# Supplementary Information (SI) for Catalysis Science & Technology.
# 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_S0928
_database_code_depnum_ccdc_archive 'CCDC 2360895'
loop_
_audit_author_name
_audit_author_address
'Jeffrey Ovens'
;University of Ottawa
Canada
;
_audit_update_record             
;
2024-07-22 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
#===============================================================================
# 5. CHEMICAL DATA

_chemical_name_systematic        
; 
;

_chemical_formula_sum            'C44 H49 Br2 Cl2 N3 Ni'
_chemical_formula_moiety         'C44 H49 Br2 Cl2 N3 Ni'
_chemical_formula_weight         909.29
#=============================================================
# 6. CRYSTAL DATA

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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'

#------------------------------------------------
_cell_length_a                   9.5290(6)
_cell_length_b                   9.7708(6)
_cell_length_c                   13.6707(9)
_cell_angle_alpha                93.325(2)
_cell_angle_beta                 107.464(2)
_cell_angle_gamma                114.272(2)
_cell_volume                     1082.49(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      26.57

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_min          0.236
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_max          0.918

_exptl_crystal_density_diffrn    1.395
_exptl_crystal_F_000             466
_exptl_absorpt_coefficient_mu    2.450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5368
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   SADABS

#=============================================================================
# 7. EXPERIMENTAL DATA

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω and φ scans'
_diffrn_ambient_temperature      203(2)
_diffrn_reflns_number            12372
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.597
_diffrn_reflns_theta_max         26.576
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_point_group_measured_fraction_full 0.934


#==========================================================================
# 8. REFINEMENT DATA

_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.
;

_reflns_number_total             8201
_reflns_number_gt                7740
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_max     0.828
_reflns_Friedel_fraction_full    0.870

_refine_special_details          none

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3246 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8201
_refine_ls_number_parameters     477
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0749
_refine_ls_wR_factor_gt          0.0732
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0170P)²] where P=(Fo²+2Fc²)/3'

#---------------------------------------------------------


#========================================================== 
# 9. General computing 

_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_cell_refinement       'Bruker SAINT'
_computing_structure_solution    
; 
 SHELXT 2014/5 (Sheldrick, 2014)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_shelx_SHELXL_version_number     2018/3

#===================================================================
# 10.  ATOMIC COORDINATES AND THERMAL PARAMETERS

_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom

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'
Br Br -0.2901 2.4595 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================
# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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
Br1 Br 0.80683(4) 0.65514(4) 0.59694(3) 0.03288(12) Uani 1 1 d . . . . .
Cl1 Cl 1.0303(4) 0.8821(4) 0.9288(2) 0.1256(11) Uani 1 1 d . . . . .
Ni1 Ni 0.52124(6) 0.47662(5) 0.48985(4) 0.02142(12) Uani 1 1 d . . . . .
N1 N 0.4300(4) 0.4389(4) 0.6201(3) 0.0205(7) Uani 1 1 d . . . . .
N2 N 0.4592(4) 0.6446(4) 0.5044(3) 0.0216(7) Uani 1 1 d . . . . .
Cl2 Cl 0.7680(4) 0.9700(4) 0.8847(2) 0.1208(10) Uani 1 1 d . . . . .
N3 N 0.5301(4) 0.5658(4) 0.3485(3) 0.0233(7) Uani 1 1 d . . . . .
C1 C 0.3818(5) 0.3010(5) 0.6640(3) 0.0221(9) Uani 1 1 d . . . . .
C2 C 0.5017(5) 0.2789(5) 0.7410(3) 0.0249(9) Uani 1 1 d . . . . .
C3 C 0.4495(6) 0.1452(5) 0.7807(4) 0.0335(11) Uani 1 1 d . . . . .
H3 H 0.526719 0.129008 0.833824 0.040 Uiso 1 1 calc R U . . .
C4 C 0.2872(7) 0.0374(6) 0.7433(4) 0.0387(12) Uani 1 1 d . . . . .
H4 H 0.254244 -0.051176 0.771424 0.046 Uiso 1 1 calc R U . . .
C5 C 0.1728(6) 0.0586(5) 0.6648(4) 0.0357(11) Uani 1 1 d . . . . .
H5 H 0.062759 -0.017425 0.638901 0.043 Uiso 1 1 calc R U . . .
C6 C 0.2160(5) 0.1898(5) 0.6228(3) 0.0266(9) Uani 1 1 d . . . . .
C7 C 0.7653(6) 0.3184(6) 0.7237(4) 0.0417(13) Uani 1 1 d . . . . .
H7A H 0.714645 0.302635 0.648265 0.062 Uiso 1 1 calc R U . . .
H7B H 0.751306 0.220802 0.742770 0.062 Uiso 1 1 calc R U . . .
H7C H 0.881864 0.387866 0.745511 0.062 Uiso 1 1 calc R U . . .
C8 C 0.6842(6) 0.3872(5) 0.7775(4) 0.0291(10) Uani 1 1 d . . . . .
H8 H 0.695916 0.483941 0.753979 0.035 Uiso 1 1 calc R U . . .
C9 C 0.7706(7) 0.4272(7) 0.8963(4) 0.0455(13) Uani 1 1 d . . . . .
H9A H 0.765220 0.334926 0.921372 0.068 Uiso 1 1 calc R U . . .
H9B H 0.716630 0.470933 0.928793 0.068 Uiso 1 1 calc R U . . .
H9C H 0.884938 0.501065 0.914214 0.068 Uiso 1 1 calc R U . . .
C10 C 0.0120(8) 0.0748(9) 0.4405(5) 0.0671(19) Uani 1 1 d . . . . .
H10A H -0.064914 0.091157 0.383316 0.101 Uiso 1 1 calc R U . . .
H10B H -0.045059 -0.022683 0.458172 0.101 Uiso 1 1 calc R U . . .
H10C H 0.100058 0.073657 0.419320 0.101 Uiso 1 1 calc R U . . .
C11 C 0.0843(6) 0.2042(6) 0.5360(4) 0.0415(12) Uani 1 1 d . . . . .
H11 H 0.135330 0.303163 0.515207 0.050 Uiso 1 1 calc R U . . .
C12 C -0.0511(7) 0.2044(8) 0.5741(6) 0.0590(16) Uani 1 1 d . . . . .
H12A H -0.128184 0.225227 0.520133 0.089 Uiso 1 1 calc R U . . .
H12B H -0.002122 0.283182 0.637274 0.089 Uiso 1 1 calc R U . . .
H12C H -0.108789 0.104943 0.589185 0.089 Uiso 1 1 calc R U . . .
C13 C 0.3449(5) 0.5660(5) 0.7388(3) 0.0242(9) Uani 1 1 d . . . . .
C14 C 0.4291(7) 0.5583(6) 0.8392(4) 0.0362(11) Uani 1 1 d . . . . .
H14 H 0.516959 0.532785 0.851247 0.043 Uiso 1 1 calc R U . . .
C15 C 0.3823(8) 0.5888(6) 0.9215(4) 0.0475(14) Uani 1 1 d . . . . .
H15 H 0.438756 0.583965 0.989525 0.057 Uiso 1 1 calc R U . . .
C16 C 0.2533(7) 0.6262(6) 0.9041(4) 0.0467(13) Uani 1 1 d . . . . .
H16 H 0.223199 0.647474 0.960516 0.056 Uiso 1 1 calc R U . . .
C17 C 0.1693(7) 0.6326(6) 0.8057(4) 0.0405(12) Uani 1 1 d . . . . .
H17 H 0.081811 0.658552 0.794465 0.049 Uiso 1 1 calc R U . . .
C18 C 0.2127(6) 0.6011(5) 0.7228(4) 0.0299(10) Uani 1 1 d . . . . .
H18 H 0.152784 0.603147 0.654820 0.036 Uiso 1 1 calc R U . . .
C19 C 0.4029(5) 0.5487(5) 0.6513(3) 0.0219(8) Uani 1 1 d . . . . .
C20 C 0.4356(5) 0.6769(5) 0.5920(3) 0.0221(8) Uani 1 1 d . . . . .
C21 C 0.4449(6) 0.8189(5) 0.6242(4) 0.0296(10) Uani 1 1 d . . . . .
H21 H 0.428419 0.841147 0.686436 0.035 Uiso 1 1 calc R U . . .
C22 C 0.4791(6) 0.9266(5) 0.5625(4) 0.0348(11) Uani 1 1 d . . . . .
H22 H 0.485018 1.023215 0.582091 0.042 Uiso 1 1 calc R U . . .
C23 C 0.5045(6) 0.8915(5) 0.4719(3) 0.0302(10) Uani 1 1 d . . . . .
H23 H 0.529779 0.964446 0.429987 0.036 Uiso 1 1 calc R U . . .
C24 C 0.4923(5) 0.7481(5) 0.4437(3) 0.0231(9) Uani 1 1 d . . . . .
C25 C 0.5151(5) 0.6903(5) 0.3485(3) 0.0231(9) Uani 1 1 d . . . . .
C26 C 0.5122(6) 0.7801(5) 0.2637(3) 0.0278(9) Uani 1 1 d . . . . .
C27 C 0.3932(7) 0.8331(6) 0.2318(4) 0.0413(12) Uani 1 1 d . . . . .
H27 H 0.309888 0.806048 0.260666 0.050 Uiso 1 1 calc R U . . .
C28 C 0.3966(9) 0.9246(7) 0.1583(5) 0.0564(16) Uani 1 1 d . . . . .
H28 H 0.317516 0.961529 0.138549 0.068 Uiso 1 1 calc R U . . .
C29 C 0.5154(10) 0.9610(7) 0.1146(5) 0.0621(19) Uani 1 1 d . . . . .
H29 H 0.516364 1.021351 0.063416 0.074 Uiso 1 1 calc R U . . .
C30 C 0.6351(8) 0.9095(6) 0.1451(4) 0.0531(15) Uani 1 1 d . . . . .
H30 H 0.717652 0.936473 0.115590 0.064 Uiso 1 1 calc R U . . .
C31 C 0.6320(6) 0.8181(5) 0.2195(4) 0.0343(11) Uani 1 1 d . . . . .
H31 H 0.711891 0.782112 0.239707 0.041 Uiso 1 1 calc R U . . .
C32 C 0.5234(5) 0.4832(5) 0.2540(3) 0.0245(9) Uani 1 1 d . . . . .
C33 C 0.6699(6) 0.4935(6) 0.2435(4) 0.0318(10) Uani 1 1 d . . . . .
C34 C 0.6534(7) 0.4112(7) 0.1503(4) 0.0449(13) Uani 1 1 d . . . . .
H34 H 0.748459 0.416802 0.139690 0.054 Uiso 1 1 calc R U . . .
C35 C 0.5017(8) 0.3219(6) 0.0734(4) 0.0460(14) Uani 1 1 d . . . . .
H35 H 0.494217 0.270866 0.010171 0.055 Uiso 1 1 calc R U . . .
C36 C 0.3626(7) 0.3081(6) 0.0897(4) 0.0386(12) Uani 1 1 d . . . . .
H36 H 0.259443 0.242638 0.038408 0.046 Uiso 1 1 calc R U . . .
C37 C 0.3681(6) 0.3878(5) 0.1797(3) 0.0315(10) Uani 1 1 d . . . . .
C38 C 0.9691(8) 0.6895(9) 0.2888(6) 0.071(2) Uani 1 1 d . . . . .
H38A H 0.997225 0.628437 0.246878 0.107 Uiso 1 1 calc R U . . .
H38B H 1.066411 0.757019 0.348473 0.107 Uiso 1 1 calc R U . . .
H38C H 0.927648 0.750440 0.246506 0.107 Uiso 1 1 calc R U . . .
C39 C 0.8360(7) 0.5828(7) 0.3278(5) 0.0487(14) Uani 1 1 d . . . . .
H39 H 0.823648 0.648431 0.379318 0.058 Uiso 1 1 calc R U . . .
C40 C 0.8926(9) 0.4763(10) 0.3852(5) 0.072(2) Uani 1 1 d . . . . .
H40A H 0.807069 0.408267 0.408375 0.108 Uiso 1 1 calc R U . . .
H40B H 0.992125 0.536458 0.445555 0.108 Uiso 1 1 calc R U . . .
H40C H 0.914988 0.416092 0.338507 0.108 Uiso 1 1 calc R U . . .
C41 C 0.1110(7) 0.4217(8) 0.1127(5) 0.0579(16) Uani 1 1 d . . . . .
H41A H 0.088403 0.369861 0.043024 0.087 Uiso 1 1 calc R U . . .
H41B H 0.174551 0.531416 0.120642 0.087 Uiso 1 1 calc R U . . .
H41C H 0.007967 0.400884 0.122404 0.087 Uiso 1 1 calc R U . . .
C42 C 0.2075(6) 0.3642(7) 0.1933(4) 0.0438(13) Uani 1 1 d . . . . .
H42 H 0.234771 0.422933 0.263444 0.053 Uiso 1 1 calc R U . . .
C43 C 0.0991(8) 0.1918(8) 0.1884(5) 0.070(2) Uani 1 1 d . . . . .
H43A H 0.056906 0.134242 0.117229 0.105 Uiso 1 1 calc R U . . .
H43B H 0.007792 0.181677 0.210010 0.105 Uiso 1 1 calc R U . . .
H43C H 0.165131 0.152060 0.234993 0.105 Uiso 1 1 calc R U . . .
C45 C 0.9058(13) 0.9364(13) 0.8395(7) 0.114(4) Uani 1 1 d . . . . .
H45A H 0.843516 0.855898 0.775515 0.136 Uiso 1 1 calc R U . . .
H45B H 0.974378 1.030103 0.821211 0.136 Uiso 1 1 calc R U . . .
Br2 Br 0.45856(6) 0.22288(5) 0.42341(4) 0.04129(14) 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
Br1 Ni1 2.4498(6) . ?
Cl1 C45 1.704(10) . ?
Ni1 N2 1.978(3) . ?
Ni1 N3 2.176(3) . ?
Ni1 N1 2.192(3) . ?
Ni1 Br2 2.3504(6) . ?
N1 C19 1.282(5) . ?
N1 C1 1.462(5) . ?
N2 C20 1.326(5) . ?
N2 C24 1.343(5) . ?
Cl2 C45 1.741(10) . ?
N3 C25 1.282(5) . ?
N3 C32 1.453(5) . ?
C1 C2 1.403(6) . ?
C1 C6 1.406(6) . ?
C2 C3 1.399(6) . ?
C2 C8 1.515(6) . ?
C3 C4 1.373(7) . ?
C3 H3 0.9400 . ?
C4 C5 1.375(7) . ?
C4 H4 0.9400 . ?
C5 C6 1.391(6) . ?
C5 H5 0.9400 . ?
C6 C11 1.508(7) . ?
C7 C8 1.518(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C8 C9 1.525(7) . ?
C8 H8 0.9900 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 C11 1.527(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 C12 1.530(8) . ?
C11 H11 0.9900 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 C14 1.391(7) . ?
C13 C18 1.397(6) . ?
C13 C19 1.487(5) . ?
C14 C15 1.387(7) . ?
C14 H14 0.9400 . ?
C15 C16 1.380(8) . ?
C15 H15 0.9400 . ?
C16 C17 1.363(8) . ?
C16 H16 0.9400 . ?
C17 C18 1.377(7) . ?
C17 H17 0.9400 . ?
C18 H18 0.9400 . ?
C19 C20 1.507(6) . ?
C20 C21 1.390(6) . ?
C21 C22 1.382(7) . ?
C21 H21 0.9400 . ?
C22 C23 1.382(6) . ?
C22 H22 0.9400 . ?
C23 C24 1.379(6) . ?
C23 H23 0.9400 . ?
C24 C25 1.498(6) . ?
C25 C26 1.495(6) . ?
C26 C31 1.377(6) . ?
C26 C27 1.399(6) . ?
C27 C28 1.382(8) . ?
C27 H27 0.9400 . ?
C28 C29 1.366(10) . ?
C28 H28 0.9400 . ?
C29 C30 1.392(10) . ?
C29 H29 0.9400 . ?
C30 C31 1.392(7) . ?
C30 H30 0.9400 . ?
C31 H31 0.9400 . ?
C32 C37 1.395(6) . ?
C32 C33 1.409(6) . ?
C33 C34 1.397(7) . ?
C33 C39 1.499(8) . ?
C34 C35 1.379(8) . ?
C34 H34 0.9400 . ?
C35 C36 1.364(8) . ?
C35 H35 0.9400 . ?
C36 C37 1.393(6) . ?
C36 H36 0.9400 . ?
C37 C42 1.521(7) . ?
C38 C39 1.537(9) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 H38C 0.9700 . ?
C39 C40 1.514(9) . ?
C39 H39 0.9900 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 H40C 0.9700 . ?
C41 C42 1.504(8) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 H41C 0.9700 . ?
C42 C43 1.557(9) . ?
C42 H42 0.9900 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 H43C 0.9700 . ?
C45 H45A 0.9800 . ?
C45 H45B 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
N2 Ni1 N3 76.90(13) . . ?
N2 Ni1 N1 77.16(13) . . ?
N3 Ni1 N1 151.54(13) . . ?
N2 Ni1 Br2 152.04(10) . . ?
N3 Ni1 Br2 98.00(10) . . ?
N1 Ni1 Br2 99.39(9) . . ?
N2 Ni1 Br1 89.17(10) . . ?
N3 Ni1 Br1 94.86(10) . . ?
N1 Ni1 Br1 96.28(9) . . ?
Br2 Ni1 Br1 118.77(3) . . ?
C19 N1 C1 119.1(3) . . ?
C19 N1 Ni1 112.6(3) . . ?
C1 N1 Ni1 127.9(3) . . ?
C20 N2 C24 121.0(4) . . ?
C20 N2 Ni1 117.9(3) . . ?
C24 N2 Ni1 117.9(3) . . ?
C25 N3 C32 120.8(3) . . ?
C25 N3 Ni1 113.4(3) . . ?
C32 N3 Ni1 124.9(3) . . ?
C2 C1 C6 121.9(4) . . ?
C2 C1 N1 119.8(4) . . ?
C6 C1 N1 118.2(4) . . ?
C3 C2 C1 117.6(4) . . ?
C3 C2 C8 119.1(4) . . ?
C1 C2 C8 123.2(4) . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 120.2(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 121.7(4) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 117.4(4) . . ?
C5 C6 C11 118.7(4) . . ?
C1 C6 C11 123.9(4) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 C7 108.8(4) . . ?
C2 C8 C9 114.0(4) . . ?
C7 C8 C9 111.1(4) . . ?
C2 C8 H8 107.6 . . ?
C7 C8 H8 107.6 . . ?
C9 C8 H8 107.6 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 C10 110.6(5) . . ?
C6 C11 C12 110.5(5) . . ?
C10 C11 C12 110.6(5) . . ?
C6 C11 H11 108.3 . . ?
C10 C11 H11 108.3 . . ?
C12 C11 H11 108.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 119.1(4) . . ?
C14 C13 C19 120.3(4) . . ?
C18 C13 C19 120.4(4) . . ?
C15 C14 C13 119.3(5) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C16 C15 C14 120.5(5) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 120.5(5) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 119.9(5) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C13 120.6(5) . . ?
C17 C18 H18 119.7 . . ?
C13 C18 H18 119.7 . . ?
N1 C19 C13 128.3(4) . . ?
N1 C19 C20 115.4(4) . . ?
C13 C19 C20 116.3(3) . . ?
N2 C20 C21 121.2(4) . . ?
N2 C20 C19 113.9(3) . . ?
C21 C20 C19 124.9(4) . . ?
C22 C21 C20 118.4(4) . . ?
C22 C21 H21 120.8 . . ?
C20 C21 H21 120.8 . . ?
C23 C22 C21 119.6(4) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C24 C23 C22 119.2(4) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
N2 C24 C23 120.5(4) . . ?
N2 C24 C25 113.1(4) . . ?
C23 C24 C25 126.4(4) . . ?
N3 C25 C26 127.5(4) . . ?
N3 C25 C24 115.4(4) . . ?
C26 C25 C24 117.0(4) . . ?
C31 C26 C27 119.2(4) . . ?
C31 C26 C25 120.2(4) . . ?
C27 C26 C25 120.6(4) . . ?
C28 C27 C26 120.8(5) . . ?
C28 C27 H27 119.6 . . ?
C26 C27 H27 119.6 . . ?
C29 C28 C27 119.6(6) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 120.5(5) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C31 C30 C29 119.7(5) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C26 C31 C30 120.1(5) . . ?
C26 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C37 C32 C33 122.6(4) . . ?
C37 C32 N3 117.4(4) . . ?
C33 C32 N3 119.9(4) . . ?
C34 C33 C32 116.5(5) . . ?
C34 C33 C39 120.5(5) . . ?
C32 C33 C39 123.0(4) . . ?
C35 C34 C33 121.9(5) . . ?
C35 C34 H34 119.0 . . ?
C33 C34 H34 119.0 . . ?
C36 C35 C34 119.5(5) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C35 C36 C37 122.2(5) . . ?
C35 C36 H36 118.9 . . ?
C37 C36 H36 118.9 . . ?
C36 C37 C32 117.1(5) . . ?
C36 C37 C42 119.2(4) . . ?
C32 C37 C42 123.7(4) . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C33 C39 C40 110.8(5) . . ?
C33 C39 C38 114.1(5) . . ?
C40 C39 C38 110.1(5) . . ?
C33 C39 H39 107.2 . . ?
C40 C39 H39 107.2 . . ?
C38 C39 H39 107.2 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C41 C42 C37 112.2(4) . . ?
C41 C42 C43 109.6(5) . . ?
C37 C42 C43 110.8(5) . . ?
C41 C42 H42 108.0 . . ?
C37 C42 H42 108.0 . . ?
C43 C42 H42 108.0 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Cl1 C45 Cl2 113.2(5) . . ?
Cl1 C45 H45A 108.9 . . ?
Cl2 C45 H45A 108.9 . . ?
Cl1 C45 H45B 108.9 . . ?
Cl2 C45 H45B 108.9 . . ?
H45A C45 H45B 107.8 . . ?

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
C19 N1 C1 C2 -102.5(5) . . . . ?
Ni1 N1 C1 C2 85.3(4) . . . . ?
C19 N1 C1 C6 80.9(5) . . . . ?
Ni1 N1 C1 C6 -91.3(4) . . . . ?
C6 C1 C2 C3 -3.7(6) . . . . ?
N1 C1 C2 C3 179.9(4) . . . . ?
C6 C1 C2 C8 172.5(4) . . . . ?
N1 C1 C2 C8 -4.0(6) . . . . ?
C1 C2 C3 C4 1.9(7) . . . . ?
C8 C2 C3 C4 -174.4(4) . . . . ?
C2 C3 C4 C5 0.6(7) . . . . ?
C3 C4 C5 C6 -1.5(8) . . . . ?
C4 C5 C6 C1 -0.2(7) . . . . ?
C4 C5 C6 C11 179.3(5) . . . . ?
C2 C1 C6 C5 2.8(6) . . . . ?
N1 C1 C6 C5 179.3(4) . . . . ?
C2 C1 C6 C11 -176.6(4) . . . . ?
N1 C1 C6 C11 -0.1(6) . . . . ?
C3 C2 C8 C7 75.8(5) . . . . ?
C1 C2 C8 C7 -100.3(5) . . . . ?
C3 C2 C8 C9 -48.8(6) . . . . ?
C1 C2 C8 C9 135.1(5) . . . . ?
C5 C6 C11 C10 -61.2(6) . . . . ?
C1 C6 C11 C10 118.2(5) . . . . ?
C5 C6 C11 C12 61.6(6) . . . . ?
C1 C6 C11 C12 -119.0(5) . . . . ?
C18 C13 C14 C15 -1.3(7) . . . . ?
C19 C13 C14 C15 174.1(5) . . . . ?
C13 C14 C15 C16 0.1(8) . . . . ?
C14 C15 C16 C17 0.5(9) . . . . ?
C15 C16 C17 C18 0.2(8) . . . . ?
C16 C17 C18 C13 -1.5(7) . . . . ?
C14 C13 C18 C17 2.1(7) . . . . ?
C19 C13 C18 C17 -173.3(4) . . . . ?
C1 N1 C19 C13 8.4(6) . . . . ?
Ni1 N1 C19 C13 -178.3(3) . . . . ?
C1 N1 C19 C20 -172.2(3) . . . . ?
Ni1 N1 C19 C20 1.1(4) . . . . ?
C14 C13 C19 N1 54.5(6) . . . . ?
C18 C13 C19 N1 -130.1(5) . . . . ?
C14 C13 C19 C20 -124.9(4) . . . . ?
C18 C13 C19 C20 50.5(5) . . . . ?
C24 N2 C20 C21 -0.2(6) . . . . ?
Ni1 N2 C20 C21 158.9(3) . . . . ?
C24 N2 C20 C19 -179.0(4) . . . . ?
Ni1 N2 C20 C19 -19.9(5) . . . . ?
N1 C19 C20 N2 11.5(5) . . . . ?
C13 C19 C20 N2 -169.0(4) . . . . ?
N1 C19 C20 C21 -167.1(4) . . . . ?
C13 C19 C20 C21 12.4(6) . . . . ?
N2 C20 C21 C22 0.2(7) . . . . ?
C19 C20 C21 C22 178.7(4) . . . . ?
C20 C21 C22 C23 -0.6(7) . . . . ?
C21 C22 C23 C24 1.2(8) . . . . ?
C20 N2 C24 C23 0.8(6) . . . . ?
Ni1 N2 C24 C23 -158.3(3) . . . . ?
C20 N2 C24 C25 179.9(4) . . . . ?
Ni1 N2 C24 C25 20.8(5) . . . . ?
C22 C23 C24 N2 -1.2(7) . . . . ?
C22 C23 C24 C25 179.7(4) . . . . ?
C32 N3 C25 C26 -8.9(7) . . . . ?
Ni1 N3 C25 C26 -178.6(3) . . . . ?
C32 N3 C25 C24 168.9(4) . . . . ?
Ni1 N3 C25 C24 -0.8(5) . . . . ?
N2 C24 C25 N3 -12.3(5) . . . . ?
C23 C24 C25 N3 166.8(4) . . . . ?
N2 C24 C25 C26 165.8(4) . . . . ?
C23 C24 C25 C26 -15.1(6) . . . . ?
N3 C25 C26 C31 -49.5(7) . . . . ?
C24 C25 C26 C31 132.7(4) . . . . ?
N3 C25 C26 C27 133.7(5) . . . . ?
C24 C25 C26 C27 -44.1(6) . . . . ?
C31 C26 C27 C28 -1.1(8) . . . . ?
C25 C26 C27 C28 175.7(5) . . . . ?
C26 C27 C28 C29 1.5(9) . . . . ?
C27 C28 C29 C30 -1.4(10) . . . . ?
C28 C29 C30 C31 1.1(10) . . . . ?
C27 C26 C31 C30 0.8(7) . . . . ?
C25 C26 C31 C30 -176.1(4) . . . . ?
C29 C30 C31 C26 -0.8(8) . . . . ?
C25 N3 C32 C37 -81.0(5) . . . . ?
Ni1 N3 C32 C37 87.5(4) . . . . ?
C25 N3 C32 C33 103.1(5) . . . . ?
Ni1 N3 C32 C33 -88.4(5) . . . . ?
C37 C32 C33 C34 4.6(7) . . . . ?
N3 C32 C33 C34 -179.8(4) . . . . ?
C37 C32 C33 C39 -173.4(5) . . . . ?
N3 C32 C33 C39 2.2(7) . . . . ?
C32 C33 C34 C35 -1.3(8) . . . . ?
C39 C33 C34 C35 176.8(5) . . . . ?
C33 C34 C35 C36 -2.6(8) . . . . ?
C34 C35 C36 C37 3.4(8) . . . . ?
C35 C36 C37 C32 -0.2(7) . . . . ?
C35 C36 C37 C42 -178.9(5) . . . . ?
C33 C32 C37 C36 -3.8(7) . . . . ?
N3 C32 C37 C36 -179.6(4) . . . . ?
C33 C32 C37 C42 174.7(5) . . . . ?
N3 C32 C37 C42 -1.0(7) . . . . ?
C34 C33 C39 C40 -74.8(7) . . . . ?
C32 C33 C39 C40 103.1(6) . . . . ?
C34 C33 C39 C38 50.1(7) . . . . ?
C32 C33 C39 C38 -132.0(5) . . . . ?
C36 C37 C42 C41 -65.4(6) . . . . ?
C32 C37 C42 C41 116.1(5) . . . . ?
C36 C37 C42 C43 57.5(6) . . . . ?
C32 C37 C42 C43 -121.0(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C23 H23 Br2 0.94 2.87 3.515(4) 126.7 1_565 yes
C45 H45A Br1 0.98 2.88 3.791(9) 154.9 . yes

_refine_diff_density_max         0.743
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.056



# start Validation Reply Form
_vrf_PLAT987_S0928               
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: Fraction of inverted structure presnt is less than 3%, thus a
BASF/TWIN refinement was not deemed necessary.
;
# end Validation Reply Form
