . ?
C21 C20 C18 C19 -52.5(14) . . . . ?
C25 C20 C18 C19 130.8(10) . . . . ?
C8 C9 C10 C11 -0.3(13) . . . . ?
C8 C9 C10 C13 -176.8(8) . . . . ?
N1 C11 C10 C9 -4.2(13) . . . . ?
N1 C11 C10 C13 172.4(8) . . . . ?
O4 C13 C10 C9 13.4(13) . . . . ?
O3 C13 C10 C9 -168.0(8) . . . . ?
O4 C13 C10 C11 -163.1(8) . . . . ?
O3 C13 C10 C11 15.6(12) . . . . ?
C45 C46 C41 C42 1.1(16) . . . . ?
C45 C46 C41 C40 -179.3(10) . . . . ?
C43 C42 C41 C46 -2.3(15) . . . . ?
C43 C42 C41 C40 178.1(9) . . . . ?
O11 C40 C41 C46 -165.0(9) . . . . ?
O12 C40 C41 C46 15.3(13) . . . . ?
O11 C40 C41 C42 14.6(13) . . . . ?
O12 C40 C41 C42 -165.2(9) . . . . ?
Ni3 O9 C52 O18 -91.6(9) 1_244 . . . ?
Ni4 O9 C52 O18 38.0(11) 1_244 . . . ?
Ni3 O9 C52 C49 89.7(7) 1_244 . . . ?
Ni4 O9 C52 C49 -140.6(6) 1_244 . . . ?
C50 C49 C52 O18 -163.6(8) . . . . ?
C48 C49 C52 O18 12.8(13) . . . . ?
C50 C49 C52 O9 15.1(12) . . . . ?
C48 C49 C52 O9 -168.5(8) . . . . ?
C23 C24 C25 C20 -2.1(16) . . . . ?
C21 C20 C25 C24 0.5(15) . . . . ?
C18 C20 C25 C24 177.4(9) . . . . ?
Ni2 O5 C14 O6 -35.9(11) 1_455 . . . ?
Ni1 O5 C14 O6 98.1(10) 1_455 . . . ?
Ni2 O5 C14 C15 140.0(6) 1_455 . . . ?
Ni1 O5 C14 C15 -86.1(8) 1_455 . . . ?
C19 C15 C14 O6 -15.0(13) . . . . ?
C16 C15 C14 O6 159.8(8) . . . . ?
C19 C15 C14 O5 168.9(8) . . . . ?
C16 C15 C14 O5 -16.2(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.134
####################################################################### 
# 
# 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_111_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1845012'
_audit_update_record             
;
2018-05-24 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H15 N3 Ni O6'
_chemical_formula_weight         440.05

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.315(2)
_cell_length_b                   10.7544(9)
_cell_length_c                   17.4714(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 131.595(8)
_cell_angle_gamma                90.00
_cell_volume                     3557.3(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6452
_cell_measurement_theta_min      2.338
_cell_measurement_theta_max      28.345

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1808
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6852
_exptl_absorpt_correction_T_max  0.8571
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8414
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3139
_reflns_number_gt                2554
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0550P)²+8.8978P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3139
_refine_ls_number_parameters     275
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1195
_refine_ls_wR_factor_gt          0.1103
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.086
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.21940(2) 0.58462(4) 0.40666(3) 0.01926(17) Uani 1 1 d . . .
O1 O 0.74109(13) 0.3293(2) 0.6501(2) 0.0289(6) Uani 1 1 d . . .
O4 O 0.31598(13) 0.5029(3) 0.5133(2) 0.0357(7) Uani 1 1 d . . .
O2B O 0.8001(8) 0.1611(15) 0.7170(13) 0.0392(18) Uani 0.330(15) 1 d PU A 2
N4 N 0.18194(16) 0.5126(3) 0.4725(2) 0.0268(7) Uani 1 1 d . . .
O3 O 0.38744(14) 0.6682(3) 0.5812(2) 0.0430(8) Uani 1 1 d . . .
N6 N 0.11641(16) 0.4832(3) 0.5119(2) 0.0276(7) Uani 1 1 d . . .
N7 N 0.68980(17) 0.0696(3) 0.8117(3) 0.0311(8) Uani 1 1 d . . .
C4 C 0.61321(18) 0.2423(3) 0.7109(3) 0.0254(8) Uani 1 1 d . . .
C2 C 0.71399(19) 0.2010(3) 0.7281(3) 0.0262(8) Uani 1 1 d . A .
C7 C 0.55179(19) 0.3207(3) 0.6727(3) 0.0264(8) Uani 1 1 d . . .
C3 C 0.65467(18) 0.2711(3) 0.6879(3) 0.0259(8) Uani 1 1 d . . .
H3 H 0.6426 0.3380 0.6451 0.031 Uiso 1 1 calc R . .
C1 C 0.76097(19) 0.2374(3) 0.7071(3) 0.0268(8) Uani 1 1 d . . .
C14 C 0.1231(2) 0.5414(4) 0.4515(3) 0.0330(9) Uani 1 1 d . . .
H14 H 0.0898 0.5965 0.4000 0.040 Uiso 1 1 calc R . .
C18 C 0.0129(2) 0.5922(4) 0.4602(4) 0.0426(11) Uani 1 1 d . . .
H18 H 0.0215 0.6553 0.4332 0.051 Uiso 1 1 calc R . .
C12 C 0.49059(19) 0.2703(4) 0.6443(3) 0.0311(9) Uani 1 1 d . . .
H12 H 0.4879 0.1851 0.6501 0.037 Uiso 1 1 calc R . .
C5 C 0.63296(19) 0.1389(3) 0.7723(3) 0.0274(8) Uani 1 1 d . . .
H5 H 0.6050 0.1166 0.7870 0.033 Uiso 1 1 calc R . .
C17 C 0.05754(19) 0.4928(4) 0.5069(3) 0.0276(8) Uani 1 1 d . . .
C10 C 0.43616(19) 0.4715(4) 0.5994(3) 0.0280(8) Uani 1 1 d . . .
C6 C 0.7298(2) 0.1009(3) 0.7901(3) 0.0307(9) Uani 1 1 d . . .
H6 H 0.7698 0.0537 0.8178 0.037 Uiso 1 1 calc R A .
C9 C 0.4980(2) 0.5229(4) 0.6288(4) 0.0410(11) Uani 1 1 d . . .
H9 H 0.5008 0.6083 0.6238 0.049 Uiso 1 1 calc R . .
C11 C 0.43313(19) 0.3454(4) 0.6072(3) 0.0319(9) Uani 1 1 d . . .
H11 H 0.3922 0.3096 0.5874 0.038 Uiso 1 1 calc R . .
C8 C 0.5548(2) 0.4492(4) 0.6649(4) 0.0395(11) Uani 1 1 d . . .
H8 H 0.5956 0.4852 0.6844 0.047 Uiso 1 1 calc R . .
C13 C 0.37500(19) 0.5544(4) 0.5615(3) 0.0297(9) Uani 1 1 d . . .
C19 C -0.0451(2) 0.5998(4) 0.4525(3) 0.0396(11) Uani 1 1 d . . .
H19 H -0.0756 0.6674 0.4200 0.048 Uiso 1 1 calc R . .
O6 O 0.12414(15) 0.6757(3) 0.2948(3) 0.0591(10) Uani 1 1 d . . .
H6A H 0.0914 0.6223 0.2537 0.089 Uiso 1 1 d R . .
H6B H 0.1285 0.7244 0.2602 0.089 Uiso 1 1 d R . .
C16 C 0.2147(3) 0.4298(5) 0.5508(4) 0.0600(15) Uani 1 1 d U . .
H16 H 0.2573 0.3900 0.5817 0.072 Uiso 1 1 calc R . .
C15 C 0.1749(3) 0.4146(6) 0.5763(4) 0.0714(18) Uani 1 1 d U . .
H15 H 0.1863 0.3653 0.6292 0.086 Uiso 1 1 calc R . .
O5 O 0.2663(3) 0.7312(6) 0.5250(4) 0.0273(14) Uani 0.50 1 d PU . .
O7 O 0.5000 0.7720(8) 0.7500 0.123(3) Uani 1 2 d SG . .
H7A H 0.4623 0.7386 0.6972 0.184 Uiso 0.50 1 d PG . .
H7B H 0.5235 0.7190 0.7981 0.184 Uiso 0.50 1 d PG . .
O2A O 0.8228(4) 0.1864(7) 0.7633(8) 0.0392(18) Uani 0.670(15) 1 d PU A 1


_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 2.040(2) 5_666 ?
Ni1 O4 2.043(3) . ?
Ni1 N4 2.067(3) . ?
Ni1 O6 2.082(3) . ?
Ni1 N7 2.102(3) 8_455 ?
Ni1 O5 2.215(6) 7_566 ?
Ni1 O5 2.216(6) . ?
O1 C1 1.247(4) . ?
O1 Ni1 2.040(2) 5_666 ?
O4 C13 1.256(5) . ?
O2B C1 1.207(15) . ?
N4 C14 1.311(5) . ?
N4 C16 1.359(5) . ?
O3 C13 1.254(5) . ?
N6 C14 1.332(5) . ?
N6 C15 1.339(6) . ?
N6 C17 1.437(5) . ?
N7 C5 1.336(5) . ?
N7 C6 1.337(5) . ?
N7 Ni1 2.101(3) 8_556 ?
C4 C3 1.385(5) . ?
C4 C5 1.388(5) . ?
C4 C7 1.482(5) . ?
C2 C6 1.384(5) . ?
C2 C3 1.385(5) . ?
C2 C1 1.511(5) . ?
C7 C12 1.385(5) . ?
C7 C8 1.395(6) . ?
C1 O2A 1.293(8) . ?
C18 C17 1.363(5) . ?
C18 C19 1.387(6) . ?
C12 C11 1.391(5) . ?
C17 C19 1.375(5) 5_566 ?
C10 C11 1.370(6) . ?
C10 C9 1.398(5) . ?
C10 C13 1.506(5) . ?
C9 C8 1.374(6) . ?
C19 C17 1.375(5) 5_566 ?
C16 C15 1.354(7) . ?
O5 O5 0.807(9) 7_566 ?
O5 Ni1 2.215(6) 7_566 ?

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 O4 87.84(10) 5_666 . ?
O1 Ni1 N4 174.50(12) 5_666 . ?
O4 Ni1 N4 92.56(11) . . ?
O1 Ni1 O6 88.09(11) 5_666 . ?
O4 Ni1 O6 175.89(11) . . ?
N4 Ni1 O6 91.44(12) . . ?
O1 Ni1 N7 90.40(12) 5_666 8_455 ?
O4 Ni1 N7 87.95(13) . 8_455 ?
N4 Ni1 N7 95.10(12) . 8_455 ?
O6 Ni1 N7 92.67(15) . 8_455 ?
O1 Ni1 O5 84.22(19) 5_666 7_566 ?
O4 Ni1 O5 102.99(15) . 7_566 ?
N4 Ni1 O5 90.34(19) . 7_566 ?
O6 Ni1 O5 76.00(16) . 7_566 ?
N7 Ni1 O5 167.57(15) 8_455 7_566 ?
O1 Ni1 O5 89.94(19) 5_666 . ?
O4 Ni1 O5 83.06(15) . . ?
N4 Ni1 O5 84.67(19) . . ?
O6 Ni1 O5 96.35(16) . . ?
N7 Ni1 O5 170.98(15) 8_455 . ?
O5 Ni1 O5 21.0(2) 7_566 . ?
C1 O1 Ni1 132.8(2) . 5_666 ?
C13 O4 Ni1 126.4(3) . . ?
C14 N4 C16 104.9(3) . . ?
C14 N4 Ni1 127.6(3) . . ?
C16 N4 Ni1 127.4(3) . . ?
C14 N6 C15 105.8(3) . . ?
C14 N6 C17 126.2(3) . . ?
C15 N6 C17 128.0(3) . . ?
C5 N7 C6 118.3(3) . . ?
C5 N7 Ni1 123.0(3) . 8_556 ?
C6 N7 Ni1 118.8(2) . 8_556 ?
C3 C4 C5 116.8(3) . . ?
C3 C4 C7 120.9(3) . . ?
C5 C4 C7 122.3(3) . . ?
C6 C2 C3 118.3(3) . . ?
C6 C2 C1 121.8(3) . . ?
C3 C2 C1 119.9(3) . . ?
C12 C7 C8 118.2(3) . . ?
C12 C7 C4 121.9(3) . . ?
C8 C7 C4 119.8(3) . . ?
C2 C3 C4 120.4(3) . . ?
O2B C1 O1 120.8(8) . . ?
O2B C1 O2A 30.6(6) . . ?
O1 C1 O2A 125.9(4) . . ?
O2B C1 C2 119.5(8) . . ?
O1 C1 C2 115.7(3) . . ?
O2A C1 C2 117.1(4) . . ?
N4 C14 N6 112.7(3) . . ?
C17 C18 C19 120.5(4) . . ?
C7 C12 C11 121.0(4) . . ?
N7 C5 C4 123.8(3) . . ?
C18 C17 C19 119.6(4) . 5_566 ?
C18 C17 N6 120.4(3) . . ?
C19 C17 N6 119.9(3) 5_566 . ?
C11 C10 C9 118.5(3) . . ?
C11 C10 C13 121.4(3) . . ?
C9 C10 C13 120.1(4) . . ?
N7 C6 C2 122.4(3) . . ?
C8 C9 C10 121.0(4) . . ?
C10 C11 C12 120.7(4) . . ?
C9 C8 C7 120.5(4) . . ?
O3 C13 O4 125.7(4) . . ?
O3 C13 C10 117.4(3) . . ?
O4 C13 C10 116.9(4) . . ?
C17 C19 C18 119.9(4) 5_566 . ?
C15 C16 N4 108.7(4) . . ?
N6 C15 C16 107.8(4) . . ?
O5 O5 Ni1 79.6(9) 7_566 7_566 ?
O5 O5 Ni1 79.5(9) 7_566 . ?
Ni1 O5 Ni1 159.0(2) 7_566 . ?

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 Ni1 O4 C13 41.7(3) 5_666 . . . ?
N4 Ni1 O4 C13 -132.8(3) . . . . ?
O6 Ni1 O4 C13 33(2) . . . . ?
N7 Ni1 O4 C13 132.1(3) 8_455 . . . ?
O5 Ni1 O4 C13 -41.9(4) 7_566 . . . ?
O5 Ni1 O4 C13 -48.5(4) . . . . ?
O1 Ni1 N4 C14 75.5(12) 5_666 . . . ?
O4 Ni1 N4 C14 169.6(3) . . . . ?
O6 Ni1 N4 C14 -9.5(4) . . . . ?
N7 Ni1 N4 C14 -102.3(4) 8_455 . . . ?
O5 Ni1 N4 C14 66.6(4) 7_566 . . . ?
O5 Ni1 N4 C14 86.8(4) . . . . ?
O1 Ni1 N4 C16 -100.8(12) 5_666 . . . ?
O4 Ni1 N4 C16 -6.7(4) . . . . ?
O6 Ni1 N4 C16 174.3(4) . . . . ?
N7 Ni1 N4 C16 81.5(4) 8_455 . . . ?
O5 Ni1 N4 C16 -109.7(4) 7_566 . . . ?
O5 Ni1 N4 C16 -89.5(4) . . . . ?
C3 C4 C7 C12 144.7(4) . . . . ?
C5 C4 C7 C12 -36.6(6) . . . . ?
C3 C4 C7 C8 -35.4(6) . . . . ?
C5 C4 C7 C8 143.3(4) . . . . ?
C6 C2 C3 C4 1.0(6) . . . . ?
C1 C2 C3 C4 -176.7(3) . . . . ?
C5 C4 C3 C2 -2.1(5) . . . . ?
C7 C4 C3 C2 176.7(4) . . . . ?
Ni1 O1 C1 O2B -20.7(12) 5_666 . . . ?
Ni1 O1 C1 O2A 15.6(8) 5_666 . . . ?
Ni1 O1 C1 C2 -177.9(2) 5_666 . . . ?
C6 C2 C1 O2B 22.6(11) . . . . ?
C3 C2 C1 O2B -159.8(10) . . . . ?
C6 C2 C1 O1 -179.9(4) . . . . ?
C3 C2 C1 O1 -2.2(5) . . . . ?
C6 C2 C1 O2A -12.2(7) . . . . ?
C3 C2 C1 O2A 165.4(6) . . . . ?
C16 N4 C14 N6 0.6(5) . . . . ?
Ni1 N4 C14 N6 -176.3(3) . . . . ?
C15 N6 C14 N4 0.9(5) . . . . ?
C17 N6 C14 N4 -178.6(3) . . . . ?
C8 C7 C12 C11 1.1(6) . . . . ?
C4 C7 C12 C11 -179.0(4) . . . . ?
C6 N7 C5 C4 -0.5(6) . . . . ?
Ni1 N7 C5 C4 178.9(3) 8_556 . . . ?
C3 C4 C5 N7 1.9(6) . . . . ?
C7 C4 C5 N7 -176.9(4) . . . . ?
C19 C18 C17 C19 -0.5(8) . . . 5_566 ?
C19 C18 C17 N6 178.1(4) . . . . ?
C14 N6 C17 C18 -20.7(6) . . . . ?
C15 N6 C17 C18 159.9(5) . . . . ?
C14 N6 C17 C19 157.9(4) . . . 5_566 ?
C15 N6 C17 C19 -21.5(7) . . . 5_566 ?
C5 N7 C6 C2 -0.7(6) . . . . ?
Ni1 N7 C6 C2 179.9(3) 8_556 . . . ?
C3 C2 C6 N7 0.5(6) . . . . ?
C1 C2 C6 N7 178.1(4) . . . . ?
C11 C10 C9 C8 -0.1(7) . . . . ?
C13 C10 C9 C8 179.1(4) . . . . ?
C9 C10 C11 C12 0.5(6) . . . . ?
C13 C10 C11 C12 -178.7(4) . . . . ?
C7 C12 C11 C10 -1.1(6) . . . . ?
C10 C9 C8 C7 0.2(7) . . . . ?
C12 C7 C8 C9 -0.7(7) . . . . ?
C4 C7 C8 C9 179.4(4) . . . . ?
Ni1 O4 C13 O3 26.4(6) . . . . ?
Ni1 O4 C13 C10 -154.1(3) . . . . ?
C11 C10 C13 O3 161.7(4) . . . . ?
C9 C10 C13 O3 -17.5(6) . . . . ?
C11 C10 C13 O4 -17.8(5) . . . . ?
C9 C10 C13 O4 163.0(4) . . . . ?
C17 C18 C19 C17 0.5(8) . . . 5_566 ?
C14 N4 C16 C15 -1.9(6) . . . . ?
Ni1 N4 C16 C15 175.0(4) . . . . ?
C14 N6 C15 C16 -2.1(7) . . . . ?
C17 N6 C15 C16 177.4(4) . . . . ?
N4 C16 C15 N6 2.5(7) . . . . ?
O1 Ni1 O5 O5 73.8(9) 5_666 . . 7_566 ?
O4 Ni1 O5 O5 161.7(9) . . . 7_566 ?
N4 Ni1 O5 O5 -105.1(9) . . . 7_566 ?
O6 Ni1 O5 O5 -14.2(9) . . . 7_566 ?
N7 Ni1 O5 O5 166.0(6) 8_455 . . 7_566 ?
O1 Ni1 O5 Ni1 73.8(9) 5_666 . . 7_566 ?
O4 Ni1 O5 Ni1 161.7(9) . . . 7_566 ?
N4 Ni1 O5 Ni1 -105.1(9) . . . 7_566 ?
O6 Ni1 O5 Ni1 -14.2(9) . . . 7_566 ?
N7 Ni1 O5 Ni1 166.0(6) 8_455 . . 7_566 ?
O5 Ni1 O5 Ni1 -0.006(2) 7_566 . . 7_566 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.083
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_111_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1845009'
_audit_update_record             
;
2018-05-24 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_audit_creation_date             2017-11-05
_chemical_formula_sum            'C27 H25 N5 Ni O6'
_chemical_formula_weight         574.230
_refine_ls_R_factor_all          0.096
_cell_length_a                   23.8398(12)
_cell_length_b                   13.0355(6)
_cell_length_c                   16.7711(8)
_cell_angle_alpha                90.000
_cell_angle_beta                 103.743(2)
_cell_angle_gamma                90.000
_cell_volume                     5062.6(4)
_cell_formula_units_Z            8
_symmetry_int_tables_number      15
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  -C_2yc

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z

loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_radius_bond
Ni ? 1.200
O ? 1.200
N ? 1.200
C ? 1.200
H ? 1.200


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_attached_hydrogens
_atom_site_calc_flag
_atom_site_thermal_displace_type
_atom_site_u_iso_or_equiv
Ni1 Ni 0.7151(0) 0.3698(0) 0.7035(0) 1.000 8 f ? d Uani 0.01938(18)
O4 O 0.2728(1) 0.2413(2) 0.1787(2) 1.000 8 f ? d Uani 0.0287(8)
O2 O 0.6797(1) 0.3711(2) 0.5787(2) 1.000 8 f ? d Uani 0.0320(8)
O1 O 0.6964(2) 0.5290(3) 0.5398(2) 1.000 8 f ? d Uani 0.0425(10)
O3 O 0.3576(1) 0.1595(2) 0.2143(2) 1.000 8 f ? d Uani 0.0371(9)
N5 N 0.3427(2) 0.5116(3) 0.2799(2) 1.000 8 f ? d Uani 0.0248(9)
N4 N 0.6569(2) 0.2571(3) 0.7125(2) 1.000 8 f ? d Uani 0.0266(9)
N1 N 0.2553(2) 0.1480(3) 0.3271(2) 1.000 8 f ? d Uani 0.0282(9)
N3 N 0.6034(2) 0.1180(3) 0.6856(2) 1.000 8 f ? d Uani 0.0263(9)
N2 N 0.3032(2) 0.1310(3) 0.4558(2) 1.000 8 f ? d Uani 0.0301(9)
C24 C 0.3552(2) 0.3373(3) 0.2420(3) 1.000 8 f ? d Uani 0.020(1)
C27 C 0.3268(2) 0.2375(3) 0.2074(3) 1.000 8 f ? d Uani 0.0236(10)
C23 C 0.4134(2) 0.3425(3) 0.2805(3) 1.000 8 f ? d Uani 0.0241(11)
H23 H 0.4371 0.2859 0.2799 1.000 8 f ? calc Uiso 0.02900
C19 C 0.4975(2) 0.4369(4) 0.3698(3) 1.000 8 f ? d Uani 0.0243(10)
C15 C 0.6665(2) 0.4501(4) 0.5336(3) 1.000 8 f ? d Uani 0.0258(11)
C20 C 0.5298(2) 0.5275(4) 0.3770(3) 1.000 8 f ? d Uani 0.0367(13)
H20 H 0.5143 0.5860 0.3482 1.000 8 f ? calc Uiso 0.04400
C22 C 0.4364(2) 0.4319(3) 0.3199(3) 1.000 8 f ? d Uani 0.0226(10)
C26 C 0.3993(2) 0.5140(3) 0.3180(3) 1.000 8 f ? d Uani 0.023(1)
H26 H 0.4142 0.5742 0.3445 1.000 8 f ? calc Uiso 0.02800
C1 C 0.2676(2) 0.2435(4) 0.3618(3) 1.000 8 f ? d Uani 0.0292(11)
H1 H 0.2572 0.3054 0.3349 1.000 8 f ? calc Uiso 0.03500
C21 C 0.5851(2) 0.5291(4) 0.4273(3) 1.000 8 f ? d Uani 0.0367(13)
H21 H 0.6067 0.5891 0.4309 1.000 8 f ? calc Uiso 0.04400
C8 C 0.5124(2) 0.0403(4) 0.6106(3) 1.000 8 f ? d Uani 0.0303(11)
C25 C 0.3220(2) 0.4237(3) 0.2432(3) 1.000 8 f ? d Uani 0.0229(10)
H25 H 0.2830 0.4207 0.2170 1.000 8 f ? calc Uiso 0.02700
C5 C 0.3931(2) 0.0660(4) 0.5534(3) 1.000 8 f ? d Uani 0.0273(11)
C7 C 0.4744(2) -0.0349(4) 0.6215(3) 1.000 8 f ? d Uani 0.0347(12)
H7 H 0.4887 -0.0948 0.6491 1.000 8 f ? calc Uiso 0.04200
C16 C 0.6090(2) 0.4446(4) 0.4723(3) 1.000 8 f ? d Uani 0.0243(10)
C12 C 0.5904(2) 0.1627(4) 0.7528(3) 1.000 8 f ? d Uani 0.0338(12)
H12 H 0.5639 0.1396 0.7813 1.000 8 f ? calc Uiso 0.04100
C6 C 0.4151(2) -0.0234(4) 0.5922(3) 1.000 8 f ? d Uani 0.0342(12)
H6 H 0.3903 -0.0760 0.5989 1.000 8 f ? calc Uiso 0.04100
C11 C 0.5768(2) 0.0263(4) 0.6431(4) 1.000 8 f ? d Uani 0.0389(13)
H11A H 0.5839 -0.0314 0.6807 1.000 8 f ? calc Uiso 0.04700
H11B H 0.5944 0.0111 0.5979 1.000 8 f ? calc Uiso 0.04700
C4 C 0.3281(2) 0.0812(4) 0.5343(3) 1.000 8 f ? d Uani 0.0344(12)
H4A H 0.3100 0.0147 0.5347 1.000 8 f ? calc Uiso 0.04100
H4B H 0.3188 0.1219 0.5778 1.000 8 f ? calc Uiso 0.04100
C9 C 0.4899(2) 0.1283(4) 0.5687(3) 1.000 8 f ? d Uani 0.0371(13)
H9 H 0.5148 0.1793 0.5593 1.000 8 f ? calc Uiso 0.04500
C2 C 0.2770(2) 0.0827(4) 0.3859(3) 1.000 8 f ? d Uani 0.0296(11)
H2 H 0.2745 0.0118 0.3800 1.000 8 f ? calc Uiso 0.03600
O6 O 0.7162(4) 0.1561(5) 0.5202(5) 1.000 8 f ? d Uani 0.123(3)
H6A H 0.7459 0.1487 0.5011 1.000 8 f ? d Uiso 0.18400
H6B H 0.6948 0.2027 0.4935 1.000 8 f ? d Uiso 0.18400
C14 C 0.6429(2) 0.1782(4) 0.6634(3) 1.000 8 f ? d Uani 0.0275(11)
H14 H 0.6585 0.1653 0.6185 1.000 8 f ? calc Uiso 0.03300
C17 C 0.5775(2) 0.3546(4) 0.4624(3) 1.000 8 f ? d Uani 0.0377(13)
H17 H 0.5936 0.2957 0.4898 1.000 8 f ? calc Uiso 0.04500
C13 C 0.6240(2) 0.2475(4) 0.7694(3) 1.000 8 f ? d Uani 0.0312(12)
H13 H 0.6247 0.2925 0.8127 1.000 8 f ? calc Uiso 0.03700
C3 C 0.2968(2) 0.2339(4) 0.4407(3) 1.000 8 f ? d Uani 0.0338(12)
H3 H 0.3100 0.2868 0.4776 1.000 8 f ? calc Uiso 0.04100
C10 C 0.4306(2) 0.1419(4) 0.5405(3) 1.000 8 f ? d Uani 0.0373(13)
H10 H 0.4162 0.2018 0.5130 1.000 8 f ? calc Uiso 0.04500
C18 C 0.5223(2) 0.3512(4) 0.4120(3) 1.000 8 f ? d Uani 0.0360(13)
H18 H 0.5017 0.2900 0.4066 1.000 8 f ? calc Uiso 0.04300
O5 O 0.7734(1) 0.4861(2) 0.6887(2) 1.000 8 f ? d Uani 0.0286(8)



loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N4 . . 2.052(4) no
Ni1 O2 . . 2.063(3) no
Ni1 N1 . 8 2.079(4) no
Ni1 O4 . 8 2.105(3) no
Ni1 O5 . . 2.109(3) no
Ni1 N5 . 3_666 2.132(4) no
O4 C27 . . 1.266(5) no
O4 Ni1 . 8_454 2.105(3) no
O2 C15 . . 1.272(6) no
O1 C15 . . 1.241(6) no
O3 C27 . . 1.243(5) no
N5 C25 . . 1.339(6) no
N5 C26 . . 1.349(5) no
N5 Ni1 . 3_666 2.132(4) no
N4 C14 . . 1.310(6) no
N4 C13 . . 1.376(6) no
N1 C2 . . 1.313(6) no
N1 C1 . . 1.376(6) no
N1 Ni1 . 8_454 2.079(4) no
N3 C14 . . 1.345(6) no
N3 C12 . . 1.369(6) no
N3 C11 . . 1.457(6) no
N2 C2 . . 1.347(6) no
N2 C3 . . 1.367(6) no
N2 C4 . . 1.461(6) no
C24 C25 . . 1.380(6) no
C24 C23 . . 1.385(6) no
C24 C27 . . 1.517(6) no
C23 C22 . . 1.387(6) no
C19 C18 . . 1.379(6) no
C19 C20 . . 1.399(6) no
C19 C22 . . 1.500(6) no
C15 C16 . . 1.508(6) no
C20 C21 . . 1.386(7) no
C22 C26 . . 1.384(6) no
C1 C3 . . 1.346(7) no
C21 C16 . . 1.380(7) no
C8 C7 . . 1.377(7) no
C8 C9 . . 1.386(7) no
C8 C11 . . 1.513(7) no
C5 C6 . . 1.376(7) no
C5 C10 . . 1.385(7) no
C5 C4 . . 1.517(7) no
C7 C6 . . 1.389(7) no
C16 C17 . . 1.380(7) no
C12 C13 . . 1.354(7) no
C9 C10 . . 1.391(7) no
C17 C18 . . 1.385(7) no

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N4 Ni1 O2 . . . 87.63(14) no
N4 Ni1 N1 . . 8 90.38(15) no
O2 Ni1 N1 . . 8 173.21(14) no
N4 Ni1 O4 . . 8 90.38(14) no
O2 Ni1 O4 . . 8 86.22(13) no
N1 Ni1 O4 8 . 8 87.30(14) no
N4 Ni1 O5 . . . 177.48(14) no
O2 Ni1 O5 . . . 89.85(13) no
N1 Ni1 O5 8 . . 92.14(14) no
O4 Ni1 O5 8 . . 89.57(12) no
N4 Ni1 N5 . . 3_666 92.27(15) no
O2 Ni1 N5 . . 3_666 90.26(14) no
N1 Ni1 N5 8 . 3_666 96.31(15) no
O4 Ni1 N5 8 . 3_666 175.50(14) no
O5 Ni1 N5 . . 3_666 87.62(13) no
C27 O4 Ni1 . . 8_454 123.4(3) no
C15 O2 Ni1 . . . 126.4(3) no
C25 N5 C26 . . . 117.1(4) no
C25 N5 Ni1 . . 3_666 120.1(3) no
C26 N5 Ni1 . . 3_666 121.8(3) no
C14 N4 C13 . . . 105.2(4) no
C14 N4 Ni1 . . . 126.2(3) no
C13 N4 Ni1 . . . 128.5(3) no
C2 N1 C1 . . . 105.2(4) no
C2 N1 Ni1 . . 8_454 133.1(3) no
C1 N1 Ni1 . . 8_454 121.6(3) no
C14 N3 C12 . . . 106.8(4) no
C14 N3 C11 . . . 126.6(4) no
C12 N3 C11 . . . 126.5(4) no
C2 N2 C3 . . . 106.8(4) no
C2 N2 C4 . . . 125.6(4) no
C3 N2 C4 . . . 127.4(4) no
C25 C24 C23 . . . 117.9(4) no
C25 C24 C27 . . . 120.0(4) no
C23 C24 C27 . . . 121.8(4) no
O3 C27 O4 . . . 126.4(4) no
O3 C27 C24 . . . 117.8(4) no
O4 C27 C24 . . . 115.7(4) no
C24 C23 C22 . . . 120.1(4) no
C18 C19 C20 . . . 118.7(4) no
C18 C19 C22 . . . 119.5(4) no
C20 C19 C22 . . . 121.8(4) no
O1 C15 O2 . . . 124.5(4) no
O1 C15 C16 . . . 120.5(4) no
O2 C15 C16 . . . 114.9(4) no
C21 C20 C19 . . . 119.3(4) no
C26 C22 C23 . . . 117.5(4) no
C26 C22 C19 . . . 120.7(4) no
C23 C22 C19 . . . 121.6(4) no
N5 C26 C22 . . . 123.7(4) no
C3 C1 N1 . . . 109.9(4) no
C16 C21 C20 . . . 122.0(5) no
C7 C8 C9 . . . 117.9(5) no
C7 C8 C11 . . . 120.7(5) no
C9 C8 C11 . . . 121.4(5) no
N5 C25 C24 . . . 123.7(4) no
C6 C5 C10 . . . 119.4(5) no
C6 C5 C4 . . . 117.7(4) no
C10 C5 C4 . . . 122.6(5) no
C8 C7 C6 . . . 121.5(5) no
C17 C16 C21 . . . 118.0(4) no
C17 C16 C15 . . . 120.2(4) no
C21 C16 C15 . . . 121.7(4) no
C13 C12 N3 . . . 106.2(4) no
C5 C6 C7 . . . 120.0(5) no
N3 C11 C8 . . . 111.3(4) no
N2 C4 C5 . . . 115.1(4) no
C8 C9 C10 . . . 121.2(5) no
N1 C2 N2 . . . 111.7(4) no
N4 C14 N3 . . . 112.0(4) no
C16 C17 C18 . . . 120.8(4) no
C12 C13 N4 . . . 109.8(4) no
C1 C3 N2 . . . 106.4(4) no
C5 C10 C9 . . . 119.9(5) no
C19 C18 C17 . . . 121.1(4) no

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N4 Ni1 O2 C15 . . . . 135.4(4) no
N1 Ni1 O2 C15 8 . . . -151.6(12) no
O4 Ni1 O2 C15 8 . . . -134.1(4) no
O5 Ni1 O2 C15 . . . . -44.5(4) no
N5 Ni1 O2 C15 3_666 . . . 43.1(4) no
O2 Ni1 N4 C14 . . . . 43.1(4) no
N1 Ni1 N4 C14 8 . . . -130.4(4) no
O4 Ni1 N4 C14 8 . . . -43.1(4) no
O5 Ni1 N4 C14 . . . . 46.(3) no
N5 Ni1 N4 C14 3_666 . . . 133.3(4) no
O2 Ni1 N4 C13 . . . . -136.4(4) no
N1 Ni1 N4 C13 8 . . . 50.1(4) no
O4 Ni1 N4 C13 8 . . . 137.4(4) no
O5 Ni1 N4 C13 . . . . -134.(3) no
N5 Ni1 N4 C13 3_666 . . . -46.2(4) no
Ni1 O4 C27 O3 8_454 . . . 40.7(6) no
Ni1 O4 C27 C24 8_454 . . . -134.6(3) no
C25 C24 C27 O3 . . . . -173.6(4) no
C23 C24 C27 O3 . . . . -0.2(7) no
C25 C24 C27 O4 . . . . 2.1(6) no
C23 C24 C27 O4 . . . . 175.5(4) no
C25 C24 C23 C22 . . . . 1.2(7) no
C27 C24 C23 C22 . . . . -172.4(4) no
Ni1 O2 C15 O1 . . . . 40.8(7) no
Ni1 O2 C15 C16 . . . . -136.4(3) no
C18 C19 C20 C21 . . . . -1.3(8) no
C22 C19 C20 C21 . . . . 176.7(5) no
C24 C23 C22 C26 . . . . -0.8(7) no
C24 C23 C22 C19 . . . . 173.3(4) no
C18 C19 C22 C26 . . . . 141.0(5) no
C20 C19 C22 C26 . . . . -37.1(7) no
C18 C19 C22 C23 . . . . -32.9(7) no
C20 C19 C22 C23 . . . . 149.1(5) no
C25 N5 C26 C22 . . . . 0.9(7) no
Ni1 N5 C26 C22 3_666 . . . 169.2(4) no
C23 C22 C26 N5 . . . . -0.3(7) no
C19 C22 C26 N5 . . . . -174.4(4) no
C2 N1 C1 C3 . . . . 0.5(6) no
Ni1 N1 C1 C3 8_454 . . . -176.0(3) no
C19 C20 C21 C16 . . . . -1.4(9) no
C26 N5 C25 C24 . . . . -0.4(7) no
Ni1 N5 C25 C24 3_666 . . . -168.9(3) no
C23 C24 C25 N5 . . . . -0.6(7) no
C27 C24 C25 N5 . . . . 173.1(4) no
C9 C8 C7 C6 . . . . -0.5(8) no
C11 C8 C7 C6 . . . . 179.9(5) no
C20 C21 C16 C17 . . . . 3.8(8) no
C20 C21 C16 C15 . . . . -173.4(5) no
O1 C15 C16 C17 . . . . 176.2(5) no
O2 C15 C16 C17 . . . . -6.5(7) no
O1 C15 C16 C21 . . . . -6.6(8) no
O2 C15 C16 C21 . . . . 170.7(5) no
C14 N3 C12 C13 . . . . -1.4(5) no
C11 N3 C12 C13 . . . . -177.8(4) no
C10 C5 C6 C7 . . . . 3.0(8) no
C4 C5 C6 C7 . . . . -170.9(5) no
C8 C7 C6 C5 . . . . -1.9(8) no
C14 N3 C11 C8 . . . . -116.2(5) no
C12 N3 C11 C8 . . . . 59.5(7) no
C7 C8 C11 N3 . . . . -134.1(5) no
C9 C8 C11 N3 . . . . 46.3(7) no
C2 N2 C4 C5 . . . . 99.0(6) no
C3 N2 C4 C5 . . . . -87.9(6) no
C6 C5 C4 N2 . . . . -142.1(5) no
C10 C5 C4 N2 . . . . 44.2(7) no
C7 C8 C9 C10 . . . . 1.8(8) no
C11 C8 C9 C10 . . . . -178.6(5) no
C1 N1 C2 N2 . . . . -1.1(5) no
Ni1 N1 C2 N2 8_454 . . . 174.9(3) no
C3 N2 C2 N1 . . . . 1.2(6) no
C4 N2 C2 N1 . . . . 175.5(4) no
C13 N4 C14 N3 . . . . -0.5(5) no
Ni1 N4 C14 N3 . . . . 180.0(3) no
C12 N3 C14 N4 . . . . 1.2(5) no
C11 N3 C14 N4 . . . . 177.6(4) no
C21 C16 C17 C18 . . . . -3.4(8) no
C15 C16 C17 C18 . . . . 173.9(5) no
N3 C12 C13 N4 . . . . 1.1(6) no
C14 N4 C13 C12 . . . . -0.4(5) no
Ni1 N4 C13 C12 . . . . 179.1(3) no
N1 C1 C3 N2 . . . . 0.2(6) no
C2 N2 C3 C1 . . . . -0.8(6) no
C4 N2 C3 C1 . . . . -174.9(4) no
C6 C5 C10 C9 . . . . -1.7(8) no
C4 C5 C10 C9 . . . . 171.8(5) no
C8 C9 C10 C5 . . . . -0.7(8) no
C20 C19 C18 C17 . . . . 1.7(8) no
C22 C19 C18 C17 . . . . -176.4(5) no
C16 C17 C18 C19 . . . . 0.7(9) no
####################################################################### 
# 
# 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_111_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1845011'
_audit_update_record             
;
2018-05-24 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H32 N6 Ni2 O9'
_chemical_formula_weight         930.20

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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   26.5859(11)
_cell_length_b                   13.3749(5)
_cell_length_c                   11.9649(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.8910(10)
_cell_angle_gamma                90.00
_cell_volume                     4203.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9454
_cell_measurement_theta_min      2.394
_cell_measurement_theta_max      28.359

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_exptl_absorpt_coefficient_mu    0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7485
_exptl_absorpt_correction_T_max  0.8934
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41160
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3709
_reflns_number_gt                2919
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0500P)²+105.6116P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3709
_refine_ls_number_parameters     278
_refine_ls_number_restraints     169
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0963
_refine_ls_wR_factor_ref         0.2132
_refine_ls_wR_factor_gt          0.1947
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.171
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.45737(3) 0.78794(7) 0.61866(8) 0.0214(3) Uani 1 1 d . . .
O5 O 0.5000 0.6998(5) 0.7500 0.0211(15) Uani 1 2 d S . .
O4 O 0.40024(18) 0.6862(4) 0.5955(5) 0.0288(13) Uani 1 1 d . . .
O1 O 0.0139(2) 0.3943(5) 0.6329(6) 0.054(2) Uani 1 1 d U . .
O2 O 0.08024(19) 0.3556(5) 0.7652(5) 0.0380(15) Uani 1 1 d . . .
O3 O 0.4143(2) 0.5992(5) 0.7563(6) 0.054(2) Uani 1 1 d . . .
N1 N 0.0876(2) 0.6185(6) 0.5021(6) 0.042(2) Uani 1 1 d U . .
C13 C 0.3863(3) 0.6309(6) 0.6698(8) 0.0313(19) Uani 1 1 d . . .
C3 C 0.1432(4) 0.4846(8) 0.6506(10) 0.061(3) Uani 1 1 d U . .
H3 H 0.1616 0.4405 0.7014 0.074 Uiso 1 1 calc R . .
C6 C 0.0647(3) 0.5481(7) 0.5553(8) 0.047(3) Uani 1 1 d U . .
H6 H 0.0293 0.5452 0.5421 0.056 Uiso 1 1 calc R . .
C8 C 0.2545(4) 0.5460(10) 0.7158(11) 0.078(4) Uani 1 1 d U . .
H8 H 0.2393 0.5202 0.7745 0.094 Uiso 1 1 calc R . .
C2 C 0.0905(3) 0.4793(8) 0.6288(9) 0.050(3) Uani 1 1 d U . .
C5 C 0.1387(3) 0.6210(7) 0.5219(8) 0.046(2) Uani 1 1 d U . .
H5 H 0.1552 0.6686 0.4841 0.055 Uiso 1 1 calc R . .
C4 C 0.1684(3) 0.5564(8) 0.5957(9) 0.052(3) Uani 1 1 d U . .
C1 C 0.0594(3) 0.4026(7) 0.6819(9) 0.046(2) Uani 1 1 d U . .
C9 C 0.3071(4) 0.5627(9) 0.7316(10) 0.070(3) Uani 1 1 d U . .
H9 H 0.3264 0.5464 0.8007 0.084 Uiso 1 1 calc R . .
C7 C 0.2252(3) 0.5678(8) 0.6129(10) 0.052(3) Uani 1 1 d U . .
C11 C 0.3012(3) 0.6201(7) 0.5453(8) 0.039(2) Uani 1 1 d U . .
H11 H 0.3168 0.6448 0.4866 0.046 Uiso 1 1 calc R . .
C10 C 0.3304(3) 0.6020(7) 0.6492(8) 0.039(2) Uani 1 1 d U . .
C12 C 0.2496(3) 0.6023(7) 0.5269(9) 0.043(2) Uani 1 1 d U . .
H12 H 0.2310 0.6137 0.4557 0.051 Uiso 1 1 calc R . .
C23 C 0.7247(4) 0.7448(10) 0.4701(11) 0.067(3) Uani 1 1 d . . .
C20A C 0.7094(13) 0.682(3) 0.384(3) 0.098(9) Uani 0.499(8) 1 d PU A 1
H20A H 0.7328 0.6383 0.3612 0.118 Uiso 0.499(8) 1 calc PR A 1
C21B C 0.7094(14) 0.761(3) 0.360(3) 0.109(11) Uani 0.501(8) 1 d PU A 2
H21B H 0.7318 0.7941 0.3203 0.131 Uiso 0.501(8) 1 calc PR A 2
C14 C 0.4888(2) 0.6202(6) 0.4678(6) 0.094(4) Uani 1 1 d GU . .
H14 H 0.4700 0.5715 0.4986 0.113 Uiso 1 1 calc R . .
N2 N 0.4911(2) 0.7176(6) 0.4954(5) 0.064(2) Uani 1 1 d GU . .
C16 C 0.5220(2) 0.7631(5) 0.4325(5) 0.084(3) Uani 1 1 d GU A .
H16 H 0.5304 0.8306 0.4346 0.101 Uiso 1 1 calc R . .
N3 N 0.53884(17) 0.6937(5) 0.3659(4) 0.116(4) Uani 1 1 d GU . .
C15 C 0.5183(2) 0.6054(6) 0.3878(6) 0.118(4) Uani 1 1 d GU A .
H15 H 0.5237 0.5448 0.3535 0.141 Uiso 1 1 calc R . .
C22B C 0.6631(3) 0.7342(9) 0.3021(7) 0.069(7) Uani 0.501(8) 1 d PGU A 2
H22B H 0.6560 0.7451 0.2245 0.083 Uiso 0.501(8) 1 calc PR A 2
C20B C 0.6913(3) 0.6769(10) 0.5160(9) 0.078(6) Uani 0.501(8) 1 d PG A 2
H20B H 0.7022 0.6478 0.5861 0.093 Uiso 0.501(8) 1 calc PR A 2
C18B C 0.6265(2) 0.6901(6) 0.3580(6) 0.055(4) Uani 0.501(8) 1 d PG A 2
C19B C 0.6441(3) 0.6535(7) 0.4603(7) 0.082(6) Uani 0.501(8) 1 d PG A 2
H19B H 0.6235 0.6107 0.4947 0.099 Uiso 0.501(8) 1 calc PR A 2
C17B C 0.5730(2) 0.7533(7) 0.2808(5) 0.052(4) Uani 0.501(8) 1 d PG A 2
H17A H 0.5738 0.8254 0.2896 0.062 Uiso 0.501(8) 1 calc PR A 2
H17B H 0.5652 0.7342 0.2018 0.062 Uiso 0.501(8) 1 calc PR A 2
C21A C 0.6911(4) 0.8296(9) 0.4721(9) 0.078(6) Uani 0.499(8) 1 d PG A 1
H21A H 0.7025 0.8844 0.5170 0.093 Uiso 0.499(8) 1 calc PR A 1
C19A C 0.6570(3) 0.6814(8) 0.3264(7) 0.092(8) Uani 0.499(8) 1 d PGU A 1
H19A H 0.6442 0.6276 0.2816 0.111 Uiso 0.499(8) 1 calc PR A 1
C22A C 0.6435(3) 0.8324(7) 0.4107(8) 0.082(6) Uani 0.499(8) 1 d PG A 1
H22A H 0.6219 0.8855 0.4192 0.099 Uiso 0.499(8) 1 calc PR A 1
C17A C 0.5753(2) 0.6588(7) 0.2920(5) 0.052(4) Uani 0.499(8) 1 d PGU A 1
H17C H 0.5615 0.6637 0.2123 0.062 Uiso 0.499(8) 1 calc PR A 1
H17D H 0.5872 0.5912 0.3100 0.062 Uiso 0.499(8) 1 calc PR A 1
C18A C 0.6284(3) 0.7603(7) 0.3399(6) 0.055(4) Uani 0.499(8) 1 d PGU A 1


_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 O4 2.026(5) . ?
Ni1 O2 2.044(6) 4_556 ?
Ni1 O1 2.057(6) 3 ?
Ni1 N2 2.067(6) . ?
Ni1 N1 2.133(7) 7_566 ?
Ni1 O5 2.143(4) . ?
O5 Ni1 2.143(4) 2_656 ?
O4 C13 1.257(10) . ?
O1 C1 1.265(10) . ?
O1 Ni1 2.057(6) 3_445 ?
O2 C1 1.236(10) . ?
O2 Ni1 2.044(6) 4_546 ?
O3 C13 1.251(10) . ?
N1 C6 1.335(11) . ?
N1 C5 1.344(10) . ?
N1 Ni1 2.133(7) 7_566 ?
C13 C10 1.517(10) . ?
C3 C2 1.387(12) . ?
C3 C4 1.391(13) . ?
C6 C2 1.379(12) . ?
C8 C7 1.384(14) . ?
C8 C9 1.398(14) . ?
C2 C1 1.517(12) . ?
C5 C4 1.390(12) . ?
C4 C7 1.500(12) . ?
C9 C10 1.350(14) . ?
C7 C12 1.378(14) . ?
C11 C12 1.376(11) . ?
C11 C10 1.381(12) . ?
C23 C21B 1.33(4) . ?
C23 C20A 1.34(3) . ?
C23 C23 1.43(2) 7_666 ?
C23 C20B 1.437(16) . ?
C23 C21A 1.446(17) . ?
C20A C19A 1.46(3) . ?
C21B C22B 1.36(4) . ?
C14 N2 1.343(3) . ?
C14 C15 1.344(3) . ?
N2 C16 1.343(3) . ?
C16 N3 1.343(3) . ?
N3 C15 1.343(3) . ?
N3 C17A 1.485(3) . ?
N3 C17B 1.669(3) . ?
C22B C18B 1.394(3) . ?
C20B C19B 1.362(3) . ?
C18B C19B 1.334(3) . ?
C18B C17B 1.786(4) . ?
C21A C22A 1.362(3) . ?
C19A C18A 1.326(3) . ?
C22A C18A 1.305(3) . ?
C17A C18A 1.979(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 O2 87.4(2) . 4_556 ?
O4 Ni1 O1 176.6(2) . 3 ?
O2 Ni1 O1 93.7(3) 4_556 3 ?
O4 Ni1 N2 89.7(3) . . ?
O2 Ni1 N2 176.5(2) 4_556 . ?
O1 Ni1 N2 89.0(3) 3 . ?
O4 Ni1 N1 88.4(2) . 7_566 ?
O2 Ni1 N1 85.4(3) 4_556 7_566 ?
O1 Ni1 N1 88.6(2) 3 7_566 ?
N2 Ni1 N1 92.5(3) . 7_566 ?
O4 Ni1 O5 91.8(2) . . ?
O2 Ni1 O5 90.23(19) 4_556 . ?
O1 Ni1 O5 91.3(2) 3 . ?
N2 Ni1 O5 92.0(2) . . ?
N1 Ni1 O5 175.6(3) 7_566 . ?
Ni1 O5 Ni1 113.3(3) . 2_656 ?
C13 O4 Ni1 126.6(5) . . ?
C1 O1 Ni1 137.1(6) . 3_445 ?
C1 O2 Ni1 124.6(5) . 4_546 ?
C6 N1 C5 117.1(7) . . ?
C6 N1 Ni1 119.2(5) . 7_566 ?
C5 N1 Ni1 123.4(6) . 7_566 ?
O3 C13 O4 125.5(7) . . ?
O3 C13 C10 119.4(8) . . ?
O4 C13 C10 115.1(7) . . ?
C2 C3 C4 119.5(9) . . ?
N1 C6 C2 123.8(8) . . ?
C7 C8 C9 120.1(10) . . ?
C6 C2 C3 118.3(8) . . ?
C6 C2 C1 117.9(7) . . ?
C3 C2 C1 123.8(8) . . ?
N1 C5 C4 123.7(8) . . ?
C5 C4 C3 117.5(8) . . ?
C5 C4 C7 118.9(8) . . ?
C3 C4 C7 123.6(8) . . ?
O2 C1 O1 127.4(8) . . ?
O2 C1 C2 118.4(7) . . ?
O1 C1 C2 114.2(8) . . ?
C10 C9 C8 121.7(9) . . ?
C12 C7 C8 117.9(9) . . ?
C12 C7 C4 120.9(9) . . ?
C8 C7 C4 121.2(10) . . ?
C12 C11 C10 121.4(9) . . ?
C9 C10 C11 117.9(8) . . ?
C9 C10 C13 122.0(8) . . ?
C11 C10 C13 120.1(8) . . ?
C7 C12 C11 120.8(9) . . ?
C21B C23 C20A 48.5(19) . . ?
C21B C23 C23 127(2) . 7_666 ?
C20A C23 C23 127(2) . 7_666 ?
C21B C23 C20B 111.7(19) . . ?
C20A C23 C20B 76.4(19) . . ?
C23 C23 C20B 117.4(14) 7_666 . ?
C21B C23 C21A 77.9(19) . . ?
C20A C23 C21A 112.8(17) . . ?
C23 C23 C21A 116.8(15) 7_666 . ?
C20B C23 C21A 94.1(9) . . ?
C23 C20A C19A 122(2) . . ?
C23 C21B C22B 125(3) . . ?
N2 C14 C15 108.0 . . ?
C16 N2 C14 108.0 . . ?
C16 N2 Ni1 124.4(4) . . ?
C14 N2 Ni1 127.5(4) . . ?
N2 C16 N3 108.0 . . ?
C15 N3 C16 108.0 . . ?
C15 N3 C17A 99.3 . . ?
C16 N3 C17A 151.4 . . ?
C15 N3 C17B 144.5 . . ?
C16 N3 C17B 107.1 . . ?
C17A N3 C17B 47.2 . . ?
N3 C15 C14 108.0 . . ?
C21B C22B C18B 120.6(16) . . ?
C19B C20B C23 122.4(7) . . ?
C19B C18B C22B 115.1 . . ?
C19B C18B C17B 141.9 . . ?
C22B C18B C17B 96.4 . . ?
C18B C19B C20B 122.0 . . ?
N3 C17B C18B 85.6 . . ?
C22A C21A C23 122.4(7) . . ?
C18A C19A C20A 117.4(14) . . ?
C18A C22A C21A 119.9 . . ?
N3 C17A C18A 96.5 . . ?
C22A C18A C19A 122.8 . . ?
C22A C18A C17A 146.1 . . ?
C19A C18A C17A 79.4 . . ?

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
O4 Ni1 O5 Ni1 -145.61(16) . . . 2_656 ?
O2 Ni1 O5 Ni1 -58.15(16) 4_556 . . 2_656 ?
O1 Ni1 O5 Ni1 35.6(2) 3 . . 2_656 ?
N2 Ni1 O5 Ni1 124.6(2) . . . 2_656 ?
N1 Ni1 O5 Ni1 -54(3) 7_566 . . 2_656 ?
O2 Ni1 O4 C13 -58.2(6) 4_556 . . . ?
O1 Ni1 O4 C13 -169(5) 3 . . . ?
N2 Ni1 O4 C13 123.9(7) . . . . ?
N1 Ni1 O4 C13 -143.6(7) 7_566 . . . ?
O5 Ni1 O4 C13 32.0(6) . . . . ?
Ni1 O4 C13 O3 -29.3(13) . . . . ?
Ni1 O4 C13 C10 150.8(6) . . . . ?
C5 N1 C6 C2 0.4(16) . . . . ?
Ni1 N1 C6 C2 175.3(9) 7_566 . . . ?
N1 C6 C2 C3 1.3(18) . . . . ?
N1 C6 C2 C1 -179.2(10) . . . . ?
C4 C3 C2 C6 -1.9(19) . . . . ?
C4 C3 C2 C1 178.6(11) . . . . ?
C6 N1 C5 C4 -1.5(16) . . . . ?
Ni1 N1 C5 C4 -176.2(9) 7_566 . . . ?
N1 C5 C4 C3 0.9(18) . . . . ?
N1 C5 C4 C7 -178.6(11) . . . . ?
C2 C3 C4 C5 0.9(19) . . . . ?
C2 C3 C4 C7 -179.6(12) . . . . ?
Ni1 O2 C1 O1 -22.9(16) 4_546 . . . ?
Ni1 O2 C1 C2 157.6(7) 4_546 . . . ?
Ni1 O1 C1 O2 -23(2) 3_445 . . . ?
Ni1 O1 C1 C2 157.0(8) 3_445 . . . ?
C6 C2 C1 O2 -164.2(10) . . . . ?
C3 C2 C1 O2 15.3(18) . . . . ?
C6 C2 C1 O1 16.2(16) . . . . ?
C3 C2 C1 O1 -164.3(12) . . . . ?
C7 C8 C9 C10 1(2) . . . . ?
C9 C8 C7 C12 2(2) . . . . ?
C9 C8 C7 C4 -176.3(12) . . . . ?
C5 C4 C7 C12 -31.1(17) . . . . ?
C3 C4 C7 C12 149.4(12) . . . . ?
C5 C4 C7 C8 147.7(13) . . . . ?
C3 C4 C7 C8 -31.8(19) . . . . ?
C8 C9 C10 C11 -3.7(19) . . . . ?
C8 C9 C10 C13 173.1(12) . . . . ?
C12 C11 C10 C9 2.3(15) . . . . ?
C12 C11 C10 C13 -174.6(9) . . . . ?
O3 C13 C10 C9 15.3(15) . . . . ?
O4 C13 C10 C9 -164.7(10) . . . . ?
O3 C13 C10 C11 -167.9(9) . . . . ?
O4 C13 C10 C11 12.1(13) . . . . ?
C8 C7 C12 C11 -3.8(17) . . . . ?
C4 C7 C12 C11 175.0(10) . . . . ?
C10 C11 C12 C7 1.5(15) . . . . ?
C21B C23 C20A C19A -68(3) . . . . ?
C23 C23 C20A C19A -177(2) 7_666 . . . ?
C20B C23 C20A C19A 69(3) . . . . ?
C21A C23 C20A C19A -20(4) . . . . ?
C20A C23 C21B C22B 58(3) . . . . ?
C23 C23 C21B C22B 168(2) 7_666 . . . ?
C20B C23 C21B C22B 12(4) . . . . ?
C21A C23 C21B C22B -78(3) . . . . ?
C15 C14 N2 C16 0.0 . . . . ?
C15 C14 N2 Ni1 -176.6(4) . . . . ?
O4 Ni1 N2 C16 153.8(3) . . . . ?
O2 Ni1 N2 C16 117(5) 4_556 . . . ?
O1 Ni1 N2 C16 -23.1(3) 3 . . . ?
N1 Ni1 N2 C16 65.5(3) 7_566 . . . ?
O5 Ni1 N2 C16 -114.4(3) . . . . ?
O4 Ni1 N2 C14 -30.0(4) . . . . ?
O2 Ni1 N2 C14 -67(5) 4_556 . . . ?
O1 Ni1 N2 C14 153.1(4) 3 . . . ?
N1 Ni1 N2 C14 -118.3(4) 7_566 . . . ?
O5 Ni1 N2 C14 61.8(4) . . . . ?
C14 N2 C16 N3 0.0 . . . . ?
Ni1 N2 C16 N3 176.8(4) . . . . ?
N2 C16 N3 C15 0.0 . . . . ?
N2 C16 N3 C17A -162.0 . . . . ?
N2 C16 N3 C17B 175.2 . . . . ?
C16 N3 C15 C14 0.1 . . . . ?
C17A N3 C15 C14 171.4 . . . . ?
C17B N3 C15 C14 -172.0 . . . . ?
N2 C14 C15 N3 -0.1 . . . . ?
C23 C21B C22B C18B 4(4) . . . . ?
C21B C23 C20B C19B -15(2) . . . . ?
C20A C23 C20B C19B -48.8(17) . . . . ?
C23 C23 C20B C19B -173.2(12) 7_666 . . . ?
C21A C23 C20B C19B 63.7(10) . . . . ?
C21B C22B C18B C19B -17(2) . . . . ?
C21B C22B C18B C17B 141(2) . . . . ?
C22B C18B C19B C20B 14.0 . . . . ?
C17B C18B C19B C20B -128.7 . . . . ?
C23 C20B C19B C18B 2.0(8) . . . . ?
C15 N3 C17B C18B -76.0 . . . . ?
C16 N3 C17B C18B 111.8 . . . . ?
C17A N3 C17B C18B -53.5 . . . . ?
C19B C18B C17B N3 -30.9 . . . . ?
C22B C18B C17B N3 -177.2 . . . . ?
C21B C23 C21A C22A 49.1(18) . . . . ?
C20A C23 C21A C22A 15(2) . . . . ?
C23 C23 C21A C22A 174.2(11) 7_666 . . . ?
C20B C23 C21A C22A -62.2(10) . . . . ?
C23 C20A C19A C18A 17(4) . . . . ?
C23 C21A C22A C18A -5.8(8) . . . . ?
C15 N3 C17A C18A -146.9 . . . . ?
C16 N3 C17A C18A 15.7 . . . . ?
C17B N3 C17A C18A 46.1 . . . . ?
C21A C22A C18A C19A 1.9 . . . . ?
C21A C22A C18A C17A 126.2 . . . . ?
C20A C19A C18A C22A -7.0(17) . . . . ?
C20A C19A C18A C17A -159.0(17) . . . . ?
N3 C17A C18A C22A 8.4 . . . . ?
N3 C17A C18A C19A 143.4 . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.088
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.130
