# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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_exp_10165
_database_code_depnum_ccdc_archive 'CCDC 1975207'
loop_
_audit_author_name
_audit_author_address
'Rong-Yun Li'
;Liaocheng University
China
;
_audit_update_record             
;
2020-01-03 deposited with the CCDC.	2020-03-16 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         ?
_chemical_formula_sum            'C40 H32 Br4 N4 Ni O12'
_chemical_formula_weight         1139.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.0144(4)
_cell_length_b                   14.3925(7)
_cell_length_c                   14.5425(5)
_cell_angle_alpha                91.472(3)
_cell_angle_beta                 106.177(3)
_cell_angle_gamma                109.433(4)
_cell_volume                     2070.02(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6168
_cell_measurement_theta_min      3.2380
_cell_measurement_theta_max      71.4890

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    5.789
_shelx_estimated_absorpt_T_min   0.543
_shelx_estimated_absorpt_T_max   0.568
_exptl_absorpt_correction_T_min  0.33602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13151
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.284
_diffrn_reflns_theta_max         67.247
_diffrn_reflns_theta_full        67.247
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7418
_reflns_number_gt                6375
_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       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0549P)²+2.8886P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7418
_refine_ls_number_parameters     552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1247
_refine_ls_wR_factor_gt          0.1181
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.51895(6) -0.01339(5) 0.75155(4) 0.02461(15) Uani 1 1 d . . . . .
Br1 Br 0.79245(5) -0.12458(4) 0.42757(4) 0.04600(14) Uani 1 1 d . . . . .
Br2 Br 0.00663(5) -0.26293(6) 0.35997(4) 0.0654(2) Uani 1 1 d . . . . .
Br3 Br 0.38154(6) -0.36448(4) 1.03725(5) 0.06383(19) Uani 1 1 d . . . . .
Br4 Br 0.15480(6) 0.10536(6) 0.99968(6) 0.0688(2) Uani 1 1 d . . . . .
N1 N 0.6106(3) -0.0569(2) 0.6614(2) 0.0281(6) Uani 1 1 d . . . . .
N2 N 0.3555(3) -0.0869(2) 0.6333(2) 0.0260(6) Uani 1 1 d . . . . .
N3 N 0.4104(3) 0.0309(2) 0.8257(2) 0.0277(6) Uani 1 1 d . . . . .
N4 N 0.4772(3) -0.1280(2) 0.8320(2) 0.0276(6) Uani 1 1 d . . . . .
O1 O 0.6975(3) 0.0729(2) 0.85227(19) 0.0311(6) Uani 1 1 d . . . . .
O2 O 0.6162(2) 0.1410(2) 0.72817(19) 0.0300(6) Uani 1 1 d . . . . .
O3 O 1.1040(3) 0.2742(2) 1.1209(2) 0.0356(6) Uani 1 1 d . . . . .
O4 O 1.2495(3) 0.4054(3) 1.0829(2) 0.0472(8) Uani 1 1 d . . . . .
O5 O 0.9593(3) 0.4832(2) 0.7775(2) 0.0418(7) Uani 1 1 d . . . . .
O6 O 1.2176(3) 0.5826(3) 0.5378(2) 0.0455(8) Uani 1 1 d . . . . .
O7 O 1.7049(3) 0.7166(3) 0.7345(2) 0.0402(7) Uani 1 1 d . . . . .
H7 H 1.771551 0.713544 0.775263 0.060 Uiso 1 1 calc R U . . .
O8 O 1.8220(3) 0.7237(3) 0.6300(2) 0.0409(7) Uani 1 1 d . . . . .
O9 O 1.5482(4) 0.5682(5) 0.2819(3) 0.0872(18) Uani 1 1 d . . . . .
O10 O 1.3277(4) 0.5045(3) 0.2545(3) 0.0588(10) Uani 1 1 d . . . . .
H10 H 1.329849 0.474233 0.206759 0.088 Uiso 1 1 calc R U . . .
O11 O 0.7388(7) 0.6342(8) 0.1773(7) 0.158(4) Uani 1 1 d . . . . .
H11D H 0.668721 0.606564 0.194356 0.190 Uiso 1 1 d R U . . .
H11B H 0.804769 0.619023 0.210266 0.190 Uiso 1 1 d R U . . .
O12 O 0.0352(4) 0.8737(3) 0.7668(3) 0.0665(11) Uani 1 1 d . . . . .
H12C H 0.013633 0.843768 0.812720 0.080 Uiso 1 1 d R U . . .
H12D H -0.019757 0.839398 0.714010 0.080 Uiso 1 1 d R U . . .
C1 C 0.7187(4) -0.0947(3) 0.5220(3) 0.0309(8) Uani 1 1 d . . . . .
C2 C 0.8022(4) -0.0537(3) 0.6130(3) 0.0379(9) Uani 1 1 d . . . . .
H2 H 0.895170 -0.038011 0.628506 0.045 Uiso 1 1 calc R U . . .
C3 C 0.7440(4) -0.0362(3) 0.6814(3) 0.0363(9) Uani 1 1 d . . . . .
H3 H 0.799662 -0.008933 0.743780 0.044 Uiso 1 1 calc R U . . .
C4 C 0.5297(3) -0.0970(3) 0.5709(3) 0.0244(7) Uani 1 1 d . . . . .
C5 C 0.5803(4) -0.1170(3) 0.4986(3) 0.0292(8) Uani 1 1 d . . . . .
H5 H 0.523512 -0.144342 0.436507 0.035 Uiso 1 1 calc R U . . .
C6 C 0.3831(3) -0.1192(3) 0.5568(3) 0.0244(7) Uani 1 1 d . . . . .
C7 C 0.2829(4) -0.1713(3) 0.4727(3) 0.0312(8) Uani 1 1 d . . . . .
H7A H 0.304110 -0.190746 0.419421 0.037 Uiso 1 1 calc R U . . .
C8 C 0.1489(4) -0.1933(3) 0.4713(3) 0.0351(9) Uani 1 1 d . . . . .
C9 C 0.1188(4) -0.1651(3) 0.5510(3) 0.0339(8) Uani 1 1 d . . . . .
H9 H 0.029885 -0.182099 0.551672 0.041 Uiso 1 1 calc R U . . .
C10 C 0.2255(4) -0.1107(3) 0.6294(3) 0.0307(8) Uani 1 1 d . . . . .
H10A H 0.206422 -0.089267 0.682832 0.037 Uiso 1 1 calc R U . . .
C11 C 0.5190(4) -0.2055(3) 0.8332(3) 0.0355(9) Uani 1 1 d . . . . .
H11 H 0.567965 -0.210973 0.791825 0.043 Uiso 1 1 calc R U . . .
C12 C 0.4925(5) -0.2777(3) 0.8933(3) 0.0426(10) Uani 1 1 d . . . . .
H12 H 0.523978 -0.330134 0.893155 0.051 Uiso 1 1 calc R U . . .
C13 C 0.4185(4) -0.2698(3) 0.9529(3) 0.0398(10) Uani 1 1 d . . . . .
C14 C 0.3727(4) -0.1901(3) 0.9529(3) 0.0352(9) Uani 1 1 d . . . . .
H14 H 0.322038 -0.184013 0.992841 0.042 Uiso 1 1 calc R U . . .
C15 C 0.4055(3) -0.1202(3) 0.8913(3) 0.0276(8) Uani 1 1 d . . . . .
C16 C 0.3668(4) -0.0306(3) 0.8873(3) 0.0280(8) Uani 1 1 d . . . . .
C17 C 0.2914(4) -0.0099(3) 0.9417(3) 0.0350(9) Uani 1 1 d . . . . .
H17 H 0.264075 -0.051154 0.985963 0.042 Uiso 1 1 calc R U . . .
C18 C 0.2583(4) 0.0748(4) 0.9277(3) 0.0397(10) Uani 1 1 d . . . . .
C19 C 0.3014(5) 0.1374(4) 0.8654(4) 0.0430(10) Uani 1 1 d . . . . .
H19 H 0.278950 0.194093 0.856346 0.052 Uiso 1 1 calc R U . . .
C20 C 0.3802(4) 0.1132(3) 0.8162(3) 0.0360(9) Uani 1 1 d . . . . .
H20 H 0.413382 0.156139 0.775018 0.043 Uiso 1 1 calc R U . . .
C21 C 0.7054(3) 0.1480(3) 0.8069(3) 0.0251(7) Uani 1 1 d . . . . .
C22 C 0.8225(3) 0.2423(3) 0.8486(3) 0.0256(7) Uani 1 1 d . . . . .
C23 C 0.9179(4) 0.2459(3) 0.9362(3) 0.0265(7) Uani 1 1 d . . . . .
H23 H 0.907295 0.190980 0.969657 0.032 Uiso 1 1 calc R U . . .
C24 C 1.0288(4) 0.3326(3) 0.9725(3) 0.0271(7) Uani 1 1 d . . . . .
C25 C 1.0457(4) 0.4143(3) 0.9215(3) 0.0300(8) Uani 1 1 d . . . . .
H25 H 1.121146 0.471849 0.945724 0.036 Uiso 1 1 calc R U . . .
C26 C 0.9494(4) 0.4094(3) 0.8342(3) 0.0299(8) Uani 1 1 d . . . . .
C27 C 0.8364(4) 0.3240(3) 0.7991(3) 0.0287(8) Uani 1 1 d . . . . .
H27 H 0.769946 0.321613 0.742237 0.034 Uiso 1 1 calc R U . . .
C28 C 1.1368(4) 0.3387(3) 1.0657(3) 0.0301(8) Uani 1 1 d . . . . .
C29 C 1.0794(4) 0.5700(3) 0.8057(3) 0.0341(9) Uani 1 1 d . . . . .
H29A H 1.158798 0.551978 0.814134 0.041 Uiso 1 1 calc R U . . .
H29B H 1.087404 0.605471 0.866025 0.041 Uiso 1 1 calc R U . . .
C30 C 1.0658(4) 0.6337(3) 0.7254(3) 0.0380(9) Uani 1 1 d . . . . .
H30A H 1.136891 0.698357 0.747009 0.046 Uiso 1 1 calc R U . . .
H30B H 0.980058 0.643505 0.713295 0.046 Uiso 1 1 calc R U . . .
C31 C 1.0731(4) 0.5916(3) 0.6307(3) 0.0387(10) Uani 1 1 d . . . . .
H31A H 1.023101 0.520629 0.618547 0.046 Uiso 1 1 calc R U . . .
H31B H 1.030940 0.621832 0.578227 0.046 Uiso 1 1 calc R U . . .
C32 C 1.2175(4) 0.6105(4) 0.6327(3) 0.0394(9) Uani 1 1 d . . . . .
H32A H 1.271579 0.680331 0.653481 0.047 Uiso 1 1 calc R U . . .
H32B H 1.256156 0.571909 0.677814 0.047 Uiso 1 1 calc R U . . .
C33 C 1.4636(4) 0.6421(3) 0.5944(3) 0.0321(8) Uani 1 1 d . . . . .
H33 H 1.466623 0.659022 0.657319 0.038 Uiso 1 1 calc R U . . .
C34 C 1.5824(4) 0.6584(3) 0.5713(3) 0.0280(8) Uani 1 1 d . . . . .
C35 C 1.5794(4) 0.6325(3) 0.4779(3) 0.0314(8) Uani 1 1 d . . . . .
H35 H 1.659361 0.643931 0.462762 0.038 Uiso 1 1 calc R U . . .
C36 C 1.4548(4) 0.5892(3) 0.4073(3) 0.0321(8) Uani 1 1 d . . . . .
C37 C 1.3356(4) 0.5738(3) 0.4295(3) 0.0349(9) Uani 1 1 d . . . . .
H37 H 1.252882 0.545626 0.381722 0.042 Uiso 1 1 calc R U . . .
C38 C 1.3399(4) 0.6003(3) 0.5228(3) 0.0337(8) Uani 1 1 d . . . . .
C39 C 1.7161(4) 0.7032(3) 0.6491(3) 0.0309(8) Uani 1 1 d . . . . .
C40 C 1.4494(5) 0.5542(3) 0.3077(3) 0.0407(10) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3 2.047(3) . ?
Ni1 N4 2.048(3) . ?
Ni1 N2 2.057(3) . ?
Ni1 O1 2.057(3) . ?
Ni1 N1 2.061(3) . ?
Ni1 O2 2.205(3) . ?
Ni1 C21 2.464(4) . ?
Br1 C1 1.885(4) . ?
Br2 C8 1.882(4) . ?
Br3 C13 1.877(4) . ?
Br4 C18 1.888(4) . ?
N1 C3 1.341(5) . ?
N1 C4 1.350(5) . ?
N2 C6 1.342(5) . ?
N2 C10 1.342(5) . ?
N3 C20 1.333(6) . ?
N3 C16 1.348(5) . ?
N4 C11 1.340(5) . ?
N4 C15 1.347(5) . ?
O1 C21 1.272(5) . ?
O2 C21 1.260(4) . ?
O3 C28 1.269(5) . ?
O4 C28 1.245(5) . ?
O5 C26 1.356(5) . ?
O5 C29 1.432(5) . ?
O6 C38 1.365(5) . ?
O6 C32 1.428(6) . ?
O7 C39 1.297(5) . ?
O8 C39 1.217(5) . ?
O9 C40 1.205(7) . ?
O10 C40 1.289(6) . ?
C1 C2 1.367(6) . ?
C1 C5 1.386(6) . ?
C2 C3 1.383(6) . ?
C4 C5 1.384(5) . ?
C4 C6 1.491(5) . ?
C6 C7 1.388(5) . ?
C7 C8 1.397(6) . ?
C8 C9 1.377(6) . ?
C9 C10 1.374(6) . ?
C11 C12 1.384(6) . ?
C12 C13 1.371(7) . ?
C13 C14 1.400(7) . ?
C14 C15 1.389(6) . ?
C15 C16 1.485(6) . ?
C16 C17 1.387(6) . ?
C17 C18 1.388(7) . ?
C18 C19 1.362(7) . ?
C19 C20 1.386(7) . ?
C21 C22 1.493(5) . ?
C22 C27 1.382(5) . ?
C22 C23 1.395(5) . ?
C23 C24 1.386(5) . ?
C24 C25 1.394(6) . ?
C24 C28 1.512(5) . ?
C25 C26 1.392(5) . ?
C26 C27 1.384(6) . ?
C29 C30 1.508(6) . ?
C30 C31 1.523(7) . ?
C31 C32 1.513(5) . ?
C33 C34 1.387(6) . ?
C33 C38 1.391(6) . ?
C34 C35 1.387(6) . ?
C34 C39 1.505(5) . ?
C35 C36 1.393(6) . ?
C36 C37 1.386(6) . ?
C36 C40 1.500(6) . ?
C37 C38 1.384(6) . ?

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
N3 Ni1 N4 79.63(13) . . ?
N3 Ni1 N2 95.32(13) . . ?
N4 Ni1 N2 93.62(12) . . ?
N3 Ni1 O1 90.89(12) . . ?
N4 Ni1 O1 95.43(11) . . ?
N2 Ni1 O1 169.82(12) . . ?
N3 Ni1 N1 172.79(13) . . ?
N4 Ni1 N1 104.29(13) . . ?
N2 Ni1 N1 78.51(12) . . ?
O1 Ni1 N1 94.71(12) . . ?
N3 Ni1 O2 90.81(12) . . ?
N4 Ni1 O2 155.29(11) . . ?
N2 Ni1 O2 110.04(11) . . ?
O1 Ni1 O2 61.71(10) . . ?
N1 Ni1 O2 87.87(12) . . ?
N3 Ni1 C21 90.49(12) . . ?
N4 Ni1 C21 125.82(12) . . ?
N2 Ni1 C21 140.50(12) . . ?
O1 Ni1 C21 31.05(12) . . ?
N1 Ni1 C21 91.98(13) . . ?
O2 Ni1 C21 30.67(11) . . ?
C3 N1 C4 118.6(3) . . ?
C3 N1 Ni1 125.1(3) . . ?
C4 N1 Ni1 115.5(2) . . ?
C6 N2 C10 118.1(3) . . ?
C6 N2 Ni1 116.3(2) . . ?
C10 N2 Ni1 125.3(3) . . ?
C20 N3 C16 119.6(4) . . ?
C20 N3 Ni1 125.2(3) . . ?
C16 N3 Ni1 115.2(3) . . ?
C11 N4 C15 118.7(3) . . ?
C11 N4 Ni1 126.1(3) . . ?
C15 N4 Ni1 115.2(3) . . ?
C21 O1 Ni1 92.4(2) . . ?
C21 O2 Ni1 86.1(2) . . ?
C26 O5 C29 118.6(3) . . ?
C38 O6 C32 117.7(3) . . ?
C2 C1 C5 121.1(4) . . ?
C2 C1 Br1 119.4(3) . . ?
C5 C1 Br1 119.5(3) . . ?
C1 C2 C3 117.8(4) . . ?
N1 C3 C2 122.7(4) . . ?
N1 C4 C5 122.1(3) . . ?
N1 C4 C6 114.4(3) . . ?
C5 C4 C6 123.5(3) . . ?
C4 C5 C1 117.6(4) . . ?
N2 C6 C7 122.7(3) . . ?
N2 C6 C4 114.4(3) . . ?
C7 C6 C4 122.9(3) . . ?
C6 C7 C8 117.2(4) . . ?
C9 C8 C7 120.9(4) . . ?
C9 C8 Br2 119.1(3) . . ?
C7 C8 Br2 120.0(3) . . ?
C10 C9 C8 117.3(4) . . ?
N2 C10 C9 123.7(4) . . ?
N4 C11 C12 122.8(4) . . ?
C13 C12 C11 118.2(4) . . ?
C12 C13 C14 120.3(4) . . ?
C12 C13 Br3 120.1(4) . . ?
C14 C13 Br3 119.5(4) . . ?
C15 C14 C13 117.6(4) . . ?
N4 C15 C14 122.3(4) . . ?
N4 C15 C16 115.0(3) . . ?
C14 C15 C16 122.7(4) . . ?
N3 C16 C17 121.3(4) . . ?
N3 C16 C15 114.9(3) . . ?
C17 C16 C15 123.8(4) . . ?
C16 C17 C18 117.4(4) . . ?
C19 C18 C17 121.8(4) . . ?
C19 C18 Br4 119.3(4) . . ?
C17 C18 Br4 118.8(4) . . ?
C18 C19 C20 117.2(4) . . ?
N3 C20 C19 122.6(4) . . ?
O2 C21 O1 119.7(3) . . ?
O2 C21 C22 121.8(3) . . ?
O1 C21 C22 118.4(3) . . ?
O2 C21 Ni1 63.21(19) . . ?
O1 C21 Ni1 56.54(18) . . ?
C22 C21 Ni1 174.9(3) . . ?
C27 C22 C23 120.9(3) . . ?
C27 C22 C21 119.7(3) . . ?
C23 C22 C21 119.3(3) . . ?
C24 C23 C22 118.9(3) . . ?
C23 C24 C25 120.5(3) . . ?
C23 C24 C28 120.6(3) . . ?
C25 C24 C28 118.8(3) . . ?
C26 C25 C24 119.8(3) . . ?
O5 C26 C27 115.9(3) . . ?
O5 C26 C25 124.2(4) . . ?
C27 C26 C25 119.9(3) . . ?
C22 C27 C26 119.9(3) . . ?
O4 C28 O3 125.0(4) . . ?
O4 C28 C24 118.5(4) . . ?
O3 C28 C24 116.5(3) . . ?
O5 C29 C30 106.2(3) . . ?
C29 C30 C31 115.0(4) . . ?
C32 C31 C30 111.8(4) . . ?
O6 C32 C31 108.5(3) . . ?
C34 C33 C38 119.6(4) . . ?
C35 C34 C33 120.8(3) . . ?
C35 C34 C39 119.7(4) . . ?
C33 C34 C39 119.5(4) . . ?
C34 C35 C36 119.0(4) . . ?
C37 C36 C35 120.5(4) . . ?
C37 C36 C40 119.7(4) . . ?
C35 C36 C40 119.7(4) . . ?
C38 C37 C36 120.0(4) . . ?
O6 C38 C37 115.9(4) . . ?
O6 C38 C33 124.1(4) . . ?
C37 C38 C33 120.0(4) . . ?
O8 C39 O7 125.4(4) . . ?
O8 C39 C34 121.0(4) . . ?
O7 C39 C34 113.7(3) . . ?
O9 C40 O10 124.2(5) . . ?
O9 C40 C36 123.5(4) . . ?
O10 C40 C36 112.2(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C30 H30B O8 0.97 2.46 3.338(5) 150.1 1_455 yes
C25 H25 Br3 0.93 2.96 3.882(4) 171.5 1_665 yes
C20 H20 O2 0.93 2.58 3.122(5) 117.5 . yes
C20 H20 Br1 0.93 3.09 3.563(4) 113.4 2_656 yes
C19 H19 O11 0.93 2.59 3.508(11) 168.5 2_666 yes
C17 H17 O1 0.93 2.32 3.134(5) 145.9 2_657 yes
C11 H11 O7 0.93 2.40 3.255(5) 152.7 1_445 yes
C10 H10A O12 0.93 2.45 3.238(6) 143.0 1_545 yes
C10 H10A N3 0.93 2.64 3.186(5) 117.9 . yes
C9 H9 Br1 0.93 3.11 3.786(4) 131.1 1_455 yes
C7 H7A O2 0.93 2.57 3.392(5) 147.7 2_656 yes
C5 H5 O2 0.93 2.47 3.339(4) 155.2 2_656 yes
C3 H3 O1 0.93 2.63 3.154(5) 116.3 . yes
O12 H12D O8 0.85 2.02 2.817(5) 155.8 1_355 yes
O12 H12C O3 0.85 2.19 2.991(5) 156.4 2_667 yes
O11 H11B Br2 0.85 2.68 3.237(9) 124.6 1_665 yes
O11 H11D O9 0.85 2.04 2.855(9) 159.2 1_455 yes
O10 H10 O4 0.82 1.86 2.609(5) 151.9 1_554 yes
O7 H7 O3 0.82 1.69 2.491(4) 164.2 2_867 yes
O7 H7 O3 0.82 1.69 2.491(4) 164.2 2_867 yes
O10 H10 O4 0.82 1.86 2.609(5) 151.9 1_554 yes
O11 H11D O9 0.85 2.04 2.855(9) 159.2 1_455 yes
O11 H11B Br2 0.85 2.68 3.237(9) 124.6 1_665 yes
O12 H12C O3 0.85 2.19 2.991(5) 156.4 2_667 yes
O12 H12D O8 0.85 2.02 2.817(5) 155.8 1_355 yes
C3 H3 O1 0.93 2.63 3.154(5) 116.3 . yes
C5 H5 O2 0.93 2.47 3.339(4) 155.2 2_656 yes
C7 H7A O2 0.93 2.57 3.392(5) 147.7 2_656 yes
C9 H9 Br1 0.93 3.11 3.786(4) 131.1 1_455 yes
C10 H10A N3 0.93 2.64 3.186(5) 117.9 . yes
C10 H10A O12 0.93 2.45 3.238(6) 143.0 1_545 yes
C11 H11 O7 0.93 2.40 3.255(5) 152.7 1_445 yes
C17 H17 O1 0.93 2.32 3.134(5) 145.9 2_657 yes
C19 H19 O11 0.93 2.59 3.508(11) 168.5 2_666 yes
C20 H20 Br1 0.93 3.09 3.563(4) 113.4 2_656 yes
C20 H20 O2 0.93 2.58 3.122(5) 117.5 . yes
C25 H25 Br3 0.93 2.96 3.882(4) 171.5 1_665 yes
C30 H30B O8 0.97 2.46 3.338(5) 150.1 1_455 yes

_refine_diff_density_max         1.346
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.097



####################################################################### 
# 
# 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_exp_10157
_database_code_depnum_ccdc_archive 'CCDC 1975208'
loop_
_audit_author_name
_audit_author_address
'Rong-Yun Li'
;Liaocheng University
China
;
_audit_update_record             
;
2020-01-03 deposited with the CCDC.	2020-03-16 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         ?
_chemical_formula_sum            'C60 H50 Br4 N4 Ni2 O23'
_chemical_formula_weight         1632.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'
Br Br -0.6763 1.2805 '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                   7.6727(4)
_cell_length_b                   17.5244(7)
_cell_length_c                   23.0349(6)
_cell_angle_alpha                94.137(3)
_cell_angle_beta                 90.844(3)
_cell_angle_gamma                97.229(4)
_cell_volume                     3063.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8279
_cell_measurement_theta_min      3.3030
_cell_measurement_theta_max      71.2210

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             1636
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    4.559
_shelx_estimated_absorpt_T_min   0.611
_shelx_estimated_absorpt_T_max   0.634
_exptl_absorpt_correction_T_min  0.46013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22513
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.549
_diffrn_reflns_theta_max         67.245
_diffrn_reflns_theta_full        67.245
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10964
_reflns_number_gt                8864
_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       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_structure_solution    'SHELXL-2018/3 '
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0645P)²+5.7287P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10964
_refine_ls_number_parameters     843
_refine_ls_number_restraints     2406
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1397
_refine_ls_wR_factor_gt          0.1296
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      0.993
_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 0.53258(9) 0.69611(3) 0.78541(3) 0.02196(15) Uani 1 1 d . U . . .
Ni2 Ni 0.19267(9) 0.02213(4) 1.23614(3) 0.02287(16) Uani 1 1 d . U . . .
Br1 Br -0.14459(8) 0.41936(3) 0.81136(3) 0.05141(16) Uani 1 1 d . U . . .
Br2 Br 0.71598(9) 0.37345(3) 0.63661(2) 0.05353(17) Uani 1 1 d . U . . .
Br3 Br -0.22958(11) -0.26487(5) 1.37630(3) 0.0797(3) Uani 1 1 d . U . . .
Br4 Br 0.62153(12) -0.28470(5) 1.19741(4) 0.0826(3) Uani 1 1 d . U . . .
N1 N 0.6028(5) 0.59998(19) 0.73810(14) 0.0262(7) Uani 1 1 d . U . . .
N2 N 0.3234(5) 0.61264(19) 0.80070(14) 0.0263(7) Uani 1 1 d . U . . .
N3 N 0.3609(5) -0.06162(19) 1.23476(13) 0.0259(6) Uani 1 1 d . U . . .
N4 N 0.0467(5) -0.0619(2) 1.27960(14) 0.0285(7) Uani 1 1 d . U . . .
O1 O 0.0143(6) 0.8824(2) 0.55388(18) 0.0584(9) Uani 1 1 d . U . . .
O2 O -0.0299(6) 0.5984(2) 0.48276(14) 0.0498(9) Uani 1 1 d . U . . .
H2 H -0.043346 0.553449 0.469108 0.075 Uiso 1 1 calc R U . . .
O3 O 0.0580(5) 0.54307(18) 0.56029(14) 0.0463(9) Uani 1 1 d . U . . .
O4 O 0.3872(4) 0.71727(16) 0.71511(11) 0.0291(6) Uani 1 1 d . U . . .
O5 O 0.2317(6) 0.8095(2) 0.74794(15) 0.0590(11) Uani 1 1 d . U . . .
O6 O 0.8730(4) 0.77137(16) 0.87318(12) 0.0327(7) Uani 1 1 d . U . . .
O7 O 0.6661(4) 0.67051(16) 0.85905(11) 0.0286(6) Uani 1 1 d . U . . .
O8 O 0.4413(4) 0.78677(16) 0.83236(11) 0.0298(6) Uani 1 1 d . U . . .
H8A H 0.514247 0.827231 0.830572 0.045 Uiso 1 1 d R U . . .
H8B H 0.342588 0.794130 0.818072 0.045 Uiso 1 1 d R U . . .
O9 O 0.7494(4) 0.76627(15) 0.75970(12) 0.0305(6) Uani 1 1 d . U . . .
H9A H 0.762613 0.808080 0.781331 0.046 Uiso 1 1 d R U . . .
H9C H 0.734374 0.776190 0.724531 0.046 Uiso 1 1 d R U . . .
O10 O 0.9601(5) 0.85030(17) 1.08801(13) 0.0408(8) Uani 1 1 d . U . . .
H10 H 1.024991 0.880771 1.109818 0.061 Uiso 1 1 calc R U . . .
O11 O 1.0527(6) 0.7624(2) 1.14140(15) 0.0578(11) Uani 1 1 d . U . . .
O12 O 0.7796(5) 0.51525(16) 1.03307(13) 0.0364(7) Uani 1 1 d . U . . .
O13 O 0.5247(5) 0.17767(17) 0.97213(12) 0.0373(7) Uani 1 1 d . U . . .
O14 O 0.2203(4) -0.05742(18) 0.86863(12) 0.0368(7) Uani 1 1 d . U . . .
O15 O 0.0832(5) -0.12292(17) 0.93778(12) 0.0371(7) Uani 1 1 d . U . . .
H15 H 0.037695 -0.150475 0.909959 0.056 Uiso 1 1 calc R U . . .
O16 O 0.1339(4) -0.02132(15) 1.14495(11) 0.0249(6) Uani 1 1 d . U . . .
O17 O 0.3223(4) 0.07992(15) 1.16876(10) 0.0255(6) Uani 1 1 d . U . . .
O18 O 0.2877(4) 0.09841(16) 1.30267(11) 0.0299(6) Uani 1 1 d . U . . .
O19 O 0.3616(5) 0.00743(19) 1.35617(13) 0.0469(9) Uani 1 1 d . U . . .
O20 O -0.0176(4) 0.08378(18) 1.22831(12) 0.0379(7) Uani 1 1 d . U . . .
H20B H -0.064540 0.089413 1.261280 0.057 Uiso 1 1 d R U . . .
H20D H -0.092670 0.059303 1.204020 0.057 Uiso 1 1 d R U . . .
O21 O 0.5528(7) 0.0695(2) 1.55780(16) 0.0668(12) Uani 1 1 d . U . . .
H21 H 0.604702 0.057472 1.586479 0.100 Uiso 1 1 calc R U . . .
O22 O 0.6689(7) 0.1869(3) 1.58917(17) 0.0741(13) Uani 1 1 d . U . . .
O23 O 0.4277(5) 0.3429(2) 1.43369(15) 0.0478(8) Uani 1 1 d . U . . .
C1 C -0.0787(10) 0.9770(4) 0.4986(4) 0.0785(17) Uani 1 1 d . U . . .
H1A H -0.141453 0.983873 0.462821 0.094 Uiso 1 1 calc R U . . .
H1B H -0.149736 0.991314 0.531088 0.094 Uiso 1 1 calc R U . . .
C2 C -0.0471(10) 0.8883(4) 0.5003(3) 0.0652(14) Uani 1 1 d . U . . .
H2A H -0.156179 0.854372 0.492712 0.078 Uiso 1 1 calc R U . . .
H2B H 0.037524 0.875158 0.471585 0.078 Uiso 1 1 calc R U . . .
C3 C 0.0521(6) 0.8146(2) 0.57322(19) 0.0333(9) Uani 1 1 d . U . . .
C4 C 0.0167(6) 0.7431(3) 0.54211(18) 0.0331(9) Uani 1 1 d . U . . .
H4 H -0.036774 0.738744 0.505323 0.040 Uiso 1 1 calc R U . . .
C5 C 0.0624(6) 0.6786(2) 0.56677(17) 0.0291(8) Uani 1 1 d . U . . .
C6 C 0.1473(6) 0.6844(2) 0.62105(17) 0.0273(8) Uani 1 1 d . U . . .
H6 H 0.181831 0.640859 0.636465 0.033 Uiso 1 1 calc R U . . .
C7 C 0.1796(6) 0.7555(2) 0.65165(17) 0.0277(8) Uani 1 1 d . U . . .
C9 C 0.0290(6) 0.6014(3) 0.53649(18) 0.0327(9) Uani 1 1 d . U . . .
C10 C 0.2727(6) 0.7615(2) 0.70947(17) 0.0294(8) Uani 1 1 d . U . . .
C11 C 0.7489(6) 0.5981(3) 0.70692(18) 0.0334(9) Uani 1 1 d . U . . .
H11 H 0.827044 0.643079 0.706182 0.040 Uiso 1 1 calc R U . . .
C12 C 0.7883(7) 0.5320(3) 0.67580(19) 0.0365(9) Uani 1 1 d . U . . .
H12 H 0.891310 0.532044 0.655044 0.044 Uiso 1 1 calc R U . . .
C13 C 0.6696(6) 0.4666(2) 0.67670(18) 0.0334(9) Uani 1 1 d . U . . .
C14 C 0.5173(6) 0.4672(2) 0.70782(19) 0.0332(9) Uani 1 1 d . U . . .
H14 H 0.436428 0.422998 0.708367 0.040 Uiso 1 1 calc R U . . .
C15 C 0.4884(6) 0.5354(2) 0.73822(17) 0.0278(8) Uani 1 1 d . U . . .
C16 C 0.3280(6) 0.5428(2) 0.77243(17) 0.0275(8) Uani 1 1 d . U . . .
C17 C 0.1904(6) 0.4839(2) 0.77502(19) 0.0335(9) Uani 1 1 d . U . . .
H17 H 0.196444 0.435416 0.756386 0.040 Uiso 1 1 calc R U . . .
C18 C 0.0450(6) 0.4987(3) 0.80576(19) 0.0335(9) Uani 1 1 d . U . . .
C19 C 0.0360(7) 0.5704(3) 0.8336(2) 0.0398(10) Uani 1 1 d . U . . .
H19 H -0.062904 0.581083 0.853950 0.048 Uiso 1 1 calc R U . . .
C20 C 0.1788(6) 0.6253(3) 0.83004(19) 0.0358(9) Uani 1 1 d . U . . .
H20A H 0.175095 0.673836 0.848912 0.043 Uiso 1 1 calc R U . . .
C21 C 0.7821(5) 0.7131(2) 0.88956(16) 0.0223(7) Uani 1 1 d . U . . .
C22 C 0.8116(5) 0.6892(2) 0.95068(16) 0.0223(7) Uani 1 1 d . U . . .
C23 C 0.7742(5) 0.6120(2) 0.96192(16) 0.0228(7) Uani 1 1 d . U . . .
H23 H 0.726967 0.575624 0.932639 0.027 Uiso 1 1 calc R U . . .
C24 C 0.8080(6) 0.5895(2) 1.01766(17) 0.0259(8) Uani 1 1 d . U . . .
C25 C 0.8745(6) 0.6439(2) 1.06153(17) 0.0271(8) Uani 1 1 d . U . . .
H25 H 0.898297 0.628655 1.098351 0.033 Uiso 1 1 calc R U . . .
C26 C 0.9055(5) 0.7211(2) 1.05068(16) 0.0250(8) Uani 1 1 d . U . . .
C27 C 0.8752(5) 0.7439(2) 0.99506(16) 0.0235(7) Uani 1 1 d . U . . .
H27 H 0.897455 0.795691 0.987703 0.028 Uiso 1 1 calc R U . . .
C28 C 0.9818(6) 0.7788(2) 1.09871(17) 0.0289(8) Uani 1 1 d . U . . .
C29 C 0.7218(6) 0.4552(2) 0.98910(17) 0.0287(8) Uani 1 1 d . U . . .
H29A H 0.806859 0.453987 0.958407 0.034 Uiso 1 1 calc R U . . .
H29B H 0.609825 0.463427 0.972174 0.034 Uiso 1 1 calc R U . . .
C30 C 0.7039(6) 0.3807(2) 1.01868(18) 0.0303(8) Uani 1 1 d . U . . .
H30A H 0.627889 0.385084 1.051706 0.036 Uiso 1 1 calc R U . . .
H30B H 0.818464 0.372054 1.033287 0.036 Uiso 1 1 calc R U . . .
C31 C 0.6285(6) 0.3116(2) 0.97785(18) 0.0293(8) Uani 1 1 d . U . . .
H31A H 0.519031 0.321756 0.960192 0.035 Uiso 1 1 calc R U . . .
H31B H 0.710266 0.303169 0.947020 0.035 Uiso 1 1 calc R U . . .
C32 C 0.5964(6) 0.2406(2) 1.01178(18) 0.0294(8) Uani 1 1 d . U . . .
H32A H 0.705842 0.229656 1.029047 0.035 Uiso 1 1 calc R U . . .
H32B H 0.514939 0.248706 1.042744 0.035 Uiso 1 1 calc R U . . .
C33 C 0.4264(5) 0.1159(2) 0.99317(16) 0.0236(7) Uani 1 1 d . U . . .
C34 C 0.3596(5) 0.0586(2) 0.95123(16) 0.0236(7) Uani 1 1 d . U . . .
H34 H 0.386496 0.063690 0.912352 0.028 Uiso 1 1 calc R U . . .
C35 C 0.2540(5) -0.0059(2) 0.96660(15) 0.0207(7) Uani 1 1 d . U . . .
C36 C 0.2120(5) -0.0147(2) 1.02479(15) 0.0216(7) Uani 1 1 d . U . . .
H36 H 0.138558 -0.057712 1.035098 0.026 Uiso 1 1 calc R U . . .
C37 C 0.2820(5) 0.0420(2) 1.06692(15) 0.0205(7) Uani 1 1 d . U . . .
C38 C 0.3905(5) 0.1070(2) 1.05145(16) 0.0236(7) Uani 1 1 d . U . . .
H38 H 0.438633 0.144194 1.080011 0.028 Uiso 1 1 calc R U . . .
C39 C 0.1850(5) -0.0646(2) 0.91890(16) 0.0237(8) Uani 1 1 d . U . . .
C40 C 0.2433(5) 0.0325(2) 1.12972(15) 0.0208(7) Uani 1 1 d . U . . .
C41 C 0.5152(6) -0.0592(3) 1.20808(18) 0.0334(8) Uani 1 1 d . U . . .
H41 H 0.567141 -0.012277 1.196148 0.040 Uiso 1 1 calc R U . . .
C42 C 0.6002(7) -0.1234(3) 1.1975(2) 0.0422(10) Uani 1 1 d . U . . .
H42 H 0.708273 -0.119967 1.179515 0.051 Uiso 1 1 calc R U . . .
C43 C 0.5202(7) -0.1925(3) 1.2145(2) 0.0406(10) Uani 1 1 d . U . . .
C44 C 0.3663(7) -0.1962(3) 1.2438(2) 0.0382(9) Uani 1 1 d . U . . .
H44 H 0.314690 -0.242420 1.257054 0.046 Uiso 1 1 calc R U . . .
C45 C 0.2891(6) -0.1293(2) 1.25311(17) 0.0281(8) Uani 1 1 d . U . . .
C46 C 0.1187(6) -0.1272(2) 1.28267(17) 0.0293(8) Uani 1 1 d . U . . .
C47 C 0.0394(7) -0.1888(3) 1.31122(19) 0.0389(10) Uani 1 1 d . U . . .
H47 H 0.090829 -0.233924 1.312699 0.047 Uiso 1 1 calc R U . . .
C48 C -0.1180(7) -0.1809(3) 1.33734(19) 0.0422(10) Uani 1 1 d . U . . .
C49 C -0.1939(7) -0.1150(3) 1.3350(2) 0.0461(11) Uani 1 1 d . U . . .
H49 H -0.301055 -0.109876 1.352248 0.055 Uiso 1 1 calc R U . . .
C50 C -0.1064(7) -0.0564(3) 1.30611(19) 0.0390(10) Uani 1 1 d . U . . .
H50 H -0.155523 -0.010630 1.304861 0.047 Uiso 1 1 calc R U . . .
C51 C 0.3491(6) 0.0759(2) 1.34933(17) 0.0301(8) Uani 1 1 d . U . . .
C52 C 0.4073(6) 0.1371(2) 1.39850(16) 0.0293(8) Uani 1 1 d . U . . .
C53 C 0.3906(6) 0.2143(3) 1.39421(18) 0.0331(9) Uani 1 1 d . U . . .
H53 H 0.342789 0.230358 1.360545 0.040 Uiso 1 1 calc R U . . .
C54 C 0.4464(6) 0.2681(3) 1.44102(19) 0.0359(9) Uani 1 1 d . U . . .
C55 C 0.5141(7) 0.2438(3) 1.49120(18) 0.0396(10) Uani 1 1 d . U . . .
H55 H 0.551004 0.279538 1.522109 0.048 Uiso 1 1 calc R U . . .
C56 C 0.5274(6) 0.1666(3) 1.49588(18) 0.0358(9) Uani 1 1 d . U . . .
C57 C 0.4761(6) 0.1131(3) 1.44917(17) 0.0335(9) Uani 1 1 d . U . . .
H57 H 0.487848 0.061262 1.451934 0.040 Uiso 1 1 calc R U . . .
C58 C 0.5916(7) 0.1425(3) 1.5524(2) 0.0445(11) Uani 1 1 d . U . . .
C59 C 0.4853(8) 0.3938(3) 1.4846(2) 0.0524(12) Uani 1 1 d . U . . .
H59A H 0.606303 0.388702 1.494617 0.063 Uiso 1 1 calc R U . . .
H59B H 0.413278 0.379765 1.517429 0.063 Uiso 1 1 calc R U . . .
C60 C 0.4705(9) 0.4733(3) 1.4726(2) 0.0551(13) Uani 1 1 d . U . . .
H60A H 0.349814 0.478391 1.462154 0.066 Uiso 1 1 calc R U . . .
H60B H 0.543924 0.487732 1.440235 0.066 Uiso 1 1 calc R U . . .
C8O C 0.1294(6) 0.8198(2) 0.62846(19) 0.0337(9) Uani 1 1 d . U . . .
H8O H 0.147401 0.867143 0.650020 0.040 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 O4 2.035(3) . ?
Ni1 O8 2.059(3) . ?
Ni1 O9 2.061(3) . ?
Ni1 N1 2.073(3) . ?
Ni1 O7 2.074(3) . ?
Ni1 N2 2.083(4) . ?
Ni2 O18 2.023(3) . ?
Ni2 N4 2.063(4) . ?
Ni2 O20 2.064(3) . ?
Ni2 N3 2.072(4) . ?
Ni2 O17 2.108(3) . ?
Ni2 O16 2.202(3) . ?
Ni2 C40 2.504(4) . ?
Br1 C18 1.894(4) . ?
Br2 C13 1.892(4) . ?
Br3 C48 1.897(5) . ?
Br4 C43 1.898(5) . ?
N1 C15 1.343(5) . ?
N1 C11 1.343(6) . ?
N2 C20 1.342(6) . ?
N2 C16 1.349(5) . ?
N3 C41 1.339(6) . ?
N3 C45 1.343(5) . ?
N4 C46 1.338(6) . ?
N4 C50 1.343(6) . ?
O1 C2 1.330(7) . ?
O1 C3 1.362(5) . ?
O2 C9 1.306(5) . ?
O3 C9 1.237(6) . ?
O4 C10 1.254(5) . ?
O5 C10 1.249(5) . ?
O6 C21 1.248(5) . ?
O7 C21 1.258(5) . ?
O10 C28 1.324(5) . ?
O11 C28 1.187(5) . ?
O12 C24 1.365(5) . ?
O12 C29 1.430(5) . ?
O13 C33 1.362(5) . ?
O13 C32 1.428(5) . ?
O14 C39 1.205(5) . ?
O15 C39 1.311(5) . ?
O16 C40 1.255(5) . ?
O17 C40 1.271(4) . ?
O18 C51 1.275(5) . ?
O19 C51 1.236(5) . ?
O21 C58 1.293(7) . ?
O22 C58 1.202(6) . ?
O23 C54 1.359(6) . ?
O23 C59 1.450(6) . ?
C1 C1 1.364(14) 2_576 ?
C1 C2 1.606(9) . ?
C3 C8O 1.388(6) . ?
C3 C4 1.392(6) . ?
C4 C5 1.382(6) . ?
C5 C6 1.392(6) . ?
C5 C9 1.467(6) . ?
C6 C7 1.379(6) . ?
C7 C8O 1.376(6) . ?
C7 C10 1.493(5) . ?
C11 C12 1.385(6) . ?
C12 C13 1.374(7) . ?
C13 C14 1.381(7) . ?
C14 C15 1.385(6) . ?
C15 C16 1.486(6) . ?
C16 C17 1.386(6) . ?
C17 C18 1.372(7) . ?
C18 C19 1.378(7) . ?
C19 C20 1.372(7) . ?
C21 C22 1.519(5) . ?
C22 C27 1.389(5) . ?
C22 C23 1.391(5) . ?
C23 C24 1.400(5) . ?
C24 C25 1.384(5) . ?
C25 C26 1.384(6) . ?
C26 C27 1.395(5) . ?
C26 C28 1.504(5) . ?
C29 C30 1.508(5) . ?
C30 C31 1.525(5) . ?
C31 C32 1.514(5) . ?
C33 C34 1.386(5) . ?
C33 C38 1.390(5) . ?
C34 C35 1.376(5) . ?
C35 C36 1.398(5) . ?
C35 C39 1.492(5) . ?
C36 C37 1.389(5) . ?
C37 C38 1.395(5) . ?
C37 C40 1.498(5) . ?
C41 C42 1.378(7) . ?
C42 C43 1.374(7) . ?
C43 C44 1.365(7) . ?
C44 C45 1.384(6) . ?
C45 C46 1.486(6) . ?
C46 C47 1.384(6) . ?
C47 C48 1.375(7) . ?
C48 C49 1.361(8) . ?
C49 C50 1.374(7) . ?
C51 C52 1.524(5) . ?
C52 C53 1.384(6) . ?
C52 C57 1.388(6) . ?
C53 C54 1.405(6) . ?
C54 C55 1.377(7) . ?
C55 C56 1.382(7) . ?
C56 C57 1.393(6) . ?
C56 C58 1.493(7) . ?
C59 C60 1.458(8) . ?
C60 C60 1.542(10) 2_668 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 O8 89.56(11) . . ?
O4 Ni1 O9 92.13(12) . . ?
O8 Ni1 O9 91.85(12) . . ?
O4 Ni1 N1 88.58(12) . . ?
O8 Ni1 N1 175.11(14) . . ?
O9 Ni1 N1 92.74(13) . . ?
O4 Ni1 O7 176.25(13) . . ?
O8 Ni1 O7 89.97(11) . . ?
O9 Ni1 O7 91.60(12) . . ?
N1 Ni1 O7 91.59(12) . . ?
O4 Ni1 N2 85.48(13) . . ?
O8 Ni1 N2 97.03(13) . . ?
O9 Ni1 N2 170.79(12) . . ?
N1 Ni1 N2 78.32(14) . . ?
O7 Ni1 N2 90.89(12) . . ?
O18 Ni2 N4 101.71(12) . . ?
O18 Ni2 O20 88.63(12) . . ?
N4 Ni2 O20 92.53(15) . . ?
O18 Ni2 N3 104.01(13) . . ?
N4 Ni2 N3 79.24(14) . . ?
O20 Ni2 N3 166.02(13) . . ?
O18 Ni2 O17 97.10(11) . . ?
N4 Ni2 O17 160.97(12) . . ?
O20 Ni2 O17 90.79(13) . . ?
N3 Ni2 O17 93.49(12) . . ?
O18 Ni2 O16 156.96(11) . . ?
N4 Ni2 O16 100.96(12) . . ?
O20 Ni2 O16 86.30(11) . . ?
N3 Ni2 O16 84.24(12) . . ?
O17 Ni2 O16 60.55(10) . . ?
O18 Ni2 C40 127.42(12) . . ?
N4 Ni2 C40 130.87(13) . . ?
O20 Ni2 C40 88.53(12) . . ?
N3 Ni2 C40 88.43(12) . . ?
O17 Ni2 C40 30.49(11) . . ?
O16 Ni2 C40 30.07(11) . . ?
C15 N1 C11 118.5(4) . . ?
C15 N1 Ni1 116.0(3) . . ?
C11 N1 Ni1 125.5(3) . . ?
C20 N2 C16 118.5(4) . . ?
C20 N2 Ni1 125.5(3) . . ?
C16 N2 Ni1 115.5(3) . . ?
C41 N3 C45 118.2(4) . . ?
C41 N3 Ni2 126.4(3) . . ?
C45 N3 Ni2 114.2(3) . . ?
C46 N4 C50 118.1(4) . . ?
C46 N4 Ni2 114.9(3) . . ?
C50 N4 Ni2 127.0(3) . . ?
C2 O1 C3 122.9(5) . . ?
C10 O4 Ni1 131.7(3) . . ?
C21 O7 Ni1 128.4(2) . . ?
C24 O12 C29 118.6(3) . . ?
C33 O13 C32 119.1(3) . . ?
C40 O16 Ni2 88.4(2) . . ?
C40 O17 Ni2 92.2(2) . . ?
C51 O18 Ni2 121.2(3) . . ?
C54 O23 C59 112.5(4) . . ?
C1 C1 C2 109.8(8) 2_576 . ?
O1 C2 C1 105.0(5) . . ?
O1 C3 C8O 115.5(4) . . ?
O1 C3 C4 124.8(4) . . ?
C8O C3 C4 119.7(4) . . ?
C5 C4 C3 118.9(4) . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 C9 121.8(4) . . ?
C6 C5 C9 116.9(4) . . ?
C7 C6 C5 119.1(4) . . ?
C8O C7 C6 120.2(4) . . ?
C8O C7 C10 120.9(4) . . ?
C6 C7 C10 118.9(4) . . ?
O3 C9 O2 122.2(4) . . ?
O3 C9 C5 121.7(4) . . ?
O2 C9 C5 116.0(4) . . ?
O5 C10 O4 125.4(4) . . ?
O5 C10 C7 118.2(4) . . ?
O4 C10 C7 116.4(3) . . ?
N1 C11 C12 122.9(4) . . ?
C13 C12 C11 117.6(4) . . ?
C12 C13 C14 120.7(4) . . ?
C12 C13 Br2 120.2(4) . . ?
C14 C13 Br2 119.1(3) . . ?
C13 C14 C15 118.1(4) . . ?
N1 C15 C14 122.2(4) . . ?
N1 C15 C16 115.2(3) . . ?
C14 C15 C16 122.6(4) . . ?
N2 C16 C17 121.5(4) . . ?
N2 C16 C15 114.9(4) . . ?
C17 C16 C15 123.6(4) . . ?
C18 C17 C16 118.4(4) . . ?
C17 C18 C19 120.9(4) . . ?
C17 C18 Br1 119.7(3) . . ?
C19 C18 Br1 119.3(4) . . ?
C20 C19 C18 117.4(4) . . ?
N2 C20 C19 123.3(4) . . ?
O6 C21 O7 125.2(3) . . ?
O6 C21 C22 119.1(3) . . ?
O7 C21 C22 115.7(3) . . ?
C27 C22 C23 120.2(3) . . ?
C27 C22 C21 120.4(3) . . ?
C23 C22 C21 119.4(3) . . ?
C22 C23 C24 119.5(3) . . ?
O12 C24 C25 115.5(3) . . ?
O12 C24 C23 124.3(3) . . ?
C25 C24 C23 120.2(4) . . ?
C24 C25 C26 120.1(4) . . ?
C25 C26 C27 120.1(4) . . ?
C25 C26 C28 119.0(3) . . ?
C27 C26 C28 120.7(3) . . ?
C22 C27 C26 119.9(3) . . ?
O11 C28 O10 123.8(4) . . ?
O11 C28 C26 124.1(4) . . ?
O10 C28 C26 112.1(3) . . ?
O12 C29 C30 106.5(3) . . ?
C29 C30 C31 112.4(3) . . ?
C32 C31 C30 109.6(3) . . ?
O13 C32 C31 107.7(3) . . ?
O13 C33 C34 114.8(3) . . ?
O13 C33 C38 125.6(3) . . ?
C34 C33 C38 119.6(4) . . ?
C35 C34 C33 120.6(3) . . ?
C34 C35 C36 120.6(3) . . ?
C34 C35 C39 117.5(3) . . ?
C36 C35 C39 121.9(3) . . ?
C37 C36 C35 118.8(3) . . ?
C36 C37 C38 120.7(3) . . ?
C36 C37 C40 119.6(3) . . ?
C38 C37 C40 119.7(3) . . ?
C33 C38 C37 119.8(3) . . ?
O14 C39 O15 124.8(3) . . ?
O14 C39 C35 122.4(4) . . ?
O15 C39 C35 112.8(3) . . ?
O16 C40 O17 118.8(3) . . ?
O16 C40 C37 121.5(3) . . ?
O17 C40 C37 119.6(3) . . ?
O16 C40 Ni2 61.56(18) . . ?
O17 C40 Ni2 57.27(18) . . ?
C37 C40 Ni2 176.9(3) . . ?
N3 C41 C42 122.8(4) . . ?
C43 C42 C41 117.9(5) . . ?
C44 C43 C42 120.6(5) . . ?
C44 C43 Br4 118.9(4) . . ?
C42 C43 Br4 120.5(4) . . ?
C43 C44 C45 118.2(4) . . ?
N3 C45 C44 122.3(4) . . ?
N3 C45 C46 115.0(4) . . ?
C44 C45 C46 122.7(4) . . ?
N4 C46 C47 122.2(4) . . ?
N4 C46 C45 115.5(4) . . ?
C47 C46 C45 122.3(4) . . ?
C48 C47 C46 117.7(5) . . ?
C49 C48 C47 121.2(5) . . ?
C49 C48 Br3 120.4(4) . . ?
C47 C48 Br3 118.4(4) . . ?
C48 C49 C50 117.5(5) . . ?
N4 C50 C49 123.2(5) . . ?
O19 C51 O18 123.0(4) . . ?
O19 C51 C52 119.5(4) . . ?
O18 C51 C52 117.5(4) . . ?
C53 C52 C57 120.1(4) . . ?
C53 C52 C51 122.2(4) . . ?
C57 C52 C51 117.7(4) . . ?
C52 C53 C54 119.6(4) . . ?
O23 C54 C55 123.5(4) . . ?
O23 C54 C53 116.5(4) . . ?
C55 C54 C53 120.0(4) . . ?
C54 C55 C56 120.4(4) . . ?
C55 C56 C57 120.0(4) . . ?
C55 C56 C58 118.3(4) . . ?
C57 C56 C58 121.7(5) . . ?
C52 C57 C56 119.9(4) . . ?
O22 C58 O21 124.0(5) . . ?
O22 C58 C56 123.3(5) . . ?
O21 C58 C56 112.7(4) . . ?
O23 C59 C60 109.5(5) . . ?
C59 C60 C60 109.0(6) . 2_668 ?
C7 C8O C3 120.7(4) . . ?

_refine_diff_density_max         1.919
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.102



