# 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 2017

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

data_2a
_database_code_depnum_ccdc_archive 'CCDC 1496539'
_audit_update_record             
;
2016-07-28 deposited with the CCDC.
2017-02-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT790_2a                  
;
PROBLEM: Centre of Gravity not Within Unit Cell: Resd.  #          1 Note
RESPONSE: No other solution find
;
# Added during the CSD deposition process: Thursday 28 July 2016 09:45 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H48 N6 O2, 2(Ag C N)'
_chemical_formula_sum            'C38 H48 Ag2 N8 O2'
_chemical_formula_weight         864.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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                   6.4200(10)
_cell_length_b                   6.9240(10)
_cell_length_c                   22.131(2)
_cell_angle_alpha                95.130(2)
_cell_angle_beta                 92.580(2)
_cell_angle_gamma                100.820(3)
_cell_volume                     960.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8953
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             442
_exptl_absorpt_coefficient_mu    1.063
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5560
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         30.03
_reflns_number_total             5559
_reflns_number_gt                4694
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0420P)²+0.1103P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5559
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1229
_refine_ls_wR_factor_gt          0.1171
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
Ag Ag 0.50578(4) 0.25152(3) 0.146840(10) 0.03959(9) Uani 1 1 d . . .
O O 0.7013(3) 0.1421(3) 0.35409(9) 0.0338(4) Uani 1 1 d . . .
N1 N 0.6024(4) 0.7829(4) 0.07414(11) 0.0392(5) Uani 1 1 d . . .
N2 N 0.5297(4) 0.7658(3) 0.16786(10) 0.0321(4) Uani 1 1 d . . .
N3 N 0.1026(4) 0.0360(4) 0.21030(14) 0.0467(6) Uani 1 1 d . . .
N4 N 0.8855(7) 0.3934(6) 0.07301(19) 0.0626(10) Uani 1 1 d . . .
C1 C 0.7224(7) 0.8262(6) 0.02092(17) 0.0581(9) Uani 1 1 d . . .
H1A H 0.7862 0.9672 0.0243 0.087 Uiso 1 1 calc . . .
H1B H 0.6269 0.7923 -0.0159 0.087 Uiso 1 1 calc . . .
H1C H 0.8349 0.7482 0.0186 0.087 Uiso 1 1 calc . . .
C2 C 0.3981(5) 0.6803(4) 0.07387(14) 0.0404(6) Uani 1 1 d . . .
H2 H 0.3065 0.6270 0.0391 0.048 Uiso 1 1 calc . . .
C3 C 0.3514(4) 0.6691(4) 0.13298(14) 0.0381(6) Uani 1 1 d . . .
H3 H 0.2210 0.6066 0.1474 0.046 Uiso 1 1 calc . . .
C4 C 0.6791(5) 0.8327(4) 0.13135(13) 0.0359(5) Uani 1 1 d . . .
H4 H 0.8177 0.9041 0.1440 0.043 Uiso 1 1 calc . . .
C5 C 0.5527(5) 0.8003(4) 0.23503(12) 0.0392(6) Uani 1 1 d . . .
H5A H 0.4215 0.8376 0.2502 0.047 Uiso 1 1 calc . . .
H5B H 0.6720 0.9121 0.2471 0.047 Uiso 1 1 calc . . .
C6 C 0.5932(4) 0.6208(4) 0.26435(11) 0.0317(5) Uani 1 1 d . . .
C7 C 0.4452(4) 0.5250(4) 0.30104(13) 0.0345(5) Uani 1 1 d . . .
H7 H 0.3151 0.5692 0.3062 0.041 Uiso 1 1 calc . . .
C8 C 0.4858(4) 0.3647(4) 0.33040(12) 0.0338(5) Uani 1 1 d . . .
H8 H 0.3834 0.2999 0.3553 0.041 Uiso 1 1 calc . . .
C9 C 0.6762(4) 0.2998(4) 0.32329(11) 0.0290(4) Uani 1 1 d . . .
C10 C 0.8244(4) 0.3929(4) 0.28619(12) 0.0332(5) Uani 1 1 d . . .
H10 H 0.9536 0.3476 0.2806 0.040 Uiso 1 1 calc . . .
C11 C 0.7821(4) 0.5531(4) 0.25730(12) 0.0344(5) Uani 1 1 d . . .
H11 H 0.8844 0.6175 0.2323 0.041 Uiso 1 1 calc . . .
C12 C 0.9132(4) 0.1065(4) 0.36163(11) 0.0307(5) Uani 1 1 d . . .
H12A H 1.0085 0.2264 0.3817 0.037 Uiso 1 1 calc . . .
H12B H 0.9666 0.0736 0.3215 0.037 Uiso 1 1 calc . . .
C13 C 0.9107(4) -0.0637(4) 0.40018(12) 0.0306(5) Uani 1 1 d . . .
H13A H 0.8232 -0.1854 0.3786 0.037 Uiso 1 1 calc . . .
H13B H 0.8461 -0.0347 0.4389 0.037 Uiso 1 1 calc . . .
C14 C 1.1369(4) -0.0964(4) 0.41339(12) 0.0323(5) Uani 1 1 d . . .
H14A H 1.2049 -0.1121 0.3744 0.039 Uiso 1 1 calc . . .
H14B H 1.2199 0.0224 0.4377 0.039 Uiso 1 1 calc . . .
C15 C 1.1456(4) -0.2765(4) 0.44750(12) 0.0308(5) Uani 1 1 d . . .
H15A H 1.0719 -0.3967 0.4219 0.037 Uiso 1 1 calc . . .
H15B H 1.0689 -0.2656 0.4851 0.037 Uiso 1 1 calc . . .
C16 C 1.3727(4) -0.2986(4) 0.46425(13) 0.0323(5) Uani 1 1 d . . .
H16A H 1.4519 -0.2998 0.4269 0.039 Uiso 1 1 calc . . .
H16B H 1.4429 -0.1821 0.4920 0.039 Uiso 1 1 calc . . .
C17 C 1.3864(4) -0.4849(4) 0.49470(12) 0.0319(5) Uani 1 1 d . . .
H17A H 1.3039 -0.6007 0.4690 0.038 Uiso 1 1 calc . . .
H17B H 1.3206 -0.4774 0.5342 0.038 Uiso 1 1 calc . . .
C18 C 0.2417(5) 0.1186(4) 0.18807(14) 0.0386(6) Uani 1 1 d . . .
C19 C 0.7797(7) 0.3543(4) 0.09535(15) 0.0417(7) 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
Ag C18 2.063(3) . ?
Ag C19 2.180(5) . ?
O C9 1.368(3) . ?
O C12 1.433(3) . ?
N1 C4 1.329(4) . ?
N1 C2 1.369(4) . ?
N1 C1 1.459(5) . ?
N2 C4 1.326(4) . ?
N2 C3 1.376(3) . ?
N2 C5 1.481(3) . ?
N3 C18 1.125(4) . ?
N4 C19 0.874(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.361(4) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.511(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.390(4) . ?
C6 C11 1.390(3) . ?
C7 C8 1.394(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.390(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(4) . ?
C10 C11 1.392(4) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.513(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.531(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.523(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.527(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.522(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C17 1.523(5) 2_846 ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?

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
C18 Ag C19 172.21(11) . . ?
C9 O C12 116.6(2) . . ?
C4 N1 C2 109.0(3) . . ?
C4 N1 C1 124.6(3) . . ?
C2 N1 C1 126.4(3) . . ?
C4 N2 C3 108.8(2) . . ?
C4 N2 C5 124.4(2) . . ?
C3 N2 C5 126.8(3) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 N1 106.9(2) . . ?
C3 C2 H2 126.5 . . ?
N1 C2 H2 126.5 . . ?
C2 C3 N2 106.7(3) . . ?
C2 C3 H3 126.6 . . ?
N2 C3 H3 126.6 . . ?
N2 C4 N1 108.6(2) . . ?
N2 C4 H4 125.7 . . ?
N1 C4 H4 125.7 . . ?
N2 C5 C6 112.6(2) . . ?
N2 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
N2 C5 H5B 109.1 . . ?
C6 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
C7 C6 C11 118.7(2) . . ?
C7 C6 C5 120.4(2) . . ?
C11 C6 C5 120.9(3) . . ?
C6 C7 C8 120.7(2) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C9 C8 C7 120.0(2) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
O C9 C10 124.5(2) . . ?
O C9 C8 115.6(2) . . ?
C10 C9 C8 119.9(2) . . ?
C9 C10 C11 119.5(2) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C6 C11 C10 121.3(2) . . ?
C6 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
O C12 C13 108.7(2) . . ?
O C12 H12A 109.9 . . ?
C13 C12 H12A 109.9 . . ?
O C12 H12B 109.9 . . ?
C13 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C12 C13 C14 110.3(2) . . ?
C12 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
C12 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C15 C14 C13 113.3(2) . . ?
C15 C14 H14A 108.9 . . ?
C13 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
C13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C14 C15 C16 112.7(2) . . ?
C14 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
C14 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C15 113.8(2) . . ?
C17 C16 H16A 108.8 . . ?
C15 C16 H16A 108.8 . . ?
C17 C16 H16B 108.8 . . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
C16 C17 C17 113.0(3) . 2_846 ?
C16 C17 H17A 109.0 . . ?
C17 C17 H17A 109.0 2_846 . ?
C16 C17 H17B 109.0 . . ?
C17 C17 H17B 109.0 2_846 . ?
H17A C17 H17B 107.8 . . ?
N3 C18 Ag 175.8(3) . . ?
N4 C19 Ag 177.1(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
C4 N1 C2 C3 0.2(3) . . . . ?
C1 N1 C2 C3 178.1(3) . . . . ?
N1 C2 C3 N2 0.0(3) . . . . ?
C4 N2 C3 C2 -0.2(3) . . . . ?
C5 N2 C3 C2 177.2(2) . . . . ?
C3 N2 C4 N1 0.3(3) . . . . ?
C5 N2 C4 N1 -177.1(2) . . . . ?
C2 N1 C4 N2 -0.3(3) . . . . ?
C1 N1 C4 N2 -178.3(3) . . . . ?
C4 N2 C5 C6 -103.3(3) . . . . ?
C3 N2 C5 C6 79.8(3) . . . . ?
N2 C5 C6 C7 -115.3(3) . . . . ?
N2 C5 C6 C11 67.4(3) . . . . ?
C11 C6 C7 C8 0.3(4) . . . . ?
C5 C6 C7 C8 -177.1(2) . . . . ?
C6 C7 C8 C9 0.2(4) . . . . ?
C12 O C9 C10 17.6(4) . . . . ?
C12 O C9 C8 -163.2(2) . . . . ?
C7 C8 C9 O 179.8(2) . . . . ?
C7 C8 C9 C10 -1.0(4) . . . . ?
O C9 C10 C11 -179.7(2) . . . . ?
C8 C9 C10 C11 1.2(4) . . . . ?
C7 C6 C11 C10 0.0(4) . . . . ?
C5 C6 C11 C10 177.3(3) . . . . ?
C9 C10 C11 C6 -0.7(4) . . . . ?
C9 O C12 C13 176.2(2) . . . . ?
O C12 C13 C14 -175.7(2) . . . . ?
C12 C13 C14 C15 -175.1(2) . . . . ?
C13 C14 C15 C16 -175.9(2) . . . . ?
C14 C15 C16 C17 -176.2(2) . . . . ?
C15 C16 C17 C17 174.2(3) . . . 2_846 ?
C19 Ag C18 N3 40(4) . . . . ?
C18 Ag C19 N4 49(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.900
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.094
####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1496540'
_audit_update_record             
;
2016-07-28 deposited with the CCDC.
2017-02-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H48 N4 Ni O2, H2 O, Ni C4 N4'
_chemical_formula_sum            'C38 H50 N8 Ni O3'
_chemical_formula_weight         725.57

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   8.8400(3)
_cell_length_b                   9.3130(4)
_cell_length_c                   24.9890(5)
_cell_angle_alpha                90.611(2)
_cell_angle_beta                 99.078(2)
_cell_angle_gamma                108.8990(13)
_cell_volume                     1917.78(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    18343
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             772
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11123
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         30.03
_reflns_number_total             11122
_reflns_number_gt                8181
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0473P)²+0.0000P] 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         11122
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1277
_refine_ls_wR_factor_gt          0.1181
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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 0.83497(2) 0.48671(2) 0.149835(9) 0.02962(8) Uani 1 1 d . . .
O1 O -0.12890(14) 0.53224(14) 0.33309(5) 0.0336(3) Uani 1 1 d . . .
O2 O 1.40824(14) 0.05684(14) 0.61667(5) 0.0321(3) Uani 1 1 d . . .
N1 N -0.57686(19) 0.72126(17) 0.07320(6) 0.0366(3) Uani 1 1 d . . .
N2 N -0.47648(16) 0.85588(14) 0.14896(5) 0.0266(3) Uani 1 1 d . . .
N3 N 1.94088(19) -0.15037(19) 0.89214(6) 0.0399(4) Uani 1 1 d . . .
N4 N 1.80284(16) -0.18846(15) 0.81109(5) 0.0268(3) Uani 1 1 d . . .
N5 N 1.1916(2) 0.6605(2) 0.18075(8) 0.0526(5) Uani 1 1 d . . .
N6 N 0.87856(19) 0.25272(19) 0.22811(7) 0.0438(4) Uani 1 1 d . . .
N7 N 0.4761(2) 0.32218(19) 0.11913(8) 0.0473(4) Uani 1 1 d . . .
N8 N 0.7991(2) 0.6955(2) 0.06115(7) 0.0549(5) Uani 1 1 d . . .
C1 C -0.6373(3) 0.5916(2) 0.03287(9) 0.0539(6) Uani 1 1 d . . .
H1A H -0.6090 0.5053 0.0482 0.081 Uiso 1 1 calc . . .
H1B H -0.5877 0.6197 0.0004 0.081 Uiso 1 1 calc . . .
H1C H -0.7554 0.5631 0.0231 0.081 Uiso 1 1 calc . . .
C2 C -0.5754(3) 0.8666(2) 0.06372(8) 0.0470(5) Uani 1 1 d . . .
H2 H -0.6112 0.9013 0.0300 0.056 Uiso 1 1 calc . . .
C3 C -0.5143(3) 0.9502(2) 0.11076(8) 0.0401(4) Uani 1 1 d . . .
H3 H -0.4996 1.0551 0.1168 0.048 Uiso 1 1 calc . . .
C4 C -0.5171(2) 0.71809(18) 0.12532(7) 0.0297(3) Uani 1 1 d . . .
H4 H -0.5056 0.6310 0.1427 0.036 Uiso 1 1 calc . . .
C5 C -0.4277(2) 0.90009(18) 0.20774(7) 0.0289(3) Uani 1 1 d . . .
H5A H -0.5250 0.8977 0.2231 0.035 Uiso 1 1 calc . . .
H5B H -0.3517 1.0059 0.2128 0.035 Uiso 1 1 calc . . .
C6 C -0.34810(19) 0.79847(17) 0.23838(6) 0.0260(3) Uani 1 1 d . . .
C7 C -0.1878(2) 0.8133(2) 0.23655(7) 0.0329(4) Uani 1 1 d . . .
H7 H -0.1300 0.8850 0.2140 0.039 Uiso 1 1 calc . . .
C8 C -0.1095(2) 0.7255(2) 0.26703(7) 0.0322(3) Uani 1 1 d . . .
H8 H 0.0000 0.7363 0.2650 0.039 Uiso 1 1 calc . . .
C9 C -0.19351(19) 0.62194(17) 0.30047(6) 0.0266(3) Uani 1 1 d . . .
C10 C -0.35497(19) 0.60524(18) 0.30236(7) 0.0287(3) Uani 1 1 d . . .
H10 H -0.4130 0.5335 0.3249 0.034 Uiso 1 1 calc . . .
C11 C -0.43116(18) 0.69266(18) 0.27161(7) 0.0278(3) Uani 1 1 d . . .
H11 H -0.5413 0.6804 0.2732 0.033 Uiso 1 1 calc . . .
C12 C 0.03836(19) 0.54941(19) 0.33402(7) 0.0306(3) Uani 1 1 d . . .
H12A H 0.1071 0.6557 0.3455 0.037 Uiso 1 1 calc . . .
H12B H 0.0559 0.5246 0.2974 0.037 Uiso 1 1 calc . . .
C13 C 0.0821(2) 0.44216(19) 0.37375(7) 0.0328(4) Uani 1 1 d . . .
H13A H 0.0179 0.3360 0.3604 0.039 Uiso 1 1 calc . . .
H13B H 0.0535 0.4614 0.4092 0.039 Uiso 1 1 calc . . .
C14 C 0.2621(2) 0.46105(18) 0.38145(7) 0.0294(3) Uani 1 1 d . . .
H14A H 0.3258 0.5686 0.3930 0.035 Uiso 1 1 calc . . .
H14B H 0.2892 0.4376 0.3461 0.035 Uiso 1 1 calc . . .
C15 C 0.3123(2) 0.35967(19) 0.42318(7) 0.0299(3) Uani 1 1 d . . .
H15A H 0.2883 0.3850 0.4588 0.036 Uiso 1 1 calc . . .
H15B H 0.2468 0.2523 0.4122 0.036 Uiso 1 1 calc . . .
C16 C 0.49094(19) 0.37642(18) 0.42941(7) 0.0280(3) Uani 1 1 d . . .
H16A H 0.5560 0.4845 0.4394 0.034 Uiso 1 1 calc . . .
H16B H 0.5139 0.3491 0.3939 0.034 Uiso 1 1 calc . . .
C17 C 0.5459(2) 0.27918(18) 0.47179(7) 0.0287(3) Uani 1 1 d . . .
H17A H 0.5210 0.3047 0.5072 0.034 Uiso 1 1 calc . . .
H17B H 0.4834 0.1707 0.4614 0.034 Uiso 1 1 calc . . .
C18 C 0.72614(19) 0.30115(18) 0.47810(7) 0.0283(3) Uani 1 1 d . . .
H18A H 0.7885 0.4094 0.4888 0.034 Uiso 1 1 calc . . .
H18B H 0.7510 0.2769 0.4425 0.034 Uiso 1 1 calc . . .
C19 C 0.7818(2) 0.20318(18) 0.51994(7) 0.0298(3) Uani 1 1 d . . .
H19A H 0.7557 0.2270 0.5554 0.036 Uiso 1 1 calc . . .
H19B H 0.7196 0.0950 0.5090 0.036 Uiso 1 1 calc . . .
C20 C 0.9615(2) 0.22440(19) 0.52707(7) 0.0301(3) Uani 1 1 d . . .
H20A H 1.0240 0.3321 0.5388 0.036 Uiso 1 1 calc . . .
H20B H 0.9883 0.2025 0.4915 0.036 Uiso 1 1 calc . . .
C21 C 1.01463(19) 0.12315(18) 0.56829(7) 0.0289(3) Uani 1 1 d . . .
H21A H 0.9922 0.1480 0.6042 0.035 Uiso 1 1 calc . . .
H21B H 0.9491 0.0157 0.5574 0.035 Uiso 1 1 calc . . .
C22 C 1.1939(2) 0.14038(19) 0.57359(7) 0.0296(3) Uani 1 1 d . . .
H22A H 1.2176 0.1166 0.5377 0.035 Uiso 1 1 calc . . .
H22B H 1.2604 0.2470 0.5854 0.035 Uiso 1 1 calc . . .
C23 C 1.23931(19) 0.03537(18) 0.61429(7) 0.0278(3) Uani 1 1 d . . .
H23A H 1.2184 0.0597 0.6505 0.033 Uiso 1 1 calc . . .
H23B H 1.1737 -0.0717 0.6028 0.033 Uiso 1 1 calc . . .
C24 C 1.47560(19) -0.02549(17) 0.65203(6) 0.0260(3) Uani 1 1 d . . .
C25 C 1.64110(19) 0.0019(2) 0.65380(7) 0.0327(4) Uani 1 1 d . . .
H25 H 1.6989 0.0744 0.6315 0.039 Uiso 1 1 calc . . .
C26 C 1.7216(2) -0.0759(2) 0.68789(7) 0.0340(4) Uani 1 1 d . . .
H26 H 1.8341 -0.0573 0.6886 0.041 Uiso 1 1 calc . . .
C27 C 1.6381(2) -0.18200(18) 0.72134(7) 0.0283(3) Uani 1 1 d . . .
C28 C 1.47396(19) -0.20820(18) 0.71918(6) 0.0271(3) Uani 1 1 d . . .
H28 H 1.4164 -0.2803 0.7417 0.033 Uiso 1 1 calc . . .
C29 C 1.39108(18) -0.13129(18) 0.68476(6) 0.0265(3) Uani 1 1 d . . .
H29 H 1.2782 -0.1510 0.6837 0.032 Uiso 1 1 calc . . .
C30 C 1.7248(2) -0.2692(2) 0.75754(7) 0.0359(4) Uani 1 1 d . . .
H30A H 1.6461 -0.3690 0.7630 0.043 Uiso 1 1 calc . . .
H30B H 1.8086 -0.2883 0.7392 0.043 Uiso 1 1 calc . . .
C31 C 1.8320(2) -0.03930(19) 0.82738(7) 0.0350(4) Uani 1 1 d . . .
H31 H 1.7979 0.0334 0.8069 0.042 Uiso 1 1 calc . . .
C32 C 1.9187(2) -0.0159(2) 0.87823(8) 0.0432(4) Uani 1 1 d . . .
H32 H 1.9571 0.0767 0.9002 0.052 Uiso 1 1 calc . . .
C33 C 1.8690(2) -0.2530(2) 0.85112(7) 0.0324(3) Uani 1 1 d . . .
H33 H 1.8654 -0.3561 0.8504 0.039 Uiso 1 1 calc . . .
C34 C 2.0322(3) -0.1791(3) 0.94360(9) 0.0677(7) Uani 1 1 d . . .
H34A H 1.9560 -0.2290 0.9676 0.102 Uiso 1 1 calc . . .
H34B H 2.1069 -0.0822 0.9614 0.102 Uiso 1 1 calc . . .
H34C H 2.0940 -0.2449 0.9358 0.102 Uiso 1 1 calc . . .
C35 C 1.0573(2) 0.59459(19) 0.16796(8) 0.0342(4) Uani 1 1 d . . .
C36 C 0.8591(2) 0.3428(2) 0.19920(8) 0.0339(4) Uani 1 1 d . . .
C37 C 0.6129(2) 0.38302(19) 0.13190(7) 0.0340(4) Uani 1 1 d . . .
C38 C 0.8133(2) 0.6187(2) 0.09599(8) 0.0383(4) Uani 1 1 d . . .
O3 O 0.6945(3) 0.8742(2) -0.01908(8) 0.0672(5) Uani 1 1 d . . .
HO1 H 0.656(4) 0.817(4) -0.0448(14) 0.092(12) Uiso 1 1 d . . .
HO2 H 0.705(4) 0.799(4) 0.0026(14) 0.104(11) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C38 1.8613(19) . ?
Ni1 C37 1.8637(18) . ?
Ni1 C36 1.8713(18) . ?
Ni1 C35 1.8727(18) . ?
O1 C9 1.3658(18) . ?
O1 C12 1.4312(19) . ?
O2 C24 1.3666(18) . ?
O2 C23 1.4324(19) . ?
N1 C4 1.330(2) . ?
N1 C2 1.373(2) . ?
N1 C1 1.465(2) . ?
N2 C4 1.320(2) . ?
N2 C3 1.379(2) . ?
N2 C5 1.478(2) . ?
N3 C33 1.322(2) . ?
N3 C32 1.370(3) . ?
N3 C34 1.482(3) . ?
N4 C33 1.327(2) . ?
N4 C31 1.373(2) . ?
N4 C30 1.478(2) . ?
N5 C35 1.137(2) . ?
N6 C36 1.150(2) . ?
N7 C37 1.147(2) . ?
N8 C38 1.150(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.337(3) . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.501(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.387(2) . ?
C6 C11 1.393(2) . ?
C7 C8 1.393(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.389(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.393(2) . ?
C10 C11 1.383(2) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.511(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.523(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.524(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.518(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.523(2) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.522(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.522(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.517(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.525(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.524(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.516(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C29 1.390(2) . ?
C24 C25 1.395(2) . ?
C25 C26 1.383(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.400(2) . ?
C26 H26 0.9500 . ?
C27 C28 1.383(2) . ?
C27 C30 1.505(2) . ?
C28 C29 1.394(2) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.352(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O3 HO1 0.79(3) . ?
O3 HO2 0.91(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
C38 Ni1 C37 88.76(8) . . ?
C38 Ni1 C36 174.92(8) . . ?
C37 Ni1 C36 90.98(7) . . ?
C38 Ni1 C35 90.51(8) . . ?
C37 Ni1 C35 178.85(8) . . ?
C36 Ni1 C35 89.82(7) . . ?
C9 O1 C12 117.64(13) . . ?
C24 O2 C23 117.55(12) . . ?
C4 N1 C2 108.34(15) . . ?
C4 N1 C1 126.07(16) . . ?
C2 N1 C1 125.58(17) . . ?
C4 N2 C3 108.34(14) . . ?
C4 N2 C5 127.11(13) . . ?
C3 N2 C5 123.66(13) . . ?
C33 N3 C32 108.56(15) . . ?
C33 N3 C34 124.52(19) . . ?
C32 N3 C34 126.90(19) . . ?
C33 N4 C31 108.59(14) . . ?
C33 N4 C30 122.38(14) . . ?
C31 N4 C30 128.84(14) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 N1 107.27(16) . . ?
C3 C2 H2 126.4 . . ?
N1 C2 H2 126.4 . . ?
C2 C3 N2 107.30(15) . . ?
C2 C3 H3 126.4 . . ?
N2 C3 H3 126.4 . . ?
N2 C4 N1 108.74(14) . . ?
N2 C4 H4 125.6 . . ?
N1 C4 H4 125.6 . . ?
N2 C5 C6 113.16(13) . . ?
N2 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
C7 C6 C11 118.49(14) . . ?
C7 C6 C5 120.84(15) . . ?
C11 C6 C5 120.58(14) . . ?
C6 C7 C8 121.54(15) . . ?
C6 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C9 C8 C7 119.20(15) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
O1 C9 C8 124.57(14) . . ?
O1 C9 C10 115.63(14) . . ?
C8 C9 C10 119.79(14) . . ?
C11 C10 C9 120.27(14) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C6 120.69(14) . . ?
C10 C11 H11 119.7 . . ?
C6 C11 H11 119.7 . . ?
O1 C12 C13 107.75(13) . . ?
O1 C12 H12A 110.2 . . ?
C13 C12 H12A 110.2 . . ?
O1 C12 H12B 110.2 . . ?
C13 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
C12 C13 C14 112.02(14) . . ?
C12 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
C12 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 C15 113.53(14) . . ?
C13 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
C13 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C16 C15 C14 113.05(13) . . ?
C16 C15 H15A 109.0 . . ?
C14 C15 H15A 109.0 . . ?
C16 C15 H15B 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C15 C16 C17 114.33(13) . . ?
C15 C16 H16A 108.7 . . ?
C17 C16 H16A 108.7 . . ?
C15 C16 H16B 108.7 . . ?
C17 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C18 C17 C16 113.16(13) . . ?
C18 C17 H17A 108.9 . . ?
C16 C17 H17A 108.9 . . ?
C18 C17 H17B 108.9 . . ?
C16 C17 H17B 108.9 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 C19 113.53(13) . . ?
C17 C18 H18A 108.9 . . ?
C19 C18 H18A 108.9 . . ?
C17 C18 H18B 108.9 . . ?
C19 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C20 C19 C18 114.27(13) . . ?
C20 C19 H19A 108.7 . . ?
C18 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C18 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 C21 113.62(13) . . ?
C19 C20 H20A 108.8 . . ?
C21 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C22 C21 C20 113.35(13) . . ?
C22 C21 H21A 108.9 . . ?
C20 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C23 C22 C21 111.10(13) . . ?
C23 C22 H22A 109.4 . . ?
C21 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
O2 C23 C22 107.86(13) . . ?
O2 C23 H23A 110.1 . . ?
C22 C23 H23A 110.1 . . ?
O2 C23 H23B 110.1 . . ?
C22 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
O2 C24 C29 124.70(14) . . ?
O2 C24 C25 115.43(14) . . ?
C29 C24 C25 119.87(14) . . ?
C26 C25 C24 120.33(15) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 120.37(15) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 118.73(14) . . ?
C28 C27 C30 120.87(15) . . ?
C26 C27 C30 120.37(15) . . ?
C27 C28 C29 121.53(15) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C24 C29 C28 119.17(14) . . ?
C24 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
N4 C30 C27 112.96(13) . . ?
N4 C30 H30A 109.0 . . ?
C27 C30 H30A 109.0 . . ?
N4 C30 H30B 109.0 . . ?
C27 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C32 C31 N4 106.74(16) . . ?
C32 C31 H31 126.6 . . ?
N4 C31 H31 126.6 . . ?
C31 C32 N3 107.29(16) . . ?
C31 C32 H32 126.4 . . ?
N3 C32 H32 126.4 . . ?
N3 C33 N4 108.81(15) . . ?
N3 C33 H33 125.6 . . ?
N4 C33 H33 125.6 . . ?
N3 C34 H34A 109.5 . . ?
N3 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N3 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N5 C35 Ni1 177.68(18) . . ?
N6 C36 Ni1 176.86(17) . . ?
N7 C37 Ni1 177.42(17) . . ?
N8 C38 Ni1 177.16(18) . . ?
HO1 O3 HO2 93(3) . . ?

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
C4 N1 C2 C3 0.0(3) . . . . ?
C1 N1 C2 C3 178.8(2) . . . . ?
N1 C2 C3 N2 0.7(3) . . . . ?
C4 N2 C3 C2 -1.1(2) . . . . ?
C5 N2 C3 C2 -170.97(17) . . . . ?
C3 N2 C4 N1 1.1(2) . . . . ?
C5 N2 C4 N1 170.50(15) . . . . ?
C2 N1 C4 N2 -0.7(2) . . . . ?
C1 N1 C4 N2 -179.47(18) . . . . ?
C4 N2 C5 C6 28.6(2) . . . . ?
C3 N2 C5 C6 -163.48(16) . . . . ?
N2 C5 C6 C7 77.58(19) . . . . ?
N2 C5 C6 C11 -105.90(17) . . . . ?
C11 C6 C7 C8 -0.1(3) . . . . ?
C5 C6 C7 C8 176.50(16) . . . . ?
C6 C7 C8 C9 -0.7(3) . . . . ?
C12 O1 C9 C8 1.9(2) . . . . ?
C12 O1 C9 C10 -177.77(14) . . . . ?
C7 C8 C9 O1 -178.48(15) . . . . ?
C7 C8 C9 C10 1.2(3) . . . . ?
O1 C9 C10 C11 178.86(14) . . . . ?
C8 C9 C10 C11 -0.8(3) . . . . ?
C9 C10 C11 C6 0.0(2) . . . . ?
C7 C6 C11 C10 0.5(2) . . . . ?
C5 C6 C11 C10 -176.14(15) . . . . ?
C9 O1 C12 C13 178.54(13) . . . . ?
O1 C12 C13 C14 -175.15(14) . . . . ?
C12 C13 C14 C15 177.41(14) . . . . ?
C13 C14 C15 C16 178.47(14) . . . . ?
C14 C15 C16 C17 178.68(13) . . . . ?
C15 C16 C17 C18 -178.61(14) . . . . ?
C16 C17 C18 C19 -179.38(13) . . . . ?
C17 C18 C19 C20 -179.59(14) . . . . ?
C18 C19 C20 C21 -178.84(14) . . . . ?
C19 C20 C21 C22 177.68(14) . . . . ?
C20 C21 C22 C23 -179.02(13) . . . . ?
C24 O2 C23 C22 178.73(13) . . . . ?
C21 C22 C23 O2 179.46(13) . . . . ?
C23 O2 C24 C29 1.8(2) . . . . ?
C23 O2 C24 C25 -178.57(14) . . . . ?
O2 C24 C25 C26 -179.54(15) . . . . ?
C29 C24 C25 C26 0.1(3) . . . . ?
C24 C25 C26 C27 -0.6(3) . . . . ?
C25 C26 C27 C28 0.6(3) . . . . ?
C25 C26 C27 C30 178.66(16) . . . . ?
C26 C27 C28 C29 -0.2(2) . . . . ?
C30 C27 C28 C29 -178.24(14) . . . . ?
O2 C24 C29 C28 179.92(14) . . . . ?
C25 C24 C29 C28 0.3(2) . . . . ?
C27 C28 C29 C24 -0.2(2) . . . . ?
C33 N4 C30 C27 171.96(15) . . . . ?
C31 N4 C30 C27 -13.6(3) . . . . ?
C28 C27 C30 N4 -94.38(19) . . . . ?
C26 C27 C30 N4 87.6(2) . . . . ?
C33 N4 C31 C32 0.4(2) . . . . ?
C30 N4 C31 C32 -174.65(17) . . . . ?
N4 C31 C32 N3 0.0(2) . . . . ?
C33 N3 C32 C31 -0.4(2) . . . . ?
C34 N3 C32 C31 178.4(2) . . . . ?
C32 N3 C33 N4 0.6(2) . . . . ?
C34 N3 C33 N4 -178.20(19) . . . . ?
C31 N4 C33 N3 -0.7(2) . . . . ?
C30 N4 C33 N3 174.80(15) . . . . ?
C38 Ni1 C35 N5 127(4) . . . . ?
C37 Ni1 C35 N5 76(6) . . . . ?
C36 Ni1 C35 N5 -58(4) . . . . ?
C38 Ni1 C36 N6 31(4) . . . . ?
C37 Ni1 C36 N6 118(3) . . . . ?
C35 Ni1 C36 N6 -63(3) . . . . ?
C38 Ni1 C37 N7 12(4) . . . . ?
C36 Ni1 C37 N7 -163(4) . . . . ?
C35 Ni1 C37 N7 63(7) . . . . ?
C37 Ni1 C38 N8 -72(4) . . . . ?
C36 Ni1 C38 N8 15(4) . . . . ?
C35 Ni1 C38 N8 108(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        30.03
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.058
