# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_jyy300
_database_code_depnum_ccdc_archive 'CCDC 2379616'
loop_
_audit_author_name
_audit_author_address
'Joseph W. Ziller'
;University of California, Irvine
United States of America
;
_audit_update_record             
;
2024-08-24 deposited with the CCDC.	2024-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H30 D6 N6 Ni O5 S'
_chemical_formula_weight         705.49

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'
D D 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   18.2951(5)
_cell_length_b                   8.7660(3)
_cell_length_c                   19.4810(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.9571(5)
_cell_angle_gamma                90
_cell_volume                     3122.44(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    9548
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      31.38

_exptl_crystal_description       hexagonal
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_F_000             1464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.429
_exptl_crystal_size_mid          0.415
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.742
_shelx_estimated_absorpt_T_min   0.741
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8092
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            80109
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.092
_diffrn_reflns_theta_max         31.652
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10013
_reflns_number_gt                9302
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+1.2489P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10013
_refine_ls_number_parameters     466
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0687
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.54154(2) 0.27637(2) 0.49093(2) 0.00988(4) Uani 1 1 d . . . . .
S1 S 0.79776(2) 0.11477(3) 0.37912(2) 0.01476(5) Uani 1 1 d . . . . .
O1 O 0.63612(4) 0.23506(8) 0.52031(3) 0.01324(12) Uani 1 1 d . . . . .
O2 O 0.58607(3) 0.38667(8) 0.42373(3) 0.01280(12) Uani 1 1 d . . . . .
O3 O 0.81993(4) 0.44536(9) 0.64414(3) 0.01688(13) Uani 1 1 d . . . . .
O4 O 0.72881(4) 0.74119(8) 0.29831(4) 0.01817(14) Uani 1 1 d . . . . .
O5 O 0.80089(4) 0.27180(8) 0.41252(4) 0.01729(14) Uani 1 1 d . . . . .
N1 N 0.50059(4) 0.15290(9) 0.55754(4) 0.01200(13) Uani 1 1 d . . . . .
N2 N 0.44736(4) 0.32130(9) 0.45748(4) 0.01176(13) Uani 1 1 d . . . . .
N3 N 0.77446(5) 0.28892(10) 0.55868(4) 0.01451(14) Uani 1 1 d . . . . .
H3 H 0.7627(9) 0.2871(17) 0.5185(8) 0.024(4) Uiso 1 1 d . . . . .
N4 N 0.83877(5) 0.50431(10) 0.53119(4) 0.01672(15) Uani 1 1 d . . . . .
H4 H 0.8433(8) 0.4609(19) 0.4933(8) 0.027(4) Uiso 1 1 d . . . . .
N5 N 0.67835(4) 0.53211(9) 0.34984(4) 0.01326(14) Uani 1 1 d . . . . .
H5 H 0.6878(8) 0.4577(18) 0.3746(8) 0.021(3) Uiso 1 1 d . . . . .
N6 N 0.80200(4) 0.54667(9) 0.33979(4) 0.01391(14) Uani 1 1 d . . . . .
H6 H 0.7995(8) 0.4582(17) 0.3571(7) 0.018(3) Uiso 1 1 d . . . . .
C1 C 0.65687(5) 0.17458(10) 0.57951(5) 0.01235(15) Uani 1 1 d . . . . .
C2 C 0.73122(5) 0.19823(11) 0.60147(5) 0.01414(16) Uani 1 1 d . . . . .
C3 C 0.75874(5) 0.13754(13) 0.66244(5) 0.01919(18) Uani 1 1 d . . . . .
H3A H 0.8086 0.1533 0.6758 0.023 Uiso 1 1 calc R U . . .
C4 C 0.71350(6) 0.05284(13) 0.70478(5) 0.02124(19) Uani 1 1 d . . . . .
H4A H 0.7325 0.0119 0.7469 0.025 Uiso 1 1 calc R U . . .
C5 C 0.64136(5) 0.02932(12) 0.68497(5) 0.01756(17) Uani 1 1 d . . . . .
H5A H 0.6110 -0.0283 0.7139 0.021 Uiso 1 1 calc R U . . .
C6 C 0.61120(5) 0.08883(10) 0.62254(5) 0.01309(15) Uani 1 1 d . . . . .
C7 C 0.53325(5) 0.07282(10) 0.60616(5) 0.01274(15) Uani 1 1 d . . . . .
C8 C 0.48945(5) -0.03753(11) 0.64784(5) 0.01534(16) Uani 1 1 d . . . . .
H8A H 0.4533 -0.0892 0.6177 0.023 Uiso 1 1 calc R U . . .
H8B H 0.4643 0.0183 0.6836 0.023 Uiso 1 1 calc R U . . .
H8C H 0.5224 -0.1133 0.6692 0.023 Uiso 1 1 calc R U . . .
C9 C 0.42099(5) 0.13237(10) 0.54629(5) 0.01369(16) Uani 1 1 d . . . . .
H9A H 0.3968 0.1332 0.5910 0.016 Uiso 1 1 calc R U . . .
H9B H 0.4112 0.0326 0.5240 0.016 Uiso 1 1 calc R U . . .
C10 C 0.39010(5) 0.25907(11) 0.50125(5) 0.01427(16) Uani 1 1 d . . . . .
H10A H 0.3492 0.2192 0.4720 0.017 Uiso 1 1 calc R U . . .
H10B H 0.3708 0.3413 0.5304 0.017 Uiso 1 1 calc R U . . .
C11 C 0.42636(5) 0.40651(10) 0.40523(5) 0.01304(15) Uani 1 1 d . . . . .
C12 C 0.34557(5) 0.42355(13) 0.38933(6) 0.02081(19) Uani 1 1 d . . . . .
H12A H 0.3210 0.4559 0.4308 0.031 Uiso 1 1 calc R U . . .
H12B H 0.3254 0.3255 0.3736 0.031 Uiso 1 1 calc R U . . .
H12C H 0.3378 0.5003 0.3532 0.031 Uiso 1 1 calc R U . . .
C13 C 0.47832(5) 0.48683(10) 0.36294(5) 0.01207(15) Uani 1 1 d . . . . .
C14 C 0.45344(5) 0.58672(10) 0.30982(5) 0.01383(16) Uani 1 1 d . . . . .
H14 H 0.4024 0.5958 0.3000 0.017 Uiso 1 1 calc R U . . .
C15 C 0.50134(5) 0.67078(10) 0.27228(5) 0.01426(16) Uani 1 1 d . . . . .
H15 H 0.4830 0.7385 0.2377 0.017 Uiso 1 1 calc R U . . .
C16 C 0.57712(5) 0.65750(10) 0.28456(5) 0.01337(15) Uani 1 1 d . . . . .
H16 H 0.6100 0.7159 0.2584 0.016 Uiso 1 1 calc R U . . .
C17 C 0.60366(5) 0.55888(10) 0.33494(4) 0.01167(15) Uani 1 1 d . . . . .
C18 C 0.55482(5) 0.47263(10) 0.37603(4) 0.01135(15) Uani 1 1 d . . . . .
C19 C 0.81186(5) 0.41436(11) 0.58325(5) 0.01331(15) Uani 1 1 d . . . . .
C20 C 0.88227(5) 0.63503(11) 0.54457(5) 0.01485(16) Uani 1 1 d . . . . .
C21 C 0.86451(6) 0.73986(12) 0.59570(5) 0.01867(18) Uani 1 1 d . . . . .
H21 H 0.8215 0.7267 0.6210 0.022 Uiso 1 1 calc R U . . .
C22 C 0.91059(6) 0.86345(12) 0.60894(5) 0.0223(2) Uani 1 1 d . . . . .
H22 H 0.8989 0.9342 0.6438 0.027 Uiso 1 1 calc R U . . .
C23 C 0.97340(7) 0.88511(12) 0.57205(6) 0.0249(2) Uani 1 1 d . . . . .
H23 H 1.0052 0.9681 0.5825 0.030 Uiso 1 1 calc R U . . .
C24 C 0.98922(6) 0.78408(13) 0.51962(6) 0.0231(2) Uani 1 1 d . . . . .
H24 H 1.0312 0.7999 0.4932 0.028 Uiso 1 1 calc R U . . .
C25 C 0.94375(6) 0.65974(11) 0.50571(5) 0.01776(17) Uani 1 1 d . . . . .
H25 H 0.9547 0.5915 0.4696 0.021 Uiso 1 1 calc R U . . .
C26 C 0.73606(5) 0.61684(10) 0.32696(5) 0.01228(15) Uani 1 1 d . . . . .
C27 C 0.87245(5) 0.60394(10) 0.32827(4) 0.01172(15) Uani 1 1 d . . . . .
C28 C 0.93042(5) 0.50080(10) 0.33853(5) 0.01284(15) Uani 1 1 d . . . . .
H28 H 0.9205 0.3976 0.3499 0.015 Uiso 1 1 calc R U . . .
C29 C 1.00233(5) 0.54858(11) 0.33220(5) 0.01405(16) Uani 1 1 d . . . . .
H29 H 1.0413 0.4781 0.3394 0.017 Uiso 1 1 calc R U . . .
C30 C 1.01753(5) 0.69944(11) 0.31534(5) 0.01585(17) Uani 1 1 d . . . . .
H30 H 1.0667 0.7328 0.3120 0.019 Uiso 1 1 calc R U . . .
C31 C 0.95992(5) 0.80058(11) 0.30345(5) 0.01609(17) Uani 1 1 d . . . . .
H31 H 0.9701 0.9029 0.2909 0.019 Uiso 1 1 calc R U . . .
C32 C 0.88746(5) 0.75466(11) 0.30955(5) 0.01424(16) Uani 1 1 d . . . . .
H32 H 0.8487 0.8249 0.3011 0.017 Uiso 1 1 calc R U . . .
C33 C 0.79481(7) -0.01984(12) 0.44812(6) 0.0250(2) Uani 1 1 d . . . . .
D33A D 0.8403(10) -0.016(2) 0.4715(9) 0.038(4) Uiso 1 1 d . . . . .
D33B D 0.7882(9) -0.119(2) 0.4290(9) 0.033(4) Uiso 1 1 d . . . . .
D33C D 0.7543(9) 0.009(2) 0.4764(8) 0.032(4) Uiso 1 1 d . . . . .
C34 C 0.70552(6) 0.09706(12) 0.34803(6) 0.01992(18) Uani 1 1 d . . . . .
D34A D 0.7016(9) 0.1677(19) 0.3108(9) 0.032(4) Uiso 1 1 d . . . . .
D34B D 0.7009(8) -0.0058(19) 0.3334(8) 0.026(4) Uiso 1 1 d . . . . .
D34C D 0.6763(9) 0.1239(19) 0.3866(8) 0.028(4) 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 O2 1.8399(7) . ?
Ni1 O1 1.8399(7) . ?
Ni1 N2 1.8633(8) . ?
Ni1 N1 1.8663(8) . ?
S1 O5 1.5227(7) . ?
S1 C34 1.7802(11) . ?
S1 C33 1.7908(11) . ?
O1 C1 1.3134(11) . ?
O2 C18 1.3122(11) . ?
O3 C19 1.2210(11) . ?
O4 C26 1.2298(11) . ?
N1 C7 1.3070(12) . ?
N1 C9 1.4762(11) . ?
N2 C11 1.3096(12) . ?
N2 C10 1.4775(11) . ?
N3 C19 1.3726(12) . ?
N3 C2 1.4135(12) . ?
N3 H3 0.805(16) . ?
N4 C19 1.3879(12) . ?
N4 C20 1.4144(12) . ?
N4 H4 0.837(16) . ?
N5 C26 1.3774(11) . ?
N5 C17 1.4069(11) . ?
N5 H5 0.825(15) . ?
N6 C26 1.3695(11) . ?
N6 C27 1.4084(11) . ?
N6 H6 0.847(15) . ?
C1 C6 1.4190(12) . ?
C1 C2 1.4271(12) . ?
C2 C3 1.3807(13) . ?
C3 C4 1.4011(14) . ?
C3 H3A 0.9500 . ?
C4 C5 1.3780(14) . ?
C4 H4A 0.9500 . ?
C5 C6 1.4176(13) . ?
C5 H5A 0.9500 . ?
C6 C7 1.4575(12) . ?
C7 C8 1.5104(12) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.5129(13) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C13 1.4600(12) . ?
C11 C12 1.5072(13) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.4186(12) . ?
C13 C18 1.4196(12) . ?
C14 C15 1.3746(13) . ?
C14 H14 0.9500 . ?
C15 C16 1.4037(12) . ?
C15 H15 0.9500 . ?
C16 C17 1.3834(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.4353(12) . ?
C20 C25 1.3939(14) . ?
C20 C21 1.4015(14) . ?
C21 C22 1.3915(15) . ?
C21 H21 0.9500 . ?
C22 C23 1.3890(17) . ?
C22 H22 0.9500 . ?
C23 C24 1.3897(16) . ?
C23 H23 0.9500 . ?
C24 C25 1.3923(14) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C27 C32 1.4003(12) . ?
C27 C28 1.4027(12) . ?
C28 C29 1.3902(12) . ?
C28 H28 0.9500 . ?
C29 C30 1.3929(13) . ?
C29 H29 0.9500 . ?
C30 C31 1.3906(14) . ?
C30 H30 0.9500 . ?
C31 C32 1.3944(13) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 D33A 0.937(18) . ?
C33 D33B 0.955(17) . ?
C33 D33C 0.972(17) . ?
C34 D34A 0.955(17) . ?
C34 D34B 0.949(16) . ?
C34 D34C 0.966(16) . ?

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
O2 Ni1 O1 83.70(3) . . ?
O2 Ni1 N2 93.83(3) . . ?
O1 Ni1 N2 177.45(3) . . ?
O2 Ni1 N1 175.96(3) . . ?
O1 Ni1 N1 93.74(3) . . ?
N2 Ni1 N1 88.70(3) . . ?
O5 S1 C34 104.22(5) . . ?
O5 S1 C33 106.06(5) . . ?
C34 S1 C33 98.35(6) . . ?
C1 O1 Ni1 126.37(6) . . ?
C18 O2 Ni1 127.79(6) . . ?
C7 N1 C9 117.80(8) . . ?
C7 N1 Ni1 129.12(6) . . ?
C9 N1 Ni1 112.64(6) . . ?
C11 N2 C10 117.66(8) . . ?
C11 N2 Ni1 129.47(6) . . ?
C10 N2 Ni1 112.68(6) . . ?
C19 N3 C2 121.82(8) . . ?
C19 N3 H3 117.9(11) . . ?
C2 N3 H3 115.2(11) . . ?
C19 N4 C20 122.48(8) . . ?
C19 N4 H4 115.7(11) . . ?
C20 N4 H4 117.3(11) . . ?
C26 N5 C17 126.38(8) . . ?
C26 N5 H5 117.9(10) . . ?
C17 N5 H5 115.7(10) . . ?
C26 N6 C27 128.03(8) . . ?
C26 N6 H6 115.2(10) . . ?
C27 N6 H6 116.8(10) . . ?
O1 C1 C6 125.05(8) . . ?
O1 C1 C2 116.64(8) . . ?
C6 C1 C2 118.31(8) . . ?
C3 C2 N3 121.94(9) . . ?
C3 C2 C1 121.18(8) . . ?
N3 C2 C1 116.86(8) . . ?
C2 C3 C4 120.35(9) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
C5 C4 C3 119.59(9) . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 H4A 120.2 . . ?
C4 C5 C6 121.75(9) . . ?
C4 C5 H5A 119.1 . . ?
C6 C5 H5A 119.1 . . ?
C5 C6 C1 118.81(8) . . ?
C5 C6 C7 120.11(8) . . ?
C1 C6 C7 120.87(8) . . ?
N1 C7 C6 121.78(8) . . ?
N1 C7 C8 119.72(8) . . ?
C6 C7 C8 118.49(8) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 110.10(7) . . ?
N1 C9 H9A 109.6 . . ?
C10 C9 H9A 109.6 . . ?
N1 C9 H9B 109.6 . . ?
C10 C9 H9B 109.6 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C9 110.34(7) . . ?
N2 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
N2 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
N2 C11 C13 122.29(8) . . ?
N2 C11 C12 118.42(8) . . ?
C13 C11 C12 119.28(8) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 118.36(8) . . ?
C14 C13 C11 120.69(8) . . ?
C18 C13 C11 120.88(8) . . ?
C15 C14 C13 121.64(8) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C16 120.58(8) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 119.57(8) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 N5 124.44(8) . . ?
C16 C17 C18 120.98(8) . . ?
N5 C17 C18 114.57(8) . . ?
O2 C18 C13 125.50(8) . . ?
O2 C18 C17 115.66(8) . . ?
C13 C18 C17 118.84(8) . . ?
O3 C19 N3 124.01(9) . . ?
O3 C19 N4 123.32(9) . . ?
N3 C19 N4 112.66(8) . . ?
C25 C20 C21 119.68(9) . . ?
C25 C20 N4 119.03(9) . . ?
C21 C20 N4 121.30(9) . . ?
C22 C21 C20 119.24(10) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C23 C22 C21 121.14(10) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C22 C23 C24 119.34(10) . . ?
C22 C23 H23 120.3 . . ?
C24 C23 H23 120.3 . . ?
C23 C24 C25 120.26(11) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C20 120.25(10) . . ?
C24 C25 H25 119.9 . . ?
C20 C25 H25 119.9 . . ?
O4 C26 N6 124.17(8) . . ?
O4 C26 N5 123.56(8) . . ?
N6 C26 N5 112.27(8) . . ?
C32 C27 C28 119.42(8) . . ?
C32 C27 N6 124.51(8) . . ?
C28 C27 N6 116.05(8) . . ?
C29 C28 C27 120.42(8) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C28 C29 C30 120.27(8) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C31 C30 C29 119.23(9) . . ?
C31 C30 H30 120.4 . . ?
C29 C30 H30 120.4 . . ?
C30 C31 C32 121.27(9) . . ?
C30 C31 H31 119.4 . . ?
C32 C31 H31 119.4 . . ?
C31 C32 C27 119.34(9) . . ?
C31 C32 H32 120.3 . . ?
C27 C32 H32 120.3 . . ?
S1 C33 D33A 106.9(11) . . ?
S1 C33 D33B 108.4(10) . . ?
D33A C33 D33B 108.9(15) . . ?
S1 C33 D33C 107.4(10) . . ?
D33A C33 D33C 113.4(14) . . ?
D33B C33 D33C 111.7(14) . . ?
S1 C34 D34A 104.4(10) . . ?
S1 C34 D34B 105.0(9) . . ?
D34A C34 D34B 112.7(13) . . ?
S1 C34 D34C 104.9(9) . . ?
D34A C34 D34C 113.8(14) . . ?
D34B C34 D34C 114.7(13) . . ?

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
O2 Ni1 O1 C1 167.16(8) . . . . ?
N1 Ni1 O1 C1 -15.97(8) . . . . ?
O1 Ni1 O2 C18 -175.48(8) . . . . ?
N2 Ni1 O2 C18 5.15(8) . . . . ?
O1 Ni1 N1 C7 1.05(8) . . . . ?
N2 Ni1 N1 C7 -179.71(8) . . . . ?
O1 Ni1 N1 C9 -170.97(6) . . . . ?
N2 Ni1 N1 C9 8.26(6) . . . . ?
O2 Ni1 N2 C11 -1.70(8) . . . . ?
N1 Ni1 N2 C11 -178.55(8) . . . . ?
O2 Ni1 N2 C10 -176.39(6) . . . . ?
N1 Ni1 N2 C10 6.77(6) . . . . ?
Ni1 O1 C1 C6 20.12(13) . . . . ?
Ni1 O1 C1 C2 -159.80(7) . . . . ?
C19 N3 C2 C3 -53.08(14) . . . . ?
C19 N3 C2 C1 125.61(10) . . . . ?
O1 C1 C2 C3 -179.05(9) . . . . ?
C6 C1 C2 C3 1.02(14) . . . . ?
O1 C1 C2 N3 2.24(13) . . . . ?
C6 C1 C2 N3 -177.69(8) . . . . ?
N3 C2 C3 C4 177.64(10) . . . . ?
C1 C2 C3 C4 -0.99(16) . . . . ?
C2 C3 C4 C5 0.50(17) . . . . ?
C3 C4 C5 C6 -0.07(17) . . . . ?
C4 C5 C6 C1 0.11(15) . . . . ?
C4 C5 C6 C7 -174.71(10) . . . . ?
O1 C1 C6 C5 179.51(9) . . . . ?
C2 C1 C6 C5 -0.57(13) . . . . ?
O1 C1 C6 C7 -5.71(14) . . . . ?
C2 C1 C6 C7 174.21(8) . . . . ?
C9 N1 C7 C6 -178.01(8) . . . . ?
Ni1 N1 C7 C6 10.31(13) . . . . ?
C9 N1 C7 C8 0.78(12) . . . . ?
Ni1 N1 C7 C8 -170.89(6) . . . . ?
C5 C6 C7 N1 164.91(9) . . . . ?
C1 C6 C7 N1 -9.80(13) . . . . ?
C5 C6 C7 C8 -13.90(13) . . . . ?
C1 C6 C7 C8 171.39(8) . . . . ?
C7 N1 C9 C10 166.21(8) . . . . ?
Ni1 N1 C9 C10 -20.78(9) . . . . ?
C11 N2 C10 C9 164.95(8) . . . . ?
Ni1 N2 C10 C9 -19.68(9) . . . . ?
N1 C9 C10 N2 25.61(10) . . . . ?
C10 N2 C11 C13 173.44(8) . . . . ?
Ni1 N2 C11 C13 -1.02(13) . . . . ?
C10 N2 C11 C12 -5.55(12) . . . . ?
Ni1 N2 C11 C12 179.99(7) . . . . ?
N2 C11 C13 C14 -175.47(9) . . . . ?
C12 C11 C13 C14 3.52(13) . . . . ?
N2 C11 C13 C18 1.49(13) . . . . ?
C12 C11 C13 C18 -179.52(9) . . . . ?
C18 C13 C14 C15 -1.21(13) . . . . ?
C11 C13 C14 C15 175.83(8) . . . . ?
C13 C14 C15 C16 1.42(14) . . . . ?
C14 C15 C16 C17 -0.02(14) . . . . ?
C15 C16 C17 N5 177.46(8) . . . . ?
C15 C16 C17 C18 -1.55(13) . . . . ?
C26 N5 C17 C16 12.78(14) . . . . ?
C26 N5 C17 C18 -168.16(8) . . . . ?
Ni1 O2 C18 C13 -6.08(13) . . . . ?
Ni1 O2 C18 C17 173.43(6) . . . . ?
C14 C13 C18 O2 179.15(8) . . . . ?
C11 C13 C18 O2 2.12(14) . . . . ?
C14 C13 C18 C17 -0.34(12) . . . . ?
C11 C13 C18 C17 -177.37(8) . . . . ?
C16 C17 C18 O2 -177.82(8) . . . . ?
N5 C17 C18 O2 3.08(11) . . . . ?
C16 C17 C18 C13 1.72(13) . . . . ?
N5 C17 C18 C13 -177.38(8) . . . . ?
C2 N3 C19 O3 11.06(14) . . . . ?
C2 N3 C19 N4 -167.97(8) . . . . ?
C20 N4 C19 O3 4.33(15) . . . . ?
C20 N4 C19 N3 -176.63(8) . . . . ?
C19 N4 C20 C25 136.76(10) . . . . ?
C19 N4 C20 C21 -43.55(14) . . . . ?
C25 C20 C21 C22 -2.95(15) . . . . ?
N4 C20 C21 C22 177.36(9) . . . . ?
C20 C21 C22 C23 0.50(16) . . . . ?
C21 C22 C23 C24 1.98(17) . . . . ?
C22 C23 C24 C25 -2.00(17) . . . . ?
C23 C24 C25 C20 -0.45(16) . . . . ?
C21 C20 C25 C24 2.94(15) . . . . ?
N4 C20 C25 C24 -177.37(9) . . . . ?
C27 N6 C26 O4 5.05(16) . . . . ?
C27 N6 C26 N5 -174.98(9) . . . . ?
C17 N5 C26 O4 11.08(15) . . . . ?
C17 N5 C26 N6 -168.89(8) . . . . ?
C26 N6 C27 C32 9.08(15) . . . . ?
C26 N6 C27 C28 -172.70(9) . . . . ?
C32 C27 C28 C29 1.90(13) . . . . ?
N6 C27 C28 C29 -176.41(8) . . . . ?
C27 C28 C29 C30 -0.24(14) . . . . ?
C28 C29 C30 C31 -1.41(14) . . . . ?
C29 C30 C31 C32 1.40(15) . . . . ?
C30 C31 C32 C27 0.26(15) . . . . ?
C28 C27 C32 C31 -1.90(14) . . . . ?
N6 C27 C32 C31 176.26(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O5 0.805(16) 2.206(16) 2.9082(11) 145.9(15) .
N4 H4 O5 0.837(16) 2.396(16) 3.1416(11) 148.7(14) .
N5 H5 O5 0.825(15) 2.717(15) 3.3966(11) 140.8(13) .
N6 H6 O5 0.847(15) 1.958(15) 2.7956(10) 169.4(14) .
C4 H4A O3 0.95 2.43 3.1697(12) 134.6 2_646
C29 H29 O3 0.95 2.64 3.2691(11) 124.5 3_766
C30 H30 O3 0.95 2.71 3.3041(12) 121.1 3_766
C34 D34B O4 0.949(16) 2.381(16) 3.2985(13) 162.5(13) 1_545
C34 D34A O4 0.955(17) 2.596(17) 3.3765(14) 139.1(13) 2_645

_refine_diff_density_max         0.485
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.054


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMSO-d6'
####################################################################### 
# 
# 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_jyy285
_database_code_depnum_ccdc_archive 'CCDC 2379617'
loop_
_audit_author_name
_audit_author_address
'Joseph W. Ziller'
;University of California, Irvine
United States of America
;
_audit_update_record             
;
2024-08-24 deposited with the CCDC.	2024-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H50 N6 Ni O8'
_chemical_formula_weight         801.57

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   23.663(3)
_cell_length_b                   7.1548(8)
_cell_length_c                   25.033(3)
_cell_angle_alpha                90
_cell_angle_beta                 113.9687(17)
_cell_angle_gamma                90
_cell_volume                     3872.7(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9986
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      29.33

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.119
_exptl_absorpt_coefficient_mu    0.562
_shelx_estimated_absorpt_T_min   0.856
_shelx_estimated_absorpt_T_max   0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6246
_exptl_absorpt_correction_T_max  0.8017
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
52637 Corrected reflections written to file jyy285s.hkl 
Estimated minimum and maximum transmission:  0.6246  0.8017 
The ratio (0.7791) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.1500 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45957
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.536
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9623
_reflns_number_gt                7289
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0471P)²+2.9990P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9623
_refine_ls_number_parameters     526
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1154
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.72171(2) 0.78030(4) 0.26985(2) 0.01047(8) Uani 1 1 d . . . . .
O1 O 0.69393(7) 0.7448(2) 0.32776(6) 0.0144(3) Uani 1 1 d . . . . .
O2 O 0.63942(7) 0.8126(2) 0.22288(6) 0.0142(3) Uani 1 1 d . . . . .
O3 O 0.59933(8) 0.5531(2) 0.45608(7) 0.0207(4) Uani 1 1 d . . . . .
O4 O 0.41892(7) 0.8868(3) 0.12255(7) 0.0239(4) Uani 1 1 d . . . . .
N1 N 0.80461(8) 0.7822(2) 0.32107(8) 0.0127(3) Uani 1 1 d . . . . .
N2 N 0.74591(8) 0.7811(2) 0.20798(8) 0.0127(3) Uani 1 1 d . . . . .
N3 N 0.63290(9) 0.5914(3) 0.38322(8) 0.0160(4) Uani 1 1 d . . . . .
H3 H 0.6226(12) 0.596(4) 0.3479(12) 0.021(7) Uiso 1 1 d . . . . .
N4 N 0.53384(9) 0.4976(3) 0.36047(8) 0.0172(4) Uani 1 1 d . . . . .
H4 H 0.5347(12) 0.465(4) 0.3287(11) 0.019(7) Uiso 1 1 d . . . . .
N5 N 0.52240(9) 0.8817(3) 0.18056(9) 0.0218(5) Uani 1 1 d . . . . .
H5 H 0.5466(13) 0.884(4) 0.2130(12) 0.023(7) Uiso 1 1 d . . . . .
N6 N 0.45354(9) 0.8999(3) 0.22245(9) 0.0215(4) Uani 1 1 d . . . . .
H6 H 0.4851(13) 0.896(4) 0.2529(12) 0.022(7) Uiso 1 1 d . . . . .
C1 C 0.72799(10) 0.7028(3) 0.38326(9) 0.0130(4) Uani 1 1 d . . . . .
C2 C 0.69546(10) 0.6322(3) 0.41611(9) 0.0137(4) Uani 1 1 d . . . . .
C3 C 0.72619(11) 0.5999(3) 0.47551(9) 0.0170(5) Uani 1 1 d . . . . .
H3A H 0.7040 0.5575 0.4974 0.020 Uiso 1 1 calc R U . . .
C4 C 0.78963(11) 0.6298(3) 0.50304(9) 0.0192(5) Uani 1 1 d . . . . .
H4A H 0.8104 0.6107 0.5440 0.023 Uiso 1 1 calc R U . . .
C5 C 0.82246(11) 0.6862(3) 0.47178(9) 0.0177(5) Uani 1 1 d . . . . .
H5A H 0.8660 0.7004 0.4912 0.021 Uiso 1 1 calc R U . . .
C6 C 0.79265(10) 0.7239(3) 0.41091(9) 0.0139(4) Uani 1 1 d . . . . .
C7 C 0.82919(10) 0.7745(3) 0.37806(9) 0.0136(4) Uani 1 1 d . . . . .
C8 C 0.89729(10) 0.8138(3) 0.41124(10) 0.0192(5) Uani 1 1 d . . . . .
H8A H 0.9103 0.9095 0.3906 0.029 Uiso 1 1 calc R U . . .
H8B H 0.9209 0.6989 0.4141 0.029 Uiso 1 1 calc R U . . .
H8C H 0.9049 0.8585 0.4506 0.029 Uiso 1 1 calc R U . . .
C9 C 0.84459(10) 0.8270(3) 0.29040(10) 0.0163(4) Uani 1 1 d . . . . .
H9A H 0.8852 0.7650 0.3102 0.020 Uiso 1 1 calc R U . . .
H9B H 0.8515 0.9636 0.2911 0.020 Uiso 1 1 calc R U . . .
C10 C 0.81362(10) 0.7601(3) 0.22827(10) 0.0154(4) Uani 1 1 d . . . . .
H10A H 0.8284 0.8342 0.2030 0.019 Uiso 1 1 calc R U . . .
H10B H 0.8241 0.6273 0.2259 0.019 Uiso 1 1 calc R U . . .
C11 C 0.71119(11) 0.7659(3) 0.15219(9) 0.0140(4) Uani 1 1 d . . . . .
C12 C 0.73943(11) 0.7170(3) 0.10956(10) 0.0189(5) Uani 1 1 d . . . . .
H12A H 0.7816 0.6707 0.1311 0.028 Uiso 1 1 calc R U . . .
H12B H 0.7404 0.8285 0.0873 0.028 Uiso 1 1 calc R U . . .
H12C H 0.7145 0.6199 0.0827 0.028 Uiso 1 1 calc R U . . .
C13 C 0.64456(10) 0.7932(3) 0.12865(9) 0.0130(4) Uani 1 1 d . . . . .
C14 C 0.60936(11) 0.7960(3) 0.06718(9) 0.0170(4) Uani 1 1 d . . . . .
H14 H 0.6297 0.7787 0.0418 0.020 Uiso 1 1 calc R U . . .
C15 C 0.54702(11) 0.8229(3) 0.04400(9) 0.0192(5) Uani 1 1 d . . . . .
H15 H 0.5246 0.8220 0.0028 0.023 Uiso 1 1 calc R U . . .
C16 C 0.51556(11) 0.8517(3) 0.07997(9) 0.0191(5) Uani 1 1 d . . . . .
H16 H 0.4721 0.8709 0.0633 0.023 Uiso 1 1 calc R U . . .
C17 C 0.54798(10) 0.8522(3) 0.13989(9) 0.0161(4) Uani 1 1 d . . . . .
C18 C 0.61313(10) 0.8195(3) 0.16544(9) 0.0132(4) Uani 1 1 d . . . . .
C19 C 0.58928(10) 0.5469(3) 0.40433(9) 0.0141(4) Uani 1 1 d . . . . .
C20 C 0.48233(10) 0.4278(3) 0.36865(9) 0.0149(4) Uani 1 1 d . . . . .
C21 C 0.44214(11) 0.3122(3) 0.32500(10) 0.0189(5) Uani 1 1 d . . . . .
H21 H 0.4512 0.2806 0.2925 0.023 Uiso 1 1 calc R U . . .
C22 C 0.38921(11) 0.2429(3) 0.32842(11) 0.0223(5) Uani 1 1 d . . . . .
H22 H 0.3618 0.1659 0.2980 0.027 Uiso 1 1 calc R U . . .
C23 C 0.37604(11) 0.2856(4) 0.37603(10) 0.0227(5) Uani 1 1 d . . . . .
H23 H 0.3402 0.2357 0.3790 0.027 Uiso 1 1 calc R U . . .
C24 C 0.41560(12) 0.4016(4) 0.41933(10) 0.0227(5) Uani 1 1 d . . . . .
H24 H 0.4067 0.4314 0.4521 0.027 Uiso 1 1 calc R U . . .
C25 C 0.46811(11) 0.4752(3) 0.41560(10) 0.0186(5) Uani 1 1 d . . . . .
H25 H 0.4942 0.5577 0.4450 0.022 Uiso 1 1 calc R U . . .
C26 C 0.46131(11) 0.8889(3) 0.17084(9) 0.0182(5) Uani 1 1 d . . . . .
C27 C 0.39762(11) 0.8762(3) 0.22884(10) 0.0199(5) Uani 1 1 d . . . . .
C28 C 0.40014(13) 0.7962(3) 0.28011(12) 0.0271(5) Uani 1 1 d . . . . .
H28 H 0.4390 0.7592 0.3093 0.032 Uiso 1 1 calc R U . . .
C29 C 0.34702(15) 0.7694(4) 0.28939(15) 0.0380(7) Uani 1 1 d . . . . .
H29 H 0.3494 0.7127 0.3245 0.046 Uiso 1 1 calc R U . . .
C30 C 0.29071(14) 0.8247(4) 0.24766(16) 0.0417(8) Uani 1 1 d . . . . .
H30 H 0.2540 0.8066 0.2538 0.050 Uiso 1 1 calc R U . . .
C31 C 0.28792(13) 0.9066(4) 0.19691(13) 0.0353(7) Uani 1 1 d . . . . .
H31 H 0.2490 0.9459 0.1684 0.042 Uiso 1 1 calc R U . . .
C32 C 0.34060(11) 0.9331(4) 0.18640(11) 0.0240(5) Uani 1 1 d . . . . .
H32 H 0.3379 0.9889 0.1510 0.029 Uiso 1 1 calc R U . . .
O5 O 0.59454(10) 1.0489(3) 0.41842(8) 0.0406(5) Uani 1 1 d . . . . .
C33 C 0.65460(13) 1.0901(4) 0.46197(11) 0.0300(6) Uani 1 1 d . . . . .
H33A H 0.6665 1.2200 0.4576 0.036 Uiso 1 1 calc R U . . .
H33B H 0.6857 1.0040 0.4586 0.036 Uiso 1 1 calc R U . . .
C34 C 0.65074(16) 1.0655(6) 0.52000(13) 0.0530(9) Uani 1 1 d . . . . .
H34A H 0.6766 1.1588 0.5488 0.064 Uiso 1 1 calc R U . . .
H34B H 0.6639 0.9384 0.5358 0.064 Uiso 1 1 calc R U . . .
C35 C 0.58256(14) 1.0963(4) 0.50532(11) 0.0355(7) Uani 1 1 d . . . . .
H35A H 0.5697 1.0321 0.5336 0.043 Uiso 1 1 calc R U . . .
H35B H 0.5726 1.2310 0.5043 0.043 Uiso 1 1 calc R U . . .
C36 C 0.55291(13) 1.0103(4) 0.44587(12) 0.0309(6) Uani 1 1 d . . . . .
H36A H 0.5477 0.8739 0.4488 0.037 Uiso 1 1 calc R U . . .
H36B H 0.5119 1.0668 0.4233 0.037 Uiso 1 1 calc R U . . .
O6 O 0.44839(13) 0.4010(5) 0.16119(10) 0.0765(9) Uani 1 1 d . . . . .
C37 C 0.43716(18) 0.3837(5) 0.10163(14) 0.0524(9) Uani 1 1 d . . . . .
H37A H 0.4588 0.2728 0.0954 0.063 Uiso 1 1 calc R U . . .
H37B H 0.4520 0.4961 0.0882 0.063 Uiso 1 1 calc R U . . .
C38 C 0.36866(16) 0.3633(5) 0.06889(12) 0.0454(8) Uani 1 1 d . . . . .
H38A H 0.3568 0.2301 0.0612 0.054 Uiso 1 1 calc R U . . .
H38B H 0.3538 0.4314 0.0312 0.054 Uiso 1 1 calc R U . . .
C39 C 0.34296(15) 0.4482(5) 0.10943(13) 0.0432(8) Uani 1 1 d . . . . .
H39A H 0.3363 0.5842 0.1027 0.052 Uiso 1 1 calc R U . . .
H39B H 0.3035 0.3882 0.1046 0.052 Uiso 1 1 calc R U . . .
C40 C 0.39264(16) 0.4086(4) 0.16861(12) 0.0391(7) Uani 1 1 d . . . . .
H40A H 0.3943 0.5089 0.1965 0.047 Uiso 1 1 calc R U . . .
H40B H 0.3848 0.2881 0.1838 0.047 Uiso 1 1 calc R U . . .
O7 O 0.58528(8) 0.9751(2) 0.30908(7) 0.0219(4) Uani 1 1 d D . . . .
H7A H 0.5864(9) 0.991(4) 0.3432(3) 0.033 Uiso 1 1 d D U . . .
H7B H 0.6186(6) 0.916(3) 0.3156(7) 0.033 Uiso 1 1 d D U . . .
O8 O 0.55244(9) 0.3545(3) 0.26169(7) 0.0287(4) Uani 1 1 d D . . . .
H8D H 0.5225(9) 0.347(3) 0.2283(6) 0.043 Uiso 1 1 d D U . . .
H8E H 0.5617(12) 0.2407(9) 0.2708(10) 0.043 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 1.8349(15) . ?
Ni1 O1 1.8363(15) . ?
Ni1 N2 1.8569(17) . ?
Ni1 N1 1.8571(18) . ?
O1 C1 1.327(2) . ?
O2 C18 1.316(2) . ?
O3 C19 1.219(2) . ?
O4 C26 1.218(3) . ?
N1 C7 1.305(3) . ?
N1 C9 1.476(3) . ?
N2 C11 1.306(3) . ?
N2 C10 1.479(3) . ?
N3 C19 1.375(3) . ?
N3 C2 1.402(3) . ?
N4 C19 1.371(3) . ?
N4 C20 1.407(3) . ?
N5 C26 1.366(3) . ?
N5 C17 1.396(3) . ?
N6 C26 1.379(3) . ?
N6 C27 1.406(3) . ?
C1 C6 1.408(3) . ?
C1 C2 1.428(3) . ?
C2 C3 1.384(3) . ?
C3 C4 1.391(3) . ?
C4 C5 1.369(3) . ?
C5 C6 1.421(3) . ?
C6 C7 1.460(3) . ?
C7 C8 1.509(3) . ?
C9 C10 1.503(3) . ?
C11 C13 1.455(3) . ?
C11 C12 1.513(3) . ?
C13 C18 1.412(3) . ?
C13 C14 1.421(3) . ?
C14 C15 1.362(3) . ?
C15 C16 1.397(3) . ?
C16 C17 1.380(3) . ?
C17 C18 1.428(3) . ?
C20 C25 1.390(3) . ?
C20 C21 1.392(3) . ?
C21 C22 1.382(3) . ?
C22 C23 1.383(3) . ?
C23 C24 1.384(4) . ?
C24 C25 1.387(3) . ?
C27 C28 1.384(3) . ?
C27 C32 1.397(3) . ?
C28 C29 1.381(4) . ?
C29 C30 1.376(5) . ?
C30 C31 1.376(4) . ?
C31 C32 1.387(4) . ?
O5 C33 1.427(3) . ?
O5 C36 1.438(3) . ?
C33 C34 1.503(4) . ?
C34 C35 1.518(4) . ?
C35 C36 1.496(4) . ?
O6 C40 1.406(4) . ?
O6 C37 1.410(4) . ?
C37 C38 1.497(5) . ?
C38 C39 1.507(4) . ?
C39 C40 1.497(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
O2 Ni1 O1 84.05(7) . . ?
O2 Ni1 N2 94.12(7) . . ?
O1 Ni1 N2 171.72(7) . . ?
O2 Ni1 N1 171.81(7) . . ?
O1 Ni1 N1 94.15(7) . . ?
N2 Ni1 N1 88.78(8) . . ?
C1 O1 Ni1 126.73(13) . . ?
C18 O2 Ni1 127.78(14) . . ?
C7 N1 C9 118.85(18) . . ?
C7 N1 Ni1 129.16(15) . . ?
C9 N1 Ni1 111.29(13) . . ?
C11 N2 C10 118.83(18) . . ?
C11 N2 Ni1 128.20(15) . . ?
C10 N2 Ni1 111.81(13) . . ?
C19 N3 C2 126.96(18) . . ?
C19 N4 C20 125.33(19) . . ?
C26 N5 C17 128.1(2) . . ?
C26 N6 C27 126.1(2) . . ?
O1 C1 C6 124.54(19) . . ?
O1 C1 C2 116.31(18) . . ?
C6 C1 C2 119.16(19) . . ?
C3 C2 N3 124.4(2) . . ?
C3 C2 C1 120.5(2) . . ?
N3 C2 C1 115.03(18) . . ?
C2 C3 C4 119.8(2) . . ?
C5 C4 C3 120.8(2) . . ?
C4 C5 C6 121.3(2) . . ?
C1 C6 C5 118.3(2) . . ?
C1 C6 C7 121.57(18) . . ?
C5 C6 C7 120.1(2) . . ?
N1 C7 C6 121.54(19) . . ?
N1 C7 C8 119.74(19) . . ?
C6 C7 C8 118.70(18) . . ?
N1 C9 C10 108.85(17) . . ?
N2 C10 C9 109.14(17) . . ?
N2 C11 C13 121.99(19) . . ?
N2 C11 C12 120.5(2) . . ?
C13 C11 C12 117.52(18) . . ?
C18 C13 C14 118.2(2) . . ?
C18 C13 C11 121.67(18) . . ?
C14 C13 C11 120.17(19) . . ?
C15 C14 C13 121.3(2) . . ?
C14 C15 C16 121.0(2) . . ?
C17 C16 C15 119.6(2) . . ?
C16 C17 N5 125.4(2) . . ?
C16 C17 C18 120.6(2) . . ?
N5 C17 C18 114.04(19) . . ?
O2 C18 C13 124.6(2) . . ?
O2 C18 C17 116.15(19) . . ?
C13 C18 C17 119.25(19) . . ?
O3 C19 N4 124.8(2) . . ?
O3 C19 N3 123.2(2) . . ?
N4 C19 N3 112.04(18) . . ?
C25 C20 C21 119.1(2) . . ?
C25 C20 N4 123.9(2) . . ?
C21 C20 N4 116.92(19) . . ?
C22 C21 C20 120.8(2) . . ?
C21 C22 C23 120.1(2) . . ?
C22 C23 C24 119.3(2) . . ?
C23 C24 C25 121.0(2) . . ?
C24 C25 C20 119.7(2) . . ?
O4 C26 N5 124.2(2) . . ?
O4 C26 N6 124.1(2) . . ?
N5 C26 N6 111.69(19) . . ?
C28 C27 C32 119.3(2) . . ?
C28 C27 N6 117.9(2) . . ?
C32 C27 N6 122.8(2) . . ?
C29 C28 C27 120.9(3) . . ?
C30 C29 C28 119.9(3) . . ?
C29 C30 C31 119.5(3) . . ?
C30 C31 C32 121.6(3) . . ?
C31 C32 C27 118.7(3) . . ?
C33 O5 C36 109.7(2) . . ?
O5 C33 C34 106.4(2) . . ?
C33 C34 C35 103.0(2) . . ?
C36 C35 C34 101.8(2) . . ?
O5 C36 C35 105.1(2) . . ?
C40 O6 C37 111.1(3) . . ?
O6 C37 C38 106.5(3) . . ?
C37 C38 C39 103.6(2) . . ?
C40 C39 C38 102.8(3) . . ?
O6 C40 C39 106.2(2) . . ?

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
O2 Ni1 O1 C1 177.74(17) . . . . ?
N1 Ni1 O1 C1 -10.28(17) . . . . ?
O1 Ni1 O2 C18 -168.27(17) . . . . ?
N2 Ni1 O2 C18 3.62(18) . . . . ?
O1 Ni1 N1 C7 -4.5(2) . . . . ?
N2 Ni1 N1 C7 -176.73(19) . . . . ?
O1 Ni1 N1 C9 -174.61(14) . . . . ?
N2 Ni1 N1 C9 13.15(14) . . . . ?
O2 Ni1 N2 C11 -13.50(19) . . . . ?
N1 Ni1 N2 C11 174.17(19) . . . . ?
O2 Ni1 N2 C10 179.10(14) . . . . ?
N1 Ni1 N2 C10 6.77(14) . . . . ?
Ni1 O1 C1 C6 16.9(3) . . . . ?
Ni1 O1 C1 C2 -163.34(14) . . . . ?
C19 N3 C2 C3 12.9(4) . . . . ?
C19 N3 C2 C1 -170.4(2) . . . . ?
O1 C1 C2 C3 -174.34(19) . . . . ?
C6 C1 C2 C3 5.4(3) . . . . ?
O1 C1 C2 N3 8.7(3) . . . . ?
C6 C1 C2 N3 -171.47(19) . . . . ?
N3 C2 C3 C4 174.2(2) . . . . ?
C1 C2 C3 C4 -2.4(3) . . . . ?
C2 C3 C4 C5 -1.7(3) . . . . ?
C3 C4 C5 C6 2.8(3) . . . . ?
O1 C1 C6 C5 175.4(2) . . . . ?
C2 C1 C6 C5 -4.3(3) . . . . ?
O1 C1 C6 C7 -7.5(3) . . . . ?
C2 C1 C6 C7 172.8(2) . . . . ?
C4 C5 C6 C1 0.3(3) . . . . ?
C4 C5 C6 C7 -176.8(2) . . . . ?
C9 N1 C7 C6 -177.64(19) . . . . ?
Ni1 N1 C7 C6 12.9(3) . . . . ?
C9 N1 C7 C8 0.8(3) . . . . ?
Ni1 N1 C7 C8 -168.68(15) . . . . ?
C1 C6 C7 N1 -7.6(3) . . . . ?
C5 C6 C7 N1 169.4(2) . . . . ?
C1 C6 C7 C8 173.9(2) . . . . ?
C5 C6 C7 C8 -9.0(3) . . . . ?
C7 N1 C9 C10 159.34(19) . . . . ?
Ni1 N1 C9 C10 -29.4(2) . . . . ?
C11 N2 C10 C9 166.76(19) . . . . ?
Ni1 N2 C10 C9 -24.5(2) . . . . ?
N1 C9 C10 N2 34.2(2) . . . . ?
C10 N2 C11 C13 -177.18(18) . . . . ?
Ni1 N2 C11 C13 16.2(3) . . . . ?
C10 N2 C11 C12 3.4(3) . . . . ?
Ni1 N2 C11 C12 -163.25(16) . . . . ?
N2 C11 C13 C18 -6.3(3) . . . . ?
C12 C11 C13 C18 173.13(19) . . . . ?
N2 C11 C13 C14 173.0(2) . . . . ?
C12 C11 C13 C14 -7.6(3) . . . . ?
C18 C13 C14 C15 -0.1(3) . . . . ?
C11 C13 C14 C15 -179.4(2) . . . . ?
C13 C14 C15 C16 1.0(3) . . . . ?
C14 C15 C16 C17 -0.3(3) . . . . ?
C15 C16 C17 N5 179.1(2) . . . . ?
C15 C16 C17 C18 -1.4(3) . . . . ?
C26 N5 C17 C16 10.1(4) . . . . ?
C26 N5 C17 C18 -169.4(2) . . . . ?
Ni1 O2 C18 C13 3.3(3) . . . . ?
Ni1 O2 C18 C17 -178.03(14) . . . . ?
C14 C13 C18 O2 177.09(19) . . . . ?
C11 C13 C18 O2 -3.6(3) . . . . ?
C14 C13 C18 C17 -1.5(3) . . . . ?
C11 C13 C18 C17 177.80(19) . . . . ?
C16 C17 C18 O2 -176.5(2) . . . . ?
N5 C17 C18 O2 3.1(3) . . . . ?
C16 C17 C18 C13 2.3(3) . . . . ?
N5 C17 C18 C13 -178.2(2) . . . . ?
C20 N4 C19 O3 -7.2(4) . . . . ?
C20 N4 C19 N3 173.5(2) . . . . ?
C2 N3 C19 O3 6.4(4) . . . . ?
C2 N3 C19 N4 -174.2(2) . . . . ?
C19 N4 C20 C25 30.9(3) . . . . ?
C19 N4 C20 C21 -152.6(2) . . . . ?
C25 C20 C21 C22 -0.9(3) . . . . ?
N4 C20 C21 C22 -177.6(2) . . . . ?
C20 C21 C22 C23 -1.0(4) . . . . ?
C21 C22 C23 C24 1.5(4) . . . . ?
C22 C23 C24 C25 -0.1(4) . . . . ?
C23 C24 C25 C20 -1.9(4) . . . . ?
C21 C20 C25 C24 2.3(3) . . . . ?
N4 C20 C25 C24 178.8(2) . . . . ?
C17 N5 C26 O4 -7.0(4) . . . . ?
C17 N5 C26 N6 173.3(2) . . . . ?
C27 N6 C26 O4 12.4(4) . . . . ?
C27 N6 C26 N5 -167.9(2) . . . . ?
C26 N6 C27 C28 146.8(2) . . . . ?
C26 N6 C27 C32 -34.5(4) . . . . ?
C32 C27 C28 C29 1.0(4) . . . . ?
N6 C27 C28 C29 179.8(2) . . . . ?
C27 C28 C29 C30 -0.9(4) . . . . ?
C28 C29 C30 C31 0.0(4) . . . . ?
C29 C30 C31 C32 0.7(4) . . . . ?
C30 C31 C32 C27 -0.5(4) . . . . ?
C28 C27 C32 C31 -0.3(4) . . . . ?
N6 C27 C32 C31 -179.0(2) . . . . ?
C36 O5 C33 C34 3.2(3) . . . . ?
O5 C33 C34 C35 -24.8(3) . . . . ?
C33 C34 C35 C36 36.0(3) . . . . ?
C33 O5 C36 C35 20.3(3) . . . . ?
C34 C35 C36 O5 -34.7(3) . . . . ?
C40 O6 C37 C38 -4.8(4) . . . . ?
O6 C37 C38 C39 22.6(4) . . . . ?
C37 C38 C39 C40 -30.7(3) . . . . ?
C37 O6 C40 C39 -15.2(4) . . . . ?
C38 C39 C40 O6 28.5(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O8 0.82(3) 2.73(3) 3.324(3) 130(2) .
N4 H4 O8 0.84(3) 2.05(3) 2.871(3) 168(3) .
N5 H5 O7 0.78(3) 2.29(3) 3.020(3) 156(3) .
N6 H6 O7 0.82(3) 2.28(3) 3.036(3) 152(2) .
C4 H4A O4 0.95 2.52 3.300(3) 139.2 4_676
C24 H24 O3 0.95 2.36 3.294(3) 166.5 3_666
O7 H7B O1 0.8500(10) 2.081(4) 2.927(2) 173(2) .
O7 H7A O5 0.8500(10) 1.861(4) 2.708(2) 174(3) .
O8 H8D O6 0.8501(10) 1.911(7) 2.733(3) 162(2) .
O8 H8E O7 0.8502(10) 2.099(6) 2.938(3) 169(3) 1_545

_refine_diff_density_max         0.716
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.078


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
####################################################################### 
# 
# 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_jyy284
_database_code_depnum_ccdc_archive 'CCDC 2379618'
loop_
_audit_author_name
_audit_author_address
'Joseph W. Ziller'
;University of California, Irvine
United States of America
;
_audit_update_record             
;
2024-08-24 deposited with the CCDC.	2024-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C92 H120 Cl N13 Ni2 O11'
_chemical_formula_weight         1736.87

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.4188(9)
_cell_length_b                   15.6518(13)
_cell_length_c                   25.611(2)
_cell_angle_alpha                97.4909(14)
_cell_angle_beta                 100.7164(14)
_cell_angle_gamma                104.6492(14)
_cell_volume                     4274.9(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    9831
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      26.22

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_F_000             1848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.172
_exptl_absorpt_coefficient_mu    0.541
_shelx_estimated_absorpt_T_min   0.870
_shelx_estimated_absorpt_T_max   0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Bruker TWINABS 2012/1'
_exptl_absorpt_special_details   
; 
HKLF 5 dataset constructed from all observations involving domain 1 
33208 Corrected reflections written to file twin5.hkl 
Reflections merged according to point-group -1 
Single reflections that also occur in composites omitted 
Minimum and maximum apparent transmission:  0.6744  0.7454 (ratio 0.9047) 
Additional spherical absorption correction applied with mu*r =  0.2000 
;
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17549
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.460
_diffrn_reflns_theta_max         26.419
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             17549
_reflns_number_gt                15615
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;An orange crystal of approximate dimensions 0.172 x 0.236 x 0.265 mm 
was mounted in a cryoloop and transferred to a Bruker SMART APEX II 
diffractometer system.  The APEX2 program package and the CELL_NOW 
were used to determine the unit-cell parameters.  Data was collected 
using a 120 sec/frame scan time.  The raw frame data was processed 
using SAINT and TWINABS to yield the reflection data file (HKLF5 format).  
Subsequent calculations were carried out using the SHELXTL program package.  
There were no systematic absences nor any diffraction symmetry other than 
the Friedel condition.  The centrosymmetric triclinic space group P-1 was 
assigned and later determined to be correct.

The structure was solved by direct methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral 
atoms were used throughout the analysis.  Hydrogen atoms H(3), H(4), H(5), 
H(6), H(9), H(10), H(11) and H(12) were located from a difference-Fourier 
map and refined (x,y,z and riding Uiso).  The remaining hydrogen atoms were 
included using a riding model.  There were three molecules of tetrahydrofuran 
solvent present.  Disordered atoms were included using multiple components, 
partial site-occupancy-factors and restraint/constraints.

Least-squares analysis yielded wR2 = 0.1368 and Goof = 1.063 for 1132 
variables refined against 17549 data (0.80 Å), R1 = 0.0519 for those 15615 
with I > 2.0sigma(I).  The structure was refined as a two-component twin, 
BASF = 0.3687.,Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0656P)²+7.1545P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17549
_refine_ls_number_parameters     1132
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1368
_refine_ls_wR_factor_gt          0.1310
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT214_jyy284              
;
PROBLEM: Atom C88 (Anion/Solvent) ADP max/min Ratio 5.5 prolat
RESPONSE: ...The THF solvent disorder contributed
to high thermal displacement parameters.
;
# end Validation Reply Form 

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.37298(4) 1.56996(3) 0.13888(2) 0.01430(11) Uani 1 1 d . . . . .
O1 O 0.4003(2) 1.57257(16) 0.21246(9) 0.0144(5) Uani 1 1 d . . . . .
O2 O 0.3733(2) 1.45174(16) 0.13291(10) 0.0154(5) Uani 1 1 d . . . . .
O3 O 0.4975(2) 1.54639(18) 0.40019(10) 0.0218(6) Uani 1 1 d . . . . .
O4 O 0.5115(3) 1.19205(19) 0.15238(11) 0.0243(6) Uani 1 1 d . . . . .
N1 N 0.3871(3) 1.6921(2) 0.14577(13) 0.0176(6) Uani 1 1 d . . . . .
N2 N 0.3304(3) 1.5619(2) 0.06421(12) 0.0161(6) Uani 1 1 d . . . . .
N3 N 0.4203(3) 1.5375(2) 0.30987(13) 0.0158(6) Uani 1 1 d . . . . .
H3 H 0.377(4) 1.511(3) 0.2855(19) 0.019 Uiso 1 1 d . U . . .
N4 N 0.3462(3) 1.4209(2) 0.35048(12) 0.0178(6) Uani 1 1 d . . . . .
H4 H 0.297(4) 1.396(3) 0.3168(18) 0.021 Uiso 1 1 d . U . . .
N5 N 0.4107(3) 1.3010(2) 0.15033(13) 0.0171(6) Uani 1 1 d . . . . .
H5 H 0.372(4) 1.332(3) 0.1681(18) 0.021 Uiso 1 1 d . U . . .
N6 N 0.3914(3) 1.2108(2) 0.21333(13) 0.0201(7) Uani 1 1 d . . . . .
H6 H 0.328(4) 1.239(3) 0.2194(18) 0.024 Uiso 1 1 d . U . . .
C1 C 0.4403(3) 1.6441(2) 0.25077(15) 0.0146(7) Uani 1 1 d . . . . .
C2 C 0.4590(3) 1.6288(2) 0.30513(15) 0.0156(7) Uani 1 1 d . . . . .
C3 C 0.5083(3) 1.6992(3) 0.34877(15) 0.0190(8) Uani 1 1 d . . . . .
H3A H 0.5223 1.6878 0.3846 0.023 Uiso 1 1 calc R U . . .
C4 C 0.5374(4) 1.7877(3) 0.33948(16) 0.0227(8) Uani 1 1 d . . . . .
H4A H 0.5718 1.8364 0.3693 0.027 Uiso 1 1 calc R U . . .
C5 C 0.5172(4) 1.8049(3) 0.28820(17) 0.0239(9) Uani 1 1 d . . . . .
H5A H 0.5364 1.8655 0.2830 0.029 Uiso 1 1 calc R U . . .
C6 C 0.4679(3) 1.7343(2) 0.24238(15) 0.0171(7) Uani 1 1 d . . . . .
C7 C 0.4371(4) 1.7554(3) 0.18863(16) 0.0202(8) Uani 1 1 d . . . . .
C8 C 0.4635(5) 1.8534(3) 0.18412(18) 0.0305(10) Uani 1 1 d . . . . .
H8A H 0.4447 1.8584 0.1459 0.046 Uiso 1 1 calc R U . . .
H8B H 0.5514 1.8843 0.2003 0.046 Uiso 1 1 calc R U . . .
H8C H 0.4115 1.8810 0.2032 0.046 Uiso 1 1 calc R U . . .
C9 C 0.3501(4) 1.7181(3) 0.09302(16) 0.0228(8) Uani 1 1 d . . . . .
H9A H 0.4250 1.7483 0.0810 0.027 Uiso 1 1 calc R U . . .
H9B H 0.2995 1.7605 0.0965 0.027 Uiso 1 1 calc R U . . .
C10 C 0.2754(4) 1.6343(3) 0.05211(16) 0.0211(8) Uani 1 1 d . . . . .
H10A H 0.1874 1.6183 0.0548 0.025 Uiso 1 1 calc R U . . .
H10B H 0.2786 1.6444 0.0150 0.025 Uiso 1 1 calc R U . . .
C11 C 0.4251(3) 1.5049(3) 0.35686(15) 0.0169(7) Uani 1 1 d . . . . .
C12 C 0.2824(4) 1.5039(3) -0.03288(15) 0.0208(8) Uani 1 1 d . . . . .
H12A H 0.2003 1.5141 -0.0369 0.031 Uiso 1 1 calc R U . . .
H12B H 0.2757 1.4472 -0.0562 0.031 Uiso 1 1 calc R U . . .
H12C H 0.3395 1.5534 -0.0433 0.031 Uiso 1 1 calc R U . . .
C13 C 0.3768(3) 1.4233(2) 0.03768(14) 0.0159(7) Uani 1 1 d . . . . .
C14 C 0.4009(4) 1.3648(3) -0.00384(15) 0.0189(8) Uani 1 1 d . . . . .
H14A H 0.3949 1.3787 -0.0391 0.023 Uiso 1 1 calc R U . . .
C15 C 0.4327(4) 1.2888(3) 0.00629(15) 0.0201(8) Uani 1 1 d . . . . .
H15A H 0.4502 1.2514 -0.0218 0.024 Uiso 1 1 calc R U . . .
C16 C 0.4398(4) 1.2654(3) 0.05758(16) 0.0192(8) Uani 1 1 d . . . . .
H16A H 0.4603 1.2119 0.0640 0.023 Uiso 1 1 calc R U . . .
C17 C 0.4167(3) 1.3208(2) 0.09861(14) 0.0159(7) Uani 1 1 d . . . . .
C18 C 0.3892(3) 1.4030(2) 0.09028(14) 0.0143(7) Uani 1 1 d . . . . .
C19 C 0.3314(3) 1.4993(3) 0.02527(15) 0.0174(7) Uani 1 1 d . . . . .
C20 C 0.3333(3) 1.3646(3) 0.38863(15) 0.0174(7) Uani 1 1 d . . . . .
C21 C 0.2615(4) 1.2754(3) 0.36865(16) 0.0218(8) Uani 1 1 d . . . . .
H21A H 0.2267 1.2560 0.3309 0.026 Uiso 1 1 calc R U . . .
C22 C 0.2410(4) 1.2156(3) 0.40329(17) 0.0290(9) Uani 1 1 d . . . . .
H22A H 0.1923 1.1552 0.3892 0.035 Uiso 1 1 calc R U . . .
C23 C 0.2906(4) 1.2427(3) 0.45817(17) 0.0285(9) Uani 1 1 d . . . . .
H23A H 0.2764 1.2013 0.4819 0.034 Uiso 1 1 calc R U . . .
C24 C 0.3611(4) 1.3305(3) 0.47815(15) 0.0234(8) Uani 1 1 d . . . . .
H24A H 0.3947 1.3492 0.5160 0.028 Uiso 1 1 calc R U . . .
C25 C 0.3843(3) 1.3927(3) 0.44417(15) 0.0201(8) Uani 1 1 d . . . . .
H25A H 0.4338 1.4528 0.4585 0.024 Uiso 1 1 calc R U . . .
C26 C 0.4429(3) 1.2309(2) 0.17025(15) 0.0180(8) Uani 1 1 d . . . . .
C27 C 0.4122(4) 1.1450(2) 0.24399(15) 0.0180(7) Uani 1 1 d . . . . .
C28 C 0.3219(4) 1.1098(3) 0.27148(16) 0.0227(8) Uani 1 1 d . . . . .
H28A H 0.2479 1.1281 0.2674 0.027 Uiso 1 1 calc R U . . .
C29 C 0.3388(4) 1.0486(3) 0.30460(18) 0.0272(9) Uani 1 1 d . . . . .
H29A H 0.2766 1.0253 0.3231 0.033 Uiso 1 1 calc R U . . .
C30 C 0.4456(4) 1.0215(3) 0.31083(17) 0.0238(8) Uani 1 1 d . . . . .
H30A H 0.4577 0.9800 0.3338 0.029 Uiso 1 1 calc R U . . .
C31 C 0.5360(4) 1.0559(2) 0.28289(16) 0.0207(8) Uani 1 1 d . . . . .
H31A H 0.6093 1.0369 0.2866 0.025 Uiso 1 1 calc R U . . .
C32 C 0.5197(3) 1.1177(2) 0.24973(15) 0.0180(7) Uani 1 1 d . . . . .
H32A H 0.5818 1.1410 0.2311 0.022 Uiso 1 1 calc R U . . .
Ni2 Ni 0.15950(4) 1.55593(3) 0.36340(2) 0.01411(11) Uani 1 1 d . . . . .
O5 O 0.1358(2) 1.55738(17) 0.29056(9) 0.0147(5) Uani 1 1 d . . . . .
O6 O 0.0829(2) 1.43353(17) 0.34377(9) 0.0150(5) Uani 1 1 d . . . . .
O7 O 0.0224(3) 1.52243(18) 0.09648(10) 0.0208(6) Uani 1 1 d . . . . .
O8 O -0.1785(3) 1.12969(18) 0.27193(11) 0.0248(6) Uani 1 1 d . . . . .
N7 N 0.2237(3) 1.6803(2) 0.38296(12) 0.0170(6) Uani 1 1 d . . . . .
N8 N 0.1960(3) 1.5509(2) 0.43676(12) 0.0167(6) Uani 1 1 d . . . . .
N9 N 0.0967(3) 1.5195(2) 0.18582(12) 0.0156(6) Uani 1 1 d . . . . .
H9 H 0.130(4) 1.492(3) 0.2092(18) 0.019 Uiso 1 1 d . U . . .
N10 N 0.0839(3) 1.4015(2) 0.12077(13) 0.0176(7) Uani 1 1 d . . . . .
H10 H 0.115(4) 1.390(3) 0.1440(19) 0.021 Uiso 1 1 d . U . . .
N11 N -0.0385(3) 1.2693(2) 0.29481(13) 0.0177(7) Uani 1 1 d . . . . .
H11 H 0.015(4) 1.298(3) 0.2843(19) 0.021 Uiso 1 1 d . U . . .
N12 N -0.0400(3) 1.1718(2) 0.21949(13) 0.0198(7) Uani 1 1 d . . . . .
H12 H 0.021(5) 1.214(3) 0.2210(19) 0.024 Uiso 1 1 d . U . . .
C33 C 0.1442(3) 1.6277(2) 0.26761(14) 0.0141(7) Uani 1 1 d . . . . .
C34 C 0.1167(3) 1.6095(2) 0.20896(14) 0.0148(7) Uani 1 1 d . . . . .
C35 C 0.1155(3) 1.6787(3) 0.18082(15) 0.0190(8) Uani 1 1 d . . . . .
H35A H 0.0958 1.6662 0.1424 0.023 Uiso 1 1 calc R U . . .
C36 C 0.1431(4) 1.7672(3) 0.20840(17) 0.0239(8) Uani 1 1 d . . . . .
H36A H 0.1409 1.8143 0.1886 0.029 Uiso 1 1 calc R U . . .
C37 C 0.1732(4) 1.7862(3) 0.26374(16) 0.0203(8) Uani 1 1 d . . . . .
H37A H 0.1929 1.8467 0.2818 0.024 Uiso 1 1 calc R U . . .
C38 C 0.1756(3) 1.7183(3) 0.29464(16) 0.0177(8) Uani 1 1 d . . . . .
C39 C 0.2168(3) 1.7409(3) 0.35338(16) 0.0189(8) Uani 1 1 d . . . . .
C40 C 0.2554(5) 1.8395(3) 0.37935(17) 0.0311(10) Uani 1 1 d . . . . .
H40A H 0.2484 1.8452 0.4171 0.047 Uiso 1 1 calc R U . . .
H40B H 0.2012 1.8700 0.3597 0.047 Uiso 1 1 calc R U . . .
H40C H 0.3417 1.8671 0.3780 0.047 Uiso 1 1 calc R U . . .
C41 C 0.2740(4) 1.7094(3) 0.44226(15) 0.0231(8) Uani 1 1 d . . . . .
H41A H 0.2131 1.7311 0.4592 0.028 Uiso 1 1 calc R U . . .
H41B H 0.3518 1.7592 0.4497 0.028 Uiso 1 1 calc R U . . .
C42 C 0.2989(4) 1.6306(3) 0.46500(15) 0.0224(8) Uani 1 1 d . . . . .
H42A H 0.3791 1.6227 0.4591 0.027 Uiso 1 1 calc R U . . .
H42B H 0.3031 1.6401 0.5044 0.027 Uiso 1 1 calc R U . . .
C43 C 0.1529(4) 1.4874(3) 0.46165(14) 0.0181(8) Uani 1 1 d . . . . .
C44 C 0.2043(4) 1.4947(3) 0.52180(15) 0.0234(9) Uani 1 1 d . . . . .
H44A H 0.2945 1.5219 0.5305 0.035 Uiso 1 1 calc R U . . .
H44B H 0.1856 1.4347 0.5310 0.035 Uiso 1 1 calc R U . . .
H44C H 0.1658 1.5324 0.5426 0.035 Uiso 1 1 calc R U . . .
C45 C 0.0577(3) 1.4056(2) 0.43265(14) 0.0156(7) Uani 1 1 d . . . . .
C46 C -0.0065(4) 1.3445(3) 0.46113(16) 0.0238(9) Uani 1 1 d . . . . .
H46A H 0.0057 1.3608 0.4992 0.029 Uiso 1 1 calc R U . . .
C47 C -0.0850(4) 1.2635(3) 0.43529(16) 0.0249(9) Uani 1 1 d . . . . .
H47A H -0.1306 1.2254 0.4550 0.030 Uiso 1 1 calc R U . . .
C48 C -0.0995(4) 1.2353(3) 0.37903(16) 0.0218(8) Uani 1 1 d . . . . .
H48A H -0.1513 1.1772 0.3614 0.026 Uiso 1 1 calc R U . . .
C49 C -0.0383(3) 1.2923(3) 0.35023(15) 0.0167(7) Uani 1 1 d . . . . .
C50 C 0.0360(3) 1.3816(2) 0.37557(15) 0.0152(7) Uani 1 1 d . . . . .
C51 C 0.0649(3) 1.4836(3) 0.13090(14) 0.0160(7) Uani 1 1 d . . . . .
C52 C 0.0707(3) 1.3486(2) 0.06998(15) 0.0161(7) Uani 1 1 d . . . . .
C53 C 0.0929(4) 1.2649(3) 0.07105(16) 0.0205(8) Uani 1 1 d . . . . .
H53A H 0.1126 1.2463 0.1047 0.025 Uiso 1 1 calc R U . . .
C54 C 0.0864(4) 1.2088(3) 0.02320(16) 0.0244(9) Uani 1 1 d . . . . .
H54A H 0.1007 1.1518 0.0242 0.029 Uiso 1 1 calc R U . . .
C55 C 0.0593(4) 1.2356(3) -0.02594(16) 0.0243(9) Uani 1 1 d . . . . .
H55A H 0.0564 1.1978 -0.0586 0.029 Uiso 1 1 calc R U . . .
C56 C 0.0364(4) 1.3178(3) -0.02710(15) 0.0212(8) Uani 1 1 d . . . . .
H56A H 0.0171 1.3361 -0.0608 0.025 Uiso 1 1 calc R U . . .
C57 C 0.0411(3) 1.3747(3) 0.02056(15) 0.0195(8) Uani 1 1 d . . . . .
H57A H 0.0241 1.4308 0.0192 0.023 Uiso 1 1 calc R U . . .
C58 C -0.0928(3) 1.1855(2) 0.26286(15) 0.0175(7) Uani 1 1 d . . . . .
C59 C -0.0858(4) 1.0982(3) 0.17600(16) 0.0202(8) Uani 1 1 d . . . . .
C60 C -0.0007(4) 1.0744(3) 0.14851(17) 0.0249(9) Uani 1 1 d . . . . .
H60A H 0.0850 1.1066 0.1599 0.030 Uiso 1 1 calc R U . . .
C61 C -0.0411(4) 1.0038(3) 0.10457(19) 0.0324(10) Uani 1 1 d . . . . .
H61A H 0.0175 0.9873 0.0864 0.039 Uiso 1 1 calc R U . . .
C62 C -0.1668(4) 0.9570(3) 0.08682(18) 0.0312(10) Uani 1 1 d . . . . .
H62A H -0.1945 0.9095 0.0563 0.037 Uiso 1 1 calc R U . . .
C63 C -0.2496(4) 0.9806(3) 0.11415(18) 0.0281(9) Uani 1 1 d . . . . .
H63A H -0.3353 0.9486 0.1024 0.034 Uiso 1 1 calc R U . . .
C64 C -0.2113(4) 1.0502(3) 0.15854(17) 0.0259(9) Uani 1 1 d . . . . .
H64A H -0.2703 1.0652 0.1770 0.031 Uiso 1 1 calc R U . . .
Cl1 Cl 0.20411(8) 1.33625(6) 0.22736(3) 0.01551(18) Uani 1 1 d . . . . .
N13 N 0.7531(3) 1.4945(2) 0.26110(12) 0.0194(7) Uani 1 1 d . . . . .
C65 C 0.8466(3) 1.5579(3) 0.30952(14) 0.0211(8) Uani 1 1 d . . . . .
H65A H 0.8852 1.5214 0.3323 0.025 Uiso 1 1 calc R U . . .
H65B H 0.9133 1.5963 0.2961 0.025 Uiso 1 1 calc R U . . .
C66 C 0.7966(4) 1.6186(3) 0.34506(16) 0.0242(9) Uani 1 1 d . . . . .
H66A H 0.7404 1.5822 0.3642 0.029 Uiso 1 1 calc R U . . .
H66B H 0.7486 1.6505 0.3225 0.029 Uiso 1 1 calc R U . . .
C67 C 0.9045(4) 1.6861(3) 0.38583(17) 0.0310(10) Uani 1 1 d . . . . .
H67A H 0.9586 1.7232 0.3663 0.037 Uiso 1 1 calc R U . . .
H67B H 0.9544 1.6534 0.4067 0.037 Uiso 1 1 calc R U . . .
C68 C 0.8621(4) 1.7477(3) 0.42494(18) 0.0355(11) Uani 1 1 d . . . . .
H68A H 0.8118 1.7798 0.4045 0.053 Uiso 1 1 calc R U . . .
H68B H 0.9351 1.7912 0.4496 0.053 Uiso 1 1 calc R U . . .
H68C H 0.8123 1.7116 0.4459 0.053 Uiso 1 1 calc R U . . .
C69 C 0.6931(3) 1.5471(3) 0.22340(15) 0.0215(8) Uani 1 1 d . . . . .
H69A H 0.6342 1.5037 0.1922 0.026 Uiso 1 1 calc R U . . .
H69B H 0.6441 1.5782 0.2429 0.026 Uiso 1 1 calc R U . . .
C70 C 0.7818(4) 1.6164(3) 0.20180(16) 0.0246(9) Uani 1 1 d . . . . .
H70A H 0.8264 1.5859 0.1793 0.030 Uiso 1 1 calc R U . . .
H70B H 0.8441 1.6590 0.2323 0.030 Uiso 1 1 calc R U . . .
C71 C 0.7088(4) 1.6672(3) 0.16809(17) 0.0260(9) Uani 1 1 d . . . . .
H71A H 0.6445 1.6238 0.1386 0.031 Uiso 1 1 calc R U . . .
H71B H 0.6659 1.6984 0.1912 0.031 Uiso 1 1 calc R U . . .
C72 C 0.7914(4) 1.7358(3) 0.14379(18) 0.0325(10) Uani 1 1 d . . . . .
H72A H 0.8288 1.7048 0.1186 0.049 Uiso 1 1 calc R U . . .
H72B H 0.8573 1.7776 0.1727 0.049 Uiso 1 1 calc R U . . .
H72C H 0.7415 1.7693 0.1244 0.049 Uiso 1 1 calc R U . . .
C73 C 0.8245(3) 1.4403(3) 0.23277(15) 0.0232(8) Uani 1 1 d . . . . .
H73A H 0.9021 1.4823 0.2291 0.028 Uiso 1 1 calc R U . . .
H73B H 0.8484 1.3991 0.2563 0.028 Uiso 1 1 calc R U . . .
C74 C 0.7559(4) 1.3852(3) 0.17743(16) 0.0239(8) Uani 1 1 d . . . . .
H74A H 0.7605 1.4243 0.1500 0.029 Uiso 1 1 calc R U . . .
H74B H 0.6672 1.3592 0.1772 0.029 Uiso 1 1 calc R U . . .
C75 C 0.8144(4) 1.3098(3) 0.16354(17) 0.0258(9) Uani 1 1 d . . . . .
H75A H 0.9061 1.3342 0.1744 0.031 Uiso 1 1 calc R U . . .
H75B H 0.7893 1.2625 0.1847 0.031 Uiso 1 1 calc R U . . .
C76 C 0.7775(4) 1.2679(3) 0.10417(17) 0.0313(10) Uani 1 1 d . . . . .
H76A H 0.8067 1.3135 0.0830 0.047 Uiso 1 1 calc R U . . .
H76B H 0.6868 1.2443 0.0929 0.047 Uiso 1 1 calc R U . . .
H76C H 0.8150 1.2188 0.0980 0.047 Uiso 1 1 calc R U . . .
C77 C 0.6487(3) 1.4335(3) 0.27939(15) 0.0212(8) Uani 1 1 d . . . . .
H77A H 0.5863 1.3969 0.2468 0.025 Uiso 1 1 calc R U . . .
H77B H 0.6076 1.4717 0.2990 0.025 Uiso 1 1 calc R U . . .
C78 C 0.6850(4) 1.3698(3) 0.31559(16) 0.0218(8) Uani 1 1 d . . . . .
H78A H 0.7655 1.4005 0.3414 0.026 Uiso 1 1 calc R U . . .
H78B H 0.6944 1.3164 0.2933 0.026 Uiso 1 1 calc R U . . .
C79 C 0.5839(3) 1.3408(3) 0.34656(15) 0.0193(7) Uani 1 1 d . . . . .
H79A H 0.5802 1.3945 0.3706 0.023 Uiso 1 1 calc R U . . .
H79B H 0.5027 1.3165 0.3203 0.023 Uiso 1 1 calc R U . . .
C80 C 0.6033(4) 1.2711(3) 0.38016(16) 0.0245(8) Uani 1 1 d . . . . .
H80A H 0.6061 1.2173 0.3567 0.037 Uiso 1 1 calc R U . . .
H80B H 0.5345 1.2553 0.3983 0.037 Uiso 1 1 calc R U . . .
H80C H 0.6819 1.2954 0.4074 0.037 Uiso 1 1 calc R U . . .
O9 O 0.4322(4) 0.9202(2) 0.05917(16) 0.0516(10) Uani 1 1 d . . . . .
C81 C 0.4374(5) 1.0084(4) 0.0840(3) 0.0575(17) Uani 1 1 d . . . . .
H81A H 0.4829 1.0534 0.0656 0.069 Uiso 1 1 calc R U . . .
H81B H 0.4818 1.0209 0.1225 0.069 Uiso 1 1 calc R U . . .
C82 C 0.3080(5) 1.0146(5) 0.0799(3) 0.070(2) Uani 1 1 d . . . . .
H82A H 0.2978 1.0691 0.0660 0.084 Uiso 1 1 calc R U . . .
H82B H 0.2858 1.0159 0.1155 0.084 Uiso 1 1 calc R U . . .
C83 C 0.2297(7) 0.9306(5) 0.0406(4) 0.082(2) Uani 1 1 d . . . . .
H83A H 0.1695 0.9446 0.0123 0.098 Uiso 1 1 calc R U . . .
H83B H 0.1837 0.8867 0.0595 0.098 Uiso 1 1 calc R U . . .
C84 C 0.3235(7) 0.8948(4) 0.0166(2) 0.068(2) Uani 1 1 d . . . . .
H84A H 0.2931 0.8286 0.0052 0.081 Uiso 1 1 calc R U . . .
H84B H 0.3401 0.9219 -0.0151 0.081 Uiso 1 1 calc R U . . .
O10 O 0.6645(6) 2.0608(4) 0.4427(3) 0.0536(16) Uani 0.55 1 d . U P A 1
C85 C 0.5872(11) 1.9817(8) 0.4458(5) 0.065(2) Uani 0.55 1 d . U P A 1
H85A H 0.5895 1.9357 0.4159 0.078 Uiso 0.55 1 calc R U P A 1
H85B H 0.5016 1.9875 0.4396 0.078 Uiso 0.55 1 calc R U P A 1
C86 C 0.6119(10) 1.9494(7) 0.4952(4) 0.057(2) Uani 0.55 1 d . U P A 1
H86A H 0.5800 1.8833 0.4907 0.068 Uiso 0.55 1 calc R U P A 1
H86B H 0.5828 1.9795 0.5246 0.068 Uiso 0.55 1 calc R U P A 1
C87 C 0.7503(10) 1.9819(7) 0.5012(4) 0.053(2) Uani 0.55 1 d . U P A 1
H87A H 0.7954 1.9863 0.5389 0.064 Uiso 0.55 1 calc R U P A 1
H87B H 0.7790 1.9416 0.4766 0.064 Uiso 0.55 1 calc R U P A 1
C88 C 0.7676(11) 2.0718(8) 0.4861(4) 0.0490(19) Uani 0.55 1 d . U P A 1
H88A H 0.7679 2.1172 0.5170 0.059 Uiso 0.55 1 calc R U P A 1
H88B H 0.8467 2.0909 0.4746 0.059 Uiso 0.55 1 calc R U P A 1
O10B O 0.7228(10) 2.0812(7) 0.4919(4) 0.063(2) Uani 0.45 1 d G U P B 2
C85B C 0.7598(13) 2.1005(6) 0.4440(4) 0.083(3) Uani 0.45 1 d G U P B 2
H85C H 0.8401 2.1481 0.4526 0.100 Uiso 0.45 1 calc R U P B 2
H85D H 0.6965 2.1209 0.4209 0.100 Uiso 0.45 1 calc R U P B 2
C86B C 0.7725(13) 2.0126(7) 0.4155(3) 0.069(2) Uani 0.45 1 d G U P B 2
H86C H 0.6916 1.9742 0.3928 0.083 Uiso 0.45 1 calc R U P B 2
H86D H 0.8339 2.0237 0.3927 0.083 Uiso 0.45 1 calc R U P B 2
C87B C 0.8172(12) 1.9706(7) 0.4626(4) 0.068(2) Uani 0.45 1 d G U P B 2
H87C H 0.9061 1.9736 0.4666 0.082 Uiso 0.45 1 calc R U P B 2
H87D H 0.7679 1.9071 0.4578 0.082 Uiso 0.45 1 calc R U P B 2
C88B C 0.7972(12) 2.0274(7) 0.5111(3) 0.064(2) Uani 0.45 1 d G U P B 2
H88C H 0.7554 1.9881 0.5335 0.077 Uiso 0.45 1 calc R U P B 2
H88D H 0.8782 2.0659 0.5336 0.077 Uiso 0.45 1 calc R U P B 2
O11 O 1.0572(3) 1.9695(3) 0.33699(15) 0.0576(10) Uani 1 1 d G U . . .
C89 C 0.9730(4) 1.9920(4) 0.36674(15) 0.0951(17) Uani 1 1 d G U . . .
H89A H 0.9774 2.0565 0.3691 0.114 Uiso 1 1 calc R U . . .
H89B H 0.9920 1.9796 0.4038 0.114 Uiso 1 1 calc R U . . .
C90 C 0.8447(3) 1.9330(5) 0.3356(2) 0.1075(19) Uani 1 1 d G U . . .
H90A H 0.8256 1.8732 0.3461 0.129 Uiso 1 1 calc R U . . .
H90B H 0.7791 1.9617 0.3415 0.129 Uiso 1 1 calc R U . . .
C91 C 0.8577(3) 1.9258(4) 0.27753(19) 0.0871(17) Uani 1 1 d G U . . .
H91A H 0.8115 1.9621 0.2580 0.104 Uiso 1 1 calc R U . . .
H91B H 0.8267 1.8626 0.2582 0.104 Uiso 1 1 calc R U . . .
C92 C 0.9965(4) 1.9626(4) 0.28272(13) 0.0689(14) Uani 1 1 d G U . . .
H92A H 1.0255 1.9218 0.2585 0.083 Uiso 1 1 calc R U . . .
H92B H 1.0153 2.0224 0.2723 0.083 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 1.838(2) . ?
Ni1 O1 1.845(2) . ?
Ni1 N1 1.860(3) . ?
Ni1 N2 1.863(3) . ?
O1 C1 1.309(4) . ?
O2 C18 1.317(4) . ?
O3 C11 1.240(4) . ?
O4 C26 1.223(5) . ?
N1 C7 1.307(5) . ?
N1 C9 1.479(5) . ?
N2 C19 1.307(5) . ?
N2 C10 1.469(5) . ?
N3 C11 1.365(5) . ?
N3 C2 1.413(5) . ?
N4 C11 1.362(5) . ?
N4 C20 1.402(5) . ?
N5 C26 1.371(5) . ?
N5 C17 1.409(5) . ?
N6 C26 1.378(5) . ?
N6 C27 1.414(5) . ?
C1 C6 1.420(5) . ?
C1 C2 1.430(5) . ?
C2 C3 1.383(5) . ?
C3 C4 1.404(6) . ?
C4 C5 1.364(6) . ?
C5 C6 1.421(5) . ?
C6 C7 1.458(5) . ?
C7 C8 1.510(5) . ?
C9 C10 1.513(6) . ?
C12 C19 1.508(5) . ?
C13 C18 1.414(5) . ?
C13 C14 1.423(5) . ?
C13 C19 1.461(5) . ?
C14 C15 1.371(6) . ?
C15 C16 1.403(5) . ?
C16 C17 1.381(5) . ?
C17 C18 1.432(5) . ?
C20 C25 1.398(5) . ?
C20 C21 1.400(5) . ?
C21 C22 1.380(6) . ?
C22 C23 1.380(6) . ?
C23 C24 1.380(6) . ?
C24 C25 1.396(6) . ?
C27 C32 1.388(5) . ?
C27 C28 1.395(5) . ?
C28 C29 1.385(6) . ?
C29 C30 1.378(6) . ?
C30 C31 1.400(6) . ?
C31 C32 1.391(5) . ?
Ni2 O5 1.838(2) . ?
Ni2 O6 1.851(3) . ?
Ni2 N7 1.862(3) . ?
Ni2 N8 1.864(3) . ?
O5 C33 1.305(4) . ?
O6 C50 1.314(4) . ?
O7 C51 1.229(5) . ?
O8 C58 1.216(5) . ?
N7 C39 1.297(5) . ?
N7 C41 1.486(5) . ?
N8 C43 1.292(5) . ?
N8 C42 1.473(5) . ?
N9 C51 1.388(5) . ?
N9 C34 1.398(5) . ?
N10 C51 1.357(5) . ?
N10 C52 1.408(5) . ?
N11 C58 1.377(5) . ?
N11 C49 1.417(5) . ?
N12 C58 1.376(5) . ?
N12 C59 1.410(5) . ?
C33 C38 1.419(5) . ?
C33 C34 1.451(5) . ?
C34 C35 1.378(5) . ?
C35 C36 1.400(6) . ?
C36 C37 1.368(6) . ?
C37 C38 1.407(6) . ?
C38 C39 1.457(5) . ?
C39 C40 1.516(5) . ?
C41 C42 1.499(6) . ?
C43 C45 1.456(5) . ?
C43 C44 1.521(5) . ?
C45 C46 1.418(5) . ?
C45 C50 1.419(5) . ?
C46 C47 1.354(6) . ?
C47 C48 1.417(5) . ?
C48 C49 1.370(5) . ?
C49 C50 1.433(5) . ?
C52 C57 1.389(5) . ?
C52 C53 1.398(5) . ?
C53 C54 1.389(6) . ?
C54 C55 1.384(6) . ?
C55 C56 1.379(6) . ?
C56 C57 1.397(5) . ?
C59 C64 1.395(6) . ?
C59 C60 1.396(5) . ?
C60 C61 1.387(6) . ?
C61 C62 1.393(6) . ?
C62 C63 1.370(6) . ?
C63 C64 1.386(6) . ?
N13 C77 1.517(5) . ?
N13 C65 1.521(5) . ?
N13 C73 1.524(5) . ?
N13 C69 1.524(5) . ?
C65 C66 1.516(5) . ?
C66 C67 1.516(6) . ?
C67 C68 1.527(6) . ?
C69 C70 1.522(5) . ?
C70 C71 1.523(6) . ?
C71 C72 1.520(6) . ?
C73 C74 1.514(6) . ?
C74 C75 1.532(6) . ?
C75 C76 1.510(6) . ?
C77 C78 1.527(5) . ?
C78 C79 1.529(5) . ?
C79 C80 1.509(5) . ?
O9 C84 1.423(7) . ?
O9 C81 1.425(6) . ?
C81 C82 1.490(8) . ?
C82 C83 1.505(10) . ?
C83 C84 1.517(11) . ?
O10 C85 1.347(12) . ?
O10 C88 1.419(12) . ?
C85 C86 1.429(14) . ?
C86 C87 1.504(15) . ?
C87 C88 1.483(14) . ?
O10B C88B 1.4100 . ?
O10B C85B 1.4151 . ?
C85B C86B 1.5243 . ?
C86B C87B 1.5147 . ?
C87B C88B 1.5170 . ?
O11 C92 1.4100 . ?
O11 C89 1.4152 . ?
C89 C90 1.5243 . ?
C90 C91 1.5147 . ?
C91 C92 1.5170 . ?

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
O2 Ni1 O1 85.84(11) . . ?
O2 Ni1 N1 175.18(13) . . ?
O1 Ni1 N1 93.82(12) . . ?
O2 Ni1 N2 92.98(12) . . ?
O1 Ni1 N2 174.81(12) . . ?
N1 Ni1 N2 87.78(14) . . ?
C1 O1 Ni1 126.8(2) . . ?
C18 O2 Ni1 125.1(2) . . ?
C7 N1 C9 118.7(3) . . ?
C7 N1 Ni1 128.6(3) . . ?
C9 N1 Ni1 112.2(2) . . ?
C19 N2 C10 120.5(3) . . ?
C19 N2 Ni1 129.8(3) . . ?
C10 N2 Ni1 109.2(2) . . ?
C11 N3 C2 126.4(3) . . ?
C11 N4 C20 128.5(3) . . ?
C26 N5 C17 125.6(3) . . ?
C26 N6 C27 125.6(3) . . ?
O1 C1 C6 125.2(3) . . ?
O1 C1 C2 116.4(3) . . ?
C6 C1 C2 118.3(3) . . ?
C3 C2 N3 123.9(3) . . ?
C3 C2 C1 121.5(3) . . ?
N3 C2 C1 114.6(3) . . ?
C2 C3 C4 119.2(4) . . ?
C5 C4 C3 120.9(4) . . ?
C4 C5 C6 121.4(4) . . ?
C1 C6 C5 118.6(4) . . ?
C1 C6 C7 121.5(3) . . ?
C5 C6 C7 119.7(4) . . ?
N1 C7 C6 121.5(3) . . ?
N1 C7 C8 120.9(4) . . ?
C6 C7 C8 117.6(3) . . ?
N1 C9 C10 108.7(3) . . ?
N2 C10 C9 107.3(3) . . ?
O3 C11 N4 123.9(4) . . ?
O3 C11 N3 123.0(3) . . ?
N4 C11 N3 113.0(3) . . ?
C18 C13 C14 118.9(3) . . ?
C18 C13 C19 120.5(3) . . ?
C14 C13 C19 120.5(3) . . ?
C15 C14 C13 121.0(3) . . ?
C14 C15 C16 120.9(3) . . ?
C17 C16 C15 119.4(3) . . ?
C16 C17 N5 124.7(3) . . ?
C16 C17 C18 121.3(3) . . ?
N5 C17 C18 113.9(3) . . ?
O2 C18 C13 125.8(3) . . ?
O2 C18 C17 115.8(3) . . ?
C13 C18 C17 118.4(3) . . ?
N2 C19 C13 120.4(3) . . ?
N2 C19 C12 120.1(3) . . ?
C13 C19 C12 119.5(3) . . ?
C25 C20 C21 119.4(4) . . ?
C25 C20 N4 124.3(3) . . ?
C21 C20 N4 116.3(3) . . ?
C22 C21 C20 120.5(4) . . ?
C21 C22 C23 120.5(4) . . ?
C24 C23 C22 119.3(4) . . ?
C23 C24 C25 121.6(4) . . ?
C24 C25 C20 118.6(4) . . ?
O4 C26 N5 123.6(3) . . ?
O4 C26 N6 124.0(3) . . ?
N5 C26 N6 112.3(3) . . ?
C32 C27 C28 119.4(4) . . ?
C32 C27 N6 123.0(3) . . ?
C28 C27 N6 117.5(3) . . ?
C29 C28 C27 120.7(4) . . ?
C30 C29 C28 120.3(4) . . ?
C29 C30 C31 119.2(4) . . ?
C32 C31 C30 120.8(4) . . ?
C27 C32 C31 119.6(4) . . ?
O5 Ni2 O6 86.43(11) . . ?
O5 Ni2 N7 93.50(13) . . ?
O6 Ni2 N7 175.30(13) . . ?
O5 Ni2 N8 174.86(13) . . ?
O6 Ni2 N8 92.72(12) . . ?
N7 Ni2 N8 87.76(14) . . ?
C33 O5 Ni2 127.0(2) . . ?
C50 O6 Ni2 125.5(2) . . ?
C39 N7 C41 118.9(3) . . ?
C39 N7 Ni2 128.8(3) . . ?
C41 N7 Ni2 111.8(2) . . ?
C43 N8 C42 121.3(3) . . ?
C43 N8 Ni2 129.7(3) . . ?
C42 N8 Ni2 108.6(2) . . ?
C51 N9 C34 126.1(3) . . ?
C51 N10 C52 127.6(3) . . ?
C58 N11 C49 125.5(3) . . ?
C58 N12 C59 125.8(3) . . ?
O5 C33 C38 126.1(3) . . ?
O5 C33 C34 115.7(3) . . ?
C38 C33 C34 118.2(3) . . ?
C35 C34 N9 125.4(3) . . ?
C35 C34 C33 120.1(3) . . ?
N9 C34 C33 114.4(3) . . ?
C34 C35 C36 120.5(4) . . ?
C37 C36 C35 120.2(4) . . ?
C36 C37 C38 121.8(4) . . ?
C37 C38 C33 119.0(3) . . ?
C37 C38 C39 120.7(3) . . ?
C33 C38 C39 120.1(3) . . ?
N7 C39 C38 122.3(3) . . ?
N7 C39 C40 120.3(3) . . ?
C38 C39 C40 117.3(3) . . ?
N7 C41 C42 108.3(3) . . ?
N8 C42 C41 107.1(3) . . ?
N8 C43 C45 121.1(3) . . ?
N8 C43 C44 120.7(3) . . ?
C45 C43 C44 118.2(3) . . ?
C46 C45 C50 118.7(3) . . ?
C46 C45 C43 120.7(3) . . ?
C50 C45 C43 120.3(3) . . ?
C47 C46 C45 121.5(4) . . ?
C46 C47 C48 120.4(4) . . ?
C49 C48 C47 119.6(4) . . ?
C48 C49 N11 124.6(4) . . ?
C48 C49 C50 121.1(3) . . ?
N11 C49 C50 114.3(3) . . ?
O6 C50 C45 125.3(3) . . ?
O6 C50 C49 116.6(3) . . ?
C45 C50 C49 118.1(3) . . ?
O7 C51 N10 125.3(3) . . ?
O7 C51 N9 122.7(4) . . ?
N10 C51 N9 112.0(3) . . ?
C57 C52 C53 119.3(3) . . ?
C57 C52 N10 124.9(3) . . ?
C53 C52 N10 115.8(3) . . ?
C54 C53 C52 120.3(4) . . ?
C55 C54 C53 120.3(4) . . ?
C56 C55 C54 119.4(4) . . ?
C55 C56 C57 121.1(4) . . ?
C52 C57 C56 119.5(4) . . ?
O8 C58 N12 123.7(3) . . ?
O8 C58 N11 123.5(3) . . ?
N12 C58 N11 112.8(3) . . ?
C64 C59 C60 119.1(4) . . ?
C64 C59 N12 123.3(4) . . ?
C60 C59 N12 117.6(4) . . ?
C61 C60 C59 120.0(4) . . ?
C60 C61 C62 120.6(4) . . ?
C63 C62 C61 118.9(4) . . ?
C62 C63 C64 121.5(4) . . ?
C63 C64 C59 119.8(4) . . ?
C77 N13 C65 110.5(3) . . ?
C77 N13 C73 111.1(3) . . ?
C65 N13 C73 106.5(3) . . ?
C77 N13 C69 106.7(3) . . ?
C65 N13 C69 110.7(3) . . ?
C73 N13 C69 111.4(3) . . ?
C66 C65 N13 116.5(3) . . ?
C65 C66 C67 109.2(3) . . ?
C66 C67 C68 112.7(4) . . ?
C70 C69 N13 116.0(3) . . ?
C69 C70 C71 109.6(3) . . ?
C72 C71 C70 112.4(4) . . ?
C74 C73 N13 115.7(3) . . ?
C73 C74 C75 109.6(3) . . ?
C76 C75 C74 113.3(4) . . ?
N13 C77 C78 116.6(3) . . ?
C77 C78 C79 109.0(3) . . ?
C80 C79 C78 114.2(3) . . ?
C84 O9 C81 104.0(5) . . ?
O9 C81 C82 108.7(5) . . ?
C81 C82 C83 103.7(6) . . ?
C82 C83 C84 103.9(6) . . ?
O9 C84 C83 104.5(5) . . ?
C85 O10 C88 102.5(7) . . ?
O10 C85 C86 116.7(9) . . ?
C85 C86 C87 92.6(9) . . ?
C88 C87 C86 102.5(10) . . ?
O10 C88 C87 104.7(8) . . ?
C88B O10B C85B 103.7 . . ?
O10B C85B C86B 105.4 . . ?
C87B C86B C85B 102.3 . . ?
C86B C87B C88B 103.7 . . ?
O10B C88B C87B 108.2 . . ?
C92 O11 C89 103.7 . . ?
O11 C89 C90 105.4 . . ?
C91 C90 C89 102.3 . . ?
C90 C91 C92 103.7 . . ?
O11 C92 C91 108.2 . . ?

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
O2 Ni1 O1 C1 163.4(3) . . . . ?
N1 Ni1 O1 C1 -11.8(3) . . . . ?
O1 Ni1 O2 C18 -161.8(3) . . . . ?
N2 Ni1 O2 C18 23.3(3) . . . . ?
O1 Ni1 N1 C7 18.0(3) . . . . ?
N2 Ni1 N1 C7 -167.0(3) . . . . ?
O1 Ni1 N1 C9 -170.5(3) . . . . ?
N2 Ni1 N1 C9 4.5(3) . . . . ?
O2 Ni1 N2 C19 -13.5(3) . . . . ?
N1 Ni1 N2 C19 161.7(3) . . . . ?
O2 Ni1 N2 C10 158.7(2) . . . . ?
N1 Ni1 N2 C10 -26.0(3) . . . . ?
Ni1 O1 C1 C6 1.4(5) . . . . ?
Ni1 O1 C1 C2 -177.5(2) . . . . ?
C11 N3 C2 C3 0.0(6) . . . . ?
C11 N3 C2 C1 -178.4(3) . . . . ?
O1 C1 C2 C3 175.9(3) . . . . ?
C6 C1 C2 C3 -3.1(5) . . . . ?
O1 C1 C2 N3 -5.6(5) . . . . ?
C6 C1 C2 N3 175.4(3) . . . . ?
N3 C2 C3 C4 -176.6(3) . . . . ?
C1 C2 C3 C4 1.7(5) . . . . ?
C2 C3 C4 C5 0.3(6) . . . . ?
C3 C4 C5 C6 -1.0(6) . . . . ?
O1 C1 C6 C5 -176.6(3) . . . . ?
C2 C1 C6 C5 2.3(5) . . . . ?
O1 C1 C6 C7 8.7(6) . . . . ?
C2 C1 C6 C7 -172.4(3) . . . . ?
C4 C5 C6 C1 -0.3(6) . . . . ?
C4 C5 C6 C7 174.5(4) . . . . ?
C9 N1 C7 C6 175.8(3) . . . . ?
Ni1 N1 C7 C6 -13.2(5) . . . . ?
C9 N1 C7 C8 -3.5(5) . . . . ?
Ni1 N1 C7 C8 167.5(3) . . . . ?
C1 C6 C7 N1 -2.7(6) . . . . ?
C5 C6 C7 N1 -177.3(4) . . . . ?
C1 C6 C7 C8 176.7(4) . . . . ?
C5 C6 C7 C8 2.0(5) . . . . ?
C7 N1 C9 C10 -170.3(3) . . . . ?
Ni1 N1 C9 C10 17.3(4) . . . . ?
C19 N2 C10 C9 -146.3(3) . . . . ?
Ni1 N2 C10 C9 40.7(4) . . . . ?
N1 C9 C10 N2 -36.9(4) . . . . ?
C20 N4 C11 O3 -2.5(6) . . . . ?
C20 N4 C11 N3 174.8(3) . . . . ?
C2 N3 C11 O3 -23.3(6) . . . . ?
C2 N3 C11 N4 159.3(3) . . . . ?
C18 C13 C14 C15 1.6(5) . . . . ?
C19 C13 C14 C15 -174.1(3) . . . . ?
C13 C14 C15 C16 1.4(6) . . . . ?
C14 C15 C16 C17 -1.3(6) . . . . ?
C15 C16 C17 N5 174.4(3) . . . . ?
C15 C16 C17 C18 -1.8(5) . . . . ?
C26 N5 C17 C16 9.4(6) . . . . ?
C26 N5 C17 C18 -174.1(3) . . . . ?
Ni1 O2 C18 C13 -17.4(5) . . . . ?
Ni1 O2 C18 C17 165.2(2) . . . . ?
C14 C13 C18 O2 178.1(3) . . . . ?
C19 C13 C18 O2 -6.3(5) . . . . ?
C14 C13 C18 C17 -4.5(5) . . . . ?
C19 C13 C18 C17 171.1(3) . . . . ?
C16 C17 C18 O2 -177.6(3) . . . . ?
N5 C17 C18 O2 5.7(5) . . . . ?
C16 C17 C18 C13 4.7(5) . . . . ?
N5 C17 C18 C13 -171.9(3) . . . . ?
C10 N2 C19 C13 -174.9(3) . . . . ?
Ni1 N2 C19 C13 -3.4(5) . . . . ?
C10 N2 C19 C12 3.5(5) . . . . ?
Ni1 N2 C19 C12 175.0(3) . . . . ?
C18 C13 C19 N2 16.8(5) . . . . ?
C14 C13 C19 N2 -167.7(3) . . . . ?
C18 C13 C19 C12 -161.6(3) . . . . ?
C14 C13 C19 C12 13.9(5) . . . . ?
C11 N4 C20 C25 13.1(6) . . . . ?
C11 N4 C20 C21 -168.5(4) . . . . ?
C25 C20 C21 C22 0.0(6) . . . . ?
N4 C20 C21 C22 -178.4(4) . . . . ?
C20 C21 C22 C23 0.1(7) . . . . ?
C21 C22 C23 C24 0.1(7) . . . . ?
C22 C23 C24 C25 -0.5(7) . . . . ?
C23 C24 C25 C20 0.7(6) . . . . ?
C21 C20 C25 C24 -0.4(6) . . . . ?
N4 C20 C25 C24 177.9(4) . . . . ?
C17 N5 C26 O4 20.9(6) . . . . ?
C17 N5 C26 N6 -160.5(3) . . . . ?
C27 N6 C26 O4 1.8(6) . . . . ?
C27 N6 C26 N5 -176.9(3) . . . . ?
C26 N6 C27 C32 26.6(6) . . . . ?
C26 N6 C27 C28 -156.5(4) . . . . ?
C32 C27 C28 C29 0.4(6) . . . . ?
N6 C27 C28 C29 -176.6(4) . . . . ?
C27 C28 C29 C30 0.0(6) . . . . ?
C28 C29 C30 C31 -0.6(6) . . . . ?
C29 C30 C31 C32 0.8(6) . . . . ?
C28 C27 C32 C31 -0.2(6) . . . . ?
N6 C27 C32 C31 176.6(3) . . . . ?
C30 C31 C32 C27 -0.5(6) . . . . ?
O6 Ni2 O5 C33 165.0(3) . . . . ?
N7 Ni2 O5 C33 -10.3(3) . . . . ?
O5 Ni2 O6 C50 -162.9(3) . . . . ?
N8 Ni2 O6 C50 22.1(3) . . . . ?
O5 Ni2 N7 C39 16.3(4) . . . . ?
N8 Ni2 N7 C39 -168.7(4) . . . . ?
O5 Ni2 N7 C41 -172.0(3) . . . . ?
N8 Ni2 N7 C41 3.0(3) . . . . ?
O6 Ni2 N8 C43 -14.5(3) . . . . ?
N7 Ni2 N8 C43 160.8(3) . . . . ?
O6 Ni2 N8 C42 158.8(2) . . . . ?
N7 Ni2 N8 C42 -25.9(3) . . . . ?
Ni2 O5 C33 C38 1.0(5) . . . . ?
Ni2 O5 C33 C34 -178.0(2) . . . . ?
C51 N9 C34 C35 -4.1(6) . . . . ?
C51 N9 C34 C33 177.7(3) . . . . ?
O5 C33 C34 C35 176.0(3) . . . . ?
C38 C33 C34 C35 -3.2(5) . . . . ?
O5 C33 C34 N9 -5.8(4) . . . . ?
C38 C33 C34 N9 175.1(3) . . . . ?
N9 C34 C35 C36 -176.7(4) . . . . ?
C33 C34 C35 C36 1.3(5) . . . . ?
C34 C35 C36 C37 0.8(6) . . . . ?
C35 C36 C37 C38 -1.0(6) . . . . ?
C36 C37 C38 C33 -0.9(6) . . . . ?
C36 C37 C38 C39 175.4(4) . . . . ?
O5 C33 C38 C37 -176.1(3) . . . . ?
C34 C33 C38 C37 3.0(5) . . . . ?
O5 C33 C38 C39 7.5(6) . . . . ?
C34 C33 C38 C39 -173.4(3) . . . . ?
C41 N7 C39 C38 176.3(3) . . . . ?
Ni2 N7 C39 C38 -12.5(6) . . . . ?
C41 N7 C39 C40 -2.1(6) . . . . ?
Ni2 N7 C39 C40 169.1(3) . . . . ?
C37 C38 C39 N7 -177.9(4) . . . . ?
C33 C38 C39 N7 -1.6(6) . . . . ?
C37 C38 C39 C40 0.5(5) . . . . ?
C33 C38 C39 C40 176.8(4) . . . . ?
C39 N7 C41 C42 -167.4(3) . . . . ?
Ni2 N7 C41 C42 20.0(4) . . . . ?
C43 N8 C42 C41 -143.8(4) . . . . ?
Ni2 N8 C42 C41 42.2(4) . . . . ?
N7 C41 C42 N8 -39.6(4) . . . . ?
C42 N8 C43 C45 -175.2(3) . . . . ?
Ni2 N8 C43 C45 -2.6(5) . . . . ?
C42 N8 C43 C44 2.3(5) . . . . ?
Ni2 N8 C43 C44 174.9(3) . . . . ?
N8 C43 C45 C46 -167.4(4) . . . . ?
C44 C43 C45 C46 15.0(5) . . . . ?
N8 C43 C45 C50 18.5(5) . . . . ?
C44 C43 C45 C50 -159.1(3) . . . . ?
C50 C45 C46 C47 1.8(6) . . . . ?
C43 C45 C46 C47 -172.5(4) . . . . ?
C45 C46 C47 C48 3.7(6) . . . . ?
C46 C47 C48 C49 -3.2(6) . . . . ?
C47 C48 C49 N11 175.3(4) . . . . ?
C47 C48 C49 C50 -2.7(6) . . . . ?
C58 N11 C49 C48 -4.5(6) . . . . ?
C58 N11 C49 C50 173.6(3) . . . . ?
Ni2 O6 C50 C45 -13.6(5) . . . . ?
Ni2 O6 C50 C49 169.3(2) . . . . ?
C46 C45 C50 O6 175.6(3) . . . . ?
C43 C45 C50 O6 -10.2(5) . . . . ?
C46 C45 C50 C49 -7.4(5) . . . . ?
C43 C45 C50 C49 166.8(3) . . . . ?
C48 C49 C50 O6 -174.7(3) . . . . ?
N11 C49 C50 O6 7.1(5) . . . . ?
C48 C49 C50 C45 8.0(5) . . . . ?
N11 C49 C50 C45 -170.2(3) . . . . ?
C52 N10 C51 O7 6.5(6) . . . . ?
C52 N10 C51 N9 -174.9(3) . . . . ?
C34 N9 C51 O7 -17.7(6) . . . . ?
C34 N9 C51 N10 163.7(3) . . . . ?
C51 N10 C52 C57 3.4(6) . . . . ?
C51 N10 C52 C53 -178.3(3) . . . . ?
C57 C52 C53 C54 0.5(6) . . . . ?
N10 C52 C53 C54 -177.9(4) . . . . ?
C52 C53 C54 C55 0.7(6) . . . . ?
C53 C54 C55 C56 -1.2(6) . . . . ?
C54 C55 C56 C57 0.5(6) . . . . ?
C53 C52 C57 C56 -1.2(5) . . . . ?
N10 C52 C57 C56 177.0(3) . . . . ?
C55 C56 C57 C52 0.8(6) . . . . ?
C59 N12 C58 O8 8.7(6) . . . . ?
C59 N12 C58 N11 -170.9(3) . . . . ?
C49 N11 C58 O8 24.7(6) . . . . ?
C49 N11 C58 N12 -155.7(3) . . . . ?
C58 N12 C59 C64 27.8(6) . . . . ?
C58 N12 C59 C60 -154.1(4) . . . . ?
C64 C59 C60 C61 -0.2(6) . . . . ?
N12 C59 C60 C61 -178.5(4) . . . . ?
C59 C60 C61 C62 1.1(7) . . . . ?
C60 C61 C62 C63 -1.3(7) . . . . ?
C61 C62 C63 C64 0.6(7) . . . . ?
C62 C63 C64 C59 0.4(7) . . . . ?
C60 C59 C64 C63 -0.6(6) . . . . ?
N12 C59 C64 C63 177.6(4) . . . . ?
C77 N13 C65 C66 -58.3(4) . . . . ?
C73 N13 C65 C66 -179.0(3) . . . . ?
C69 N13 C65 C66 59.7(4) . . . . ?
N13 C65 C66 C67 -171.6(3) . . . . ?
C65 C66 C67 C68 -177.6(4) . . . . ?
C77 N13 C69 C70 177.4(3) . . . . ?
C65 N13 C69 C70 57.1(4) . . . . ?
C73 N13 C69 C70 -61.3(4) . . . . ?
N13 C69 C70 C71 -176.2(3) . . . . ?
C69 C70 C71 C72 -178.3(4) . . . . ?
C77 N13 C73 C74 70.9(4) . . . . ?
C65 N13 C73 C74 -168.7(3) . . . . ?
C69 N13 C73 C74 -47.9(5) . . . . ?
N13 C73 C74 C75 -158.8(3) . . . . ?
C73 C74 C75 C76 -163.9(4) . . . . ?
C65 N13 C77 C78 -62.6(4) . . . . ?
C73 N13 C77 C78 55.4(4) . . . . ?
C69 N13 C77 C78 176.9(3) . . . . ?
N13 C77 C78 C79 159.0(3) . . . . ?
C77 C78 C79 C80 174.8(3) . . . . ?
C84 O9 C81 C82 32.6(7) . . . . ?
O9 C81 C82 C83 -11.8(8) . . . . ?
C81 C82 C83 C84 -12.1(8) . . . . ?
C81 O9 C84 C83 -39.7(6) . . . . ?
C82 C83 C84 O9 32.2(7) . . . . ?
C88 O10 C85 C86 16.3(16) . . . . ?
O10 C85 C86 C87 -38.2(15) . . . . ?
C85 C86 C87 C88 42.5(12) . . . . ?
C85 O10 C88 C87 14.8(14) . . . . ?
C86 C87 C88 O10 -38.4(13) . . . . ?
C88B O10B C85B C86B 42.0 . . . . ?
O10B C85B C86B C87B -33.4 . . . . ?
C85B C86B C87B C88B 12.3 . . . . ?
C85B O10B C88B C87B -34.0 . . . . ?
C86B C87B C88B O10B 12.4 . . . . ?
C92 O11 C89 C90 42.0 . . . . ?
O11 C89 C90 C91 -33.4 . . . . ?
C89 C90 C91 C92 12.3 . . . . ?
C89 O11 C92 C91 -34.0 . . . . ?
C90 C91 C92 O11 12.5 . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 Cl1 0.72(5) 2.95(5) 3.588(3) 149(5) .
N4 H4 Cl1 0.91(5) 2.30(5) 3.202(3) 170(4) .
N5 H5 Cl1 0.87(5) 2.66(5) 3.444(3) 150(4) .
N6 H6 Cl1 0.97(5) 2.34(5) 3.284(3) 166(4) .
N9 H9 O5 0.87(5) 2.18(4) 2.599(4) 109(3) .
N9 H9 Cl1 0.87(5) 2.84(5) 3.599(3) 147(4) .
N10 H10 Cl1 0.71(5) 2.53(5) 3.228(3) 174(5) .
N11 H11 Cl1 0.78(5) 2.81(5) 3.541(3) 158(4) .
N12 H12 Cl1 0.82(5) 2.41(5) 3.235(3) 179(5) .

_refine_diff_density_max         2.139
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.092


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
####################################################################### 
# 
# 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_jyy321
_database_code_depnum_ccdc_archive 'CCDC 2379619'
loop_
_audit_author_name
_audit_author_address
'Lauren M. Anderson-Sanchez'
;University of California, Irvine
United States of America
;
_audit_update_record             
;
2024-08-24 deposited with the CCDC.	2024-10-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26.83 H28 N4 Ni O3.50'
_chemical_formula_weight         521.24

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'

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

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

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

_cell_length_a                   11.6000(10)
_cell_length_b                   16.4750(15)
_cell_length_c                   21.5479(19)
_cell_angle_alpha                72.4119(14)
_cell_angle_beta                 88.1460(15)
_cell_angle_gamma                71.8599(15)
_cell_volume                     3721.7(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    9885
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      30.43

_exptl_crystal_description       rod
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_F_000             1638
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.171
_exptl_absorpt_coefficient_mu    0.820
_shelx_estimated_absorpt_T_min   0.753
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6621
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
76873 Corrected reflections written to file jyy321s.hkl 
Estimated minimum and maximum transmission:  0.6621  0.7461 
The ratio (0.8874) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            73631
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.922
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             20850
_reflns_number_gt                15415
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0687P)²+3.8075P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         20850
_refine_ls_number_parameters     983
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1397
_refine_ls_wR_factor_gt          0.1261
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.45256(3) 0.67083(2) 0.50037(2) 0.01291(7) Uani 1 1 d . . . . .
O1 O 0.32819(16) 0.65181(13) 0.46022(9) 0.0177(4) Uani 1 1 d . . . . .
O2 O 0.33262(15) 0.71246(12) 0.55122(8) 0.0167(4) Uani 1 1 d . . . . .
O3 O 0.19947(17) 0.83682(14) 0.81041(9) 0.0220(4) Uani 1 1 d . . . . .
N1 N 0.57746(18) 0.68170(14) 0.54656(10) 0.0145(4) Uani 1 1 d . . . . .
N2 N 0.56869(18) 0.63400(14) 0.44470(10) 0.0146(4) Uani 1 1 d . . . . .
N3 N 0.35961(19) 0.85851(14) 0.74966(10) 0.0151(4) Uani 1 1 d . . . . .
H3 H 0.425(3) 0.864(2) 0.7536(16) 0.023(8) Uiso 1 1 d . . . . .
N4 N 0.33710(19) 0.89393(15) 0.84350(11) 0.0158(4) Uani 1 1 d . . . . .
H4 H 0.388(3) 0.914(2) 0.8320(16) 0.020(8) Uiso 1 1 d . . . . .
C1 C 0.6976(2) 0.64659(18) 0.52234(12) 0.0178(5) Uani 1 1 d . . . . .
H1A H 0.7349 0.5822 0.5465 0.021 Uiso 1 1 calc R U . . .
H1B H 0.7522 0.6794 0.5291 0.021 Uiso 1 1 calc R U . . .
C2 C 0.6804(2) 0.65893(18) 0.45027(13) 0.0173(5) Uani 1 1 d . . . . .
C3 C 0.7944(2) 0.6008(2) 0.42858(15) 0.0275(6) Uani 1 1 d . . . . .
H3A H 0.8066 0.5374 0.4521 0.041 Uiso 1 1 calc R U . . .
H3B H 0.8650 0.6168 0.4381 0.041 Uiso 1 1 calc R U . . .
H3C H 0.7849 0.6108 0.3816 0.041 Uiso 1 1 calc R U . . .
C4 C 0.6545(3) 0.75724(19) 0.41039(13) 0.0233(6) Uani 1 1 d . . . . .
H4A H 0.5802 0.7938 0.4241 0.035 Uiso 1 1 calc R U . . .
H4B H 0.6438 0.7640 0.3640 0.035 Uiso 1 1 calc R U . . .
H4C H 0.7229 0.7772 0.4174 0.035 Uiso 1 1 calc R U . . .
C5 C 0.5581(2) 0.59495(17) 0.40270(12) 0.0177(5) Uani 1 1 d . . . . .
H5 H 0.6276 0.5754 0.3799 0.021 Uiso 1 1 calc R U . . .
C6 C 0.4489(2) 0.57868(17) 0.38775(12) 0.0166(5) Uani 1 1 d . . . . .
C7 C 0.4505(2) 0.53790(18) 0.33828(13) 0.0197(5) Uani 1 1 d . . . . .
H7 H 0.5247 0.5172 0.3194 0.024 Uiso 1 1 calc R U . . .
C8 C 0.3468(3) 0.52772(19) 0.31713(13) 0.0224(5) Uani 1 1 d . . . . .
H8 H 0.3487 0.5015 0.2833 0.027 Uiso 1 1 calc R U . . .
C9 C 0.2390(3) 0.55642(19) 0.34607(13) 0.0220(5) Uani 1 1 d . . . . .
H9 H 0.1670 0.5495 0.3318 0.026 Uiso 1 1 calc R U . . .
C10 C 0.2349(2) 0.59486(19) 0.39537(13) 0.0206(5) Uani 1 1 d . . . . .
H10 H 0.1608 0.6118 0.4154 0.025 Uiso 1 1 calc R U . . .
C82 C 0.3389(2) 0.60932(17) 0.41640(12) 0.0162(5) Uani 1 1 d . . . . .
C12 C 0.3432(2) 0.74853(16) 0.59711(12) 0.0145(5) Uani 1 1 d . . . . .
C13 C 0.2354(2) 0.79114(17) 0.62244(12) 0.0170(5) Uani 1 1 d . . . . .
H13 H 0.1594 0.7955 0.6043 0.020 Uiso 1 1 calc R U . . .
C14 C 0.2369(2) 0.82672(17) 0.67265(12) 0.0169(5) Uani 1 1 d . . . . .
H14 H 0.1627 0.8548 0.6887 0.020 Uiso 1 1 calc R U . . .
C15 C 0.3480(2) 0.82133(16) 0.69990(12) 0.0141(4) Uani 1 1 d . . . . .
C16 C 0.4540(2) 0.78134(16) 0.67486(12) 0.0149(5) Uani 1 1 d . . . . .
H16 H 0.5292 0.7788 0.6928 0.018 Uiso 1 1 calc R U . . .
C17 C 0.4557(2) 0.74407(16) 0.62383(12) 0.0139(4) Uani 1 1 d . . . . .
C18 C 0.5720(2) 0.70439(17) 0.59975(12) 0.0156(5) Uani 1 1 d . . . . .
C19 C 0.6866(2) 0.6918(2) 0.63809(13) 0.0220(5) Uani 1 1 d . . . . .
H19A H 0.7554 0.6483 0.6260 0.033 Uiso 1 1 calc R U . . .
H19B H 0.6765 0.6694 0.6849 0.033 Uiso 1 1 calc R U . . .
H19C H 0.7021 0.7494 0.6282 0.033 Uiso 1 1 calc R U . . .
C20 C 0.2903(2) 0.86096(16) 0.80172(12) 0.0148(5) Uani 1 1 d . . . . .
C21 C 0.2928(2) 0.90818(16) 0.90220(12) 0.0143(5) Uani 1 1 d . . . . .
C22 C 0.3437(2) 0.95812(17) 0.92844(12) 0.0174(5) Uani 1 1 d . . . . .
H22 H 0.4075 0.9784 0.9076 0.021 Uiso 1 1 calc R U . . .
C23 C 0.3013(3) 0.97825(18) 0.98505(13) 0.0214(5) Uani 1 1 d . . . . .
H23 H 0.3356 1.0127 1.0025 0.026 Uiso 1 1 calc R U . . .
C24 C 0.2089(3) 0.94794(18) 1.01598(13) 0.0217(5) Uani 1 1 d . . . . .
H24 H 0.1790 0.9624 1.0542 0.026 Uiso 1 1 calc R U . . .
C25 C 0.1607(2) 0.89658(17) 0.99089(13) 0.0191(5) Uani 1 1 d . . . . .
H25 H 0.0983 0.8751 1.0125 0.023 Uiso 1 1 calc R U . . .
C26 C 0.2024(2) 0.87578(17) 0.93423(12) 0.0167(5) Uani 1 1 d . . . . .
H26 H 0.1693 0.8398 0.9177 0.020 Uiso 1 1 calc R U . . .
Ni2 Ni 1.25512(3) 0.37792(2) 0.90064(2) 0.01223(7) Uani 1 1 d . . . . .
O4 O 1.15376(15) 0.31371(12) 0.94167(8) 0.0168(4) Uani 1 1 d . . . . .
O5 O 1.13323(15) 0.42904(12) 0.83532(8) 0.0152(3) Uani 1 1 d . . . . .
O6 O 0.93452(16) 0.69890(14) 0.55808(9) 0.0249(4) Uani 1 1 d . . . . .
N5 N 1.34559(18) 0.45257(14) 0.85944(10) 0.0135(4) Uani 1 1 d . . . . .
N6 N 1.38015(18) 0.32068(14) 0.96529(10) 0.0134(4) Uani 1 1 d . . . . .
N7 N 1.14087(19) 0.63217(15) 0.57807(10) 0.0165(4) Uani 1 1 d . . . . .
H7A H 1.205(3) 0.640(2) 0.5673(14) 0.013(7) Uiso 1 1 d . . . . .
N8 N 1.0639(2) 0.74039(16) 0.48145(11) 0.0200(5) Uani 1 1 d . . . . .
H8A H 1.135(3) 0.726(2) 0.4712(15) 0.021(8) Uiso 1 1 d . . . . .
C27 C 1.4421(2) 0.44643(17) 0.90529(12) 0.0160(5) Uani 1 1 d . . . . .
H27A H 1.4089 0.4876 0.9314 0.019 Uiso 1 1 calc R U . . .
H27B H 1.5088 0.4639 0.8808 0.019 Uiso 1 1 calc R U . . .
C28 C 1.4902(2) 0.35016(16) 0.95001(12) 0.0146(5) Uani 1 1 d . . . . .
C29 C 1.5573(2) 0.34958(18) 1.01039(12) 0.0184(5) Uani 1 1 d . . . . .
H29A H 1.4999 0.3843 1.0345 0.028 Uiso 1 1 calc R U . . .
H29B H 1.6220 0.3765 0.9967 0.028 Uiso 1 1 calc R U . . .
H29C H 1.5930 0.2876 1.0385 0.028 Uiso 1 1 calc R U . . .
C30 C 1.5739(2) 0.28905(18) 0.91480(13) 0.0191(5) Uani 1 1 d . . . . .
H30A H 1.5300 0.2924 0.8755 0.029 Uiso 1 1 calc R U . . .
H30B H 1.6000 0.2270 0.9439 0.029 Uiso 1 1 calc R U . . .
H30C H 1.6453 0.3085 0.9024 0.029 Uiso 1 1 calc R U . . .
C31 C 1.3858(2) 0.25197(16) 1.01557(12) 0.0150(5) Uani 1 1 d . . . . .
H31 H 1.4594 0.2250 1.0424 0.018 Uiso 1 1 calc R U . . .
C32 C 1.2905(2) 0.21327(17) 1.03410(12) 0.0147(5) Uani 1 1 d . . . . .
C33 C 1.3109(2) 0.13904(17) 1.09124(12) 0.0169(5) Uani 1 1 d . . . . .
H33 H 1.3879 0.1151 1.1149 0.020 Uiso 1 1 calc R U . . .
C34 C 1.2215(2) 0.10075(18) 1.11325(12) 0.0195(5) Uani 1 1 d . . . . .
H34 H 1.2366 0.0502 1.1513 0.023 Uiso 1 1 calc R U . . .
C35 C 1.1074(2) 0.13781(18) 1.07830(13) 0.0196(5) Uani 1 1 d . . . . .
H35 H 1.0444 0.1128 1.0937 0.023 Uiso 1 1 calc R U . . .
C36 C 1.0854(2) 0.20950(18) 1.02230(13) 0.0196(5) Uani 1 1 d . . . . .
H36 H 1.0072 0.2336 0.9999 0.023 Uiso 1 1 calc R U . . .
C37 C 1.1770(2) 0.24809(16) 0.99745(12) 0.0150(5) Uani 1 1 d . . . . .
C38 C 1.1421(2) 0.47613(16) 0.77487(11) 0.0128(4) Uani 1 1 d . . . . .
C39 C 1.0551(2) 0.48460(17) 0.72696(12) 0.0154(5) Uani 1 1 d . . . . .
H39 H 0.9960 0.4547 0.7394 0.019 Uiso 1 1 calc R U . . .
C40 C 1.0532(2) 0.53470(17) 0.66311(12) 0.0159(5) Uani 1 1 d . . . . .
H40 H 0.9943 0.5384 0.6319 0.019 Uiso 1 1 calc R U . . .
C41 C 1.1387(2) 0.58062(16) 0.64380(11) 0.0145(5) Uani 1 1 d . . . . .
C42 C 1.2254(2) 0.57255(16) 0.68969(12) 0.0139(4) Uani 1 1 d . . . . .
H42 H 1.2839 0.6028 0.6764 0.017 Uiso 1 1 calc R U . . .
C43 C 1.2302(2) 0.52071(16) 0.75587(11) 0.0125(4) Uani 1 1 d . . . . .
C44 C 1.3244(2) 0.51347(16) 0.80268(12) 0.0138(4) Uani 1 1 d . . . . .
C45 C 1.3949(2) 0.57955(18) 0.78523(13) 0.0192(5) Uani 1 1 d . . . . .
H45A H 1.3962 0.6039 0.8214 0.029 Uiso 1 1 calc R U . . .
H45B H 1.3558 0.6286 0.7459 0.029 Uiso 1 1 calc R U . . .
H45C H 1.4784 0.5490 0.7771 0.029 Uiso 1 1 calc R U . . .
C46 C 1.0382(2) 0.69106(18) 0.54101(12) 0.0172(5) Uani 1 1 d . . . . .
C47 C 0.9720(2) 0.80364(18) 0.43339(13) 0.0212(5) Uani 1 1 d . . . . .
C48 C 0.8814(3) 0.8705(2) 0.44895(16) 0.0289(6) Uani 1 1 d . . . . .
H48 H 0.8793 0.8742 0.4921 0.035 Uiso 1 1 calc R U . . .
C49 C 0.7928(3) 0.9324(2) 0.40077(19) 0.0370(8) Uani 1 1 d . . . . .
H49 H 0.7308 0.9787 0.4113 0.044 Uiso 1 1 calc R U . . .
C50 C 0.7944(3) 0.9273(2) 0.33822(17) 0.0386(8) Uani 1 1 d . . . . .
H50 H 0.7328 0.9689 0.3060 0.046 Uiso 1 1 calc R U . . .
C51 C 0.8861(3) 0.8614(2) 0.32229(15) 0.0345(8) Uani 1 1 d . . . . .
H51 H 0.8883 0.8586 0.2789 0.041 Uiso 1 1 calc R U . . .
C52 C 0.9754(3) 0.7989(2) 0.36990(13) 0.0266(6) Uani 1 1 d . . . . .
H52 H 1.0381 0.7533 0.3590 0.032 Uiso 1 1 calc R U . . .
Ni3 Ni 0.63729(3) 0.94584(2) 0.73475(2) 0.01302(7) Uani 1 1 d . . . . .
O7 O 0.49751(15) 1.00874(11) 0.76566(8) 0.0148(3) Uani 1 1 d . . . . .
O8 O 0.59491(15) 0.84669(11) 0.77866(9) 0.0152(3) Uani 1 1 d . . . . .
O9 O 0.73089(16) 0.43464(12) 0.83701(9) 0.0182(4) Uani 1 1 d . . . . .
N9 N 0.7729(2) 0.87996(15) 0.70264(12) 0.0237(5) Uani 1 1 d D . . . .
N10 N 0.6836(2) 1.04518(15) 0.69267(11) 0.0195(4) Uani 1 1 d . . . . .
N11 N 0.87857(19) 0.48750(14) 0.86220(11) 0.0164(4) Uani 1 1 d . . . . .
H11 H 0.958(3) 0.478(2) 0.8599(15) 0.018(8) Uiso 1 1 d . . . . .
N12 N 0.92878(19) 0.34203(14) 0.86355(11) 0.0165(4) Uani 1 1 d . . . . .
H12 H 0.991(3) 0.341(2) 0.8756(16) 0.023(9) Uiso 1 1 d . . . . .
C53 C 0.8002(4) 0.9411(2) 0.64094(19) 0.0325(4) Uani 0.85 1 d D . P A 1
H53A H 0.8827 0.9135 0.6286 0.039 Uiso 0.85 1 calc R U P A 1
H53B H 0.7408 0.9521 0.6049 0.039 Uiso 0.85 1 calc R U P A 1
C54 C 0.7922(3) 1.0270(2) 0.65276(16) 0.0325(4) Uani 1 1 d D . . . .
C55 C 0.7837(3) 1.1016(2) 0.59105(16) 0.0325(4) Uani 1 1 d . . . . .
H55A H 0.7063 1.1165 0.5665 0.049 Uiso 1 1 calc R U . . .
H55B H 0.8511 1.0827 0.5646 0.049 Uiso 1 1 calc R U . . .
H55C H 0.7880 1.1545 0.6016 0.049 Uiso 1 1 calc R U . . .
C56 C 0.9079(3) 1.0133(2) 0.69565(16) 0.0325(4) Uani 1 1 d . . . . .
H56A H 0.8995 1.0684 0.7066 0.049 Uiso 1 1 calc R U . . .
H56B H 0.9804 0.9995 0.6712 0.049 Uiso 1 1 calc R U . . .
H56C H 0.9159 0.9636 0.7359 0.049 Uiso 1 1 calc R U . . .
C57 C 0.6402(2) 1.12323(18) 0.70062(14) 0.0219(5) Uani 1 1 d . . . . .
H57 H 0.6798 1.1663 0.6809 0.026 Uiso 1 1 calc R U . . .
C58 C 0.5372(2) 1.15038(17) 0.73675(12) 0.0172(5) Uani 1 1 d . . . . .
C59 C 0.5015(2) 1.23890(17) 0.73999(13) 0.0199(5) Uani 1 1 d . . . . .
H59 H 0.5519 1.2753 0.7235 0.024 Uiso 1 1 calc R U . . .
C60 C 0.3953(3) 1.27339(18) 0.76649(13) 0.0219(5) Uani 1 1 d . . . . .
H60 H 0.3726 1.3329 0.7689 0.026 Uiso 1 1 calc R U . . .
C61 C 0.3207(2) 1.21965(18) 0.79000(13) 0.0210(5) Uani 1 1 d . . . . .
H61 H 0.2458 1.2437 0.8071 0.025 Uiso 1 1 calc R U . . .
C62 C 0.3549(2) 1.13217(18) 0.78854(12) 0.0187(5) Uani 1 1 d . . . . .
H62 H 0.3029 1.0970 0.8046 0.022 Uiso 1 1 calc R U . . .
C63 C 0.4660(2) 1.09383(16) 0.76354(11) 0.0145(5) Uani 1 1 d . . . . .
C64 C 0.6677(2) 0.76251(16) 0.79723(12) 0.0143(5) Uani 1 1 d . . . . .
C65 C 0.6208(2) 0.69756(17) 0.83848(12) 0.0158(5) Uani 1 1 d . . . . .
H65 H 0.5403 0.7162 0.8516 0.019 Uiso 1 1 calc R U . . .
C66 C 0.6881(2) 0.60796(17) 0.86030(12) 0.0165(5) Uani 1 1 d . . . . .
H66 H 0.6543 0.5658 0.8884 0.020 Uiso 1 1 calc R U . . .
C67 C 0.8064(2) 0.57908(16) 0.84095(12) 0.0147(5) Uani 1 1 d . . . . .
C68 C 0.8537(2) 0.64161(17) 0.80003(13) 0.0169(5) Uani 1 1 d . . . . .
H68 H 0.9339 0.6217 0.7869 0.020 Uiso 1 1 calc R U . . .
C69 C 0.7875(2) 0.73386(17) 0.77699(13) 0.0163(5) Uani 1 1 d . . . . .
C70 C 0.8337(2) 0.79532(18) 0.72566(15) 0.0232(6) Uani 1 1 d . . . . .
C71 C 0.9527(3) 0.7560(2) 0.69804(19) 0.0379(8) Uani 1 1 d . . . . .
H71A H 0.9437 0.7128 0.6773 0.057 Uiso 1 1 calc R U . . .
H71B H 1.0170 0.7256 0.7334 0.057 Uiso 1 1 calc R U . . .
H71C H 0.9743 0.8043 0.6656 0.057 Uiso 1 1 calc R U . . .
C72 C 0.8371(2) 0.42187(16) 0.85286(12) 0.0143(5) Uani 1 1 d . . . . .
C73 C 0.9263(2) 0.26427(16) 0.85039(12) 0.0154(5) Uani 1 1 d . . . . .
C74 C 1.0307(2) 0.18956(17) 0.87026(12) 0.0182(5) Uani 1 1 d . . . . .
H74 H 1.0986 0.1936 0.8912 0.022 Uiso 1 1 calc R U . . .
C75 C 1.0361(3) 0.10982(18) 0.85972(14) 0.0235(6) Uani 1 1 d . . . . .
H75 H 1.1075 0.0594 0.8738 0.028 Uiso 1 1 calc R U . . .
C76 C 0.9388(3) 0.10263(19) 0.82893(15) 0.0268(6) Uani 1 1 d . . . . .
H76 H 0.9422 0.0477 0.8221 0.032 Uiso 1 1 calc R U . . .
C77 C 0.8356(3) 0.17763(19) 0.80817(15) 0.0265(6) Uani 1 1 d . . . . .
H77 H 0.7685 0.1734 0.7866 0.032 Uiso 1 1 calc R U . . .
C78 C 0.8284(2) 0.25830(17) 0.81818(13) 0.0191(5) Uani 1 1 d . . . . .
H78 H 0.7576 0.3089 0.8032 0.023 Uiso 1 1 calc R U . . .
O10 O 1.2147(2) 0.66035(19) 0.89399(15) 0.0522(7) Uani 1 1 d . . . . .
H10A H 1.2080 0.7121 0.8692 0.078 Uiso 1 1 calc R U . . .
C79 C 1.0932(4) 0.5752(3) 0.95167(19) 0.0477(9) Uani 1 1 d . . . . .
H79A H 1.0183 0.5610 0.9479 0.071 Uiso 1 1 calc R U . . .
H79B H 1.0897 0.6001 0.9879 0.071 Uiso 1 1 calc R U . . .
H79C H 1.1631 0.5205 0.9599 0.071 Uiso 1 1 calc R U . . .
C80 C 1.1060(3) 0.6422(2) 0.89004(18) 0.0395(8) Uani 1 1 d . . . . .
H80A H 1.1052 0.6187 0.8530 0.047 Uiso 1 1 calc R U . . .
H80B H 1.0367 0.6983 0.8823 0.047 Uiso 1 1 calc R U . . .
C53A C 0.8583(15) 0.9331(10) 0.6773(11) 0.0325(4) Uani 0.15 1 d D . P A 2
H53C H 0.9183 0.9226 0.7128 0.039 Uiso 0.15 1 calc R U P A 2
H53D H 0.9032 0.9128 0.6420 0.039 Uiso 0.15 1 calc R U P A 2
O11 O 0.5068(5) 0.9533(4) 0.5223(3) 0.0589(16) Uani 0.5 1 d . . P B -2
C11 C 0.4014(7) 0.9418(5) 0.5089(3) 0.0372(15) Uani 0.5 1 d . . P B -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 1.8353(17) . ?
Ni1 N2 1.857(2) . ?
Ni1 O1 1.8585(17) . ?
Ni1 N1 1.867(2) . ?
O1 C82 1.317(3) . ?
O2 C12 1.324(3) . ?
O3 C20 1.227(3) . ?
N1 C18 1.302(3) . ?
N1 C1 1.477(3) . ?
N2 C5 1.287(3) . ?
N2 C2 1.494(3) . ?
N3 C20 1.362(3) . ?
N3 C15 1.414(3) . ?
N3 H3 0.80(3) . ?
N4 C20 1.383(3) . ?
N4 C21 1.408(3) . ?
N4 H4 0.76(3) . ?
C1 C2 1.516(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C4 1.525(4) . ?
C2 C3 1.526(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.439(3) . ?
C5 H5 0.9500 . ?
C6 C82 1.414(4) . ?
C6 C7 1.418(4) . ?
C7 C8 1.375(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.391(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.384(4) . ?
C9 H9 0.9500 . ?
C10 C82 1.414(3) . ?
C10 H10 0.9500 . ?
C12 C13 1.412(3) . ?
C12 C17 1.415(3) . ?
C13 C14 1.380(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.401(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.380(3) . ?
C16 C17 1.409(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.458(3) . ?
C18 C19 1.513(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 C26 1.393(3) . ?
C21 C22 1.397(3) . ?
C22 C23 1.394(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.383(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.398(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
Ni2 O5 1.8332(17) . ?
Ni2 N6 1.849(2) . ?
Ni2 O4 1.8507(17) . ?
Ni2 N5 1.867(2) . ?
O4 C37 1.319(3) . ?
O5 C38 1.319(3) . ?
O6 C46 1.226(3) . ?
N5 C44 1.299(3) . ?
N5 C27 1.477(3) . ?
N6 C31 1.295(3) . ?
N6 C28 1.496(3) . ?
N7 C46 1.368(3) . ?
N7 C41 1.418(3) . ?
N7 H7A 0.81(3) . ?
N8 C46 1.376(3) . ?
N8 C47 1.422(3) . ?
N8 H8A 0.82(3) . ?
C27 C28 1.522(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C30 1.529(3) . ?
C28 C29 1.534(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.430(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.413(3) . ?
C32 C37 1.418(3) . ?
C33 C34 1.376(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.406(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.374(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.413(3) . ?
C36 H36 0.9500 . ?
C38 C39 1.414(3) . ?
C38 C43 1.417(3) . ?
C39 C40 1.371(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.407(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.381(3) . ?
C42 C43 1.416(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.465(3) . ?
C44 C45 1.510(3) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C47 C48 1.382(4) . ?
C47 C52 1.393(4) . ?
C48 C49 1.397(4) . ?
C48 H48 0.9500 . ?
C49 C50 1.375(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.382(5) . ?
C50 H50 0.9500 . ?
C51 C52 1.397(4) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
Ni3 O8 1.8278(17) . ?
Ni3 N10 1.846(2) . ?
Ni3 O7 1.8568(17) . ?
Ni3 N9 1.858(2) . ?
O7 C63 1.321(3) . ?
O8 C64 1.325(3) . ?
O9 C72 1.225(3) . ?
N9 C70 1.296(4) . ?
N9 C53 1.498(4) . ?
N9 C53A 1.504(15) . ?
N10 C57 1.289(3) . ?
N10 C54 1.505(4) . ?
N11 C72 1.380(3) . ?
N11 C67 1.417(3) . ?
N11 H11 0.88(3) . ?
N12 C72 1.370(3) . ?
N12 C73 1.402(3) . ?
N12 H12 0.77(3) . ?
C53 C54 1.486(5) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C53A 1.434(15) . ?
C54 C55 1.494(4) . ?
C54 C56 1.573(5) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C58 1.432(4) . ?
C57 H57 0.9500 . ?
C58 C59 1.410(4) . ?
C58 C63 1.417(3) . ?
C59 C60 1.372(4) . ?
C59 H59 0.9500 . ?
C60 C61 1.402(4) . ?
C60 H60 0.9500 . ?
C61 C62 1.381(4) . ?
C61 H61 0.9500 . ?
C62 C63 1.415(4) . ?
C62 H62 0.9500 . ?
C64 C65 1.410(3) . ?
C64 C69 1.421(3) . ?
C65 C66 1.377(3) . ?
C65 H65 0.9500 . ?
C66 C67 1.401(3) . ?
C66 H66 0.9500 . ?
C67 C68 1.382(4) . ?
C68 C69 1.410(3) . ?
C68 H68 0.9500 . ?
C69 C70 1.469(4) . ?
C70 C71 1.518(4) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C73 C78 1.393(4) . ?
C73 C74 1.397(3) . ?
C74 C75 1.382(4) . ?
C74 H74 0.9500 . ?
C75 C76 1.382(4) . ?
C75 H75 0.9500 . ?
C76 C77 1.393(4) . ?
C76 H76 0.9500 . ?
C77 C78 1.387(4) . ?
C77 H77 0.9500 . ?
C78 H78 0.9500 . ?
O10 C80 1.393(4) . ?
O10 H10A 0.8400 . ?
C79 C80 1.486(5) . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9900 . ?
C80 H80B 0.9900 . ?
C53A H53C 0.9900 . ?
C53A H53D 0.9900 . ?
O11 C11 1.346(9) . ?

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
O2 Ni1 N2 176.65(9) . . ?
O2 Ni1 O1 83.66(8) . . ?
N2 Ni1 O1 94.72(8) . . ?
O2 Ni1 N1 94.99(8) . . ?
N2 Ni1 N1 86.86(9) . . ?
O1 Ni1 N1 175.24(9) . . ?
C82 O1 Ni1 126.96(16) . . ?
C12 O2 Ni1 126.66(15) . . ?
C18 N1 C1 119.1(2) . . ?
C18 N1 Ni1 128.29(17) . . ?
C1 N1 Ni1 111.95(15) . . ?
C5 N2 C2 120.7(2) . . ?
C5 N2 Ni1 126.72(18) . . ?
C2 N2 Ni1 112.54(15) . . ?
C20 N3 C15 127.2(2) . . ?
C20 N3 H3 115(2) . . ?
C15 N3 H3 114(2) . . ?
C20 N4 C21 128.8(2) . . ?
C20 N4 H4 118(2) . . ?
C21 N4 H4 113(2) . . ?
N1 C1 C2 108.5(2) . . ?
N1 C1 H1A 110.0 . . ?
C2 C1 H1A 110.0 . . ?
N1 C1 H1B 110.0 . . ?
C2 C1 H1B 110.0 . . ?
H1A C1 H1B 108.4 . . ?
N2 C2 C1 104.22(19) . . ?
N2 C2 C4 108.0(2) . . ?
C1 C2 C4 110.6(2) . . ?
N2 C2 C3 114.3(2) . . ?
C1 C2 C3 109.4(2) . . ?
C4 C2 C3 110.2(2) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 124.8(2) . . ?
N2 C5 H5 117.6 . . ?
C6 C5 H5 117.6 . . ?
C82 C6 C7 119.7(2) . . ?
C82 C6 C5 122.0(2) . . ?
C7 C6 C5 118.0(2) . . ?
C8 C7 C6 121.3(2) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C7 C8 C9 119.0(2) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C10 C9 C8 121.1(2) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C82 121.2(2) . . ?
C9 C10 H10 119.4 . . ?
C82 C10 H10 119.4 . . ?
O1 C82 C10 118.8(2) . . ?
O1 C82 C6 123.6(2) . . ?
C10 C82 C6 117.6(2) . . ?
O2 C12 C13 117.7(2) . . ?
O2 C12 C17 124.0(2) . . ?
C13 C12 C17 118.2(2) . . ?
C14 C13 C12 122.2(2) . . ?
C14 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C13 C14 C15 119.8(2) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 118.6(2) . . ?
C16 C15 N3 116.9(2) . . ?
C14 C15 N3 124.3(2) . . ?
C15 C16 C17 123.0(2) . . ?
C15 C16 H16 118.5 . . ?
C17 C16 H16 118.5 . . ?
C16 C17 C12 118.1(2) . . ?
C16 C17 C18 119.2(2) . . ?
C12 C17 C18 122.7(2) . . ?
N1 C18 C17 121.4(2) . . ?
N1 C18 C19 120.9(2) . . ?
C17 C18 C19 117.7(2) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 C20 N3 124.7(2) . . ?
O3 C20 N4 124.8(2) . . ?
N3 C20 N4 110.4(2) . . ?
C26 C21 C22 119.6(2) . . ?
C26 C21 N4 123.7(2) . . ?
C22 C21 N4 116.7(2) . . ?
C23 C22 C21 120.2(2) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.1(2) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 119.6(2) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.9(2) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C21 C26 C25 119.5(2) . . ?
C21 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
O5 Ni2 N6 176.89(9) . . ?
O5 Ni2 O4 83.69(7) . . ?
N6 Ni2 O4 95.32(8) . . ?
O5 Ni2 N5 93.70(8) . . ?
N6 Ni2 N5 87.53(9) . . ?
O4 Ni2 N5 174.53(9) . . ?
C37 O4 Ni2 127.49(15) . . ?
C38 O5 Ni2 125.95(15) . . ?
C44 N5 C27 119.4(2) . . ?
C44 N5 Ni2 129.37(17) . . ?
C27 N5 Ni2 110.48(15) . . ?
C31 N6 C28 119.3(2) . . ?
C31 N6 Ni2 126.07(17) . . ?
C28 N6 Ni2 113.89(15) . . ?
C46 N7 C41 122.8(2) . . ?
C46 N7 H7A 117(2) . . ?
C41 N7 H7A 116(2) . . ?
C46 N8 C47 122.8(2) . . ?
C46 N8 H8A 117(2) . . ?
C47 N8 H8A 119(2) . . ?
N5 C27 C28 108.61(19) . . ?
N5 C27 H27A 110.0 . . ?
C28 C27 H27A 110.0 . . ?
N5 C27 H27B 110.0 . . ?
C28 C27 H27B 110.0 . . ?
H27A C27 H27B 108.3 . . ?
N6 C28 C27 104.96(18) . . ?
N6 C28 C30 107.7(2) . . ?
C27 C28 C30 111.2(2) . . ?
N6 C28 C29 113.4(2) . . ?
C27 C28 C29 108.5(2) . . ?
C30 C28 C29 111.0(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N6 C31 C32 125.5(2) . . ?
N6 C31 H31 117.2 . . ?
C32 C31 H31 117.2 . . ?
C33 C32 C37 119.8(2) . . ?
C33 C32 C31 118.3(2) . . ?
C37 C32 C31 121.9(2) . . ?
C34 C33 C32 121.3(2) . . ?
C34 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
C33 C34 C35 118.7(2) . . ?
C33 C34 H34 120.6 . . ?
C35 C34 H34 120.6 . . ?
C36 C35 C34 121.2(2) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C35 C36 C37 121.2(2) . . ?
C35 C36 H36 119.4 . . ?
C37 C36 H36 119.4 . . ?
O4 C37 C36 119.1(2) . . ?
O4 C37 C32 123.2(2) . . ?
C36 C37 C32 117.7(2) . . ?
O5 C38 C39 117.2(2) . . ?
O5 C38 C43 124.2(2) . . ?
C39 C38 C43 118.6(2) . . ?
C40 C39 C38 122.0(2) . . ?
C40 C39 H39 119.0 . . ?
C38 C39 H39 119.0 . . ?
C39 C40 C41 120.0(2) . . ?
C39 C40 H40 120.0 . . ?
C41 C40 H40 120.0 . . ?
C42 C41 C40 119.0(2) . . ?
C42 C41 N7 119.3(2) . . ?
C40 C41 N7 121.7(2) . . ?
C41 C42 C43 122.3(2) . . ?
C41 C42 H42 118.9 . . ?
C43 C42 H42 118.9 . . ?
C42 C43 C38 118.1(2) . . ?
C42 C43 C44 120.4(2) . . ?
C38 C43 C44 121.5(2) . . ?
N5 C44 C43 120.7(2) . . ?
N5 C44 C45 119.9(2) . . ?
C43 C44 C45 119.3(2) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O6 C46 N7 124.4(2) . . ?
O6 C46 N8 123.2(2) . . ?
N7 C46 N8 112.4(2) . . ?
C48 C47 C52 120.0(3) . . ?
C48 C47 N8 120.6(3) . . ?
C52 C47 N8 119.4(3) . . ?
C47 C48 C49 119.6(3) . . ?
C47 C48 H48 120.2 . . ?
C49 C48 H48 120.2 . . ?
C50 C49 C48 120.7(3) . . ?
C50 C49 H49 119.6 . . ?
C48 C49 H49 119.6 . . ?
C49 C50 C51 119.8(3) . . ?
C49 C50 H50 120.1 . . ?
C51 C50 H50 120.1 . . ?
C50 C51 C52 120.2(3) . . ?
C50 C51 H51 119.9 . . ?
C52 C51 H51 119.9 . . ?
C47 C52 C51 119.7(3) . . ?
C47 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
O8 Ni3 N10 178.13(9) . . ?
O8 Ni3 O7 84.79(8) . . ?
N10 Ni3 O7 95.48(9) . . ?
O8 Ni3 N9 93.35(9) . . ?
N10 Ni3 N9 86.43(10) . . ?
O7 Ni3 N9 177.29(9) . . ?
C63 O7 Ni3 126.30(16) . . ?
C64 O8 Ni3 126.41(15) . . ?
C70 N9 C53 123.5(2) . . ?
C70 N9 C53A 110.0(6) . . ?
C70 N9 Ni3 128.4(2) . . ?
C53 N9 Ni3 108.0(2) . . ?
C53A N9 Ni3 111.6(7) . . ?
C57 N10 C54 119.1(2) . . ?
C57 N10 Ni3 125.68(19) . . ?
C54 N10 Ni3 114.74(18) . . ?
C72 N11 C67 121.1(2) . . ?
C72 N11 H11 115(2) . . ?
C67 N11 H11 115(2) . . ?
C72 N12 C73 128.3(2) . . ?
C72 N12 H12 116(2) . . ?
C73 N12 H12 115(2) . . ?
C54 C53 N9 107.9(3) . . ?
C54 C53 H53A 110.1 . . ?
N9 C53 H53A 110.1 . . ?
C54 C53 H53B 110.1 . . ?
N9 C53 H53B 110.1 . . ?
H53A C53 H53B 108.4 . . ?
C53A C54 C55 136.6(9) . . ?
C53 C54 C55 112.7(3) . . ?
C53A C54 N10 107.6(7) . . ?
C53 C54 N10 104.9(3) . . ?
C55 C54 N10 113.4(3) . . ?
C53A C54 C56 70.7(9) . . ?
C53 C54 C56 109.4(3) . . ?
C55 C54 C56 108.5(3) . . ?
N10 C54 C56 107.8(2) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N10 C57 C58 125.3(2) . . ?
N10 C57 H57 117.3 . . ?
C58 C57 H57 117.3 . . ?
C59 C58 C63 120.3(2) . . ?
C59 C58 C57 117.7(2) . . ?
C63 C58 C57 121.7(2) . . ?
C60 C59 C58 121.1(2) . . ?
C60 C59 H59 119.5 . . ?
C58 C59 H59 119.5 . . ?
C59 C60 C61 119.1(2) . . ?
C59 C60 H60 120.4 . . ?
C61 C60 H60 120.4 . . ?
C62 C61 C60 120.8(2) . . ?
C62 C61 H61 119.6 . . ?
C60 C61 H61 119.6 . . ?
C61 C62 C63 121.3(2) . . ?
C61 C62 H62 119.4 . . ?
C63 C62 H62 119.4 . . ?
O7 C63 C62 119.2(2) . . ?
O7 C63 C58 123.5(2) . . ?
C62 C63 C58 117.3(2) . . ?
O8 C64 C65 117.0(2) . . ?
O8 C64 C69 124.3(2) . . ?
C65 C64 C69 118.6(2) . . ?
C66 C65 C64 122.0(2) . . ?
C66 C65 H65 119.0 . . ?
C64 C65 H65 119.0 . . ?
C65 C66 C67 119.9(2) . . ?
C65 C66 H66 120.1 . . ?
C67 C66 H66 120.1 . . ?
C68 C67 C66 119.0(2) . . ?
C68 C67 N11 119.3(2) . . ?
C66 C67 N11 121.6(2) . . ?
C67 C68 C69 122.6(2) . . ?
C67 C68 H68 118.7 . . ?
C69 C68 H68 118.7 . . ?
C68 C69 C64 117.9(2) . . ?
C68 C69 C70 120.4(2) . . ?
C64 C69 C70 121.0(2) . . ?
N9 C70 C69 121.4(2) . . ?
N9 C70 C71 120.6(2) . . ?
C69 C70 C71 117.9(2) . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
O9 C72 N12 125.0(2) . . ?
O9 C72 N11 123.4(2) . . ?
N12 C72 N11 111.6(2) . . ?
C78 C73 C74 119.2(2) . . ?
C78 C73 N12 124.2(2) . . ?
C74 C73 N12 116.6(2) . . ?
C75 C74 C73 120.6(2) . . ?
C75 C74 H74 119.7 . . ?
C73 C74 H74 119.7 . . ?
C76 C75 C74 120.6(2) . . ?
C76 C75 H75 119.7 . . ?
C74 C75 H75 119.7 . . ?
C75 C76 C77 118.6(3) . . ?
C75 C76 H76 120.7 . . ?
C77 C76 H76 120.7 . . ?
C78 C77 C76 121.6(3) . . ?
C78 C77 H77 119.2 . . ?
C76 C77 H77 119.2 . . ?
C77 C78 C73 119.3(2) . . ?
C77 C78 H78 120.4 . . ?
C73 C78 H78 120.4 . . ?
C80 O10 H10A 109.5 . . ?
C80 C79 H79A 109.5 . . ?
C80 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C80 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
O10 C80 C79 109.9(3) . . ?
O10 C80 H80A 109.7 . . ?
C79 C80 H80A 109.7 . . ?
O10 C80 H80B 109.7 . . ?
C79 C80 H80B 109.7 . . ?
H80A C80 H80B 108.2 . . ?
C54 C53A N9 110.4(11) . . ?
C54 C53A H53C 109.6 . . ?
N9 C53A H53C 109.6 . . ?
C54 C53A H53D 109.6 . . ?
N9 C53A H53D 109.6 . . ?
H53C C53A H53D 108.1 . . ?

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
O2 Ni1 O1 C82 -171.7(2) . . . . ?
N2 Ni1 O1 C82 11.3(2) . . . . ?
O1 Ni1 O2 C12 -176.0(2) . . . . ?
N1 Ni1 O2 C12 8.6(2) . . . . ?
O2 Ni1 N1 C18 5.1(2) . . . . ?
N2 Ni1 N1 C18 -177.7(2) . . . . ?
O2 Ni1 N1 C1 175.64(17) . . . . ?
N2 Ni1 N1 C1 -7.16(17) . . . . ?
O1 Ni1 N2 C5 -10.4(2) . . . . ?
N1 Ni1 N2 C5 165.1(2) . . . . ?
O1 Ni1 N2 C2 166.49(17) . . . . ?
N1 Ni1 N2 C2 -18.01(17) . . . . ?
C18 N1 C1 C2 -158.6(2) . . . . ?
Ni1 N1 C1 C2 29.9(2) . . . . ?
C5 N2 C2 C1 -145.8(2) . . . . ?
Ni1 N2 C2 C1 37.1(2) . . . . ?
C5 N2 C2 C4 96.6(3) . . . . ?
Ni1 N2 C2 C4 -80.5(2) . . . . ?
C5 N2 C2 C3 -26.4(3) . . . . ?
Ni1 N2 C2 C3 156.47(19) . . . . ?
N1 C1 C2 N2 -41.5(3) . . . . ?
N1 C1 C2 C4 74.3(3) . . . . ?
N1 C1 C2 C3 -164.1(2) . . . . ?
C2 N2 C5 C6 -171.6(2) . . . . ?
Ni1 N2 C5 C6 5.0(4) . . . . ?
N2 C5 C6 C82 3.4(4) . . . . ?
N2 C5 C6 C7 177.6(2) . . . . ?
C82 C6 C7 C8 0.3(4) . . . . ?
C5 C6 C7 C8 -174.0(2) . . . . ?
C6 C7 C8 C9 -1.4(4) . . . . ?
C7 C8 C9 C10 0.1(4) . . . . ?
C8 C9 C10 C82 2.3(4) . . . . ?
Ni1 O1 C82 C10 174.67(18) . . . . ?
Ni1 O1 C82 C6 -6.8(4) . . . . ?
C9 C10 C82 O1 175.3(2) . . . . ?
C9 C10 C82 C6 -3.4(4) . . . . ?
C7 C6 C82 O1 -176.5(2) . . . . ?
C5 C6 C82 O1 -2.5(4) . . . . ?
C7 C6 C82 C10 2.0(4) . . . . ?
C5 C6 C82 C10 176.1(2) . . . . ?
Ni1 O2 C12 C13 168.69(18) . . . . ?
Ni1 O2 C12 C17 -13.7(3) . . . . ?
O2 C12 C13 C14 176.6(2) . . . . ?
C17 C12 C13 C14 -1.1(4) . . . . ?
C12 C13 C14 C15 0.2(4) . . . . ?
C13 C14 C15 C16 0.9(4) . . . . ?
C13 C14 C15 N3 177.5(2) . . . . ?
C20 N3 C15 C16 -145.3(2) . . . . ?
C20 N3 C15 C14 38.2(4) . . . . ?
C14 C15 C16 C17 -1.2(4) . . . . ?
N3 C15 C16 C17 -178.0(2) . . . . ?
C15 C16 C17 C12 0.3(4) . . . . ?
C15 C16 C17 C18 179.0(2) . . . . ?
O2 C12 C17 C16 -176.7(2) . . . . ?
C13 C12 C17 C16 0.9(3) . . . . ?
O2 C12 C17 C18 4.6(4) . . . . ?
C13 C12 C17 C18 -177.8(2) . . . . ?
C1 N1 C18 C17 176.5(2) . . . . ?
Ni1 N1 C18 C17 -13.5(4) . . . . ?
C1 N1 C18 C19 -2.4(4) . . . . ?
Ni1 N1 C18 C19 167.50(19) . . . . ?
C16 C17 C18 N1 -169.3(2) . . . . ?
C12 C17 C18 N1 9.4(4) . . . . ?
C16 C17 C18 C19 9.7(3) . . . . ?
C12 C17 C18 C19 -171.7(2) . . . . ?
C15 N3 C20 O3 -6.1(4) . . . . ?
C15 N3 C20 N4 173.5(2) . . . . ?
C21 N4 C20 O3 -1.1(4) . . . . ?
C21 N4 C20 N3 179.3(2) . . . . ?
C20 N4 C21 C26 11.7(4) . . . . ?
C20 N4 C21 C22 -168.0(2) . . . . ?
C26 C21 C22 C23 -2.4(4) . . . . ?
N4 C21 C22 C23 177.4(2) . . . . ?
C21 C22 C23 C24 0.6(4) . . . . ?
C22 C23 C24 C25 1.0(4) . . . . ?
C23 C24 C25 C26 -0.9(4) . . . . ?
C22 C21 C26 C25 2.4(4) . . . . ?
N4 C21 C26 C25 -177.3(2) . . . . ?
C24 C25 C26 C21 -0.8(4) . . . . ?
O5 Ni2 O4 C37 174.8(2) . . . . ?
N6 Ni2 O4 C37 -2.2(2) . . . . ?
O4 Ni2 O5 C38 -164.6(2) . . . . ?
N5 Ni2 O5 C38 20.3(2) . . . . ?
O5 Ni2 N5 C44 -3.4(2) . . . . ?
N6 Ni2 N5 C44 173.7(2) . . . . ?
O5 Ni2 N5 C27 166.57(16) . . . . ?
N6 Ni2 N5 C27 -16.29(16) . . . . ?
O4 Ni2 N6 C31 7.0(2) . . . . ?
N5 Ni2 N6 C31 -177.6(2) . . . . ?
O4 Ni2 N6 C28 177.01(16) . . . . ?
N5 Ni2 N6 C28 -7.67(17) . . . . ?
C44 N5 C27 C28 -152.9(2) . . . . ?
Ni2 N5 C27 C28 36.0(2) . . . . ?
C31 N6 C28 C27 -161.1(2) . . . . ?
Ni2 N6 C28 C27 28.2(2) . . . . ?
C31 N6 C28 C30 80.4(3) . . . . ?
Ni2 N6 C28 C30 -90.3(2) . . . . ?
C31 N6 C28 C29 -42.9(3) . . . . ?
Ni2 N6 C28 C29 146.44(17) . . . . ?
N5 C27 C28 N6 -40.0(2) . . . . ?
N5 C27 C28 C30 76.2(2) . . . . ?
N5 C27 C28 C29 -161.5(2) . . . . ?
C28 N6 C31 C32 -176.4(2) . . . . ?
Ni2 N6 C31 C32 -6.9(4) . . . . ?
N6 C31 C32 C33 -178.9(2) . . . . ?
N6 C31 C32 C37 0.1(4) . . . . ?
C37 C32 C33 C34 -1.6(4) . . . . ?
C31 C32 C33 C34 177.5(2) . . . . ?
C32 C33 C34 C35 -1.0(4) . . . . ?
C33 C34 C35 C36 1.6(4) . . . . ?
C34 C35 C36 C37 0.6(4) . . . . ?
Ni2 O4 C37 C36 177.43(18) . . . . ?
Ni2 O4 C37 C32 -3.0(4) . . . . ?
C35 C36 C37 O4 176.4(2) . . . . ?
C35 C36 C37 C32 -3.2(4) . . . . ?
C33 C32 C37 O4 -175.9(2) . . . . ?
C31 C32 C37 O4 5.0(4) . . . . ?
C33 C32 C37 C36 3.7(4) . . . . ?
C31 C32 C37 C36 -175.4(2) . . . . ?
Ni2 O5 C38 C39 159.58(17) . . . . ?
Ni2 O5 C38 C43 -22.7(3) . . . . ?
O5 C38 C39 C40 177.6(2) . . . . ?
C43 C38 C39 C40 -0.3(4) . . . . ?
C38 C39 C40 C41 -0.9(4) . . . . ?
C39 C40 C41 C42 1.5(4) . . . . ?
C39 C40 C41 N7 179.1(2) . . . . ?
C46 N7 C41 C42 -136.5(3) . . . . ?
C46 N7 C41 C40 45.9(4) . . . . ?
C40 C41 C42 C43 -1.0(4) . . . . ?
N7 C41 C42 C43 -178.7(2) . . . . ?
C41 C42 C43 C38 -0.1(4) . . . . ?
C41 C42 C43 C44 179.5(2) . . . . ?
O5 C38 C43 C42 -177.0(2) . . . . ?
C39 C38 C43 C42 0.7(3) . . . . ?
O5 C38 C43 C44 3.5(4) . . . . ?
C39 C38 C43 C44 -178.8(2) . . . . ?
C27 N5 C44 C43 179.4(2) . . . . ?
Ni2 N5 C44 C43 -11.4(3) . . . . ?
C27 N5 C44 C45 -2.5(3) . . . . ?
Ni2 N5 C44 C45 166.72(18) . . . . ?
C42 C43 C44 N5 -165.8(2) . . . . ?
C38 C43 C44 N5 13.8(4) . . . . ?
C42 C43 C44 C45 16.1(3) . . . . ?
C38 C43 C44 C45 -164.3(2) . . . . ?
C41 N7 C46 O6 -7.4(4) . . . . ?
C41 N7 C46 N8 173.4(2) . . . . ?
C47 N8 C46 O6 -1.6(4) . . . . ?
C47 N8 C46 N7 177.6(2) . . . . ?
C46 N8 C47 C48 52.6(4) . . . . ?
C46 N8 C47 C52 -128.7(3) . . . . ?
C52 C47 C48 C49 0.6(4) . . . . ?
N8 C47 C48 C49 179.3(3) . . . . ?
C47 C48 C49 C50 0.4(5) . . . . ?
C48 C49 C50 C51 -1.4(5) . . . . ?
C49 C50 C51 C52 1.4(5) . . . . ?
C48 C47 C52 C51 -0.6(4) . . . . ?
N8 C47 C52 C51 -179.3(3) . . . . ?
C50 C51 C52 C47 -0.4(4) . . . . ?
O8 Ni3 O7 C63 168.54(19) . . . . ?
N10 Ni3 O7 C63 -9.6(2) . . . . ?
O7 Ni3 O8 C64 -160.4(2) . . . . ?
N9 Ni3 O8 C64 21.6(2) . . . . ?
O8 Ni3 N9 C70 -22.5(3) . . . . ?
N10 Ni3 N9 C70 155.6(3) . . . . ?
O8 Ni3 N9 C53 154.7(2) . . . . ?
N10 Ni3 N9 C53 -27.2(2) . . . . ?
O8 Ni3 N9 C53A -164.0(9) . . . . ?
N10 Ni3 N9 C53A 14.1(9) . . . . ?
O7 Ni3 N10 C57 14.0(3) . . . . ?
N9 Ni3 N10 C57 -167.9(3) . . . . ?
O7 Ni3 N10 C54 -174.0(2) . . . . ?
N9 Ni3 N10 C54 4.1(2) . . . . ?
C70 N9 C53 C54 -137.4(3) . . . . ?
Ni3 N9 C53 C54 45.2(3) . . . . ?
N9 C53 C54 C55 -164.2(3) . . . . ?
N9 C53 C54 N10 -40.4(4) . . . . ?
N9 C53 C54 C56 75.0(3) . . . . ?
C57 N10 C54 C53A 150.8(10) . . . . ?
Ni3 N10 C54 C53A -21.7(10) . . . . ?
C57 N10 C54 C53 -167.5(3) . . . . ?
Ni3 N10 C54 C53 20.0(3) . . . . ?
C57 N10 C54 C55 -44.1(4) . . . . ?
Ni3 N10 C54 C55 143.4(2) . . . . ?
C57 N10 C54 C56 76.0(3) . . . . ?
Ni3 N10 C54 C56 -96.5(2) . . . . ?
C54 N10 C57 C58 179.5(3) . . . . ?
Ni3 N10 C57 C58 -8.9(4) . . . . ?
N10 C57 C58 C59 -179.5(3) . . . . ?
N10 C57 C58 C63 -5.1(4) . . . . ?
C63 C58 C59 C60 -2.7(4) . . . . ?
C57 C58 C59 C60 171.7(2) . . . . ?
C58 C59 C60 C61 -0.7(4) . . . . ?
C59 C60 C61 C62 2.0(4) . . . . ?
C60 C61 C62 C63 0.2(4) . . . . ?
Ni3 O7 C63 C62 179.09(17) . . . . ?
Ni3 O7 C63 C58 -0.3(3) . . . . ?
C61 C62 C63 O7 177.1(2) . . . . ?
C61 C62 C63 C58 -3.5(4) . . . . ?
C59 C58 C63 O7 -175.9(2) . . . . ?
C57 C58 C63 O7 9.9(4) . . . . ?
C59 C58 C63 C62 4.7(4) . . . . ?
C57 C58 C63 C62 -169.5(2) . . . . ?
Ni3 O8 C64 C65 171.33(16) . . . . ?
Ni3 O8 C64 C69 -10.4(3) . . . . ?
O8 C64 C65 C66 179.4(2) . . . . ?
C69 C64 C65 C66 1.0(4) . . . . ?
C64 C65 C66 C67 -0.6(4) . . . . ?
C65 C66 C67 C68 0.0(4) . . . . ?
C65 C66 C67 N11 -179.9(2) . . . . ?
C72 N11 C67 C68 -125.2(3) . . . . ?
C72 N11 C67 C66 54.7(3) . . . . ?
C66 C67 C68 C69 0.2(4) . . . . ?
N11 C67 C68 C69 -179.9(2) . . . . ?
C67 C68 C69 C64 0.1(4) . . . . ?
C67 C68 C69 C70 -170.2(2) . . . . ?
O8 C64 C69 C68 -179.0(2) . . . . ?
C65 C64 C69 C68 -0.7(4) . . . . ?
O8 C64 C69 C70 -8.7(4) . . . . ?
C65 C64 C69 C70 169.6(2) . . . . ?
C53 N9 C70 C69 -165.6(3) . . . . ?
C53A N9 C70 C69 153.1(10) . . . . ?
Ni3 N9 C70 C69 11.2(4) . . . . ?
C53 N9 C70 C71 11.7(5) . . . . ?
C53A N9 C70 C71 -29.5(10) . . . . ?
Ni3 N9 C70 C71 -171.5(2) . . . . ?
C68 C69 C70 N9 178.3(3) . . . . ?
C64 C69 C70 N9 8.3(4) . . . . ?
C68 C69 C70 C71 0.9(4) . . . . ?
C64 C69 C70 C71 -169.1(3) . . . . ?
C73 N12 C72 O9 9.7(4) . . . . ?
C73 N12 C72 N11 -170.4(2) . . . . ?
C67 N11 C72 O9 -13.4(4) . . . . ?
C67 N11 C72 N12 166.7(2) . . . . ?
C72 N12 C73 C78 5.6(4) . . . . ?
C72 N12 C73 C74 -175.8(2) . . . . ?
C78 C73 C74 C75 -1.7(4) . . . . ?
N12 C73 C74 C75 179.6(2) . . . . ?
C73 C74 C75 C76 0.5(4) . . . . ?
C74 C75 C76 C77 0.6(4) . . . . ?
C75 C76 C77 C78 -0.5(5) . . . . ?
C76 C77 C78 C73 -0.7(4) . . . . ?
C74 C73 C78 C77 1.8(4) . . . . ?
N12 C73 C78 C77 -179.6(3) . . . . ?
C55 C54 C53A N9 -128.0(9) . . . . ?
N10 C54 C53A N9 31.9(16) . . . . ?
C56 C54 C53A N9 135.2(16) . . . . ?
C70 N9 C53A C54 -179.0(11) . . . . ?
Ni3 N9 C53A C54 -30.3(17) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O8 0.80(3) 1.97(3) 2.754(3) 166(3) .
N4 H4 O7 0.76(3) 2.43(3) 3.150(3) 161(3) .
N7 H7A O2 0.81(3) 2.13(3) 2.884(3) 154(3) 1_655
N8 H8A O1 0.82(3) 2.24(3) 3.043(3) 165(3) 1_655
N11 H11 O5 0.88(3) 2.06(3) 2.906(3) 160(3) .
N12 H12 O4 0.77(3) 2.24(3) 2.986(3) 161(3) .
N12 H12 O5 0.77(3) 2.49(3) 3.090(3) 135(3) .
O10 H10A O3 0.84 2.04 2.875(3) 177.4 1_655

_refine_diff_density_max         1.414
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.098


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Ethanol'
####################################################################### 
# 
# 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_jyy315
_database_code_depnum_ccdc_archive 'CCDC 2379620'
loop_
_audit_author_name
_audit_author_address
'Jae Elise Payong'
;University of California, Irvine
United States of America
;
_audit_update_record             
;
2024-08-24 deposited with the CCDC.	2024-10-25 downloaded from the CCDC.
;
_audit_creation_date             2024-08-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'1(C32 H30 N6 Ni O2 S2), C2 H6 O S, 0.6[C2H6SO]'
_chemical_formula_sum            'C35.20 H39.60 N6 Ni O3.60 S3.60'
_chemical_formula_weight         778.45
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.4469(4)
_cell_length_b                   14.7117(5)
_cell_length_c                   18.4767(7)
_cell_angle_alpha                79.477(2)
_cell_angle_beta                 86.598(2)
_cell_angle_gamma                88.997(2)
_cell_volume                     3587.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9420
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      72.16
_cell_measurement_theta_min      3.55
_shelx_estimated_absorpt_T_max   0.771
_shelx_estimated_absorpt_T_min   0.347
_exptl_absorpt_coefficient_mu    3.119
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1153 before and 0.0796 after correction.
The Ratio of minimum to maximum transmission is 0.6972.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       trapezoidal
_exptl_crystal_F_000             1629
_exptl_crystal_size_max          0.431
_exptl_crystal_size_mid          0.323
_exptl_crystal_size_min          0.088
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            94171
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.674
_diffrn_reflns_theta_min         2.436
_diffrn_ambient_temperature      93.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker X8 Prospector APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           0.65
_diffrn_source_power             0.029094000000000002
_diffrn_source_voltage           44.76
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10805
_reflns_number_total             13642
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.148
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         13642
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0742
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0810P)²+14.9981P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.2016
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4A-C19 \\sim N4B-C19
 with sigma of 0.02
 N4A-C20A \\sim N4B-C20B
 with sigma of 0.02
 C20A-C21A \\sim C20B-C21B
 with sigma of 0.02
 C20A-C25A \\sim C20B-C25B
 with sigma of 0.02
 C22A-C21A \\sim C22B-C21B
 with sigma of 0.02
 C22A-C23A \\sim C22B-C23B
 with sigma of 0.02
 C25A-C24A \\sim C25B-C24B
 with sigma of 0.02
 C24A-C23A \\sim C24B-C23B
 with sigma of 0.02
 N4A-C21A \\sim N4B-C21B
 with sigma of 0.04
 N4A-C25A \\sim N4B-C25B
 with sigma of 0.04
 C19-C20A \\sim C19-C20B
 with sigma of 0.04
 C20A-C22A \\sim C20B-C22B
 with sigma of 0.04
 C20A-C24A \\sim C20B-C24B
 with sigma of 0.04
 C22A-C24A \\sim C22B-C24B
 with sigma of 0.04
 C21A-C25A \\sim C21B-C25B
 with sigma of 0.04
 C21A-C23A \\sim C21B-C23B
 with sigma of 0.04
 C25A-C23A \\sim C25B-C23B
 with sigma of 0.04
 N12B-C62A \\sim N12B-C62B
 with sigma of 0.02
 C62A-C63A \\sim C62B-C63B
 with sigma of 0.02
 C62A-C67B \\sim C62B-C67A
 with sigma of 0.02
 C63A-C64A \\sim C63B-C64B
 with sigma of 0.02
 C64A-C65B \\sim C64B-C65A
 with sigma of 0.02
 C65B-C66B \\sim C65A-C66A
 with sigma of 0.02
 C67B-C66B \\sim C67A-C66A
 with sigma of 0.02
 N12B-C63A \\sim N12B-C63B
 with sigma of 0.04
 N12B-C67B \\sim N12B-C67A
 with sigma of 0.04
 C62A-C64A \\sim C62B-C64B
 with sigma of 0.04
 C62A-C66B \\sim C62B-C66A
 with sigma of 0.04
 C63A-C65B \\sim C63B-C65A
 with sigma of 0.04
 C63A-C67B \\sim C63B-C67A
 with sigma of 0.04
 C64A-C66B \\sim C64B-C66A
 with sigma of 0.04
 C65B-C67B \\sim C65A-C67A
 with sigma of 0.04
 N12B-C61 \\sim N12A-C61
 with sigma of 0.02
 N12B-C62A \\sim N12A-C62A
 with sigma of 0.02
 N12B-C62B \\sim N12A-C62B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N12A \\sim C62A \\sim C63A \\sim C64A \\sim C65A \\sim C66A \\sim C67A: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(N12A) \\sim Ueq, Uanis(C62A) \\sim Ueq, Uanis(C67A) \\sim Ueq,
Uanis(C66A) \\sim Ueq, Uanis(C65A) \\sim Ueq, Uanis(C64A) \\sim Ueq,
Uanis(C63A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C23B) = Uanis(C22B) = Uanis(C24B) = Uanis(C21B) = Uanis(C25B) =
Uanis(N4B) = Uanis(C20B)
Uanis(N4A) = Uanis(C24A) = Uanis(C20A) = Uanis(C25A) = Uanis(C22A) =
Uanis(C23A) = Uanis(C21A)
Uanis(N12B) = Uanis(C62B) = Uanis(C63B) = Uanis(C64B) = Uanis(C65B) =
Uanis(C66B) = Uanis(C67B)
Uanis(C34) = Uanis(S3) = Uanis(O3) = Uanis(C35)
4. Others
 Fixed Sof: N12B(0.35) H12D(0.35) N4A(0.5) H4A(0.5) C62A(0.65) C63A(0.65)
 H63A(0.65) C64A(0.65) H64A(0.65) C65B(0.35) H65B(0.35) C20A(0.5) C67B(0.35)
 H67B(0.35) C22A(0.5) H22A(0.5) C66B(0.35) H66B(0.35) C21A(0.5) H21A(0.5)
 C25A(0.5) H25A(0.5) C24A(0.5) H24A(0.5) C23A(0.5) H23A(0.5) C23B(0.5)
 H23B(0.5) C24B(0.5) H24B(0.5) C25B(0.5) H25B(0.5) C20B(0.5) C21B(0.5)
 H21B(0.5) C22B(0.5) H22B(0.5) N4B(0.5) H4B(0.5) C64B(0.35) H64B(0.35)
 C63B(0.35) H63B(0.35) C62B(0.35) C65A(0.65) H65A(0.65) C66A(0.65) H66A(0.65)
 C67A(0.65) H67A(0.65) N12A(0.65) H12E(0.65)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C44(H44A,H44B), C9(H9A,H9B), C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), N11(H11), N9(H9), N6(H6), N12B(H12D), N10(H10), C4(H4),
 C5(H5A), C3(H3A), C51(H51), C49(H49), C14(H14), C40(H40), C38(H38), N4A(H4A),
 C16(H16), C50(H50), C39(H39), C15(H15), C63A(H63A), C59(H59), C56(H56),
 C60(H60), C29(H29), C58(H58), C57(H57), C33(H33), C32(H32), C64A(H64A),
 C65B(H65B), C30(H30), C31(H31), C67B(H67B), C22A(H22A), C66B(H66B), C21A(H21A),
  C25A(H25A), C24A(H24A), C23A(H23A), C23B(H23B), C24B(H24B), C25B(H25B),
 C21B(H21B), C22B(H22B), N4B(H4B), C64B(H64B), C63B(H63B), C65A(H65A),
 C66A(H66A), C67A(H67A), N12A(H12E)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C43(H43A,H43B,H43C), C47(H47A,H47B,
 H47C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.75885(5) 0.63921(5) 0.52411(4) 0.02208(17) Uani 1 1 d . . . . .
Ni2 Ni 0.74232(5) 0.85663(5) 0.42160(4) 0.02429(18) Uani 1 1 d . . . . .
S6 S 0.66408(9) 1.02251(8) 0.18158(7) 0.0351(3) Uani 1 1 d . . . . .
S5 S 0.29174(8) 0.76369(9) 0.31255(7) 0.0370(3) Uani 1 1 d . . . . .
S1 S 1.08214(10) 0.88886(8) 0.66243(7) 0.0389(3) Uani 1 1 d . . . . .
S2 S 0.49669(9) 0.77271(9) 0.82308(7) 0.0416(3) Uani 1 1 d . . . . .
S3 S 0.87461(11) 0.52467(9) 0.76417(8) 0.0469(3) Uani 1 1 d . . . . .
S4 S 0.76368(10) 0.58510(9) 0.19743(8) 0.0428(3) Uani 1 1 d . . . . .
O1 O 0.8654(2) 0.66042(19) 0.57672(15) 0.0230(6) Uani 1 1 d . . . . .
O2 O 0.6821(2) 0.66482(19) 0.60371(16) 0.0243(6) Uani 1 1 d . . . . .
O4 O 0.7687(2) 0.8312(2) 0.32948(17) 0.0283(6) Uani 1 1 d . . . . .
O5 O 0.6136(2) 0.8525(2) 0.39767(16) 0.0281(6) Uani 1 1 d . . . . .
O6 O 0.6201(2) 0.9258(2) 0.19269(18) 0.0357(7) Uani 1 1 d . . . . .
O3 O 0.8369(3) 0.6214(2) 0.7677(2) 0.0469(3) Uani 1 1 d . . . . .
N2 N 0.6496(3) 0.6237(2) 0.47067(19) 0.0248(7) Uani 1 1 d . . . . .
N3 N 0.9791(3) 0.7342(2) 0.6601(2) 0.0274(8) Uani 1 1 d . . . . .
H3 H 0.9302 0.6981 0.6813 0.033 Uiso 1 1 calc R U . . .
N1 N 0.8397(3) 0.6056(2) 0.44815(19) 0.0247(7) Uani 1 1 d . . . . .
N8 N 0.7091(3) 0.8799(2) 0.5157(2) 0.0270(8) Uani 1 1 d . . . . .
N5 N 0.6149(3) 0.6817(3) 0.7361(2) 0.0274(8) Uani 1 1 d . . . . .
H5 H 0.6766 0.6651 0.7261 0.033 Uiso 1 1 calc R U . . .
N7 N 0.8761(3) 0.8699(2) 0.4373(2) 0.0276(8) Uani 1 1 d . . . . .
N11 N 0.4539(3) 0.8585(3) 0.3279(2) 0.0316(8) Uani 1 1 d . . . . .
H11 H 0.5113 0.8796 0.3068 0.038 Uiso 1 1 calc R U . . .
N9 N 0.7557(3) 0.7614(3) 0.2113(2) 0.0319(8) Uani 1 1 d . . . . .
H9 H 0.7198 0.8125 0.2076 0.038 Uiso 1 1 calc R U . . .
N6 N 0.6886(3) 0.7217(3) 0.8307(2) 0.0350(9) Uani 1 1 d . . . . .
H6 H 0.7389 0.6935 0.8113 0.042 Uiso 1 1 calc R U . . .
N12B N 0.424(2) 0.854(3) 0.2106(6) 0.059(3) Uani 0.35 1 d D . P A 2
H12D H 0.4840 0.8793 0.2047 0.070 Uiso 0.35 1 calc R U P A 2
C1 C 0.9598(3) 0.6689(3) 0.5524(2) 0.0231(8) Uani 1 1 d . . . . .
C2 C 1.0248(3) 0.7098(3) 0.5963(2) 0.0249(9) Uani 1 1 d . . . . .
C13 C 0.5201(3) 0.6323(3) 0.5640(2) 0.0249(9) Uani 1 1 d . . . . .
C18 C 0.5850(3) 0.6521(3) 0.6164(2) 0.0255(9) Uani 1 1 d . . . . .
C7 C 0.9362(3) 0.5999(3) 0.4404(2) 0.0250(9) Uani 1 1 d . . . . .
N10 N 0.6207(3) 0.7122(3) 0.1647(3) 0.0424(10) Uani 1 1 d . . . . .
H10 H 0.5972 0.7678 0.1673 0.051 Uiso 1 1 calc R U . . .
C6 C 1.0003(3) 0.6396(3) 0.4883(2) 0.0241(8) Uani 1 1 d . . . . .
C17 C 0.5447(3) 0.6599(3) 0.6874(2) 0.0269(9) Uani 1 1 d . . . . .
C41 C 0.9481(3) 0.8157(3) 0.3304(3) 0.0274(9) Uani 1 1 d . . . . .
C37 C 0.8511(3) 0.7652(3) 0.2375(2) 0.0283(9) Uani 1 1 d . . . . .
C53 C 0.5322(3) 0.8620(3) 0.4392(2) 0.0256(9) Uani 1 1 d . . . . .
C48 C 0.5301(3) 0.8730(3) 0.5132(2) 0.0272(9) Uani 1 1 d . . . . .
C36 C 0.8545(3) 0.8045(3) 0.3021(2) 0.0261(9) Uani 1 1 d . . . . .
C4 C 1.1648(3) 0.6880(3) 0.5133(3) 0.0298(10) Uani 1 1 d . . . . .
H4 H 1.2338 0.6954 0.4994 0.036 Uiso 1 1 calc R U . . .
C11 C 0.5541(3) 0.6283(3) 0.4892(2) 0.0248(9) Uani 1 1 d . . . . .
C52 C 0.4416(3) 0.8619(3) 0.4036(2) 0.0268(9) Uani 1 1 d . . . . .
C5 C 1.1031(3) 0.6502(3) 0.4699(2) 0.0280(9) Uani 1 1 d . . . . .
H5A H 1.1305 0.6309 0.4266 0.034 Uiso 1 1 calc R U . . .
C3 C 1.1259(3) 0.7153(3) 0.5778(3) 0.0296(9) Uani 1 1 d . . . . .
H3A H 1.1692 0.7378 0.6092 0.036 Uiso 1 1 calc R U . . .
C42 C 0.9552(3) 0.8580(3) 0.3955(2) 0.0259(9) Uani 1 1 d . . . . .
C46 C 0.6216(3) 0.8792(3) 0.5506(2) 0.0278(9) Uani 1 1 d . . . . .
C51 C 0.3504(3) 0.8699(3) 0.4421(3) 0.0309(10) Uani 1 1 d . . . . .
H51 H 0.2900 0.8697 0.4180 0.037 Uiso 1 1 calc R U . . .
C10 C 0.6806(3) 0.6167(3) 0.3935(2) 0.0290(9) Uani 1 1 d . . . . .
H10A H 0.6860 0.6790 0.3625 0.035 Uiso 1 1 calc R U . . .
H10B H 0.6313 0.5808 0.3728 0.035 Uiso 1 1 calc R U . . .
C8 C 0.9843(3) 0.5531(3) 0.3815(3) 0.0320(10) Uani 1 1 d . . . . .
H8A H 0.9877 0.5964 0.3344 0.048 Uiso 1 1 calc R U . . .
H8B H 0.9450 0.4992 0.3769 0.048 Uiso 1 1 calc R U . . .
H8C H 1.0518 0.5330 0.3946 0.048 Uiso 1 1 calc R U . . .
C49 C 0.4352(3) 0.8806(3) 0.5505(3) 0.0331(10) Uani 1 1 d . . . . .
H49 H 0.4322 0.8873 0.6008 0.040 Uiso 1 1 calc R U . . .
C14 C 0.4177(3) 0.6171(3) 0.5867(3) 0.0322(10) Uani 1 1 d . . . . .
H14 H 0.3731 0.6038 0.5520 0.039 Uiso 1 1 calc R U . . .
C40 C 1.0340(3) 0.7865(3) 0.2929(3) 0.0319(10) Uani 1 1 d . . . . .
H40 H 1.0974 0.7929 0.3115 0.038 Uiso 1 1 calc R U . . .
C12 C 0.4788(3) 0.6299(3) 0.4311(3) 0.0317(10) Uani 1 1 d . . . . .
H12A H 0.4667 0.5665 0.4243 0.047 Uiso 1 1 calc R U . . .
H12B H 0.5048 0.6667 0.3844 0.047 Uiso 1 1 calc R U . . .
H12C H 0.4163 0.6573 0.4471 0.047 Uiso 1 1 calc R U . . .
C38 C 0.9368(3) 0.7387(3) 0.2021(3) 0.0333(10) Uani 1 1 d . . . . .
H38 H 0.9332 0.7134 0.1585 0.040 Uiso 1 1 calc R U . . .
N4A N 0.9534(12) 0.7954(10) 0.7616(6) 0.0608(15) Uani 0.5 1 d D . P B 1
H4A H 0.9174 0.7454 0.7766 0.073 Uiso 0.5 1 calc R U P B 1
C44 C 0.8851(3) 0.9164(3) 0.5006(3) 0.0304(10) Uani 1 1 d . . . . .
H44A H 0.8832 0.9843 0.4842 0.037 Uiso 1 1 calc R U . . .
H44B H 0.9492 0.8995 0.5234 0.037 Uiso 1 1 calc R U . . .
C16 C 0.4453(3) 0.6429(4) 0.7076(3) 0.0365(11) Uani 1 1 d . . . . .
H16 H 0.4202 0.6461 0.7563 0.044 Uiso 1 1 calc R U . . .
C27 C 0.6021(3) 0.7240(3) 0.7956(2) 0.0320(10) Uani 1 1 d . . . . .
C50 C 0.3485(3) 0.8783(3) 0.5158(3) 0.0362(11) Uani 1 1 d . . . . .
H50 H 0.2864 0.8825 0.5424 0.043 Uiso 1 1 calc R U . . .
C9 C 0.7801(3) 0.5686(3) 0.3954(3) 0.0309(10) Uani 1 1 d . . . . .
H9A H 0.7713 0.5011 0.4114 0.037 Uiso 1 1 calc R U . . .
H9B H 0.8145 0.5800 0.3457 0.037 Uiso 1 1 calc R U . . .
C39 C 1.0285(3) 0.7491(3) 0.2304(3) 0.0339(10) Uani 1 1 d . . . . .
H39 H 1.0877 0.7303 0.2064 0.041 Uiso 1 1 calc R U . . .
C43 C 1.0547(3) 0.8915(3) 0.4131(3) 0.0328(10) Uani 1 1 d . . . . .
H43A H 1.0736 0.8572 0.4609 0.049 Uiso 1 1 calc R U . . .
H43B H 1.0501 0.9576 0.4150 0.049 Uiso 1 1 calc R U . . .
H43C H 1.1051 0.8816 0.3747 0.049 Uiso 1 1 calc R U . . .
C15 C 0.3820(3) 0.6211(4) 0.6565(3) 0.0388(11) Uani 1 1 d . . . . .
H15 H 0.3137 0.6090 0.6704 0.047 Uiso 1 1 calc R U . . .
C47 C 0.6144(4) 0.8871(3) 0.6307(3) 0.0364(11) Uani 1 1 d . . . . .
H47A H 0.6106 0.9525 0.6351 0.055 Uiso 1 1 calc R U . . .
H47B H 0.6734 0.8587 0.6545 0.055 Uiso 1 1 calc R U . . .
H47C H 0.5545 0.8553 0.6548 0.055 Uiso 1 1 calc R U . . .
C61 C 0.3918(3) 0.8279(3) 0.2819(3) 0.0328(10) Uani 1 1 d D . . . .
C19 C 0.9996(4) 0.8056(3) 0.6938(3) 0.0335(10) Uani 1 1 d D . . . .
C55 C 0.5588(4) 0.6511(4) 0.1324(3) 0.0410(12) Uani 1 1 d . . . . .
C28 C 0.7089(4) 0.7582(4) 0.8943(3) 0.0403(12) Uani 1 1 d . . . . .
C54 C 0.7128(4) 0.6891(4) 0.1912(3) 0.0369(11) Uani 1 1 d . . . . .
C62A C 0.3852(9) 0.8415(14) 0.1437(4) 0.036(2) Uani 0.65 1 d D U P A 1
C68 C 0.6638(5) 1.0501(4) 0.2708(3) 0.0464(13) Uani 1 1 d . . . . .
H68A H 0.5954 1.0625 0.2878 0.070 Uiso 1 1 calc R U . . .
H68B H 0.7047 1.1050 0.2692 0.070 Uiso 1 1 calc R U . . .
H68C H 0.6913 0.9980 0.3048 0.070 Uiso 1 1 calc R U . . .
C63A C 0.4327(8) 0.8901(7) 0.0795(5) 0.038(2) Uani 0.65 1 d D U P A 1
H63A H 0.4880 0.9281 0.0830 0.046 Uiso 0.65 1 calc R U P A 1
C59 C 0.4583(5) 0.5203(4) 0.1437(3) 0.0508(14) Uani 1 1 d . . . . .
H59 H 0.4314 0.4654 0.1730 0.061 Uiso 1 1 calc R U . . .
C56 C 0.5393(4) 0.6764(4) 0.0600(3) 0.0457(13) Uani 1 1 d . . . . .
H56 H 0.5684 0.7306 0.0312 0.055 Uiso 1 1 calc R U . . .
C60 C 0.5185(4) 0.5753(4) 0.1762(3) 0.0496(14) Uani 1 1 d . . . . .
H60 H 0.5309 0.5604 0.2271 0.060 Uiso 1 1 calc R U . . .
C69 C 0.7948(4) 1.0083(4) 0.1674(4) 0.0551(16) Uani 1 1 d . . . . .
H69A H 0.8195 0.9632 0.2084 0.083 Uiso 1 1 calc R U . . .
H69B H 0.8278 1.0677 0.1651 0.083 Uiso 1 1 calc R U . . .
H69C H 0.8093 0.9860 0.1211 0.083 Uiso 1 1 calc R U . . .
C34 C 0.7793(4) 0.4725(4) 0.7250(3) 0.0469(3) Uani 1 1 d . . . . .
H34A H 0.7164 0.4766 0.7538 0.070 Uiso 1 1 calc R U . . .
H34B H 0.7963 0.4073 0.7252 0.070 Uiso 1 1 calc R U . . .
H34C H 0.7724 0.5044 0.6741 0.070 Uiso 1 1 calc R U . . .
C29 C 0.7639(4) 0.7032(5) 0.9465(3) 0.0512(14) Uani 1 1 d . . . . .
H29 H 0.7831 0.6427 0.9399 0.061 Uiso 1 1 calc R U . . .
C58 C 0.4365(5) 0.5420(4) 0.0714(3) 0.0517(14) Uani 1 1 d . . . . .
H58 H 0.3948 0.5032 0.0507 0.062 Uiso 1 1 calc R U . . .
C57 C 0.4764(4) 0.6223(4) 0.0284(3) 0.0516(14) Uani 1 1 d . . . . .
H57 H 0.4610 0.6398 -0.0218 0.062 Uiso 1 1 calc R U . . .
C33 C 0.6803(5) 0.8471(4) 0.9034(3) 0.0543(15) Uani 1 1 d . . . . .
H33 H 0.6422 0.8854 0.8681 0.065 Uiso 1 1 calc R U . . .
C32 C 0.7095(5) 0.8786(5) 0.9666(4) 0.0614(18) Uani 1 1 d . . . . .
H32 H 0.6910 0.9391 0.9736 0.074 Uiso 1 1 calc R U . . .
C64A C 0.4006(9) 0.8839(9) 0.0109(6) 0.046(3) Uani 0.65 1 d D U P A 1
H64A H 0.4318 0.9202 -0.0320 0.055 Uiso 0.65 1 calc R U P A 1
C65B C 0.313(3) 0.837(4) 0.0071(12) 0.059(3) Uani 0.35 1 d D . P A 2
H65B H 0.2915 0.8245 -0.0382 0.070 Uiso 0.35 1 calc R U P A 2
C30 C 0.7911(5) 0.7355(5) 1.0081(3) 0.0642(18) Uani 1 1 d . . . . .
H30 H 0.8286 0.6971 1.0438 0.077 Uiso 1 1 calc R U . . .
C31 C 0.7637(6) 0.8239(6) 1.0177(4) 0.068(2) Uani 1 1 d . . . . .
H31 H 0.7827 0.8463 1.0599 0.081 Uiso 1 1 calc R U . . .
C20A C 0.9583(12) 0.8590(9) 0.8112(6) 0.0608(15) Uani 0.5 1 d D . P B 1
C67B C 0.2793(13) 0.8365(16) 0.1366(9) 0.059(3) Uani 0.35 1 d D . P A 2
H67B H 0.2336 0.8338 0.1781 0.070 Uiso 0.35 1 calc R U P A 2
C35 C 0.8617(4) 0.4632(4) 0.8559(3) 0.0469(3) Uani 1 1 d . . . . .
H35A H 0.8989 0.4948 0.8880 0.070 Uiso 1 1 calc R U . . .
H35B H 0.8880 0.4003 0.8580 0.070 Uiso 1 1 calc R U . . .
H35C H 0.7911 0.4605 0.8727 0.070 Uiso 1 1 calc R U . . .
C22A C 0.9817(11) 0.8829(9) 0.9346(7) 0.0608(15) Uani 0.5 1 d D . P B 1
H22A H 0.9970 0.8608 0.9843 0.073 Uiso 0.5 1 calc R U P B 1
C66B C 0.2454(14) 0.8273(16) 0.0685(8) 0.059(3) Uani 0.35 1 d D . P A 2
H66B H 0.1772 0.8149 0.0638 0.070 Uiso 0.35 1 calc R U P A 2
C21A C 0.9797(10) 0.8229(9) 0.8847(6) 0.0608(15) Uani 0.5 1 d D . P B 1
H21A H 0.9925 0.7587 0.8998 0.073 Uiso 0.5 1 calc R U P B 1
C25A C 0.9428(11) 0.9509(8) 0.7885(7) 0.0608(15) Uani 0.5 1 d D . P B 1
H25A H 0.9318 0.9761 0.7385 0.073 Uiso 0.5 1 calc R U P B 1
C24A C 0.9438(11) 1.0080(8) 0.8429(6) 0.0608(15) Uani 0.5 1 d D . P B 1
H24A H 0.9312 1.0723 0.8280 0.073 Uiso 0.5 1 calc R U P B 1
C23A C 0.9604(12) 0.9789(9) 0.9096(7) 0.0608(15) Uani 0.5 1 d D . P B 1
H23A H 0.9586 1.0206 0.9433 0.073 Uiso 0.5 1 calc R U P B 1
C23B C 0.8883(10) 1.0239(7) 0.8734(7) 0.0547(13) Uani 0.5 1 d D . P B 2
H23B H 0.8786 1.0731 0.9000 0.066 Uiso 0.5 1 calc R U P B 2
C24B C 0.8463(10) 1.0276(7) 0.8121(6) 0.0547(13) Uani 0.5 1 d D . P B 2
H24B H 0.8064 1.0801 0.7947 0.066 Uiso 0.5 1 calc R U P B 2
C25B C 0.8570(10) 0.9562(7) 0.7691(7) 0.0547(13) Uani 0.5 1 d D . P B 2
H25B H 0.8224 0.9592 0.7253 0.066 Uiso 0.5 1 calc R U P B 2
C20B C 0.9177(10) 0.8845(8) 0.7926(7) 0.0547(13) Uani 0.5 1 d D . P B 2
C21B C 0.9651(10) 0.8775(8) 0.8598(6) 0.0547(13) Uani 0.5 1 d D . P B 2
H21B H 1.0073 0.8262 0.8759 0.066 Uiso 0.5 1 calc R U P B 2
C22B C 0.9498(10) 0.9459(8) 0.9019(7) 0.0547(13) Uani 0.5 1 d D . P B 2
H22B H 0.9788 0.9416 0.9481 0.066 Uiso 0.5 1 calc R U P B 2
N4B N 0.9349(11) 0.8073(9) 0.7551(7) 0.0547(13) Uani 0.5 1 d D . P B 2
H4B H 0.9012 0.7566 0.7726 0.066 Uiso 0.5 1 calc R U P B 2
C64B C 0.417(2) 0.865(2) 0.0114(11) 0.059(3) Uani 0.35 1 d D . P A 2
H64B H 0.4605 0.8805 -0.0311 0.070 Uiso 0.35 1 calc R U P A 2
C63B C 0.4453(18) 0.868(2) 0.0812(11) 0.059(3) Uani 0.35 1 d D . P A 2
H63B H 0.5124 0.8829 0.0872 0.070 Uiso 0.35 1 calc R U P A 2
C62B C 0.380(3) 0.850(4) 0.1433(8) 0.059(3) Uani 0.35 1 d D . P A 2
C65A C 0.3254(13) 0.8269(18) 0.0038(7) 0.055(4) Uani 0.65 1 d D U P A 1
H65A H 0.3042 0.8230 -0.0436 0.066 Uiso 0.65 1 calc R U P A 1
C66A C 0.2791(6) 0.7739(7) 0.0666(5) 0.047(2) Uani 0.65 1 d D U P A 1
H66A H 0.2257 0.7344 0.0618 0.056 Uiso 0.65 1 calc R U P A 1
C67A C 0.3106(6) 0.7784(7) 0.1364(4) 0.046(2) Uani 0.65 1 d D U P A 1
H67A H 0.2818 0.7392 0.1787 0.055 Uiso 0.65 1 calc R U P A 1
N12A N 0.4233(8) 0.8561(14) 0.2105(3) 0.0330(17) Uani 0.65 1 d D U P A 1
H12E H 0.4776 0.8898 0.2045 0.040 Uiso 0.65 1 calc R U P A 1
C20 C 0.7996(3) 0.8866(3) 0.5558(3) 0.0305(9) Uani 1 1 d . . . . .
H20A H 0.8149 0.8258 0.5862 0.037 Uiso 1 1 calc R U . . .
H20B H 0.7889 0.9320 0.5890 0.037 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.841(3) . ?
Ni1 O2 1.838(3) . ?
Ni1 N2 1.857(4) . ?
Ni1 N1 1.857(4) . ?
Ni2 O4 1.822(3) . ?
Ni2 O5 1.817(3) . ?
Ni2 N8 1.859(4) . ?
Ni2 N7 1.858(4) . ?
S6 O6 1.524(3) . ?
S6 C68 1.768(5) . ?
S6 C69 1.776(5) . ?
S5 C61 1.667(5) . ?
S1 C19 1.667(5) . ?
S2 C27 1.671(5) . ?
S3 O3 1.513(4) . ?
S3 C34 1.762(6) . ?
S3 C35 1.770(6) . ?
S4 C54 1.653(5) . ?
O1 C1 1.321(5) . ?
O2 C18 1.324(5) . ?
O4 C36 1.315(5) . ?
O5 C53 1.319(5) . ?
N2 C11 1.313(5) . ?
N2 C10 1.483(5) . ?
N3 H3 0.8800 . ?
N3 C2 1.398(6) . ?
N3 C19 1.356(6) . ?
N1 C7 1.300(5) . ?
N1 C9 1.480(5) . ?
N8 C46 1.308(6) . ?
N8 C20 1.476(6) . ?
N5 H5 0.8800 . ?
N5 C17 1.421(6) . ?
N5 C27 1.361(6) . ?
N7 C42 1.306(6) . ?
N7 C44 1.471(6) . ?
N11 H11 0.8800 . ?
N11 C52 1.409(6) . ?
N11 C61 1.364(6) . ?
N9 H9 0.8800 . ?
N9 C37 1.404(5) . ?
N9 C54 1.338(6) . ?
N6 H6 0.8800 . ?
N6 C27 1.362(6) . ?
N6 C28 1.420(6) . ?
N12B H12D 0.8800 . ?
N12B C61 1.354(15) . ?
N12B C62B 1.423(16) . ?
C1 C2 1.436(6) . ?
C1 C6 1.411(6) . ?
C2 C3 1.382(6) . ?
C13 C18 1.413(6) . ?
C13 C11 1.442(6) . ?
C13 C14 1.424(6) . ?
C18 C17 1.413(6) . ?
C7 C6 1.472(6) . ?
C7 C8 1.501(6) . ?
N10 H10 0.8800 . ?
N10 C55 1.461(6) . ?
N10 C54 1.373(6) . ?
C6 C5 1.407(6) . ?
C17 C16 1.381(6) . ?
C41 C36 1.414(6) . ?
C41 C42 1.462(6) . ?
C41 C40 1.413(6) . ?
C37 C36 1.420(6) . ?
C37 C38 1.377(6) . ?
C53 C48 1.405(6) . ?
C53 C52 1.418(6) . ?
C48 C46 1.458(6) . ?
C48 C49 1.426(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.378(6) . ?
C4 C3 1.396(7) . ?
C11 C12 1.514(6) . ?
C52 C51 1.394(6) . ?
C5 H5A 0.9500 . ?
C3 H3A 0.9500 . ?
C42 C43 1.507(6) . ?
C46 C47 1.504(6) . ?
C51 H51 0.9500 . ?
C51 C50 1.389(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.502(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C49 H49 0.9500 . ?
C49 C50 1.367(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.361(7) . ?
C40 H40 0.9500 . ?
C40 C39 1.371(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C38 H38 0.9500 . ?
C38 C39 1.390(7) . ?
N4A H4A 0.8800 . ?
N4A C19 1.349(11) . ?
N4A C20A 1.429(12) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C20 1.506(6) . ?
C16 H16 0.9500 . ?
C16 C15 1.391(7) . ?
C50 H50 0.9500 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C39 H39 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C15 H15 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C61 N12A 1.353(8) . ?
C19 N4B 1.390(11) . ?
C55 C56 1.361(8) . ?
C55 C60 1.353(7) . ?
C28 C29 1.382(8) . ?
C28 C33 1.393(8) . ?
C62A C63A 1.393(11) . ?
C62A C67A 1.407(14) . ?
C62A N12A 1.418(9) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C63A H63A 0.9500 . ?
C63A C64A 1.383(10) . ?
C59 H59 0.9500 . ?
C59 C60 1.389(8) . ?
C59 C58 1.365(8) . ?
C56 H56 0.9500 . ?
C56 C57 1.394(8) . ?
C60 H60 0.9500 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C29 H29 0.9500 . ?
C29 C30 1.381(8) . ?
C58 H58 0.9500 . ?
C58 C57 1.394(8) . ?
C57 H57 0.9500 . ?
C33 H33 0.9500 . ?
C33 C32 1.409(8) . ?
C32 H32 0.9500 . ?
C32 C31 1.362(10) . ?
C64A H64A 0.9500 . ?
C64A C65A 1.35(2) . ?
C65B H65B 0.9500 . ?
C65B C66B 1.40(2) . ?
C65B C64B 1.47(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.384(10) . ?
C31 H31 0.9500 . ?
C20A C21A 1.409(16) . ?
C20A C25A 1.357(16) . ?
C67B H67B 0.9500 . ?
C67B C66B 1.392(16) . ?
C67B C62B 1.39(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C22A H22A 0.9500 . ?
C22A C21A 1.391(13) . ?
C22A C23A 1.433(18) . ?
C66B H66B 0.9500 . ?
C21A H21A 0.9500 . ?
C25A H25A 0.9500 . ?
C25A C24A 1.424(13) . ?
C24A H24A 0.9500 . ?
C24A C23A 1.260(17) . ?
C23A H23A 0.9500 . ?
C23B H23B 0.9500 . ?
C23B C24B 1.287(16) . ?
C23B C22B 1.441(19) . ?
C24B H24B 0.9500 . ?
C24B C25B 1.429(12) . ?
C25B H25B 0.9500 . ?
C25B C20B 1.347(16) . ?
C20B C21B 1.415(16) . ?
C20B N4B 1.443(11) . ?
C21B H21B 0.9500 . ?
C21B C22B 1.387(13) . ?
C22B H22B 0.9500 . ?
N4B H4B 0.8800 . ?
C64B H64B 0.9500 . ?
C64B C63B 1.376(15) . ?
C63B H63B 0.9500 . ?
C63B C62B 1.391(18) . ?
C65A H65A 0.9500 . ?
C65A C66A 1.394(15) . ?
C66A H66A 0.9500 . ?
C66A C67A 1.393(10) . ?
C67A H67A 0.9500 . ?
N12A H12E 0.8800 . ?
C20 H20A 0.9900 . ?
C20 H20B 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
O1 Ni1 N2 177.26(14) . . ?
O1 Ni1 N1 93.20(14) . . ?
O2 Ni1 O1 85.11(12) . . ?
O2 Ni1 N2 93.78(14) . . ?
O2 Ni1 N1 175.81(15) . . ?
N1 Ni1 N2 88.07(15) . . ?
O4 Ni2 N8 177.14(15) . . ?
O4 Ni2 N7 93.30(15) . . ?
O5 Ni2 O4 83.30(13) . . ?
O5 Ni2 N8 94.09(15) . . ?
O5 Ni2 N7 174.14(15) . . ?
N7 Ni2 N8 89.39(16) . . ?
O6 S6 C68 105.3(2) . . ?
O6 S6 C69 106.0(2) . . ?
C68 S6 C69 97.7(3) . . ?
O3 S3 C34 105.1(2) . . ?
O3 S3 C35 105.3(2) . . ?
C34 S3 C35 99.7(3) . . ?
C1 O1 Ni1 127.0(3) . . ?
C18 O2 Ni1 126.7(3) . . ?
C36 O4 Ni2 126.9(3) . . ?
C53 O5 Ni2 127.9(3) . . ?
C11 N2 Ni1 129.7(3) . . ?
C11 N2 C10 118.6(4) . . ?
C10 N2 Ni1 111.3(3) . . ?
C2 N3 H3 115.4 . . ?
C19 N3 H3 115.4 . . ?
C19 N3 C2 129.1(4) . . ?
C7 N1 Ni1 130.2(3) . . ?
C7 N1 C9 118.0(4) . . ?
C9 N1 Ni1 111.2(3) . . ?
C46 N8 Ni2 129.1(3) . . ?
C46 N8 C20 119.5(4) . . ?
C20 N8 Ni2 110.7(3) . . ?
C17 N5 H5 114.8 . . ?
C27 N5 H5 114.8 . . ?
C27 N5 C17 130.5(4) . . ?
C42 N7 Ni2 129.8(3) . . ?
C42 N7 C44 119.5(4) . . ?
C44 N7 Ni2 109.6(3) . . ?
C52 N11 H11 114.6 . . ?
C61 N11 H11 114.6 . . ?
C61 N11 C52 130.9(4) . . ?
C37 N9 H9 116.2 . . ?
C54 N9 H9 116.2 . . ?
C54 N9 C37 127.6(4) . . ?
C27 N6 H6 115.4 . . ?
C27 N6 C28 129.1(4) . . ?
C28 N6 H6 115.4 . . ?
C61 N12B H12D 114.0 . . ?
C61 N12B C62B 131.9(18) . . ?
C62B N12B H12D 114.0 . . ?
O1 C1 C2 116.4(4) . . ?
O1 C1 C6 124.9(4) . . ?
C6 C1 C2 118.7(4) . . ?
N3 C2 C1 114.9(3) . . ?
C3 C2 N3 124.7(4) . . ?
C3 C2 C1 120.2(4) . . ?
C18 C13 C11 122.2(4) . . ?
C18 C13 C14 118.1(4) . . ?
C14 C13 C11 119.7(4) . . ?
O2 C18 C13 124.5(4) . . ?
O2 C18 C17 116.8(4) . . ?
C13 C18 C17 118.6(4) . . ?
N1 C7 C6 121.0(4) . . ?
N1 C7 C8 120.3(4) . . ?
C6 C7 C8 118.7(4) . . ?
C55 N10 H10 117.6 . . ?
C54 N10 H10 117.6 . . ?
C54 N10 C55 124.8(4) . . ?
C1 C6 C7 120.7(4) . . ?
C5 C6 C1 119.0(4) . . ?
C5 C6 C7 120.3(4) . . ?
C18 C17 N5 114.9(4) . . ?
C16 C17 N5 123.6(4) . . ?
C16 C17 C18 121.4(4) . . ?
C36 C41 C42 120.7(4) . . ?
C40 C41 C36 118.0(4) . . ?
C40 C41 C42 121.3(4) . . ?
N9 C37 C36 114.9(4) . . ?
C38 C37 N9 123.7(4) . . ?
C38 C37 C36 121.3(4) . . ?
O5 C53 C48 125.2(4) . . ?
O5 C53 C52 115.2(4) . . ?
C48 C53 C52 119.7(4) . . ?
C53 C48 C46 121.5(4) . . ?
C53 C48 C49 117.8(4) . . ?
C49 C48 C46 120.7(4) . . ?
O4 C36 C41 124.8(4) . . ?
O4 C36 C37 116.2(4) . . ?
C41 C36 C37 118.9(4) . . ?
C5 C4 H4 120.1 . . ?
C5 C4 C3 119.9(4) . . ?
C3 C4 H4 120.1 . . ?
N2 C11 C13 120.7(4) . . ?
N2 C11 C12 119.6(4) . . ?
C13 C11 C12 119.6(4) . . ?
N11 C52 C53 114.3(4) . . ?
C51 C52 N11 125.0(4) . . ?
C51 C52 C53 120.6(4) . . ?
C6 C5 H5A 119.2 . . ?
C4 C5 C6 121.6(4) . . ?
C4 C5 H5A 119.2 . . ?
C2 C3 C4 120.5(4) . . ?
C2 C3 H3A 119.8 . . ?
C4 C3 H3A 119.8 . . ?
N7 C42 C41 120.9(4) . . ?
N7 C42 C43 119.6(4) . . ?
C41 C42 C43 119.5(4) . . ?
N8 C46 C48 121.5(4) . . ?
N8 C46 C47 119.6(4) . . ?
C48 C46 C47 118.9(4) . . ?
C52 C51 H51 120.2 . . ?
C50 C51 C52 119.6(4) . . ?
C50 C51 H51 120.2 . . ?
N2 C10 H10A 110.4 . . ?
N2 C10 H10B 110.4 . . ?
N2 C10 C9 106.8(4) . . ?
H10A C10 H10B 108.6 . . ?
C9 C10 H10A 110.4 . . ?
C9 C10 H10B 110.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C48 C49 H49 119.2 . . ?
C50 C49 C48 121.7(4) . . ?
C50 C49 H49 119.2 . . ?
C13 C14 H14 119.1 . . ?
C15 C14 C13 121.8(4) . . ?
C15 C14 H14 119.1 . . ?
C41 C40 H40 119.1 . . ?
C39 C40 C41 121.8(4) . . ?
C39 C40 H40 119.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C37 C38 H38 120.2 . . ?
C37 C38 C39 119.6(4) . . ?
C39 C38 H38 120.2 . . ?
C19 N4A H4A 117.3 . . ?
C19 N4A C20A 125.3(11) . . ?
C20A N4A H4A 117.3 . . ?
N7 C44 H44A 110.0 . . ?
N7 C44 H44B 110.0 . . ?
N7 C44 C20 108.4(4) . . ?
H44A C44 H44B 108.4 . . ?
C20 C44 H44A 110.0 . . ?
C20 C44 H44B 110.0 . . ?
C17 C16 H16 120.1 . . ?
C17 C16 C15 119.8(4) . . ?
C15 C16 H16 120.1 . . ?
N5 C27 S2 125.9(4) . . ?
N5 C27 N6 110.3(4) . . ?
N6 C27 S2 123.8(4) . . ?
C51 C50 H50 119.7 . . ?
C49 C50 C51 120.6(4) . . ?
C49 C50 H50 119.7 . . ?
N1 C9 C10 107.8(4) . . ?
N1 C9 H9A 110.1 . . ?
N1 C9 H9B 110.1 . . ?
C10 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
H9A C9 H9B 108.5 . . ?
C40 C39 C38 120.4(4) . . ?
C40 C39 H39 119.8 . . ?
C38 C39 H39 119.8 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C14 C15 C16 120.2(4) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N11 C61 S5 122.8(4) . . ?
N12B C61 S5 126.2(9) . . ?
N12B C61 N11 111.0(9) . . ?
N12A C61 S5 126.3(5) . . ?
N12A C61 N11 110.9(5) . . ?
N3 C19 S1 125.7(4) . . ?
N3 C19 N4B 111.3(6) . . ?
N4A C19 S1 122.7(7) . . ?
N4A C19 N3 111.2(7) . . ?
N4B C19 S1 122.7(6) . . ?
C56 C55 N10 118.0(5) . . ?
C60 C55 N10 119.2(5) . . ?
C60 C55 C56 122.7(5) . . ?
C29 C28 N6 117.0(5) . . ?
C29 C28 C33 120.1(5) . . ?
C33 C28 N6 122.8(5) . . ?
N9 C54 S4 124.6(4) . . ?
N9 C54 N10 111.4(4) . . ?
N10 C54 S4 124.0(4) . . ?
C63A C62A C67A 118.0(7) . . ?
C63A C62A N12A 115.4(9) . . ?
C67A C62A N12A 126.4(9) . . ?
S6 C68 H68A 109.5 . . ?
S6 C68 H68B 109.5 . . ?
S6 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C62A C63A H63A 119.5 . . ?
C64A C63A C62A 121.0(8) . . ?
C64A C63A H63A 119.5 . . ?
C60 C59 H59 118.8 . . ?
C58 C59 H59 118.8 . . ?
C58 C59 C60 122.4(5) . . ?
C55 C56 H56 120.2 . . ?
C55 C56 C57 119.6(5) . . ?
C57 C56 H56 120.2 . . ?
C55 C60 C59 117.4(5) . . ?
C55 C60 H60 121.3 . . ?
C59 C60 H60 121.3 . . ?
S6 C69 H69A 109.5 . . ?
S6 C69 H69B 109.5 . . ?
S6 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
S3 C34 H34A 109.5 . . ?
S3 C34 H34B 109.5 . . ?
S3 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C28 C29 H29 119.7 . . ?
C30 C29 C28 120.6(6) . . ?
C30 C29 H29 119.7 . . ?
C59 C58 H58 120.6 . . ?
C59 C58 C57 118.8(6) . . ?
C57 C58 H58 120.6 . . ?
C56 C57 H57 120.5 . . ?
C58 C57 C56 119.0(6) . . ?
C58 C57 H57 120.5 . . ?
C28 C33 H33 120.9 . . ?
C28 C33 C32 118.2(6) . . ?
C32 C33 H33 120.9 . . ?
C33 C32 H32 119.4 . . ?
C31 C32 C33 121.3(7) . . ?
C31 C32 H32 119.4 . . ?
C63A C64A H64A 119.5 . . ?
C65A C64A C63A 121.0(11) . . ?
C65A C64A H64A 119.5 . . ?
C66B C65B H65B 119.3 . . ?
C66B C65B C64B 121.3(19) . . ?
C64B C65B H65B 119.3 . . ?
C29 C30 H30 120.0 . . ?
C29 C30 C31 120.0(7) . . ?
C31 C30 H30 120.0 . . ?
C32 C31 C30 119.9(6) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C21A C20A N4A 117.6(12) . . ?
C25A C20A N4A 121.3(12) . . ?
C25A C20A C21A 121.1(10) . . ?
C66B C67B H67B 120.2 . . ?
C62B C67B H67B 120.2 . . ?
C62B C67B C66B 119.7(16) . . ?
S3 C35 H35A 109.5 . . ?
S3 C35 H35B 109.5 . . ?
S3 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C21A C22A H22A 120.7 . . ?
C21A C22A C23A 118.6(12) . . ?
C23A C22A H22A 120.7 . . ?
C65B C66B H66B 120.4 . . ?
C67B C66B C65B 119.2(16) . . ?
C67B C66B H66B 120.4 . . ?
C20A C21A H21A 120.6 . . ?
C22A C21A C20A 118.8(12) . . ?
C22A C21A H21A 120.6 . . ?
C20A C25A H25A 121.5 . . ?
C20A C25A C24A 117.1(12) . . ?
C24A C25A H25A 121.5 . . ?
C25A C24A H24A 117.9 . . ?
C23A C24A C25A 124.2(12) . . ?
C23A C24A H24A 117.9 . . ?
C22A C23A H23A 120.0 . . ?
C24A C23A C22A 120.1(11) . . ?
C24A C23A H23A 120.0 . . ?
C24B C23B H23B 119.7 . . ?
C24B C23B C22B 120.7(10) . . ?
C22B C23B H23B 119.7 . . ?
C23B C24B H24B 118.6 . . ?
C23B C24B C25B 122.8(12) . . ?
C25B C24B H24B 118.6 . . ?
C24B C25B H25B 121.1 . . ?
C20B C25B C24B 117.8(12) . . ?
C20B C25B H25B 121.1 . . ?
C25B C20B C21B 121.1(10) . . ?
C25B C20B N4B 123.8(12) . . ?
C21B C20B N4B 115.0(12) . . ?
C20B C21B H21B 120.2 . . ?
C22B C21B C20B 119.7(12) . . ?
C22B C21B H21B 120.2 . . ?
C23B C22B H22B 121.1 . . ?
C21B C22B C23B 117.7(12) . . ?
C21B C22B H22B 121.1 . . ?
C19 N4B C20B 126.2(10) . . ?
C19 N4B H4B 116.9 . . ?
C20B N4B H4B 116.9 . . ?
C65B C64B H64B 122.3 . . ?
C63B C64B C65B 115.4(18) . . ?
C63B C64B H64B 122.3 . . ?
C64B C63B H63B 118.7 . . ?
C64B C63B C62B 122.7(17) . . ?
C62B C63B H63B 118.7 . . ?
C67B C62B N12B 125(2) . . ?
C67B C62B C63B 120.7(15) . . ?
C63B C62B N12B 114(2) . . ?
C64A C65A H65A 120.2 . . ?
C64A C65A C66A 119.6(11) . . ?
C66A C65A H65A 120.2 . . ?
C65A C66A H66A 119.8 . . ?
C67A C66A C65A 120.5(8) . . ?
C67A C66A H66A 119.8 . . ?
C62A C67A H67A 120.2 . . ?
C66A C67A C62A 119.6(8) . . ?
C66A C67A H67A 120.2 . . ?
C61 N12A C62A 132.0(8) . . ?
C61 N12A H12E 114.0 . . ?
C62A N12A H12E 114.0 . . ?
N8 C20 C44 108.8(4) . . ?
N8 C20 H20A 109.9 . . ?
N8 C20 H20B 109.9 . . ?
C44 C20 H20A 109.9 . . ?
C44 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O3 0.88 2.13 2.971(5) 158.6 .
N5 H5 O3 0.88 2.37 3.157(5) 149.0 .
N11 H11 O6 0.88 2.49 3.277(5) 149.4 .
N9 H9 O6 0.88 2.11 2.984(5) 172.5 .
N6 H6 O3 0.88 1.91 2.785(5) 173.1 .
N12B H12D O6 0.88 1.95 2.83(2) 176.0 .
N10 H10 O6 0.88 2.48 3.278(5) 150.5 .
N4A H4A O3 0.88 2.17 3.006(15) 157.5 .
N4B H4B O3 0.88 2.20 3.022(13) 155.0 .
N12A H12E O6 0.88 1.99 2.835(9) 161.5 .

_smtbx_masks_special_details     
;
A solvent mask was calculated and 102 electrons were 
found in a volume of 357Å³ in 1 void per unit cell. 
This is consistent with the presence of 
0.6[C2H6SO] per Asymmetric Unit 
which account for 101 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 1.000 357.4 102.0 '2.4 C2H6SO'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DMSO/methyl tert-butyl ether'
