# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_s2a
_database_code_depnum_ccdc_archive 'CCDC 2288764'
loop_
_audit_author_name
_audit_author_address
'Yohei Haketa'
;Ritsumeikan University
Japan
;
_audit_update_record             
;
2024-04-11 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;

_vrf_PLAT971_s2a                 
;
PROBLEM: 
Check Calcd Resid. Dens. 1.02A From Br2 1.61 eA-3
Check Calcd Resid. Dens. 1.39A From C2 1.59 eA-3
Check Calcd Resid. Dens. 1.48A From C17 1.55 eA-3

RESPONSE: The residual electron density around Br2, C2, and C17 
could not be assigned with reasonable atoms. 
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H16 Br2 N2 O3'
_chemical_formula_sum            'C18 H16 Br2 N2 O3'
_chemical_formula_weight         468.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 0.0022 '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'
Br Br -1.0373 3.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0085 0.0044 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0146 0.0081 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.3326(2)
_cell_length_b                   12.8054(3)
_cell_length_c                   32.7329(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3492.67(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    32477
_cell_measurement_theta_min      3.128
_cell_measurement_theta_max      29.211

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_absorpt_coefficient_mu    6.459
_shelx_estimated_absorpt_T_min   0.079
_shelx_estimated_absorpt_T_max   0.247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.81032
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'DECTRIS EIGER X 1M'
_diffrn_measurement_method       'Shutterless ω scans'
_diffrn_detector_area_resol_mean 13.33
_diffrn_reflns_number            32477
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         3.128
_diffrn_reflns_theta_max         29.211
_diffrn_reflns_theta_full        29.091
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             3101
_reflns_number_gt                3050
_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       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalMaker X (CrystalMaker Software Ltd.)'
_computing_publication_material  
'Yadokari-XG (K. Wakita, Yadokari-XG, Software for Crystal Structure Analyses, 2001)'
_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)+(0.0424P)²+20.7615P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3101
_refine_ls_number_parameters     229
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1234
_refine_ls_wR_factor_gt          0.1231
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.121
_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
C1 C 0.5448(5) 0.9632(3) 0.35441(13) 0.0177(8) Uani 1 1 d . . . . .
C2 C 0.5874(5) 0.9056(3) 0.32065(14) 0.0205(9) Uani 1 1 d . . . . .
H2 H 0.6400 0.9299 0.2967 0.025 Uiso 1 1 calc R U . . .
C3 C 0.5362(5) 0.8028(3) 0.32911(13) 0.0195(9) Uani 1 1 d . . . . .
H3 H 0.5506 0.7442 0.3117 0.023 Uiso 1 1 calc R U . . .
C4 C 0.4616(5) 0.8014(3) 0.36690(13) 0.0167(8) Uani 1 1 d . . . . .
C5 C 0.3889(5) 0.7170(3) 0.38868(12) 0.0153(8) Uani 1 1 d . . . . .
C6 C 0.3851(5) 0.6145(3) 0.36723(13) 0.0152(8) Uani 1 1 d . . . . .
C7 C 0.3185(5) 0.6073(3) 0.32843(13) 0.0150(8) Uani 1 1 d . . . . .
H7 H 0.2718 0.6670 0.3160 0.018 Uiso 1 1 calc R U . . .
C8 C 0.3209(5) 0.5116(3) 0.30787(12) 0.0149(8) Uani 1 1 d . . . . .
C9 C 0.1704(6) 0.5796(4) 0.25226(14) 0.0224(9) Uani 1 1 d . . . . .
H9 H 0.0759 0.5914 0.2695 0.034 Uiso 1 1 calc R U . . .
H9A H 0.1360 0.5606 0.2246 0.034 Uiso 1 1 calc R U . . .
H9B H 0.2350 0.6435 0.2511 0.034 Uiso 1 1 calc R U . . .
C10 C 0.3905(5) 0.4239(3) 0.32581(13) 0.0156(8) Uani 1 1 d . . . . .
C11 C 0.5386(6) 0.3137(3) 0.28354(14) 0.0231(9) Uani 1 1 d . . . . .
H11 H 0.5560 0.3710 0.2642 0.035 Uiso 1 1 calc R U . . .
H11A H 0.5331 0.2474 0.2687 0.035 Uiso 1 1 calc R U . . .
H11B H 0.6276 0.3114 0.3031 0.035 Uiso 1 1 calc R U . . .
C12 C 0.4570(5) 0.4313(3) 0.36485(12) 0.0155(8) Uani 1 1 d . . . . .
C13 C 0.6063(6) 0.3495(3) 0.41780(14) 0.0247(10) Uani 1 1 d . . . . .
H13 H 0.6961 0.3985 0.4155 0.037 Uiso 1 1 calc R U . . .
H13A H 0.6471 0.2804 0.4254 0.037 Uiso 1 1 calc R U . . .
H13B H 0.5316 0.3741 0.4388 0.037 Uiso 1 1 calc R U . . .
C14 C 0.4545(5) 0.5270(3) 0.38561(13) 0.0165(8) Uani 1 1 d . . . . .
H14 H 0.5000 0.5324 0.4121 0.020 Uiso 1 1 calc R U . . .
C15 C 0.3251(5) 0.7269(3) 0.42740(13) 0.0199(9) Uani 1 1 d . . . . .
C16 C 0.2387(6) 0.6508(4) 0.45123(14) 0.0227(9) Uani 1 1 d . . . . .
H16 H 0.2172 0.5806 0.4437 0.027 Uiso 1 1 calc R U . . .
C17 C 0.1939(6) 0.6981(4) 0.48632(14) 0.0258(10) Uani 1 1 d . . . . .
H17 H 0.1349 0.6690 0.5084 0.031 Uiso 1 1 calc R U . . .
C18 C 0.2559(6) 0.8024(4) 0.48263(13) 0.0240(10) Uani 1 1 d . . . . .
N1 N 0.4693(4) 0.9027(3) 0.38197(11) 0.0161(7) Uani 1 1 d . . . . .
H1 H 0.4311 0.9238 0.4056 0.019 Uiso 1 1 calc R U . . .
N2 N 0.3323(5) 0.8218(3) 0.44907(11) 0.0220(8) Uani 1 1 d . . . . .
O1 O 0.2641(4) 0.4971(2) 0.26907(8) 0.0184(6) Uani 1 1 d . . . . .
O2 O 0.3912(3) 0.3305(2) 0.30504(9) 0.0171(6) Uani 1 1 d . . . . .
O3 O 0.5250(4) 0.3428(2) 0.37969(9) 0.0198(6) Uani 1 1 d . . . . .
Br1 Br 0.57823(6) 1.10499(3) 0.36394(2) 0.02361(18) Uani 1 1 d . . . . .
Br2 Br 0.23085(8) 0.90666(4) 0.52248(2) 0.0366(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.345(6) . ?
C1 C2 1.375(6) . ?
C1 Br1 1.863(4) . ?
C2 C3 1.411(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(6) . ?
C3 H3 0.9500 . ?
C4 N1 1.389(5) . ?
C4 C5 1.430(6) . ?
C5 C15 1.380(6) . ?
C5 C6 1.489(5) . ?
C6 C7 1.389(6) . ?
C6 C14 1.397(6) . ?
C7 C8 1.399(6) . ?
C7 H7 0.9500 . ?
C8 O1 1.368(5) . ?
C8 C10 1.394(6) . ?
C9 O1 1.424(5) . ?
C9 H9 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 O2 1.376(5) . ?
C10 C12 1.396(6) . ?
C11 O2 1.431(5) . ?
C11 H11 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 O3 1.357(5) . ?
C12 C14 1.401(6) . ?
C13 O3 1.422(5) . ?
C13 H13 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 H14 0.9500 . ?
C15 N2 1.409(6) . ?
C15 C16 1.440(6) . ?
C16 C17 1.351(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.438(7) . ?
C17 H17 0.9500 . ?
C18 N2 1.294(6) . ?
C18 Br2 1.878(4) . ?
N1 H1 0.8800 . ?

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
N1 C1 C2 110.5(4) . . ?
N1 C1 Br1 121.3(3) . . ?
C2 C1 Br1 128.2(3) . . ?
C1 C2 C3 105.3(4) . . ?
C1 C2 H2 127.3 . . ?
C3 C2 H2 127.3 . . ?
C4 C3 C2 108.9(4) . . ?
C4 C3 H3 125.6 . . ?
C2 C3 H3 125.6 . . ?
C3 C4 N1 106.5(4) . . ?
C3 C4 C5 130.2(4) . . ?
N1 C4 C5 123.3(4) . . ?
C15 C5 C4 123.5(4) . . ?
C15 C5 C6 120.4(4) . . ?
C4 C5 C6 116.1(4) . . ?
C7 C6 C14 120.4(4) . . ?
C7 C6 C5 119.8(4) . . ?
C14 C6 C5 119.7(4) . . ?
C6 C7 C8 119.5(4) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
O1 C8 C10 115.2(4) . . ?
O1 C8 C7 124.1(4) . . ?
C10 C8 C7 120.6(4) . . ?
O1 C9 H9 109.5 . . ?
O1 C9 H9A 109.5 . . ?
H9 C9 H9A 109.5 . . ?
O1 C9 H9B 109.5 . . ?
H9 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O2 C10 C8 119.6(4) . . ?
O2 C10 C12 120.6(4) . . ?
C8 C10 C12 119.8(4) . . ?
O2 C11 H11 109.5 . . ?
O2 C11 H11A 109.5 . . ?
H11 C11 H11A 109.5 . . ?
O2 C11 H11B 109.5 . . ?
H11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O3 C12 C10 115.9(4) . . ?
O3 C12 C14 124.3(4) . . ?
C10 C12 C14 119.8(4) . . ?
O3 C13 H13 109.5 . . ?
O3 C13 H13A 109.5 . . ?
H13 C13 H13A 109.5 . . ?
O3 C13 H13B 109.5 . . ?
H13 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C6 C14 C12 119.9(4) . . ?
C6 C14 H14 120.0 . . ?
C12 C14 H14 120.0 . . ?
C5 C15 N2 121.7(4) . . ?
C5 C15 C16 128.9(4) . . ?
N2 C15 C16 109.4(4) . . ?
C17 C16 C15 107.2(4) . . ?
C17 C16 H16 126.4 . . ?
C15 C16 H16 126.4 . . ?
C16 C17 C18 104.2(4) . . ?
C16 C17 H17 127.9 . . ?
C18 C17 H17 127.9 . . ?
N2 C18 C17 115.3(4) . . ?
N2 C18 Br2 120.5(4) . . ?
C17 C18 Br2 124.2(3) . . ?
C1 N1 C4 108.7(3) . . ?
C1 N1 H1 125.6 . . ?
C4 N1 H1 125.6 . . ?
C18 N2 C15 103.9(4) . . ?
C8 O1 C9 116.6(3) . . ?
C10 O2 C11 112.1(3) . . ?
C12 O3 C13 117.5(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -1.2(5) . . . . ?
Br1 C1 C2 C3 179.4(3) . . . . ?
C1 C2 C3 C4 1.4(5) . . . . ?
C2 C3 C4 N1 -1.0(5) . . . . ?
C2 C3 C4 C5 179.4(4) . . . . ?
C3 C4 C5 C15 176.8(5) . . . . ?
N1 C4 C5 C15 -2.7(7) . . . . ?
C3 C4 C5 C6 -3.0(7) . . . . ?
N1 C4 C5 C6 177.5(4) . . . . ?
C15 C5 C6 C7 126.0(5) . . . . ?
C4 C5 C6 C7 -54.1(6) . . . . ?
C15 C5 C6 C14 -56.6(6) . . . . ?
C4 C5 C6 C14 123.3(4) . . . . ?
C14 C6 C7 C8 0.2(6) . . . . ?
C5 C6 C7 C8 177.6(4) . . . . ?
C6 C7 C8 O1 -177.5(4) . . . . ?
C6 C7 C8 C10 -0.6(6) . . . . ?
O1 C8 C10 O2 -2.9(6) . . . . ?
C7 C8 C10 O2 179.9(4) . . . . ?
O1 C8 C10 C12 177.9(4) . . . . ?
C7 C8 C10 C12 0.7(6) . . . . ?
O2 C10 C12 O3 2.0(6) . . . . ?
C8 C10 C12 O3 -178.8(4) . . . . ?
O2 C10 C12 C14 -179.7(4) . . . . ?
C8 C10 C12 C14 -0.5(6) . . . . ?
C7 C6 C14 C12 0.0(6) . . . . ?
C5 C6 C14 C12 -177.5(4) . . . . ?
O3 C12 C14 C6 178.3(4) . . . . ?
C10 C12 C14 C6 0.2(6) . . . . ?
C4 C5 C15 N2 -2.2(7) . . . . ?
C6 C5 C15 N2 177.6(4) . . . . ?
C4 C5 C15 C16 174.8(4) . . . . ?
C6 C5 C15 C16 -5.3(7) . . . . ?
C5 C15 C16 C17 -177.1(5) . . . . ?
N2 C15 C16 C17 0.2(5) . . . . ?
C15 C16 C17 C18 -0.2(5) . . . . ?
C16 C17 C18 N2 0.1(6) . . . . ?
C16 C17 C18 Br2 179.8(4) . . . . ?
C2 C1 N1 C4 0.6(5) . . . . ?
Br1 C1 N1 C4 -179.9(3) . . . . ?
C3 C4 N1 C1 0.3(5) . . . . ?
C5 C4 N1 C1 179.9(4) . . . . ?
C17 C18 N2 C15 0.0(5) . . . . ?
Br2 C18 N2 C15 -179.7(3) . . . . ?
C5 C15 N2 C18 177.5(4) . . . . ?
C16 C15 N2 C18 -0.1(5) . . . . ?
C10 C8 O1 C9 170.5(4) . . . . ?
C7 C8 O1 C9 -12.4(6) . . . . ?
C8 C10 O2 C11 96.0(5) . . . . ?
C12 C10 O2 C11 -84.8(5) . . . . ?
C10 C12 O3 C13 174.7(4) . . . . ?
C14 C12 O3 C13 -3.5(6) . . . . ?

_refine_diff_density_max         1.755
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.109

####################################################################### 
# 
# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 2288766'
loop_
_audit_author_name
_audit_author_address
'Yohei Haketa'
;Ritsumeikan University
Japan
;
_audit_update_record             
;
2024-04-11 deposited with the CCDC.	2024-04-16 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         'C36 H30 N4 Ni O6'
_chemical_formula_sum            'C36 H30 N4 Ni O6'
_chemical_formula_weight         673.35

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   19.513(8)
_cell_length_b                   3.9317(17)
_cell_length_c                   18.474(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.947(15)
_cell_angle_gamma                90
_cell_volume                     1406.9(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    5249
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      34.79
_exptl_crystal_description       plate

_exptl_crystal_colour            brown

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_F_000             700
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.750
_shelx_estimated_absorpt_T_min   0.942
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_process_details   
;
SADABS Sheldrick 1996
;


_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'

_diffrn_measurement_device_type  'Bruker D8 goniometer'

_diffrn_measurement_method       'omega scans'

_diffrn_detector_area_resol_mean 7.391

_diffrn_reflns_number            14567
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.340
_diffrn_reflns_theta_max         35.034
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.809
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             5039
_reflns_number_gt                3697
_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 Instrument Service V6.2.14 (Bruker AXS Inc., 2020)'

_computing_cell_refinement       'APEX3 v2019.11 (Bruker AXS Inc., 2019)'

_computing_data_reduction        'SAINT V8.40B (Bruker AXS Inc., 2013)'

_computing_structure_solution    'SHELXT (Sheldrick, 2013)'

_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'



_computing_molecular_graphics    'CrystalMaker X (CrystalMaker Software Ltd.)'

_diffrn_source_type              ?


_diffrn_radiation_monochromator  'Incoatec Helios multilayered confocal mirror'

_computing_publication_material  
'Yadokari-XG (K. Wakita, Yadokari-XG, Software for Crystal Structure Analyses, 2001)'
_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)+(0.0142P)²+4.7335P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5039
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0834
_refine_ls_wR_factor_ref         0.1758
_refine_ls_wR_factor_gt          0.1605
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.150
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.49136(14) 0.2662(8) 0.36455(17) 0.0137(5) Uani 1 1 d . . . . .
C2 C 0.44438(15) 0.1545(8) 0.30393(18) 0.0164(6) Uani 1 1 d . . . . .
H2 H 0.4563 0.0625 0.2596 0.020 Uiso 1 1 calc R U . . .
C3 C 0.37813(15) 0.2055(8) 0.32187(18) 0.0165(6) Uani 1 1 d . . . . .
H3 H 0.3364 0.1540 0.2919 0.020 Uiso 1 1 calc R U . . .
C4 C 0.38379(14) 0.3500(8) 0.39383(18) 0.0151(6) Uani 1 1 d . . . . .
C5 C 0.33495(14) 0.4473(8) 0.44192(17) 0.0147(6) Uani 1 1 d . . . . .
C6 C 0.35505(14) 0.5606(8) 0.51487(17) 0.0155(6) Uani 1 1 d . . . . .
C7 C 0.31842(15) 0.6943(8) 0.57091(18) 0.0158(6) Uani 1 1 d . . . . .
H7 H 0.2697 0.7181 0.5685 0.019 Uiso 1 1 calc R U . . .
C8 C 0.36672(15) 0.7840(8) 0.62988(18) 0.0168(6) Uani 1 1 d . . . . .
H8 H 0.3571 0.8788 0.6749 0.020 Uiso 1 1 calc R U . . .
C9 C 0.43289(15) 0.7063(8) 0.60965(18) 0.0159(6) Uani 1 1 d . . . . .
C10 C 0.26034(14) 0.4369(7) 0.41296(17) 0.0133(5) Uani 1 1 d . . . . .
C11 C 0.23966(14) 0.5625(7) 0.34309(17) 0.0151(6) Uani 1 1 d . . . . .
H11 H 0.2728 0.6601 0.3156 0.018 Uiso 1 1 calc R U . . .
C12 C 0.17023(15) 0.5456(8) 0.31318(17) 0.0162(6) Uani 1 1 d . . . . .
C13 C 0.19415(18) 0.8053(9) 0.2035(2) 0.0231(7) Uani 1 1 d . . . . .
H13 H 0.2168 0.9971 0.2306 0.035 Uiso 1 1 calc R U . . .
H13A H 0.1702 0.8869 0.1571 0.035 Uiso 1 1 calc R U . . .
H13B H 0.2289 0.6364 0.1941 0.035 Uiso 1 1 calc R U . . .
C14 C 0.12070(15) 0.4039(8) 0.35318(18) 0.0170(6) Uani 1 1 d . . . . .
C15 C 0.00180(16) 0.5718(9) 0.3441(2) 0.0256(8) Uani 1 1 d . . . . .
H15 H 0.0017 0.5446 0.3968 0.038 Uiso 1 1 calc R U . . .
H15A H -0.0433 0.5046 0.3189 0.038 Uiso 1 1 calc R U . . .
H15B H 0.0109 0.8102 0.3330 0.038 Uiso 1 1 calc R U . . .
C16 C 0.14143(15) 0.2875(8) 0.42353(19) 0.0176(6) Uani 1 1 d . . . . .
C17 C 0.10756(17) 0.0123(10) 0.5282(2) 0.0244(7) Uani 1 1 d . . . . .
H17 H 0.1403 -0.1737 0.5242 0.037 Uiso 1 1 calc R U . . .
H17A H 0.0662 -0.0766 0.5468 0.037 Uiso 1 1 calc R U . . .
H17B H 0.1290 0.1855 0.5617 0.037 Uiso 1 1 calc R U . . .
C18 C 0.21094(15) 0.3053(8) 0.45387(18) 0.0155(6) Uani 1 1 d . . . . .
H18 H 0.2243 0.2277 0.5022 0.019 Uiso 1 1 calc R U . . .
N1 N 0.45377(13) 0.3780(8) 0.41510(15) 0.0172(5) Uani 1 1 d . . . . .
N2 N 0.42367(13) 0.5717(7) 0.54240(15) 0.0182(6) Uani 1 1 d . . . . .
O1 O 0.14555(11) 0.6536(7) 0.24527(14) 0.0223(5) Uani 1 1 d . . . . .
O2 O 0.05461(11) 0.3610(7) 0.31989(14) 0.0251(6) Uani 1 1 d . . . . .
O3 O 0.08913(11) 0.1585(7) 0.45888(14) 0.0227(5) Uani 1 1 d . . . . .
Ni1 Ni 0.5000 0.5000 0.5000 0.01667(15) Uani 1 2 d S . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.330(4) . ?
C1 C2 1.428(4) . ?
C1 C9 1.501(4) 3_666 ?
C2 C3 1.388(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.438(5) . ?
C3 H3 0.9500 . ?
C4 N1 1.379(4) . ?
C4 C5 1.432(4) . ?
C5 C6 1.429(4) . ?
C5 C10 1.490(4) . ?
C6 N2 1.374(4) . ?
C6 C7 1.427(4) . ?
C7 C8 1.397(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.420(4) . ?
C8 H8 0.9500 . ?
C9 N2 1.342(4) . ?
C9 C1 1.501(4) 3_666 ?
C10 C18 1.395(4) . ?
C10 C11 1.395(4) . ?
C11 C12 1.401(4) . ?
C11 H11 0.9500 . ?
C12 O1 1.357(4) . ?
C12 C14 1.401(5) . ?
C13 O1 1.424(4) . ?
C13 H13 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 O2 1.370(3) . ?
C14 C16 1.391(5) . ?
C15 O2 1.435(4) . ?
C15 H15 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 O3 1.373(4) . ?
C16 C18 1.405(4) . ?
C17 O3 1.410(4) . ?
C17 H17 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 H18 0.9500 . ?
N1 Ni1 1.778(3) . ?
N2 Ni1 1.787(3) . ?
Ni1 N1 1.778(3) 3_666 ?
Ni1 N2 1.787(3) 3_666 ?

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
N1 C1 C2 107.2(3) . . ?
N1 C1 C9 111.0(3) . 3_666 ?
C2 C1 C9 141.7(3) . 3_666 ?
C3 C2 C1 107.3(3) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
C2 C3 C4 108.0(3) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 H3 126.0 . . ?
N1 C4 C5 120.8(3) . . ?
N1 C4 C3 104.9(3) . . ?
C5 C4 C3 134.2(3) . . ?
C6 C5 C4 122.8(3) . . ?
C6 C5 C10 119.5(3) . . ?
C4 C5 C10 117.7(3) . . ?
N2 C6 C7 105.7(3) . . ?
N2 C6 C5 120.2(3) . . ?
C7 C6 C5 134.0(3) . . ?
C8 C7 C6 108.0(3) . . ?
C8 C7 H7 126.0 . . ?
C6 C7 H7 126.0 . . ?
C7 C8 C9 106.8(3) . . ?
C7 C8 H8 126.6 . . ?
C9 C8 H8 126.6 . . ?
N2 C9 C8 107.7(3) . . ?
N2 C9 C1 109.8(3) . 3_666 ?
C8 C9 C1 142.4(3) . 3_666 ?
C18 C10 C11 119.4(3) . . ?
C18 C10 C5 121.7(3) . . ?
C11 C10 C5 118.9(3) . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
O1 C12 C14 115.0(3) . . ?
O1 C12 C11 124.6(3) . . ?
C14 C12 C11 120.4(3) . . ?
O1 C13 H13 109.5 . . ?
O1 C13 H13A 109.5 . . ?
H13 C13 H13A 109.5 . . ?
O1 C13 H13B 109.5 . . ?
H13 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O2 C14 C16 122.0(3) . . ?
O2 C14 C12 118.9(3) . . ?
C16 C14 C12 118.8(3) . . ?
O2 C15 H15 109.5 . . ?
O2 C15 H15A 109.5 . . ?
H15 C15 H15A 109.5 . . ?
O2 C15 H15B 109.5 . . ?
H15 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C16 C14 114.6(3) . . ?
O3 C16 C18 124.4(3) . . ?
C14 C16 C18 120.9(3) . . ?
O3 C17 H17 109.5 . . ?
O3 C17 H17A 109.5 . . ?
H17 C17 H17A 109.5 . . ?
O3 C17 H17B 109.5 . . ?
H17 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C10 C18 C16 120.0(3) . . ?
C10 C18 H18 120.0 . . ?
C16 C18 H18 120.0 . . ?
C1 N1 C4 112.6(3) . . ?
C1 N1 Ni1 116.4(2) . . ?
C4 N1 Ni1 130.7(2) . . ?
C9 N2 C6 111.7(3) . . ?
C9 N2 Ni1 116.3(2) . . ?
C6 N2 Ni1 131.2(2) . . ?
C12 O1 C13 116.6(2) . . ?
C14 O2 C15 117.5(3) . . ?
C16 O3 C17 117.4(2) . . ?
N1 Ni1 N1 180.0 3_666 . ?
N1 Ni1 N2 93.92(12) 3_666 3_666 ?
N1 Ni1 N2 86.08(12) . 3_666 ?
N1 Ni1 N2 86.08(12) 3_666 . ?
N1 Ni1 N2 93.92(12) . . ?
N2 Ni1 N2 180.0 3_666 . ?

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
N1 C1 C2 C3 -0.3(4) . . . . ?
C9 C1 C2 C3 178.3(4) 3_666 . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
C2 C3 C4 N1 0.1(4) . . . . ?
C2 C3 C4 C5 -177.8(3) . . . . ?
N1 C4 C5 C6 -3.3(5) . . . . ?
C3 C4 C5 C6 174.3(3) . . . . ?
N1 C4 C5 C10 175.1(3) . . . . ?
C3 C4 C5 C10 -7.3(5) . . . . ?
C4 C5 C6 N2 -1.7(5) . . . . ?
C10 C5 C6 N2 180.0(3) . . . . ?
C4 C5 C6 C7 174.3(3) . . . . ?
C10 C5 C6 C7 -4.1(5) . . . . ?
N2 C6 C7 C8 0.6(4) . . . . ?
C5 C6 C7 C8 -175.8(3) . . . . ?
C6 C7 C8 C9 0.3(4) . . . . ?
C7 C8 C9 N2 -1.0(4) . . . . ?
C7 C8 C9 C1 175.6(4) . . . 3_666 ?
C6 C5 C10 C18 -44.8(4) . . . . ?
C4 C5 C10 C18 136.8(3) . . . . ?
C6 C5 C10 C11 135.1(3) . . . . ?
C4 C5 C10 C11 -43.3(4) . . . . ?
C18 C10 C11 C12 -2.3(4) . . . . ?
C5 C10 C11 C12 177.7(3) . . . . ?
C10 C11 C12 O1 -178.4(3) . . . . ?
C10 C11 C12 C14 0.3(5) . . . . ?
O1 C12 C14 O2 5.1(4) . . . . ?
C11 C12 C14 O2 -173.7(3) . . . . ?
O1 C12 C14 C16 -179.8(3) . . . . ?
C11 C12 C14 C16 1.4(5) . . . . ?
O2 C14 C16 O3 -6.1(5) . . . . ?
C12 C14 C16 O3 178.9(3) . . . . ?
O2 C14 C16 C18 173.8(3) . . . . ?
C12 C14 C16 C18 -1.1(5) . . . . ?
C11 C10 C18 C16 2.6(4) . . . . ?
C5 C10 C18 C16 -177.5(3) . . . . ?
O3 C16 C18 C10 179.1(3) . . . . ?
C14 C16 C18 C10 -0.9(5) . . . . ?
C2 C1 N1 C4 0.3(4) . . . . ?
C9 C1 N1 C4 -178.7(3) 3_666 . . . ?
C2 C1 N1 Ni1 174.9(2) . . . . ?
C9 C1 N1 Ni1 -4.1(4) 3_666 . . . ?
C5 C4 N1 C1 178.0(3) . . . . ?
C3 C4 N1 C1 -0.2(4) . . . . ?
C5 C4 N1 Ni1 4.4(5) . . . . ?
C3 C4 N1 Ni1 -173.9(2) . . . . ?
C8 C9 N2 C6 1.5(4) . . . . ?
C1 C9 N2 C6 -176.4(3) 3_666 . . . ?
C8 C9 N2 Ni1 172.6(2) . . . . ?
C1 C9 N2 Ni1 -5.3(4) 3_666 . . . ?
C7 C6 N2 C9 -1.3(4) . . . . ?
C5 C6 N2 C9 175.7(3) . . . . ?
C7 C6 N2 Ni1 -170.7(2) . . . . ?
C5 C6 N2 Ni1 6.3(5) . . . . ?
C14 C12 O1 C13 178.8(3) . . . . ?
C11 C12 O1 C13 -2.4(5) . . . . ?
C16 C14 O2 C15 74.0(4) . . . . ?
C12 C14 O2 C15 -111.0(4) . . . . ?
C14 C16 O3 C17 175.2(3) . . . . ?
C18 C16 O3 C17 -4.8(5) . . . . ?
C1 N1 Ni1 N2 5.8(3) . . . 3_666 ?
C4 N1 Ni1 N2 179.2(3) . . . 3_666 ?
C1 N1 Ni1 N2 -174.2(3) . . . . ?
C4 N1 Ni1 N2 -0.8(3) . . . . ?
C9 N2 Ni1 N1 6.3(3) . . . 3_666 ?
C6 N2 Ni1 N1 175.3(3) . . . 3_666 ?
C9 N2 Ni1 N1 -173.7(3) . . . . ?
C6 N2 Ni1 N1 -4.7(3) . . . . ?

_refine_diff_density_max         0.959
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.131

####################################################################### 
# 
# 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_s3a
_database_code_depnum_ccdc_archive 'CCDC 2288765'
loop_
_audit_author_name
_audit_author_address
'Yohei Haketa'
;Ritsumeikan University
Japan
;
_audit_update_record             
;
2024-04-11 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 Br4 N4 Ni O6'
_chemical_formula_sum            'C36 H30 Br4 N4 Ni O6'
_chemical_formula_weight         992.99

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'
Br Br -0.6763 1.2805 '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'

_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                   8.98210(10)
_cell_length_b                   31.6135(3)
_cell_length_c                   12.7862(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.9760(10)
_cell_angle_gamma                90
_cell_volume                     3630.19(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    22881
_cell_measurement_theta_min      3.729
_cell_measurement_theta_max      73.522

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_F_000             1960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    6.361
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.33154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.8140
_diffrn_reflns_number            22881
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.729
_diffrn_reflns_theta_max         73.522
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             7103
_reflns_number_gt                6946
_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       'CrysAlis PRO (Rigaku OD)'
_computing_cell_refinement       'CrysAlis PRO (Rigaku OD)'
_computing_data_reduction        'CrysAlis PRO (Rigaku OD)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'CrystalMaker X (CrystalMaker Software Ltd.)'
_computing_publication_material  
'Yadokari-XG (K. Wakita, Yadokari-XG, Software for Crystal Structure Analyses, 2001)'
_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)+(0.0479P)²+7.5342P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7103
_refine_ls_number_parameters     486
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0946
_refine_ls_wR_factor_gt          0.0941
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_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 0.55513(6) 0.69038(2) 0.45596(4) 0.02419(12) Uani 1 1 d . . . . .
Br1 Br 0.83508(4) 0.64307(2) 0.59364(3) 0.03019(9) Uani 1 1 d . . . . .
Br2 Br 0.20666(4) 0.70564(2) 0.32698(3) 0.03984(11) Uani 1 1 d . . . . .
Br3 Br 0.43839(4) 0.71768(2) 0.70190(3) 0.02896(9) Uani 1 1 d . . . . .
Br4 Br 0.75639(4) 0.68915(2) 0.22682(3) 0.03772(10) Uani 1 1 d . . . . .
N1 N 0.7297(3) 0.71963(8) 0.5138(2) 0.0235(5) Uani 1 1 d . . . . .
N2 N 0.4651(3) 0.74436(8) 0.4114(2) 0.0250(5) Uani 1 1 d . . . . .
N3 N 0.4062(3) 0.65977(8) 0.53767(19) 0.0221(5) Uani 1 1 d . . . . .
N4 N 0.5440(3) 0.64692(8) 0.3464(2) 0.0247(5) Uani 1 1 d . . . . .
O1 O 1.0122(3) 0.91245(7) 0.4183(2) 0.0362(5) Uani 1 1 d . . . . .
O4 O -0.1285(2) 0.52312(7) 0.36500(18) 0.0301(5) Uani 1 1 d . . . . .
O5 O 0.0234(3) 0.45198(7) 0.32589(17) 0.0300(5) Uani 1 1 d . . . . .
O6 O 0.3184(3) 0.45009(7) 0.33077(18) 0.0322(5) Uani 1 1 d . . . . .
C1 C 0.8409(3) 0.70158(10) 0.5669(3) 0.0273(6) Uani 1 1 d . . . . .
C2 C 0.9491(4) 0.73031(10) 0.6032(3) 0.0324(7) Uani 1 1 d . . . . .
H2 H 1.038354 0.724156 0.641167 0.039 Uiso 1 1 calc R U . . .
C3 C 0.8976(4) 0.76923(10) 0.5719(3) 0.0295(7) Uani 1 1 d . . . . .
H3 H 0.944339 0.795688 0.585226 0.035 Uiso 1 1 calc R U . . .
C4 C 0.7611(3) 0.76272(9) 0.5157(2) 0.0237(6) Uani 1 1 d . . . . .
C5 C 0.6651(3) 0.79333(9) 0.4722(2) 0.0237(6) Uani 1 1 d . . . . .
C6 C 0.5278(3) 0.78485(9) 0.4215(2) 0.0250(6) Uani 1 1 d . . . . .
C7 C 0.4308(4) 0.81447(10) 0.3725(3) 0.0293(7) Uani 1 1 d . . . . .
H7 H 0.446572 0.844110 0.367409 0.035 Uiso 1 1 calc R U . . .
C8 C 0.3107(4) 0.79274(11) 0.3340(3) 0.0337(7) Uani 1 1 d . . . . .
H8 H 0.227229 0.804086 0.297014 0.040 Uiso 1 1 calc R U . . .
C9 C 0.3356(3) 0.75035(10) 0.3601(3) 0.0293(6) Uani 1 1 d . . . . .
C10 C 0.7086(3) 0.83892(9) 0.4825(2) 0.0239(6) Uani 1 1 d . . . . .
C11 C 0.8427(3) 0.85306(9) 0.4426(2) 0.0240(6) Uani 1 1 d . . . . .
H11 H 0.907123 0.833877 0.408355 0.029 Uiso 1 1 calc R U . . .
C12 C 0.8822(4) 0.89550(10) 0.4529(2) 0.0282(6) Uani 1 1 d . . . . .
C13 C 0.7887(4) 0.92348(11) 0.5039(3) 0.0424(9) Uani 1 1 d . . . . .
C14 C 0.6533(4) 0.90906(11) 0.5431(3) 0.0362(8) Uani 1 1 d . . . . .
C15 C 0.6138(4) 0.86699(10) 0.5329(2) 0.0266(6) Uani 1 1 d . . . . .
H15 H 0.522276 0.857204 0.560135 0.032 Uiso 1 1 calc R U . . .
C16 C 1.1168(4) 0.88379(12) 0.3741(3) 0.0402(8) Uani 1 1 d . . . . .
H16A H 1.205101 0.899454 0.352183 0.060 Uiso 1 1 calc R U . . .
H16B H 1.145924 0.862584 0.426489 0.060 Uiso 1 1 calc R U . . .
H16C H 1.071154 0.869659 0.313339 0.060 Uiso 1 1 calc R U . . .
O2A O 0.8503(4) 0.96221(12) 0.5379(3) 0.0287(13) Uani 0.654(10) 1 d . . P A 1
C17A C 0.7929(6) 0.9957(2) 0.4754(4) 0.0350(15) Uani 0.654(10) 1 d . . P A 1
H17A H 0.835969 1.022561 0.499350 0.053 Uiso 0.654(10) 1 calc R U P A 1
H17B H 0.818726 0.990908 0.402223 0.053 Uiso 0.654(10) 1 calc R U P A 1
H17C H 0.684363 0.996757 0.481545 0.053 Uiso 0.654(10) 1 calc R U P A 1
O2B O 0.7958(7) 0.9683(2) 0.4740(5) 0.023(2) Uani 0.346(10) 1 d . . P A 2
C17B C 0.8398(11) 0.9902(3) 0.5680(7) 0.029(3) Uani 0.346(10) 1 d . . P A 2
H17D H 0.846811 1.020586 0.553780 0.044 Uiso 0.346(10) 1 calc R U P A 2
H17E H 0.765696 0.985282 0.622090 0.044 Uiso 0.346(10) 1 calc R U P A 2
H17F H 0.936931 0.979644 0.592429 0.044 Uiso 0.346(10) 1 calc R U P A 2
O3A O 0.5787(5) 0.93731(13) 0.6015(4) 0.0303(10) Uani 0.686(9) 1 d . . P B 3
C18A C 0.4371(7) 0.92342(19) 0.6393(5) 0.0332(13) Uani 0.686(9) 1 d . . P B 3
H18A H 0.392127 0.946043 0.680616 0.050 Uiso 0.686(9) 1 calc R U P B 3
H18B H 0.371264 0.916461 0.579862 0.050 Uiso 0.686(9) 1 calc R U P B 3
H18C H 0.451218 0.898292 0.683256 0.050 Uiso 0.686(9) 1 calc R U P B 3
O3B O 0.5424(12) 0.9434(3) 0.5629(9) 0.0303(10) Uani 0.314(9) 1 d . . P B 4
C18B C 0.4017(17) 0.9306(5) 0.5998(11) 0.0332(13) Uani 0.314(9) 1 d . . P B 4
H18D H 0.338784 0.955561 0.609872 0.050 Uiso 0.314(9) 1 calc R U P B 4
H18E H 0.354104 0.911691 0.548541 0.050 Uiso 0.314(9) 1 calc R U P B 4
H18F H 0.414793 0.915711 0.666525 0.050 Uiso 0.314(9) 1 calc R U P B 4
C19 C 0.3576(3) 0.67078(9) 0.6317(2) 0.0239(6) Uani 1 1 d . . . . .
C20 C 0.2473(3) 0.64351(10) 0.6700(2) 0.0263(6) Uani 1 1 d . . . . .
H20 H 0.196833 0.645585 0.734490 0.032 Uiso 1 1 calc R U . . .
C21 C 0.2286(3) 0.61309(10) 0.5934(2) 0.0244(6) Uani 1 1 d . . . . .
H21 H 0.162749 0.589603 0.595694 0.029 Uiso 1 1 calc R U . . .
C22 C 0.3257(3) 0.62332(9) 0.5108(2) 0.0216(6) Uani 1 1 d . . . . .
C23 C 0.3455(3) 0.60127(9) 0.4173(2) 0.0229(6) Uani 1 1 d . . . . .
C24 C 0.4456(3) 0.61300(10) 0.3387(2) 0.0248(6) Uani 1 1 d . . . . .
C25 C 0.4593(4) 0.59406(12) 0.2383(2) 0.0332(7) Uani 1 1 d . . . . .
H25 H 0.404257 0.570529 0.212320 0.040 Uiso 1 1 calc R U . . .
C26 C 0.5667(4) 0.61612(13) 0.1860(3) 0.0359(8) Uani 1 1 d . . . . .
H26 H 0.601378 0.610944 0.117413 0.043 Uiso 1 1 calc R U . . .
C27 C 0.6141(3) 0.64763(10) 0.2548(3) 0.0282(6) Uani 1 1 d . . . . .
C28 C 0.2570(3) 0.56212(10) 0.3974(2) 0.0231(6) Uani 1 1 d . . . . .
C29 C 0.1014(3) 0.56284(10) 0.3966(2) 0.0238(6) Uani 1 1 d . . . . .
H29 H 0.049604 0.588114 0.413009 0.029 Uiso 1 1 calc R U . . .
C30 C 0.0231(3) 0.52607(10) 0.3715(2) 0.0247(6) Uani 1 1 d . . . . .
C31 C 0.0992(3) 0.48888(10) 0.3482(2) 0.0250(6) Uani 1 1 d . . . . .
C32 C 0.2544(3) 0.48811(10) 0.3525(2) 0.0252(6) Uani 1 1 d . . . . .
C33 C 0.3333(3) 0.52471(10) 0.3771(2) 0.0242(6) Uani 1 1 d . . . . .
H33 H 0.439085 0.524226 0.380033 0.029 Uiso 1 1 calc R U . . .
C34 C -0.2109(3) 0.55848(12) 0.4017(3) 0.0349(7) Uani 1 1 d . . . . .
H34A H -0.317724 0.552814 0.393237 0.052 Uiso 1 1 calc R U . . .
H34B H -0.186999 0.563284 0.475823 0.052 Uiso 1 1 calc R U . . .
H34C H -0.184782 0.583675 0.361302 0.052 Uiso 1 1 calc R U . . .
C35 C -0.0212(4) 0.44829(11) 0.2193(3) 0.0386(8) Uani 1 1 d . . . . .
H35A H -0.074250 0.421508 0.208683 0.058 Uiso 1 1 calc R U . . .
H35B H -0.087071 0.471893 0.200470 0.058 Uiso 1 1 calc R U . . .
H35C H 0.066972 0.448919 0.175258 0.058 Uiso 1 1 calc R U . . .
C36 C 0.4777(4) 0.44805(13) 0.3359(3) 0.0432(9) Uani 1 1 d . . . . .
H36A H 0.510300 0.419316 0.318816 0.065 Uiso 1 1 calc R U . . .
H36B H 0.519397 0.468053 0.285693 0.065 Uiso 1 1 calc R U . . .
H36C H 0.512422 0.455372 0.406681 0.065 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 N1 1.955(3) . ?
Ni1 N4 1.964(3) . ?
Ni1 N3 1.966(3) . ?
Ni1 N2 1.969(3) . ?
Br1 C1 1.882(3) . ?
Br2 C9 1.872(3) . ?
Br3 C19 1.873(3) . ?
Br4 C27 1.871(3) . ?
N1 C1 1.327(4) . ?
N1 C4 1.391(4) . ?
N2 C9 1.338(4) . ?
N2 C6 1.404(4) . ?
N3 C19 1.332(4) . ?
N3 C22 1.400(4) . ?
N4 C27 1.339(4) . ?
N4 C24 1.392(4) . ?
O1 C12 1.366(4) . ?
O1 C16 1.428(4) . ?
O4 C30 1.366(3) . ?
O4 C34 1.425(4) . ?
O5 C31 1.378(4) . ?
O5 C35 1.418(4) . ?
O6 C32 1.363(4) . ?
O6 C36 1.433(4) . ?
C1 C2 1.404(4) . ?
C2 C3 1.372(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.426(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.404(4) . ?
C5 C6 1.409(4) . ?
C5 C10 1.499(4) . ?
C6 C7 1.418(4) . ?
C7 C8 1.363(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.398(5) . ?
C8 H8 0.9500 . ?
C10 C11 1.390(4) . ?
C10 C15 1.395(4) . ?
C11 C12 1.393(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(5) . ?
C13 C14 1.400(5) . ?
C13 O2A 1.409(5) . ?
C13 O2B 1.470(8) . ?
C14 O3A 1.350(5) . ?
C14 C15 1.382(4) . ?
C14 O3B 1.499(11) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O2A C17A 1.418(7) . ?
C17A H17A 0.9800 . ?
C17A H17B 0.9800 . ?
C17A H17C 0.9800 . ?
O2B C17B 1.436(12) . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 0.9800 . ?
O3A C18A 1.437(7) . ?
C18A H18A 0.9800 . ?
C18A H18B 0.9800 . ?
C18A H18C 0.9800 . ?
O3B C18B 1.416(19) . ?
C18B H18D 0.9800 . ?
C18B H18E 0.9800 . ?
C18B H18F 0.9800 . ?
C19 C20 1.407(4) . ?
C20 C21 1.381(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.419(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.398(4) . ?
C23 C24 1.409(4) . ?
C23 C28 1.491(4) . ?
C24 C25 1.424(4) . ?
C25 C26 1.374(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.390(5) . ?
C26 H26 0.9500 . ?
C28 C33 1.394(4) . ?
C28 C29 1.398(4) . ?
C29 C30 1.393(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.394(4) . ?
C31 C32 1.394(4) . ?
C32 C33 1.390(4) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?

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
N1 Ni1 N4 129.18(11) . . ?
N1 Ni1 N3 125.46(11) . . ?
N4 Ni1 N3 90.46(10) . . ?
N1 Ni1 N2 91.30(11) . . ?
N4 Ni1 N2 112.59(11) . . ?
N3 Ni1 N2 107.50(11) . . ?
C1 N1 C4 105.2(2) . . ?
C1 N1 Ni1 125.6(2) . . ?
C4 N1 Ni1 129.1(2) . . ?
C9 N2 C6 105.1(3) . . ?
C9 N2 Ni1 127.9(2) . . ?
C6 N2 Ni1 127.0(2) . . ?
C19 N3 C22 105.1(2) . . ?
C19 N3 Ni1 126.0(2) . . ?
C22 N3 Ni1 128.9(2) . . ?
C27 N4 C24 105.0(3) . . ?
C27 N4 Ni1 126.4(2) . . ?
C24 N4 Ni1 127.8(2) . . ?
C12 O1 C16 116.8(3) . . ?
C30 O4 C34 116.7(2) . . ?
C31 O5 C35 113.5(2) . . ?
C32 O6 C36 117.1(3) . . ?
N1 C1 C2 113.7(3) . . ?
N1 C1 Br1 119.5(2) . . ?
C2 C1 Br1 126.7(2) . . ?
C3 C2 C1 104.8(3) . . ?
C3 C2 H2 127.6 . . ?
C1 C2 H2 127.6 . . ?
C2 C3 C4 107.5(3) . . ?
C2 C3 H3 126.2 . . ?
C4 C3 H3 126.2 . . ?
N1 C4 C5 123.1(3) . . ?
N1 C4 C3 108.8(3) . . ?
C5 C4 C3 128.1(3) . . ?
C4 C5 C6 125.3(3) . . ?
C4 C5 C10 118.1(3) . . ?
C6 C5 C10 116.6(3) . . ?
N2 C6 C5 124.2(3) . . ?
N2 C6 C7 108.6(3) . . ?
C5 C6 C7 127.2(3) . . ?
C8 C7 C6 107.7(3) . . ?
C8 C7 H7 126.2 . . ?
C6 C7 H7 126.2 . . ?
C7 C8 C9 105.9(3) . . ?
C7 C8 H8 127.0 . . ?
C9 C8 H8 127.0 . . ?
N2 C9 C8 112.7(3) . . ?
N2 C9 Br2 122.2(2) . . ?
C8 C9 Br2 125.0(2) . . ?
C11 C10 C15 120.3(3) . . ?
C11 C10 C5 120.2(3) . . ?
C15 C10 C5 119.5(3) . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
O1 C12 C13 115.4(3) . . ?
O1 C12 C11 124.4(3) . . ?
C13 C12 C11 120.2(3) . . ?
C12 C13 C14 119.8(3) . . ?
C12 C13 O2A 117.4(3) . . ?
C14 C13 O2A 120.7(3) . . ?
C12 C13 O2B 117.6(4) . . ?
C14 C13 O2B 116.7(4) . . ?
O3A C14 C15 124.0(3) . . ?
O3A C14 C13 115.2(3) . . ?
C15 C14 C13 120.2(3) . . ?
C15 C14 O3B 122.9(5) . . ?
C13 C14 O3B 114.1(5) . . ?
C14 C15 C10 119.9(3) . . ?
C14 C15 H15 120.1 . . ?
C10 C15 H15 120.1 . . ?
O1 C16 H16A 109.5 . . ?
O1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 O2A C17A 109.7(4) . . ?
O2A C17A H17A 109.5 . . ?
O2A C17A H17B 109.5 . . ?
H17A C17A H17B 109.5 . . ?
O2A C17A H17C 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
C17B O2B C13 105.0(6) . . ?
O2B C17B H17D 109.5 . . ?
O2B C17B H17E 109.5 . . ?
H17D C17B H17E 109.5 . . ?
O2B C17B H17F 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
C14 O3A C18A 115.8(4) . . ?
O3A C18A H18A 109.5 . . ?
O3A C18A H18B 109.5 . . ?
H18A C18A H18B 109.5 . . ?
O3A C18A H18C 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C18B O3B C14 116.6(9) . . ?
O3B C18B H18D 109.5 . . ?
O3B C18B H18E 109.5 . . ?
H18D C18B H18E 109.5 . . ?
O3B C18B H18F 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
N3 C19 C20 113.4(3) . . ?
N3 C19 Br3 120.6(2) . . ?
C20 C19 Br3 125.9(2) . . ?
C21 C20 C19 104.9(3) . . ?
C21 C20 H20 127.5 . . ?
C19 C20 H20 127.5 . . ?
C20 C21 C22 107.5(3) . . ?
C20 C21 H21 126.3 . . ?
C22 C21 H21 126.3 . . ?
C23 C22 N3 123.2(3) . . ?
C23 C22 C21 127.7(3) . . ?
N3 C22 C21 109.0(2) . . ?
C22 C23 C24 124.8(3) . . ?
C22 C23 C28 119.0(3) . . ?
C24 C23 C28 116.2(3) . . ?
N4 C24 C23 124.4(3) . . ?
N4 C24 C25 108.8(3) . . ?
C23 C24 C25 126.7(3) . . ?
C26 C25 C24 107.3(3) . . ?
C26 C25 H25 126.3 . . ?
C24 C25 H25 126.3 . . ?
C25 C26 C27 105.4(3) . . ?
C25 C26 H26 127.3 . . ?
C27 C26 H26 127.3 . . ?
N4 C27 C26 113.4(3) . . ?
N4 C27 Br4 120.8(2) . . ?
C26 C27 Br4 125.8(2) . . ?
C33 C28 C29 120.5(3) . . ?
C33 C28 C23 118.3(3) . . ?
C29 C28 C23 121.2(3) . . ?
C30 C29 C28 119.3(3) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
O4 C30 C29 124.7(3) . . ?
O4 C30 C31 114.9(3) . . ?
C29 C30 C31 120.4(3) . . ?
O5 C31 C30 121.1(3) . . ?
O5 C31 C32 118.9(3) . . ?
C30 C31 C32 119.9(3) . . ?
O6 C32 C33 124.4(3) . . ?
O6 C32 C31 115.6(3) . . ?
C33 C32 C31 120.0(3) . . ?
C32 C33 C28 119.8(3) . . ?
C32 C33 H33 120.1 . . ?
C28 C33 H33 120.1 . . ?
O4 C34 H34A 109.5 . . ?
O4 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
O4 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O5 C35 H35A 109.5 . . ?
O5 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O5 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O6 C36 H36A 109.5 . . ?
O6 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O6 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 N1 C1 C2 -1.3(4) . . . . ?
Ni1 N1 C1 C2 -177.5(2) . . . . ?
C4 N1 C1 Br1 174.9(2) . . . . ?
Ni1 N1 C1 Br1 -1.2(4) . . . . ?
N1 C1 C2 C3 1.6(4) . . . . ?
Br1 C1 C2 C3 -174.3(3) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
C1 N1 C4 C5 -176.6(3) . . . . ?
Ni1 N1 C4 C5 -0.6(4) . . . . ?
C1 N1 C4 C3 0.5(3) . . . . ?
Ni1 N1 C4 C3 176.5(2) . . . . ?
C2 C3 C4 N1 0.4(4) . . . . ?
C2 C3 C4 C5 177.3(3) . . . . ?
N1 C4 C5 C6 -0.4(5) . . . . ?
C3 C4 C5 C6 -176.9(3) . . . . ?
N1 C4 C5 C10 177.8(3) . . . . ?
C3 C4 C5 C10 1.3(5) . . . . ?
C9 N2 C6 C5 179.2(3) . . . . ?
Ni1 N2 C6 C5 -4.1(4) . . . . ?
C9 N2 C6 C7 -1.0(4) . . . . ?
Ni1 N2 C6 C7 175.8(2) . . . . ?
C4 C5 C6 N2 2.9(5) . . . . ?
C10 C5 C6 N2 -175.4(3) . . . . ?
C4 C5 C6 C7 -177.0(3) . . . . ?
C10 C5 C6 C7 4.8(5) . . . . ?
N2 C6 C7 C8 0.5(4) . . . . ?
C5 C6 C7 C8 -179.7(3) . . . . ?
C6 C7 C8 C9 0.2(4) . . . . ?
C6 N2 C9 C8 1.1(4) . . . . ?
Ni1 N2 C9 C8 -175.6(2) . . . . ?
C6 N2 C9 Br2 -179.7(2) . . . . ?
Ni1 N2 C9 Br2 3.6(4) . . . . ?
C7 C8 C9 N2 -0.9(4) . . . . ?
C7 C8 C9 Br2 -180.0(3) . . . . ?
C4 C5 C10 C11 58.4(4) . . . . ?
C6 C5 C10 C11 -123.2(3) . . . . ?
C4 C5 C10 C15 -121.3(3) . . . . ?
C6 C5 C10 C15 57.1(4) . . . . ?
C15 C10 C11 C12 -0.1(4) . . . . ?
C5 C10 C11 C12 -179.8(3) . . . . ?
C16 O1 C12 C13 174.4(3) . . . . ?
C16 O1 C12 C11 -3.7(5) . . . . ?
C10 C11 C12 O1 178.7(3) . . . . ?
C10 C11 C12 C13 0.7(5) . . . . ?
O1 C12 C13 C14 -179.5(4) . . . . ?
C11 C12 C13 C14 -1.2(6) . . . . ?
O1 C12 C13 O2A -15.7(5) . . . . ?
C11 C12 C13 O2A 162.6(3) . . . . ?
O1 C12 C13 O2B 28.7(6) . . . . ?
C11 C12 C13 O2B -153.1(4) . . . . ?
C12 C13 C14 O3A 172.7(4) . . . . ?
C12 C13 C14 C15 1.2(6) . . . . ?
O2A C13 C14 C15 -162.0(4) . . . . ?
O2B C13 C14 C15 153.3(5) . . . . ?
C12 C13 C14 O3B -160.5(6) . . . . ?
O3A C14 C15 C10 -171.3(4) . . . . ?
C13 C14 C15 C10 -0.6(6) . . . . ?
O3B C14 C15 C10 159.4(6) . . . . ?
C11 C10 C15 C14 0.1(5) . . . . ?
C5 C10 C15 C14 179.8(3) . . . . ?
C12 C13 O2A C17A 109.0(5) . . . . ?
C14 C13 O2A C17A -87.4(5) . . . . ?
C12 C13 O2B C17B -119.3(6) . . . . ?
C14 C13 O2B C17B 87.9(7) . . . . ?
C15 C14 O3A C18A -10.9(7) . . . . ?
C13 C14 O3A C18A 178.0(4) . . . . ?
C15 C14 O3B C18B 17.2(12) . . . . ?
C13 C14 O3B C18B 178.3(8) . . . . ?
C22 N3 C19 C20 -0.1(3) . . . . ?
Ni1 N3 C19 C20 178.2(2) . . . . ?
C22 N3 C19 Br3 178.3(2) . . . . ?
Ni1 N3 C19 Br3 -3.4(3) . . . . ?
N3 C19 C20 C21 0.7(4) . . . . ?
Br3 C19 C20 C21 -177.6(2) . . . . ?
C19 C20 C21 C22 -1.0(3) . . . . ?
C19 N3 C22 C23 -179.1(3) . . . . ?
Ni1 N3 C22 C23 2.7(4) . . . . ?
C19 N3 C22 C21 -0.6(3) . . . . ?
Ni1 N3 C22 C21 -178.8(2) . . . . ?
C20 C21 C22 C23 179.5(3) . . . . ?
C20 C21 C22 N3 1.1(3) . . . . ?
N3 C22 C23 C24 -1.0(5) . . . . ?
C21 C22 C23 C24 -179.2(3) . . . . ?
N3 C22 C23 C28 178.4(3) . . . . ?
C21 C22 C23 C28 0.2(5) . . . . ?
C27 N4 C24 C23 -178.2(3) . . . . ?
Ni1 N4 C24 C23 -7.7(4) . . . . ?
C27 N4 C24 C25 -0.7(3) . . . . ?
Ni1 N4 C24 C25 169.7(2) . . . . ?
C22 C23 C24 N4 3.6(5) . . . . ?
C28 C23 C24 N4 -175.8(3) . . . . ?
C22 C23 C24 C25 -173.4(3) . . . . ?
C28 C23 C24 C25 7.2(5) . . . . ?
N4 C24 C25 C26 0.7(4) . . . . ?
C23 C24 C25 C26 178.1(3) . . . . ?
C24 C25 C26 C27 -0.4(4) . . . . ?
C24 N4 C27 C26 0.5(4) . . . . ?
Ni1 N4 C27 C26 -170.2(2) . . . . ?
C24 N4 C27 Br4 178.7(2) . . . . ?
Ni1 N4 C27 Br4 8.1(4) . . . . ?
C25 C26 C27 N4 0.0(4) . . . . ?
C25 C26 C27 Br4 -178.2(3) . . . . ?
C22 C23 C28 C33 -123.4(3) . . . . ?
C24 C23 C28 C33 56.1(4) . . . . ?
C22 C23 C28 C29 58.1(4) . . . . ?
C24 C23 C28 C29 -122.4(3) . . . . ?
C33 C28 C29 C30 -2.3(4) . . . . ?
C23 C28 C29 C30 176.2(3) . . . . ?
C34 O4 C30 C29 -9.7(5) . . . . ?
C34 O4 C30 C31 171.7(3) . . . . ?
C28 C29 C30 O4 -178.0(3) . . . . ?
C28 C29 C30 C31 0.5(5) . . . . ?
C35 O5 C31 C30 85.4(4) . . . . ?
C35 O5 C31 C32 -97.9(4) . . . . ?
O4 C30 C31 O5 -3.1(4) . . . . ?
C29 C30 C31 O5 178.3(3) . . . . ?
O4 C30 C31 C32 -179.8(3) . . . . ?
C29 C30 C31 C32 1.6(5) . . . . ?
C36 O6 C32 C33 1.3(5) . . . . ?
C36 O6 C32 C31 -179.2(3) . . . . ?
O5 C31 C32 O6 1.8(4) . . . . ?
C30 C31 C32 O6 178.6(3) . . . . ?
O5 C31 C32 C33 -178.6(3) . . . . ?
C30 C31 C32 C33 -1.9(5) . . . . ?
O6 C32 C33 C28 179.6(3) . . . . ?
C31 C32 C33 C28 0.0(4) . . . . ?
C29 C28 C33 C32 2.1(4) . . . . ?
C23 C28 C33 C32 -176.5(3) . . . . ?

_refine_diff_density_max         1.893
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_1b
_database_code_depnum_ccdc_archive 'CCDC 2288767'
loop_
_audit_author_name
_audit_author_address
'Yohei Haketa'
;Ritsumeikan University
Japan
;
_audit_update_record             
;
2024-04-11 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H66 N4 Ni O6, 0.67(C H4 O)'
_chemical_formula_sum            'C54.67 H68.67 N4 Ni O6.67'
_chemical_formula_weight         947.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0045 0.0022 '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 0.0085 0.0044 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3081 1.4105 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0146 0.0081 '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                   13.0251(4)
_cell_length_b                   13.0786(4)
_cell_length_c                   22.9482(9)
_cell_angle_alpha                95.536(2)
_cell_angle_beta                 105.627(2)
_cell_angle_gamma                95.810(3)
_cell_volume                     3714.0(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    39849
_cell_measurement_theta_min      1.801
_cell_measurement_theta_max      29.238

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_F_000             1518
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.632
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.626
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.81082
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_diffrn_radiation_monochromator  'Si(111) Channel Cut'
_diffrn_measurement_device_type  'DECTRIS EIGER X 1M'
_diffrn_measurement_method       'Shutterless ω scans'
_diffrn_detector_area_resol_mean 13.33
_diffrn_reflns_number            39849
_diffrn_reflns_av_unetI/netI     0.1424
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.801
_diffrn_reflns_theta_max         29.238
_diffrn_reflns_theta_full        29.110
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             13559
_reflns_number_gt                8925
_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       'Rapid Auto(Rigaku)'
_computing_cell_refinement       'Rapid Auto(Rigaku)'
_computing_data_reduction        'Rapid Auto(Rigaku)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'CrystalMaker X (CrystalMaker Software Ltd.)'
_computing_publication_material  
'Yadokari-XG (K. Wakita, Yadokari-XG, Software for Crystal Structure Analyses, 2001)'
_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)+(0.1373P)²+1.5882P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0091(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13559
_refine_ls_number_parameters     949
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1214
_refine_ls_R_factor_gt           0.0875
_refine_ls_wR_factor_ref         0.2634
_refine_ls_wR_factor_gt          0.2344
_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
C1 C 0.2077(4) 0.1298(4) 0.2576(2) 0.0454(12) Uani 1 1 d . . . . .
H1 H 0.2833 0.1288 0.2675 0.054 Uiso 1 1 calc R U . . .
C2 C 0.1472(4) 0.1254(4) 0.1968(2) 0.0478(12) Uani 1 1 d . . . . .
C3 C 0.3005(5) 0.0977(7) 0.1615(3) 0.090(2) Uani 1 1 d . . . . .
H3 H 0.3115 0.0334 0.1805 0.108 Uiso 1 1 calc R U . . .
H3A H 0.3476 0.1566 0.1896 0.108 Uiso 1 1 calc R U . . .
C4 C 0.3261(6) 0.0883(8) 0.0985(3) 0.107(3) Uani 1 1 d . . . . .
H4 H 0.3079 0.1505 0.0786 0.129 Uiso 1 1 calc R U . . .
H4A H 0.4042 0.0861 0.1054 0.129 Uiso 1 1 calc R U . . .
C5 C 0.2665(9) -0.0045(8) 0.0577(4) 0.125(3) Uani 1 1 d . . . . .
H5 H 0.1882 -0.0014 0.0491 0.150 Uiso 1 1 calc R U . . .
H5A H 0.2828 -0.0670 0.0777 0.150 Uiso 1 1 calc R U . . .
C6 C 0.2985(8) -0.0113(9) -0.0032(4) 0.155(4) Uani 1 1 d . . . . .
H6 H 0.2630 0.0380 -0.0287 0.232 Uiso 1 1 calc R U . . .
H6A H 0.2760 -0.0817 -0.0249 0.232 Uiso 1 1 calc R U . . .
H6B H 0.3767 0.0055 0.0057 0.232 Uiso 1 1 calc R U . . .
C7 C 0.0376(4) 0.1330(4) 0.1819(2) 0.0501(12) Uani 1 1 d . . . . .
C8 C -0.0023(7) 0.2022(6) 0.0864(3) 0.095(2) Uani 1 1 d . . . . .
H8 H -0.0578 0.1878 0.0464 0.114 Uiso 1 1 calc R U . . .
H8A H 0.0680 0.1951 0.0787 0.114 Uiso 1 1 calc R U . . .
C9 C -0.0003(5) 0.3126(6) 0.1116(3) 0.082(2) Uani 1 1 d . . . . .
H9 H 0.0579 0.3276 0.1504 0.098 Uiso 1 1 calc R U . . .
H9A H -0.0689 0.3182 0.1217 0.098 Uiso 1 1 calc R U . . .
C10 C 0.0153(7) 0.3974(7) 0.0730(4) 0.103(3) Uani 1 1 d . . . . .
H10 H 0.0804 0.3874 0.0598 0.124 Uiso 1 1 calc R U . . .
H10A H -0.0463 0.3851 0.0357 0.124 Uiso 1 1 calc R U . . .
C11 C 0.0256(7) 0.5007(7) 0.0962(4) 0.104(3) Uani 1 1 d . . . . .
H11 H -0.0431 0.5168 0.1021 0.157 Uiso 1 1 calc R U . . .
H11A H 0.0459 0.5442 0.0676 0.157 Uiso 1 1 calc R U . . .
H11B H 0.0813 0.5142 0.1355 0.157 Uiso 1 1 calc R U . . .
C12 C -0.0118(4) 0.1384(4) 0.2280(2) 0.0442(11) Uani 1 1 d . . . . .
C13 C -0.1825(4) 0.1123(4) 0.2505(2) 0.0462(12) Uani 1 1 d . . . . .
H13 H -0.1736 0.1684 0.2844 0.055 Uiso 1 1 calc R U . . .
H13A H -0.1584 0.0496 0.2680 0.055 Uiso 1 1 calc R U . . .
C14 C -0.2970(4) 0.0904(6) 0.2132(3) 0.0745(19) Uani 1 1 d . . . . .
H14 H -0.3161 0.1493 0.1903 0.089 Uiso 1 1 calc R U . . .
H14A H -0.3439 0.0830 0.2405 0.089 Uiso 1 1 calc R U . . .
C15 C -0.3178(6) -0.0169(6) 0.1649(3) 0.084(2) Uani 1 1 d . . . . .
H15 H -0.2700 -0.0086 0.1381 0.101 Uiso 1 1 calc R U . . .
H15A H -0.2969 -0.0748 0.1884 0.101 Uiso 1 1 calc R U . . .
C16 C -0.4243(7) -0.0439(7) 0.1279(4) 0.113(3) Uani 1 1 d . . . . .
H16 H -0.4712 -0.0617 0.1534 0.169 Uiso 1 1 calc R U . . .
H16A H -0.4279 -0.1037 0.0979 0.169 Uiso 1 1 calc R U . . .
H16B H -0.4479 0.0148 0.1068 0.169 Uiso 1 1 calc R U . . .
C17 C 0.0457(4) 0.1405(4) 0.2890(2) 0.0422(11) Uani 1 1 d . . . . .
H17 H 0.0101 0.1450 0.3200 0.051 Uiso 1 1 calc R U . . .
C18 C 0.1558(4) 0.1358(3) 0.3040(2) 0.0415(11) Uani 1 1 d . . . . .
C19 C 0.2202(4) 0.1380(3) 0.3681(2) 0.0407(11) Uani 1 1 d . . . . .
C20 C 0.1801(3) 0.0750(3) 0.4064(2) 0.0379(10) Uani 1 1 d . . . . .
C21 C 0.0842(4) 0.0013(3) 0.3973(2) 0.0394(11) Uani 1 1 d . . . . .
H21 H 0.0327 -0.0238 0.3593 0.047 Uiso 1 1 calc R U . . .
C22 C 0.0810(4) -0.0258(3) 0.4532(2) 0.0403(11) Uani 1 1 d . . . . .
H22 H 0.0266 -0.0723 0.4609 0.048 Uiso 1 1 calc R U . . .
C23 C 0.1744(3) 0.0287(3) 0.4978(2) 0.0385(11) Uani 1 1 d . . . . .
C24 C 0.2271(3) 0.0486(3) 0.5644(2) 0.0368(10) Uani 1 1 d . . . . .
C25 C 0.2149(4) 0.0248(4) 0.6209(2) 0.0418(11) Uani 1 1 d . . . . .
H25 H 0.1596 -0.0227 0.6268 0.050 Uiso 1 1 calc R U . . .
C26 C 0.2980(4) 0.0832(3) 0.6663(2) 0.0417(11) Uani 1 1 d . . . . .
H26 H 0.3098 0.0837 0.7090 0.050 Uiso 1 1 calc R U . . .
C27 C 0.3631(4) 0.1428(3) 0.6371(2) 0.0413(11) Uani 1 1 d . . . . .
C28 C 0.4569(4) 0.2208(3) 0.6590(2) 0.0411(11) Uani 1 1 d . . . . .
C29 C 0.5051(4) 0.2479(3) 0.7256(2) 0.0443(12) Uani 1 1 d . . . . .
C30 C 0.4413(4) 0.2691(4) 0.7646(2) 0.0471(12) Uani 1 1 d . . . . .
H30 H 0.3660 0.2688 0.7482 0.057 Uiso 1 1 calc R U . . .
C31 C 0.4880(4) 0.2904(4) 0.8264(2) 0.0552(14) Uani 1 1 d . . . . .
C32 C 0.3229(4) 0.3287(5) 0.8438(3) 0.0600(14) Uani 1 1 d . . . . .
H32 H 0.2813 0.2619 0.8220 0.072 Uiso 1 1 calc R U . . .
H32A H 0.3158 0.3804 0.8146 0.072 Uiso 1 1 calc R U . . .
C33 C 0.2807(5) 0.3648(5) 0.8962(3) 0.0727(17) Uani 1 1 d . . . . .
H33 H 0.3252 0.4302 0.9181 0.087 Uiso 1 1 calc R U . . .
H33A H 0.2064 0.3802 0.8796 0.087 Uiso 1 1 calc R U . . .
C34 C 0.2801(5) 0.2895(6) 0.9410(3) 0.082(2) Uani 1 1 d . . . . .
H34 H 0.3549 0.2776 0.9601 0.098 Uiso 1 1 calc R U . . .
H34A H 0.2393 0.2225 0.9191 0.098 Uiso 1 1 calc R U . . .
C35 C 0.2294(6) 0.3272(8) 0.9916(3) 0.115(3) Uani 1 1 d . . . . .
H35 H 0.2704 0.3927 1.0142 0.172 Uiso 1 1 calc R U . . .
H35A H 0.2309 0.2750 1.0197 0.172 Uiso 1 1 calc R U . . .
H35B H 0.1548 0.3377 0.9731 0.172 Uiso 1 1 calc R U . . .
C36 C 0.5971(5) 0.2842(6) 0.8516(3) 0.078(2) Uani 1 1 d . . . . .
C37 C 0.6797(9) 0.3723(9) 0.9461(8) 0.058(3) Uani 0.62(3) 1 d . . P A 1
H83 H 0.6256 0.4209 0.9373 0.070 Uiso 0.62(3) 1 calc R U P A 1
H84 H 0.7444 0.4002 0.9350 0.070 Uiso 0.62(3) 1 calc R U P A 1
C38 C 0.7081(8) 0.3541(8) 1.0135(4) 0.120(2) Uani 1 1 d . U . . .
H85 H 0.7584 0.3016 1.0189 0.144 Uiso 0.62(3) 1 calc R U P A 1
H86 H 0.7480 0.4195 1.0382 0.144 Uiso 0.62(3) 1 calc R U P A 1
H87 H 0.7779 0.3307 1.0326 0.144 Uiso 0.38(3) 1 calc R U P A 2
H88 H 0.7167 0.4290 1.0096 0.144 Uiso 0.38(3) 1 calc R U P A 2
C39 C 0.6245(8) 0.3218(8) 1.0389(4) 0.120(2) Uani 1 1 d . U . . .
H39 H 0.5844 0.2561 1.0147 0.144 Uiso 1 1 calc R U . . .
H39A H 0.5741 0.3742 1.0341 0.144 Uiso 1 1 calc R U . . .
C40 C 0.6571(10) 0.3057(10) 1.1033(5) 0.178(5) Uani 1 1 d . . . . .
H40 H 0.7065 0.2533 1.1089 0.268 Uiso 1 1 calc R U . . .
H40A H 0.5933 0.2819 1.1158 0.268 Uiso 1 1 calc R U . . .
H40B H 0.6932 0.3710 1.1284 0.268 Uiso 1 1 calc R U . . .
C41 C 0.6609(4) 0.2647(5) 0.8129(3) 0.0684(17) Uani 1 1 d . . . . .
C42 C 0.8353(5) 0.2201(7) 0.8044(3) 0.098(2) Uani 1 1 d . . . . .
H42 H 0.7978 0.1553 0.7780 0.118 Uiso 1 1 calc R U . . .
H42A H 0.8497 0.2719 0.7779 0.118 Uiso 1 1 calc R U . . .
C43 C 0.9363(5) 0.2005(8) 0.8456(4) 0.103(3) Uani 1 1 d . . . . .
H43 H 0.9214 0.1566 0.8760 0.123 Uiso 1 1 calc R U . . .
H43A H 0.9785 0.2668 0.8678 0.123 Uiso 1 1 calc R U . . .
C44 C 1.0060(7) 0.1407(8) 0.8047(6) 0.135(4) Uani 1 1 d . . . . .
H44 H 1.0716 0.1232 0.8333 0.162 Uiso 1 1 calc R U . . .
H44A H 0.9622 0.0746 0.7834 0.162 Uiso 1 1 calc R U . . .
C45 C 1.0375(7) 0.1959(8) 0.7608(5) 0.131(3) Uani 1 1 d . . . . .
H45 H 0.9733 0.2107 0.7307 0.196 Uiso 1 1 calc R U . . .
H45A H 1.0788 0.1540 0.7402 0.196 Uiso 1 1 calc R U . . .
H45B H 1.0821 0.2612 0.7811 0.196 Uiso 1 1 calc R U . . .
C46 C 0.6159(4) 0.2499(4) 0.7506(2) 0.0508(13) Uani 1 1 d . . . . .
H46 H 0.6605 0.2410 0.7243 0.061 Uiso 1 1 calc R U . . .
C47 C 0.5033(4) 0.2745(4) 0.6193(2) 0.0428(11) Uani 1 1 d . . . . .
C48 C 0.5807(4) 0.3674(4) 0.6300(2) 0.0451(12) Uani 1 1 d . . . . .
H48 H 0.6215 0.4030 0.6686 0.054 Uiso 1 1 calc R U . . .
C49 C 0.5842(4) 0.3942(3) 0.5741(2) 0.0440(12) Uani 1 1 d . . . . .
H49 H 0.6277 0.4518 0.5670 0.053 Uiso 1 1 calc R U . . .
C50 C 0.5101(3) 0.3193(3) 0.5283(2) 0.0395(11) Uani 1 1 d . . . . .
C51 C 0.4562(3) 0.3004(3) 0.4625(2) 0.0390(11) Uani 1 1 d . . . . .
C52 C 0.4461(4) 0.3507(4) 0.4093(2) 0.0424(11) Uani 1 1 d . . . . .
H52 H 0.4900 0.4108 0.4054 0.051 Uiso 1 1 calc R U . . .
C53 C 0.3605(4) 0.2952(4) 0.3644(2) 0.0427(11) Uani 1 1 d . . . . .
H53 H 0.3349 0.3103 0.3237 0.051 Uiso 1 1 calc R U . . .
N1 N 0.3164(3) 0.1183(3) 0.57549(17) 0.0370(9) Uani 1 1 d . . . . .
N2 N 0.2308(3) 0.0851(3) 0.46750(17) 0.0369(9) Uani 1 1 d . . . . .
N3 N 0.3797(3) 0.2171(3) 0.44850(18) 0.0387(9) Uani 1 1 d . . . . .
N4 N 0.4665(3) 0.2491(3) 0.55758(18) 0.0388(9) Uani 1 1 d . . . . .
Ni1 Ni 0.35458(4) 0.15989(4) 0.51191(3) 0.0389(2) Uani 1 1 d . . . . .
O1 O 0.4333(3) 0.3167(3) 0.86815(17) 0.0698(11) Uani 1 1 d . . . . .
O2 O 0.6368(6) 0.2709(8) 0.9140(5) 0.058(3) Uani 0.62(3) 1 d . . P A 1
O3 O 0.7681(4) 0.2588(5) 0.8412(2) 0.1050(18) Uani 1 1 d . . . . .
O4 O -0.1205(3) 0.1437(3) 0.20990(15) 0.0519(9) Uani 1 1 d . . . . .
O5 O -0.0231(3) 0.1248(3) 0.12260(16) 0.0635(10) Uani 1 1 d . . . . .
O6 O 0.1903(3) 0.1145(3) 0.14855(16) 0.0617(10) Uani 1 1 d . . . . .
C54 C 0.4003(3) -0.0405(3) 0.3803(2) 0.0375(10) Uani 1 1 d . . . . .
C55 C 0.4068(4) -0.0155(3) 0.3225(2) 0.0413(11) Uani 1 1 d . . . . .
H55 H 0.3589 -0.0443 0.2841 0.050 Uiso 1 1 calc R U . . .
C56 C 0.4956(3) 0.0585(3) 0.3324(2) 0.0390(11) Uani 1 1 d . . . . .
H56 H 0.5200 0.0882 0.3016 0.047 Uiso 1 1 calc R U . . .
C57 C 0.5441(3) 0.0828(3) 0.3961(2) 0.0372(10) Uani 1 1 d . . . . .
C58 C 0.6377(4) 0.1508(3) 0.4347(2) 0.0379(10) Uani 1 1 d . . . . .
C59 C 0.6708(3) 0.1554(3) 0.4986(2) 0.0386(11) Uani 1 1 d . . . . .
C60 C 0.7529(3) 0.2216(3) 0.5478(2) 0.0409(11) Uani 1 1 d . . . . .
H60 H 0.8027 0.2757 0.5425 0.049 Uiso 1 1 calc R U . . .
C61 C 0.7461(4) 0.1928(3) 0.6025(2) 0.0422(11) Uani 1 1 d . . . . .
H61 H 0.7897 0.2230 0.6418 0.051 Uiso 1 1 calc R U . . .
C62 C 0.6610(4) 0.1085(3) 0.5893(2) 0.0385(10) Uani 1 1 d . . . . .
C63 C 0.6986(3) 0.2206(3) 0.4045(2) 0.0371(10) Uani 1 1 d . . . . .
C64 C 0.8108(4) 0.2372(3) 0.4249(2) 0.0397(11) Uani 1 1 d . . . . .
H64 H 0.8479 0.2005 0.4561 0.048 Uiso 1 1 calc R U . . .
C65 C 0.8682(4) 0.3074(3) 0.3996(2) 0.0405(11) Uani 1 1 d . . . . .
C66 C 1.0368(3) 0.2832(4) 0.4676(2) 0.0429(11) Uani 1 1 d . . . . .
H66 H 1.0319 0.2075 0.4565 0.052 Uiso 1 1 calc R U . . .
H66A H 1.0065 0.2957 0.5024 0.052 Uiso 1 1 calc R U . . .
C67 C 1.1519(3) 0.3322(3) 0.4845(2) 0.0440(12) Uani 1 1 d . . . . .
H67 H 1.1794 0.3204 0.4485 0.053 Uiso 1 1 calc R U . . .
H67A H 1.1945 0.2966 0.5170 0.053 Uiso 1 1 calc R U . . .
C68 C 1.1710(4) 0.4479(3) 0.5064(2) 0.0453(12) Uani 1 1 d . . . . .
H68 H 1.1451 0.4861 0.4712 0.054 Uiso 1 1 calc R U . . .
H68A H 1.1292 0.4628 0.5357 0.054 Uiso 1 1 calc R U . . .
C69 C 1.2884(4) 0.4854(4) 0.5367(2) 0.0542(13) Uani 1 1 d . . . . .
H69 H 1.3124 0.4529 0.5739 0.081 Uiso 1 1 calc R U . . .
H69A H 1.2985 0.5609 0.5472 0.081 Uiso 1 1 calc R U . . .
H69B H 1.3305 0.4667 0.5087 0.081 Uiso 1 1 calc R U . . .
C70 C 0.8141(4) 0.3605(3) 0.3536(2) 0.0439(12) Uani 1 1 d . . . . .
C71 C 0.8985(4) 0.3966(4) 0.2771(2) 0.0523(13) Uani 1 1 d . . . . .
H71 H 0.8328 0.3710 0.2433 0.063 Uiso 1 1 calc R U . . .
H71A H 0.9412 0.3386 0.2858 0.063 Uiso 1 1 calc R U . . .
C72 C 0.9645(4) 0.4856(4) 0.2596(3) 0.0619(15) Uani 1 1 d . . . . .
H72 H 0.9795 0.4618 0.2209 0.074 Uiso 1 1 calc R U . . .
H72A H 0.9206 0.5431 0.2522 0.074 Uiso 1 1 calc R U . . .
C73 C 1.0701(4) 0.5270(4) 0.3068(3) 0.0649(16) Uani 1 1 d . . . . .
H73 H 1.0556 0.5515 0.3456 0.078 Uiso 1 1 calc R U . . .
H73A H 1.1048 0.5871 0.2928 0.078 Uiso 1 1 calc R U . . .
C74 C 1.1469(5) 0.4460(5) 0.3182(3) 0.0749(18) Uani 1 1 d . . . . .
H74 H 1.1191 0.3926 0.3392 0.112 Uiso 1 1 calc R U . . .
H74A H 1.2178 0.4793 0.3435 0.112 Uiso 1 1 calc R U . . .
H74B H 1.1533 0.4141 0.2791 0.112 Uiso 1 1 calc R U . . .
C75 C 0.7024(4) 0.3416(4) 0.3313(2) 0.0421(11) Uani 1 1 d . . . . .
C76 C 0.5445(4) 0.3748(5) 0.2582(3) 0.0648(16) Uani 1 1 d . . . . .
H76 H 0.5042 0.3865 0.2887 0.078 Uiso 1 1 calc R U . . .
H76A H 0.5259 0.3016 0.2394 0.078 Uiso 1 1 calc R U . . .
C77 C 0.5167(5) 0.4464(5) 0.2100(3) 0.081(2) Uani 1 1 d . . . . .
H77 H 0.5194 0.5172 0.2305 0.097 Uiso 1 1 calc R U . B 3
H77A H 0.5721 0.4486 0.1878 0.097 Uiso 1 1 calc R U . B 3
C78 C 0.4075(6) 0.4156(6) 0.1644(4) 0.075(3) Uani 0.847(15) 1 d . . P C 3
H91 H 0.4000 0.4597 0.1312 0.090 Uiso 0.847(15) 1 calc R U P C 3
H92 H 0.4020 0.3428 0.1462 0.090 Uiso 0.847(15) 1 calc R U P C 3
C79 C 0.3178(8) 0.4261(9) 0.1932(5) 0.089(3) Uani 0.847(15) 1 d . . P C 3
H93 H 0.3197 0.3763 0.2226 0.134 Uiso 0.847(15) 1 calc R U P C 3
H94 H 0.2487 0.4124 0.1616 0.134 Uiso 0.847(15) 1 calc R U P C 3
H95 H 0.3264 0.4966 0.2143 0.134 Uiso 0.847(15) 1 calc R U P C 3
O7 O 0.9783(2) 0.3292(2) 0.41644(14) 0.0434(8) Uani 1 1 d . . . . .
O8 O 0.8699(2) 0.4369(2) 0.33129(15) 0.0473(8) Uani 1 1 d . . . . .
O9 O 0.6574(2) 0.3982(3) 0.28656(16) 0.0512(9) Uani 1 1 d . . . . .
N5 N 0.6196(3) 0.0890(3) 0.52822(17) 0.0360(8) Uani 1 1 d . . . . .
N6 N 0.4834(3) 0.0200(3) 0.42260(17) 0.0381(9) Uani 1 1 d . . . . .
Ni2 Ni 0.5000 0.0000 0.5000 0.0380(3) Uani 1 2 d S . P . .
C80 C 0.8558(6) 0.6912(6) 0.3534(3) 0.082(2) Uani 1 1 d . . . . .
H80 H 0.8206 0.7295 0.3797 0.123 Uiso 1 1 calc R U . . .
H80A H 0.9003 0.7402 0.3377 0.123 Uiso 1 1 calc R U . . .
H80B H 0.9013 0.6457 0.3771 0.123 Uiso 1 1 calc R U . . .
O10 O 0.7794(4) 0.6328(3) 0.3058(2) 0.0873(14) Uani 1 1 d . . . . .
H10B H 0.7827 0.5696 0.3088 0.131 Uiso 1 1 calc R U . . .
C81 C 0.3166(4) 0.2103(3) 0.3899(2) 0.0395(11) Uani 1 1 d . . . . .
C82 C 0.6449(4) 0.2716(3) 0.3566(2) 0.0418(11) Uani 1 1 d . . . . .
H82 H 0.5688 0.2583 0.3412 0.050 Uiso 1 1 calc R U . . .
O11 O 0.6450(13) 0.3455(12) 0.9099(8) 0.070(6) Uani 0.38(3) 1 d . . P A 2
C83 C 0.635(2) 0.2803(19) 0.9513(15) 0.100(8) Uani 0.38(3) 1 d . . P A 2
H89 H 0.6659 0.2154 0.9443 0.120 Uiso 0.38(3) 1 calc R U P A 2
H90 H 0.5597 0.2636 0.9517 0.120 Uiso 0.38(3) 1 calc R U P A 2
C84 C 0.392(2) 0.462(3) 0.2085(16) 0.042(11) Uani 0.153(15) 1 d . . P C 4
H96 H 0.3832 0.4681 0.2503 0.050 Uiso 0.153(15) 1 calc R U P C 4
H97 H 0.3714 0.5250 0.1900 0.050 Uiso 0.153(15) 1 calc R U P C 4
C85 C 0.322(3) 0.362(4) 0.169(2) 0.074(16) Uani 0.153(15) 1 d . . P C 4
H98 H 0.3650 0.3254 0.1468 0.110 Uiso 0.153(15) 1 calc R U P C 4
H99 H 0.2597 0.3821 0.1389 0.110 Uiso 0.153(15) 1 calc R U P C 4
H100 H 0.2964 0.3170 0.1949 0.110 Uiso 0.153(15) 1 calc R U P C 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.398(7) . ?
C1 C18 1.407(6) . ?
C2 O6 1.372(5) . ?
C2 C7 1.392(7) . ?
C3 O6 1.429(7) . ?
C3 C4 1.564(9) . ?
C4 C5 1.467(12) . ?
C5 C6 1.560(10) . ?
C7 O5 1.365(6) . ?
C7 C12 1.379(7) . ?
C8 O5 1.421(8) . ?
C8 C9 1.497(10) . ?
C9 C10 1.516(9) . ?
C10 C11 1.383(10) . ?
C12 O4 1.376(5) . ?
C12 C17 1.393(7) . ?
C13 O4 1.449(5) . ?
C13 C14 1.490(7) . ?
C14 C15 1.654(10) . ?
C15 C16 1.406(9) . ?
C17 C18 1.390(6) . ?
C18 C19 1.480(7) . ?
C19 C20 1.424(6) . ?
C19 C81 1.432(6) . ?
C20 N2 1.366(6) . ?
C20 C21 1.452(6) . ?
C21 C22 1.373(6) . ?
C22 C23 1.431(6) . ?
C23 N2 1.354(5) . ?
C23 C24 1.482(6) . ?
C24 N1 1.353(5) . ?
C24 C25 1.408(6) . ?
C25 C26 1.382(6) . ?
C26 C27 1.431(6) . ?
C27 N1 1.371(6) . ?
C27 C28 1.451(6) . ?
C28 C47 1.422(6) . ?
C28 C29 1.479(7) . ?
C29 C46 1.399(7) . ?
C29 C30 1.402(6) . ?
C30 C31 1.374(7) . ?
C31 O1 1.376(6) . ?
C31 C36 1.397(8) . ?
C32 O1 1.427(6) . ?
C32 C33 1.507(7) . ?
C33 C34 1.491(9) . ?
C34 C35 1.548(9) . ?
C36 C41 1.393(8) . ?
C36 O2 1.418(12) . ?
C36 O11 1.437(19) . ?
C37 O2 1.43(2) . ?
C37 C38 1.539(17) . ?
C38 C39 1.414(11) . ?
C38 C83 1.64(3) . ?
C39 C40 1.468(12) . ?
C41 C46 1.378(7) . ?
C41 O3 1.386(7) . ?
C42 C43 1.462(9) . ?
C42 O3 1.463(8) . ?
C43 C44 1.666(12) . ?
C44 C45 1.418(12) . ?
C47 N4 1.362(6) . ?
C47 C48 1.454(6) . ?
C48 C49 1.373(7) . ?
C49 C50 1.435(6) . ?
C50 N4 1.355(5) . ?
C50 C51 1.468(7) . ?
C51 N3 1.351(5) . ?
C51 C52 1.424(6) . ?
C52 C53 1.380(6) . ?
C53 C81 1.442(6) . ?
N1 Ni1 1.778(3) . ?
N2 Ni1 1.788(4) . ?
N3 C81 1.364(6) . ?
N3 Ni1 1.789(4) . ?
N4 Ni1 1.784(4) . ?
C54 N6 1.361(5) . ?
C54 C55 1.417(6) . ?
C54 C62 1.481(6) 2_656 ?
C55 C56 1.384(6) . ?
C56 C57 1.417(6) . ?
C57 N6 1.376(5) . ?
C57 C58 1.452(6) . ?
C58 C59 1.406(6) . ?
C58 C63 1.487(6) . ?
C59 N5 1.380(5) . ?
C59 C60 1.463(6) . ?
C60 C61 1.368(7) . ?
C61 C62 1.430(6) . ?
C62 N5 1.347(6) . ?
C62 C54 1.481(6) 2_656 ?
C63 C64 1.397(6) . ?
C63 C82 1.403(6) . ?
C64 C65 1.392(6) . ?
C65 O7 1.372(5) . ?
C65 C70 1.391(7) . ?
C66 O7 1.437(6) . ?
C66 C67 1.501(6) . ?
C67 C68 1.521(6) . ?
C68 C69 1.507(6) . ?
C70 O8 1.392(5) . ?
C70 C75 1.394(6) . ?
C71 O8 1.459(6) . ?
C71 C72 1.525(7) . ?
C72 C73 1.513(8) . ?
C73 C74 1.523(8) . ?
C75 O9 1.362(6) . ?
C75 C82 1.390(6) . ?
C76 O9 1.427(6) . ?
C76 C77 1.511(7) . ?
C77 C78 1.510(9) . ?
C77 C84 1.65(3) . ?
C78 C79 1.501(13) . ?
N5 Ni2 1.773(3) . ?
N6 Ni2 1.779(4) . ?
Ni2 N5 1.773(3) 2_656 ?
Ni2 N6 1.778(4) 2_656 ?
C80 O10 1.367(7) . ?
O11 C83 1.36(4) . ?
C84 C85 1.57(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C18 119.4(4) . . ?
O6 C2 C7 115.8(4) . . ?
O6 C2 C1 123.3(4) . . ?
C7 C2 C1 120.9(4) . . ?
O6 C3 C4 105.8(5) . . ?
C5 C4 C3 112.4(7) . . ?
C4 C5 C6 109.9(8) . . ?
O5 C7 C12 119.7(5) . . ?
O5 C7 C2 121.3(4) . . ?
C12 C7 C2 118.7(5) . . ?
O5 C8 C9 117.1(6) . . ?
C8 C9 C10 118.9(6) . . ?
C11 C10 C9 120.7(7) . . ?
O4 C12 C7 115.5(4) . . ?
O4 C12 C17 122.6(4) . . ?
C7 C12 C17 121.8(4) . . ?
O4 C13 C14 106.6(4) . . ?
C13 C14 C15 111.0(5) . . ?
C16 C15 C14 114.8(6) . . ?
C18 C17 C12 119.5(4) . . ?
C17 C18 C1 119.7(4) . . ?
C17 C18 C19 121.4(4) . . ?
C1 C18 C19 119.0(4) . . ?
C20 C19 C81 122.9(4) . . ?
C20 C19 C18 119.1(4) . . ?
C81 C19 C18 117.7(4) . . ?
N2 C20 C19 120.3(4) . . ?
N2 C20 C21 105.3(4) . . ?
C19 C20 C21 134.1(4) . . ?
C22 C21 C20 108.0(4) . . ?
C21 C22 C23 107.6(4) . . ?
N2 C23 C22 106.9(4) . . ?
N2 C23 C24 110.5(4) . . ?
C22 C23 C24 142.5(4) . . ?
N1 C24 C25 108.0(4) . . ?
N1 C24 C23 109.4(4) . . ?
C25 C24 C23 142.5(4) . . ?
C26 C25 C24 107.6(4) . . ?
C25 C26 C27 107.5(4) . . ?
N1 C27 C26 106.5(4) . . ?
N1 C27 C28 119.4(4) . . ?
C26 C27 C28 134.1(5) . . ?
C47 C28 C27 122.9(4) . . ?
C47 C28 C29 118.4(4) . . ?
C27 C28 C29 118.7(4) . . ?
C46 C29 C30 119.1(5) . . ?
C46 C29 C28 119.6(4) . . ?
C30 C29 C28 121.3(4) . . ?
C31 C30 C29 119.8(5) . . ?
C30 C31 O1 124.2(5) . . ?
C30 C31 C36 120.9(5) . . ?
O1 C31 C36 114.9(5) . . ?
O1 C32 C33 107.9(5) . . ?
C34 C33 C32 114.9(6) . . ?
C33 C34 C35 112.8(6) . . ?
C41 C36 C31 119.2(5) . . ?
C41 C36 O2 118.7(6) . . ?
C31 C36 O2 120.2(6) . . ?
C41 C36 O11 119.2(7) . . ?
C31 C36 O11 114.7(8) . . ?
O2 C37 C38 103.3(9) . . ?
C39 C38 C37 119.1(9) . . ?
C39 C38 C83 85.3(14) . . ?
C38 C39 C40 116.4(10) . . ?
C46 C41 O3 124.0(5) . . ?
C46 C41 C36 120.1(5) . . ?
O3 C41 C36 115.9(5) . . ?
C43 C42 O3 108.3(6) . . ?
C42 C43 C44 108.7(7) . . ?
C45 C44 C43 116.7(8) . . ?
C41 C46 C29 120.6(5) . . ?
N4 C47 C28 121.1(4) . . ?
N4 C47 C48 106.2(4) . . ?
C28 C47 C48 132.2(4) . . ?
C49 C48 C47 107.6(4) . . ?
C48 C49 C50 107.5(4) . . ?
N4 C50 C49 107.3(4) . . ?
N4 C50 C51 110.3(4) . . ?
C49 C50 C51 141.7(4) . . ?
N3 C51 C52 107.8(4) . . ?
N3 C51 C50 111.2(4) . . ?
C52 C51 C50 140.0(4) . . ?
C53 C52 C51 106.8(4) . . ?
C52 C53 C81 108.2(4) . . ?
C24 N1 C27 110.5(4) . . ?
C24 N1 Ni1 118.0(3) . . ?
C27 N1 Ni1 131.5(3) . . ?
C23 N2 C20 112.1(4) . . ?
C23 N2 Ni1 117.0(3) . . ?
C20 N2 Ni1 131.0(3) . . ?
C51 N3 C81 111.4(4) . . ?
C51 N3 Ni1 115.9(3) . . ?
C81 N3 Ni1 130.0(3) . . ?
C50 N4 C47 111.3(4) . . ?
C50 N4 Ni1 116.5(3) . . ?
C47 N4 Ni1 130.6(3) . . ?
N1 Ni1 N4 94.20(17) . . ?
N1 Ni1 N2 84.78(17) . . ?
N4 Ni1 N2 171.64(16) . . ?
N1 Ni1 N3 171.04(16) . . ?
N4 Ni1 N3 85.64(17) . . ?
N2 Ni1 N3 94.08(17) . . ?
C31 O1 C32 116.4(4) . . ?
C36 O2 C37 106.1(10) . . ?
C41 O3 C42 118.9(5) . . ?
C12 O4 C13 117.3(4) . . ?
C7 O5 C8 119.0(5) . . ?
C2 O6 C3 117.5(4) . . ?
N6 C54 C55 106.4(4) . . ?
N6 C54 C62 110.0(4) . 2_656 ?
C55 C54 C62 143.5(4) . 2_656 ?
C56 C55 C54 107.6(4) . . ?
C55 C56 C57 108.8(4) . . ?
N6 C57 C56 105.2(4) . . ?
N6 C57 C58 119.3(4) . . ?
C56 C57 C58 135.5(4) . . ?
C59 C58 C57 123.1(4) . . ?
C59 C58 C63 119.2(4) . . ?
C57 C58 C63 117.6(4) . . ?
N5 C59 C58 121.1(4) . . ?
N5 C59 C60 104.3(4) . . ?
C58 C59 C60 134.5(4) . . ?
C61 C60 C59 108.9(4) . . ?
C60 C61 C62 107.0(4) . . ?
N5 C62 C61 108.0(4) . . ?
N5 C62 C54 110.4(4) . 2_656 ?
C61 C62 C54 141.5(4) . 2_656 ?
C64 C63 C82 119.4(4) . . ?
C64 C63 C58 119.6(4) . . ?
C82 C63 C58 121.0(4) . . ?
C65 C64 C63 120.1(4) . . ?
O7 C65 C70 115.3(4) . . ?
O7 C65 C64 124.6(4) . . ?
C70 C65 C64 120.1(4) . . ?
O7 C66 C67 107.6(4) . . ?
C66 C67 C68 115.3(4) . . ?
C69 C68 C67 111.7(4) . . ?
C65 C70 O8 120.7(4) . . ?
C65 C70 C75 120.2(4) . . ?
O8 C70 C75 119.0(4) . . ?
O8 C71 C72 107.1(4) . . ?
C73 C72 C71 114.8(5) . . ?
C72 C73 C74 112.7(5) . . ?
O9 C75 C82 124.7(4) . . ?
O9 C75 C70 115.5(4) . . ?
C82 C75 C70 119.7(4) . . ?
O9 C76 C77 106.7(4) . . ?
C78 C77 C76 114.4(5) . . ?
C76 C77 C84 102.0(14) . . ?
C79 C78 C77 112.0(8) . . ?
C65 O7 C66 117.0(3) . . ?
C70 O8 C71 112.3(3) . . ?
C75 O9 C76 117.7(4) . . ?
C62 N5 C59 111.8(4) . . ?
C62 N5 Ni2 117.0(3) . . ?
C59 N5 Ni2 130.4(3) . . ?
C54 N6 C57 112.0(4) . . ?
C54 N6 Ni2 116.5(3) . . ?
C57 N6 Ni2 131.4(3) . . ?
N5 Ni2 N5 180.0 . 2_656 ?
N5 Ni2 N6 85.75(16) . 2_656 ?
N5 Ni2 N6 94.25(16) 2_656 2_656 ?
N5 Ni2 N6 94.25(16) . . ?
N5 Ni2 N6 85.75(16) 2_656 . ?
N6 Ni2 N6 180.0 2_656 . ?
N3 C81 C19 121.0(4) . . ?
N3 C81 C53 105.8(4) . . ?
C19 C81 C53 132.7(5) . . ?
C75 C82 C63 120.4(4) . . ?
C83 O11 C36 104.7(18) . . ?
O11 C83 C38 98.8(15) . . ?
C85 C84 C77 105(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 C1 C2 O6 -176.8(4) . . . . ?
C18 C1 C2 C7 3.9(7) . . . . ?
O6 C3 C4 C5 -66.4(9) . . . . ?
C3 C4 C5 C6 -178.0(7) . . . . ?
O6 C2 C7 O5 3.2(7) . . . . ?
C1 C2 C7 O5 -177.4(4) . . . . ?
O6 C2 C7 C12 176.5(4) . . . . ?
C1 C2 C7 C12 -4.1(8) . . . . ?
O5 C8 C9 C10 -176.6(6) . . . . ?
C8 C9 C10 C11 -175.2(8) . . . . ?
O5 C7 C12 O4 -5.3(7) . . . . ?
C2 C7 C12 O4 -178.7(4) . . . . ?
O5 C7 C12 C17 176.0(4) . . . . ?
C2 C7 C12 C17 2.6(7) . . . . ?
O4 C13 C14 C15 70.9(6) . . . . ?
C13 C14 C15 C16 179.6(6) . . . . ?
O4 C12 C17 C18 -179.4(4) . . . . ?
C7 C12 C17 C18 -0.8(7) . . . . ?
C12 C17 C18 C1 0.5(7) . . . . ?
C12 C17 C18 C19 179.9(4) . . . . ?
C2 C1 C18 C17 -2.0(7) . . . . ?
C2 C1 C18 C19 178.6(4) . . . . ?
C17 C18 C19 C20 45.2(6) . . . . ?
C1 C18 C19 C20 -135.4(5) . . . . ?
C17 C18 C19 C81 -129.8(5) . . . . ?
C1 C18 C19 C81 49.6(6) . . . . ?
C81 C19 C20 N2 3.0(7) . . . . ?
C18 C19 C20 N2 -171.7(4) . . . . ?
C81 C19 C20 C21 176.2(4) . . . . ?
C18 C19 C20 C21 1.5(8) . . . . ?
N2 C20 C21 C22 2.0(5) . . . . ?
C19 C20 C21 C22 -171.9(5) . . . . ?
C20 C21 C22 C23 -0.7(5) . . . . ?
C21 C22 C23 N2 -0.8(5) . . . . ?
C21 C22 C23 C24 175.1(6) . . . . ?
N2 C23 C24 N1 0.4(5) . . . . ?
C22 C23 C24 N1 -175.4(5) . . . . ?
N2 C23 C24 C25 176.0(5) . . . . ?
C22 C23 C24 C25 0.1(11) . . . . ?
N1 C24 C25 C26 1.0(5) . . . . ?
C23 C24 C25 C26 -174.6(6) . . . . ?
C24 C25 C26 C27 -0.7(5) . . . . ?
C25 C26 C27 N1 0.2(5) . . . . ?
C25 C26 C27 C28 176.6(5) . . . . ?
N1 C27 C28 C47 0.5(7) . . . . ?
C26 C27 C28 C47 -175.6(5) . . . . ?
N1 C27 C28 C29 178.8(4) . . . . ?
C26 C27 C28 C29 2.8(8) . . . . ?
C47 C28 C29 C46 -51.2(6) . . . . ?
C27 C28 C29 C46 130.4(5) . . . . ?
C47 C28 C29 C30 130.5(5) . . . . ?
C27 C28 C29 C30 -47.9(6) . . . . ?
C46 C29 C30 C31 -0.7(7) . . . . ?
C28 C29 C30 C31 177.7(5) . . . . ?
C29 C30 C31 O1 177.0(5) . . . . ?
C29 C30 C31 C36 -4.5(8) . . . . ?
O1 C32 C33 C34 -63.9(7) . . . . ?
C32 C33 C34 C35 -176.3(6) . . . . ?
C30 C31 C36 C41 5.5(10) . . . . ?
O1 C31 C36 C41 -175.8(6) . . . . ?
C30 C31 C36 O2 -158.4(7) . . . . ?
O1 C31 C36 O2 20.3(10) . . . . ?
C30 C31 C36 O11 156.2(9) . . . . ?
O1 C31 C36 O11 -25.2(11) . . . . ?
O2 C37 C38 C39 -65.5(11) . . . . ?
C37 C38 C39 C40 179.9(10) . . . . ?
C83 C38 C39 C40 143.5(13) . . . . ?
C31 C36 C41 C46 -1.2(10) . . . . ?
O2 C36 C41 C46 162.9(7) . . . . ?
O11 C36 C41 C46 -150.6(10) . . . . ?
C31 C36 C41 O3 -179.5(6) . . . . ?
O2 C36 C41 O3 -15.4(10) . . . . ?
O11 C36 C41 O3 31.1(12) . . . . ?
O3 C42 C43 C44 172.0(7) . . . . ?
C42 C43 C44 C45 62.1(10) . . . . ?
O3 C41 C46 C29 174.2(6) . . . . ?
C36 C41 C46 C29 -3.9(9) . . . . ?
C30 C29 C46 C41 4.9(8) . . . . ?
C28 C29 C46 C41 -173.5(5) . . . . ?
C27 C28 C47 N4 -5.4(7) . . . . ?
C29 C28 C47 N4 176.3(4) . . . . ?
C27 C28 C47 C48 165.7(5) . . . . ?
C29 C28 C47 C48 -12.7(8) . . . . ?
N4 C47 C48 C49 1.5(5) . . . . ?
C28 C47 C48 C49 -170.5(5) . . . . ?
C47 C48 C49 C50 -0.1(5) . . . . ?
C48 C49 C50 N4 -1.3(5) . . . . ?
C48 C49 C50 C51 167.9(6) . . . . ?
N4 C50 C51 N3 -1.5(5) . . . . ?
C49 C50 C51 N3 -170.5(5) . . . . ?
N4 C50 C51 C52 165.1(5) . . . . ?
C49 C50 C51 C52 -3.9(10) . . . . ?
N3 C51 C52 C53 1.1(5) . . . . ?
C50 C51 C52 C53 -165.8(5) . . . . ?
C51 C52 C53 C81 0.3(5) . . . . ?
C25 C24 N1 C27 -0.8(5) . . . . ?
C23 C24 N1 C27 176.3(3) . . . . ?
C25 C24 N1 Ni1 178.1(3) . . . . ?
C23 C24 N1 Ni1 -4.8(5) . . . . ?
C26 C27 N1 C24 0.4(5) . . . . ?
C28 C27 N1 C24 -176.7(4) . . . . ?
C26 C27 N1 Ni1 -178.3(3) . . . . ?
C28 C27 N1 Ni1 4.6(6) . . . . ?
C22 C23 N2 C20 2.2(5) . . . . ?
C24 C23 N2 C20 -175.2(3) . . . . ?
C22 C23 N2 Ni1 -178.7(3) . . . . ?
C24 C23 N2 Ni1 4.0(5) . . . . ?
C19 C20 N2 C23 172.3(4) . . . . ?
C21 C20 N2 C23 -2.6(5) . . . . ?
C19 C20 N2 Ni1 -6.7(6) . . . . ?
C21 C20 N2 Ni1 178.4(3) . . . . ?
C52 C51 N3 C81 -2.2(5) . . . . ?
C50 C51 N3 C81 168.8(4) . . . . ?
C52 C51 N3 Ni1 -165.3(3) . . . . ?
C50 C51 N3 Ni1 5.7(5) . . . . ?
C49 C50 N4 C47 2.4(5) . . . . ?
C51 C50 N4 C47 -170.5(4) . . . . ?
C49 C50 N4 Ni1 169.6(3) . . . . ?
C51 C50 N4 Ni1 -3.4(5) . . . . ?
C28 C47 N4 C50 170.7(4) . . . . ?
C48 C47 N4 C50 -2.4(5) . . . . ?
C28 C47 N4 Ni1 5.8(7) . . . . ?
C48 C47 N4 Ni1 -167.3(3) . . . . ?
C24 N1 Ni1 N4 177.5(3) . . . . ?
C27 N1 Ni1 N4 -3.9(4) . . . . ?
C24 N1 Ni1 N2 5.8(3) . . . . ?
C27 N1 Ni1 N2 -175.6(4) . . . . ?
C50 N4 Ni1 N1 -165.7(3) . . . . ?
C47 N4 Ni1 N1 -1.5(4) . . . . ?
C50 N4 Ni1 N3 5.3(3) . . . . ?
C47 N4 Ni1 N3 169.5(4) . . . . ?
C23 N2 Ni1 N1 -5.4(3) . . . . ?
C20 N2 Ni1 N1 173.6(4) . . . . ?
C23 N2 Ni1 N3 -176.5(3) . . . . ?
C20 N2 Ni1 N3 2.5(4) . . . . ?
C51 N3 Ni1 N4 -6.2(3) . . . . ?
C81 N3 Ni1 N4 -165.6(4) . . . . ?
C51 N3 Ni1 N2 165.4(3) . . . . ?
C81 N3 Ni1 N2 6.1(4) . . . . ?
C30 C31 O1 C32 -4.4(8) . . . . ?
C36 C31 O1 C32 177.0(5) . . . . ?
C33 C32 O1 C31 -175.9(5) . . . . ?
C41 C36 O2 C37 98.8(9) . . . . ?
C31 C36 O2 C37 -97.2(9) . . . . ?
C38 C37 O2 C36 173.3(7) . . . . ?
C46 C41 O3 C42 -9.3(10) . . . . ?
C36 C41 O3 C42 168.9(7) . . . . ?
C43 C42 O3 C41 -168.1(7) . . . . ?
C7 C12 O4 C13 158.3(4) . . . . ?
C17 C12 O4 C13 -23.0(6) . . . . ?
C14 C13 O4 C12 -161.1(5) . . . . ?
C12 C7 O5 C8 121.0(6) . . . . ?
C2 C7 O5 C8 -65.7(7) . . . . ?
C9 C8 O5 C7 -52.4(9) . . . . ?
C7 C2 O6 C3 -174.9(5) . . . . ?
C1 C2 O6 C3 5.7(8) . . . . ?
C4 C3 O6 C2 179.9(6) . . . . ?
N6 C54 C55 C56 1.1(5) . . . . ?
C62 C54 C55 C56 -177.1(6) 2_656 . . . ?
C54 C55 C56 C57 -1.5(5) . . . . ?
C55 C56 C57 N6 1.3(5) . . . . ?
C55 C56 C57 C58 178.6(5) . . . . ?
N6 C57 C58 C59 0.6(6) . . . . ?
C56 C57 C58 C59 -176.4(5) . . . . ?
N6 C57 C58 C63 -177.6(4) . . . . ?
C56 C57 C58 C63 5.4(7) . . . . ?
C57 C58 C59 N5 4.7(7) . . . . ?
C63 C58 C59 N5 -177.1(4) . . . . ?
C57 C58 C59 C60 -172.9(4) . . . . ?
C63 C58 C59 C60 5.2(8) . . . . ?
N5 C59 C60 C61 -0.4(5) . . . . ?
C58 C59 C60 C61 177.5(5) . . . . ?
C59 C60 C61 C62 0.2(5) . . . . ?
C60 C61 C62 N5 0.1(5) . . . . ?
C60 C61 C62 C54 -175.0(6) . . . 2_656 ?
C59 C58 C63 C64 41.2(6) . . . . ?
C57 C58 C63 C64 -140.6(4) . . . . ?
C59 C58 C63 C82 -137.5(5) . . . . ?
C57 C58 C63 C82 40.7(6) . . . . ?
C82 C63 C64 C65 2.8(7) . . . . ?
C58 C63 C64 C65 -175.9(4) . . . . ?
C63 C64 C65 O7 180.0(4) . . . . ?
C63 C64 C65 C70 -0.5(7) . . . . ?
O7 C66 C67 C68 63.6(5) . . . . ?
C66 C67 C68 C69 166.0(4) . . . . ?
O7 C65 C70 O8 -5.6(6) . . . . ?
C64 C65 C70 O8 174.8(4) . . . . ?
O7 C65 C70 C75 177.7(4) . . . . ?
C64 C65 C70 C75 -1.9(7) . . . . ?
O8 C71 C72 C73 63.2(6) . . . . ?
C71 C72 C73 C74 62.4(6) . . . . ?
C65 C70 C75 O9 179.7(4) . . . . ?
O8 C70 C75 O9 2.9(6) . . . . ?
C65 C70 C75 C82 1.9(7) . . . . ?
O8 C70 C75 C82 -174.9(4) . . . . ?
O9 C76 C77 C78 165.0(6) . . . . ?
O9 C76 C77 C84 -149.7(12) . . . . ?
C76 C77 C78 C79 67.2(9) . . . . ?
C70 C65 O7 C66 174.5(4) . . . . ?
C64 C65 O7 C66 -6.0(6) . . . . ?
C67 C66 O7 C65 -170.0(4) . . . . ?
C65 C70 O8 C71 94.5(5) . . . . ?
C75 C70 O8 C71 -88.7(5) . . . . ?
C72 C71 O8 C70 -176.6(4) . . . . ?
C82 C75 O9 C76 -8.1(7) . . . . ?
C70 C75 O9 C76 174.2(5) . . . . ?
C77 C76 O9 C75 -178.8(5) . . . . ?
C61 C62 N5 C59 -0.4(5) . . . . ?
C54 C62 N5 C59 176.3(3) 2_656 . . . ?
C61 C62 N5 Ni2 -171.2(3) . . . . ?
C54 C62 N5 Ni2 5.5(5) 2_656 . . . ?
C58 C59 N5 C62 -177.8(4) . . . . ?
C60 C59 N5 C62 0.5(5) . . . . ?
C58 C59 N5 Ni2 -8.5(6) . . . . ?
C60 C59 N5 Ni2 169.7(3) . . . . ?
C55 C54 N6 C57 -0.2(5) . . . . ?
C62 C54 N6 C57 178.6(4) 2_656 . . . ?
C55 C54 N6 Ni2 -176.6(3) . . . . ?
C62 C54 N6 Ni2 2.2(5) 2_656 . . . ?
C56 C57 N6 C54 -0.7(5) . . . . ?
C58 C57 N6 C54 -178.5(4) . . . . ?
C56 C57 N6 Ni2 175.1(3) . . . . ?
C58 C57 N6 Ni2 -2.8(6) . . . . ?
C62 N5 Ni2 N6 -5.6(3) . . . 2_656 ?
C59 N5 Ni2 N6 -174.4(4) . . . 2_656 ?
C62 N5 Ni2 N6 174.4(3) . . . . ?
C59 N5 Ni2 N6 5.6(4) . . . . ?
C54 N6 Ni2 N5 175.7(3) . . . . ?
C57 N6 Ni2 N5 0.1(4) . . . . ?
C54 N6 Ni2 N5 -4.3(3) . . . 2_656 ?
C57 N6 Ni2 N5 -179.9(4) . . . 2_656 ?
C51 N3 C81 C19 -170.1(4) . . . . ?
Ni1 N3 C81 C19 -10.0(6) . . . . ?
C51 N3 C81 C53 2.3(5) . . . . ?
Ni1 N3 C81 C53 162.4(3) . . . . ?
C20 C19 C81 N3 4.9(7) . . . . ?
C18 C19 C81 N3 179.7(4) . . . . ?
C20 C19 C81 C53 -165.2(5) . . . . ?
C18 C19 C81 C53 9.6(7) . . . . ?
C52 C53 C81 N3 -1.6(5) . . . . ?
C52 C53 C81 C19 169.6(5) . . . . ?
O9 C75 C82 C63 -177.1(4) . . . . ?
C70 C75 C82 C63 0.4(7) . . . . ?
C64 C63 C82 C75 -2.8(7) . . . . ?
C58 C63 C82 C75 175.9(4) . . . . ?
C41 C36 O11 C83 -116.8(16) . . . . ?
C31 C36 O11 C83 92.5(17) . . . . ?
C36 O11 C83 C38 171.9(13) . . . . ?
C39 C38 C83 O11 135.9(18) . . . . ?
C76 C77 C84 C85 -80(3) . . . . ?

_refine_diff_density_max         1.245
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.099

