# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_C2
_database_code_depnum_ccdc_archive 'CCDC 1042276'
_audit_update_record             
;
2015-01-06 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H32 Br2 F2 N2 Ni'
_chemical_formula_weight         809.22

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'
F F 0.0171 0.0103 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   10.338(2)
_cell_length_b                   10.828(2)
_cell_length_c                   32.153(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.32(3)
_cell_angle_gamma                90.00
_cell_volume                     3577.3(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.99
_cell_measurement_theta_max      27.45

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          .00
_exptl_crystal_size_mid          .00
_exptl_crystal_size_min          .00
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    2.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.3811
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            30438
_diffrn_reflns_av_R_equivalents  0.1122
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         27.45
_reflns_number_total             8154
_reflns_number_gt                6897
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Siemens SMART'
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_reduction        'Siemens XPREP'
_computing_structure_solution    'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1076P)²+10.3833P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8154
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_ref          0.1051
_refine_ls_R_factor_gt           0.0893
_refine_ls_wR_factor_ref         0.2315
_refine_ls_wR_factor_gt          0.2192
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.54262(6) 0.03418(7) 0.144137(19) 0.0394(2) Uani 1 1 d . . .
Br2 Br 0.31810(6) 0.08208(7) 0.240159(19) 0.0381(2) Uani 1 1 d . . .
Ni1 Ni 0.39184(7) -0.03930(7) 0.18783(2) 0.0270(2) Uani 1 1 d . . .
N1 N 0.2334(4) -0.1133(4) 0.15437(13) 0.0230(9) Uani 1 1 d . . .
C21 C 0.1221(5) -0.0467(5) 0.13587(16) 0.0233(10) Uani 1 1 d . . .
C30 C 0.2706(5) 0.0804(6) 0.04045(17) 0.0273(11) Uani 1 1 d . . .
F1 F 0.3666(4) 0.3569(4) -0.03955(13) 0.0541(11) Uani 1 1 d . . .
C22 C 0.1275(5) 0.0105(5) 0.09681(16) 0.0248(11) Uani 1 1 d . . .
C26 C 0.0140(5) -0.0343(5) 0.15831(17) 0.0279(12) Uani 1 1 d . . .
N2 N 0.4475(4) -0.2180(5) 0.19394(13) 0.0275(10) Uani 1 1 d . . .
C9 C 0.3485(6) -0.4239(5) 0.17049(17) 0.0292(12) Uani 1 1 d . . .
C36 C 0.2186(5) -0.1455(5) 0.05095(16) 0.0266(11) Uani 1 1 d . . .
C29 C 0.2400(5) -0.0205(5) 0.07106(16) 0.0248(11) Uani 1 1 d . . .
H29A H 0.3194 -0.0286 0.0917 0.030 Uiso 1 1 calc R . .
C37 C 0.0958(6) -0.1841(6) 0.03308(17) 0.0314(12) Uani 1 1 d . . .
H37A H 0.0235 -0.1300 0.0334 0.038 Uiso 1 1 calc R . .
C23 C 0.0208(5) 0.0835(5) 0.08057(17) 0.0275(11) Uani 1 1 d . . .
H23A H 0.0231 0.1234 0.0544 0.033 Uiso 1 1 calc R . .
C24 C -0.0880(5) 0.0981(5) 0.10219(18) 0.0280(11) Uani 1 1 d . . .
C11 C 0.2382(5) -0.2317(5) 0.15504(15) 0.0245(11) Uani 1 1 d . . .
C25 C -0.0905(5) 0.0375(6) 0.13998(17) 0.0297(12) Uani 1 1 d . . .
H25A H -0.1661 0.0448 0.1542 0.036 Uiso 1 1 calc R . .
C5 C 0.1740(7) -0.5604(6) 0.13823(19) 0.0366(14) Uani 1 1 d . . .
C13 C 0.5732(5) -0.2634(6) 0.21180(18) 0.0293(12) Uani 1 1 d . . .
C8 C 0.4252(6) -0.5259(6) 0.18315(19) 0.0374(14) Uani 1 1 d . . .
H8A H 0.5093 -0.5157 0.1979 0.045 Uiso 1 1 calc R . .
C1 C 0.1528(6) -0.3324(6) 0.13841(17) 0.0304(12) Uani 1 1 d . . .
C14 C 0.6621(6) -0.3083(7) 0.1855(2) 0.0371(14) Uani 1 1 d . . .
C28 C 0.0087(6) -0.0927(6) 0.20050(18) 0.0355(14) Uani 1 1 d . . .
H28A H 0.0888 -0.1396 0.2082 0.053 Uiso 1 1 calc R . .
H28B H -0.0663 -0.1483 0.1994 0.053 Uiso 1 1 calc R . .
H28C H 0.0002 -0.0281 0.2214 0.053 Uiso 1 1 calc R . .
C2 C 0.0284(6) -0.3386(6) 0.11729(17) 0.0323(12) Uani 1 1 d . . .
H2A H -0.0218 -0.2661 0.1110 0.039 Uiso 1 1 calc R . .
C10 C 0.2231(6) -0.4424(5) 0.14839(17) 0.0299(12) Uani 1 1 d . . .
C35 C 0.2402(6) 0.0683(7) -0.00250(19) 0.0386(14) Uani 1 1 d . . .
H35A H 0.1967 -0.0036 -0.0137 0.046 Uiso 1 1 calc R . .
C18 C 0.6037(6) -0.2545(6) 0.25497(18) 0.0338(13) Uani 1 1 d . . .
C4 C 0.0460(8) -0.5639(7) 0.1153(2) 0.0457(17) Uani 1 1 d . . .
H4A H 0.0078 -0.6411 0.1071 0.055 Uiso 1 1 calc R . .
C20 C 0.5071(6) -0.2059(7) 0.28298(19) 0.0425(16) Uani 1 1 d . . .
H20A H 0.4274 -0.1803 0.2658 0.064 Uiso 1 1 calc R . .
H20B H 0.5448 -0.1350 0.2989 0.064 Uiso 1 1 calc R . .
H20C H 0.4865 -0.2710 0.3024 0.064 Uiso 1 1 calc R . .
C3 C -0.0210(7) -0.4570(6) 0.1054(2) 0.0397(15) Uani 1 1 d . . .
H3A H -0.1044 -0.4624 0.0899 0.048 Uiso 1 1 calc R . .
C31 C 0.3316(7) 0.1882(6) 0.05551(19) 0.0423(15) Uani 1 1 d . . .
H31A H 0.3522 0.1981 0.0849 0.051 Uiso 1 1 calc R . .
C33 C 0.3328(6) 0.2661(6) -0.0132(2) 0.0377(14) Uani 1 1 d . . .
C17 C 0.7262(6) -0.2976(7) 0.2719(2) 0.0416(16) Uani 1 1 d . . .
H17A H 0.7484 -0.2952 0.3014 0.050 Uiso 1 1 calc R . .
C7 C 0.3754(8) -0.6429(6) 0.1735(2) 0.0500(18) Uani 1 1 d . . .
H7A H 0.4263 -0.7130 0.1824 0.060 Uiso 1 1 calc R . .
C41 C 0.3233(6) -0.2271(6) 0.0497(2) 0.0374(14) Uani 1 1 d . . .
H41A H 0.4078 -0.2027 0.0614 0.045 Uiso 1 1 calc R . .
C34 C 0.2741(7) 0.1636(7) -0.0298(2) 0.0457(17) Uani 1 1 d . . .
H34A H 0.2556 0.1551 -0.0592 0.055 Uiso 1 1 calc R . .
C12 C 0.3604(5) -0.2897(5) 0.17595(16) 0.0269(11) Uani 1 1 d . . .
C27 C -0.2014(6) 0.1767(6) 0.0843(2) 0.0366(14) Uani 1 1 d . . .
H27A H -0.2688 0.1762 0.1035 0.055 Uiso 1 1 calc R . .
H27B H -0.2373 0.1432 0.0571 0.055 Uiso 1 1 calc R . .
H27C H -0.1717 0.2616 0.0807 0.055 Uiso 1 1 calc R . .
C19 C 0.6314(7) -0.3107(8) 0.1380(2) 0.0472(17) Uani 1 1 d . . .
H19A H 0.7058 -0.3447 0.1254 0.071 Uiso 1 1 calc R . .
H19B H 0.6139 -0.2265 0.1277 0.071 Uiso 1 1 calc R . .
H19C H 0.5546 -0.3623 0.1304 0.071 Uiso 1 1 calc R . .
C16 C 0.8154(6) -0.3434(8) 0.2469(2) 0.0490(19) Uani 1 1 d . . .
H16A H 0.8988 -0.3697 0.2590 0.059 Uiso 1 1 calc R . .
C15 C 0.7821(6) -0.3506(8) 0.2038(2) 0.0512(19) Uani 1 1 d . . .
H15A H 0.8422 -0.3849 0.1867 0.061 Uiso 1 1 calc R . .
C6 C 0.2543(8) -0.6610(7) 0.1515(2) 0.0487(17) Uani 1 1 d . . .
H6A H 0.2249 -0.7426 0.1452 0.058 Uiso 1 1 calc R . .
C32 C 0.3636(8) 0.2830(7) 0.0288(2) 0.0494(17) Uani 1 1 d . . .
H32A H 0.4052 0.3563 0.0395 0.059 Uiso 1 1 calc R . .
C38 C 0.0778(6) -0.3006(6) 0.01487(19) 0.0384(14) Uani 1 1 d . . .
H38A H -0.0057 -0.3265 0.0027 0.046 Uiso 1 1 calc R . .
C39 C 0.1839(7) -0.3770(6) 0.0150(2) 0.0426(15) Uani 1 1 d . . .
C40 C 0.3055(7) -0.3436(7) 0.0314(2) 0.0472(17) Uani 1 1 d . . .
H40A H 0.3769 -0.3983 0.0304 0.057 Uiso 1 1 calc R . .
F2 F 0.1661(5) -0.4903(4) -0.00269(16) 0.0634(13) 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 2.3490(11) . ?
Br2 Ni1 2.3285(10) . ?
Ni1 N2 2.022(5) . ?
Ni1 N1 2.024(4) . ?
N1 C11 1.283(7) . ?
N1 C21 1.431(7) . ?
C21 C26 1.401(8) . ?
C21 C22 1.407(7) . ?
C30 C35 1.388(8) . ?
C30 C31 1.388(9) . ?
C30 C29 1.527(8) . ?
F1 C33 1.368(7) . ?
C22 C23 1.409(8) . ?
C22 C29 1.537(7) . ?
C26 C25 1.408(8) . ?
C26 C28 1.503(8) . ?
N2 C12 1.278(7) . ?
N2 C13 1.447(7) . ?
C9 C8 1.394(9) . ?
C9 C10 1.422(8) . ?
C9 C12 1.467(8) . ?
C36 C37 1.399(8) . ?
C36 C41 1.401(8) . ?
C36 C29 1.506(8) . ?
C37 C38 1.395(9) . ?
C23 C24 1.395(8) . ?
C24 C25 1.384(8) . ?
C24 C27 1.510(8) . ?
C11 C1 1.467(8) . ?
C11 C12 1.502(7) . ?
C5 C10 1.400(8) . ?
C5 C6 1.407(10) . ?
C5 C4 1.443(10) . ?
C13 C18 1.393(8) . ?
C13 C14 1.404(8) . ?
C8 C7 1.389(10) . ?
C1 C2 1.389(8) . ?
C1 C10 1.413(8) . ?
C14 C15 1.391(8) . ?
C14 C19 1.523(9) . ?
C2 C3 1.416(9) . ?
C35 C34 1.422(9) . ?
C18 C17 1.402(8) . ?
C18 C20 1.511(9) . ?
C4 C3 1.368(10) . ?
C31 C32 1.401(9) . ?
C33 C34 1.346(10) . ?
C33 C32 1.365(10) . ?
C17 C16 1.382(10) . ?
C7 C6 1.383(11) . ?
C41 C40 1.396(9) . ?
C16 C15 1.393(10) . ?
C38 C39 1.374(10) . ?
C39 F2 1.356(8) . ?
C39 C40 1.357(10) . ?

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 N1 82.98(18) . . ?
N2 Ni1 Br2 125.60(13) . . ?
N1 Ni1 Br2 107.31(13) . . ?
N2 Ni1 Br1 100.48(13) . . ?
N1 Ni1 Br1 111.58(12) . . ?
Br2 Ni1 Br1 122.18(4) . . ?
C11 N1 C21 122.6(5) . . ?
C11 N1 Ni1 111.0(4) . . ?
C21 N1 Ni1 126.0(3) . . ?
C26 C21 C22 122.0(5) . . ?
C26 C21 N1 118.9(5) . . ?
C22 C21 N1 118.9(5) . . ?
C35 C30 C31 118.1(6) . . ?
C35 C30 C29 122.2(5) . . ?
C31 C30 C29 119.7(5) . . ?
C21 C22 C23 118.1(5) . . ?
C21 C22 C29 119.4(5) . . ?
C23 C22 C29 122.0(5) . . ?
C21 C26 C25 117.1(5) . . ?
C21 C26 C28 122.4(5) . . ?
C25 C26 C28 120.5(5) . . ?
C12 N2 C13 122.0(5) . . ?
C12 N2 Ni1 111.0(4) . . ?
C13 N2 Ni1 126.7(4) . . ?
C8 C9 C10 119.5(6) . . ?
C8 C9 C12 135.4(6) . . ?
C10 C9 C12 105.0(5) . . ?
C37 C36 C41 118.0(6) . . ?
C37 C36 C29 121.9(5) . . ?
C41 C36 C29 120.1(5) . . ?
C36 C29 C30 113.4(4) . . ?
C36 C29 C22 110.1(4) . . ?
C30 C29 C22 114.4(5) . . ?
C38 C37 C36 121.0(6) . . ?
C24 C23 C22 121.4(5) . . ?
C25 C24 C23 118.5(5) . . ?
C25 C24 C27 120.9(5) . . ?
C23 C24 C27 120.6(5) . . ?
N1 C11 C1 135.8(5) . . ?
N1 C11 C12 117.1(5) . . ?
C1 C11 C12 107.1(5) . . ?
C24 C25 C26 122.8(5) . . ?
C10 C5 C6 116.7(6) . . ?
C10 C5 C4 115.6(6) . . ?
C6 C5 C4 127.7(6) . . ?
C18 C13 C14 122.2(5) . . ?
C18 C13 N2 117.9(5) . . ?
C14 C13 N2 119.8(5) . . ?
C7 C8 C9 118.2(7) . . ?
C2 C1 C10 119.7(6) . . ?
C2 C1 C11 134.6(6) . . ?
C10 C1 C11 105.7(5) . . ?
C15 C14 C13 118.1(6) . . ?
C15 C14 C19 119.8(6) . . ?
C13 C14 C19 122.1(5) . . ?
C1 C2 C3 117.6(6) . . ?
C5 C10 C1 123.5(6) . . ?
C5 C10 C9 122.1(6) . . ?
C1 C10 C9 114.4(5) . . ?
C30 C35 C34 120.0(6) . . ?
C13 C18 C17 117.5(6) . . ?
C13 C18 C20 121.7(5) . . ?
C17 C18 C20 120.8(6) . . ?
C3 C4 C5 120.6(6) . . ?
C4 C3 C2 123.0(6) . . ?
C30 C31 C32 122.0(6) . . ?
C34 C33 C32 123.2(6) . . ?
C34 C33 F1 118.9(6) . . ?
C32 C33 F1 117.9(6) . . ?
C16 C17 C18 121.6(6) . . ?
C6 C7 C8 122.4(7) . . ?
C40 C41 C36 121.0(6) . . ?
C33 C34 C35 119.0(6) . . ?
N2 C12 C9 134.6(5) . . ?
N2 C12 C11 117.6(5) . . ?
C9 C12 C11 107.8(5) . . ?
C17 C16 C15 119.5(6) . . ?
C14 C15 C16 120.9(6) . . ?
C7 C6 C5 121.1(7) . . ?
C33 C32 C31 117.6(7) . . ?
C39 C38 C37 118.3(6) . . ?
F2 C39 C40 118.8(7) . . ?
F2 C39 C38 118.2(6) . . ?
C40 C39 C38 123.1(6) . . ?
C39 C40 C41 118.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.655
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.164
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.152 0.099 0.615 43.6 -1.7
2 0.348 0.599 0.885 43.6 -2.8
3 0.652 0.401 0.115 43.6 -1.7
4 0.848 0.901 0.385 43.6 -2.8
_platon_squeeze_details          
; ?
;
####################################################################### 
# 
# 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_C5
_database_code_depnum_ccdc_archive 'CCDC 1042277'
_audit_update_record             
;
2015-01-06 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H68 Br4 F4 N4 Ni2'
_chemical_formula_weight         1646.48

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   19.295(4)
_cell_length_b                   11.616(2)
_cell_length_c                   35.044(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.03(3)
_cell_angle_gamma                90.00
_cell_volume                     7811(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.06
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          .00
_exptl_crystal_size_mid          .00
_exptl_crystal_size_min          .00
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3328
_exptl_absorpt_coefficient_mu    2.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_correction_T_min  0.5479
_exptl_absorpt_correction_T_max  1.0000

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       'ω scans at fixed χ = 45°'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            52967
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0863
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.06
_diffrn_reflns_theta_max         27.48
_reflns_number_total             17699
_reflns_number_gt                11467
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0934P)²+15.7394P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         17699
_refine_ls_number_parameters     893
_refine_ls_number_restraints     0
_refine_ls_R_factor_ref          0.1234
_refine_ls_R_factor_gt           0.0827
_refine_ls_wR_factor_ref         0.2346
_refine_ls_wR_factor_gt          0.2077
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.12972(4) 1.04131(5) 0.327524(18) 0.04210(18) Uani 1 1 d . . .
Br2 Br 0.25043(3) 0.75015(6) 0.35064(2) 0.0480(2) Uani 1 1 d . . .
Ni1 Ni 0.14300(4) 0.84330(6) 0.33924(2) 0.03030(19) Uani 1 1 d . . .
N1 N 0.0886(2) 0.7753(4) 0.38068(13) 0.0278(10) Uani 1 1 d . . .
N2 N 0.0660(2) 0.7714(4) 0.30335(12) 0.0259(9) Uani 1 1 d . . .
C24 C 0.1206(3) 0.8805(5) 0.48097(16) 0.0323(12) Uani 1 1 d . . .
H24 H 0.1143 0.9489 0.4951 0.039 Uiso 1 1 calc R . .
C9 C -0.0396(3) 0.6466(4) 0.31216(14) 0.0237(11) Uani 1 1 d . . .
C12 C 0.0227(3) 0.7152(4) 0.32231(15) 0.0242(11) Uani 1 1 d . . .
C22 C 0.1091(3) 0.7766(5) 0.42133(16) 0.0287(12) Uani 1 1 d . . .
C1 C -0.0178(3) 0.6470(5) 0.38024(16) 0.0302(12) Uani 1 1 d . . .
C11 C 0.0363(3) 0.7162(4) 0.36569(15) 0.0241(11) Uani 1 1 d . . .
C10 C -0.0612(3) 0.6080(5) 0.34763(15) 0.0284(12) Uani 1 1 d . . .
C26 C 0.1605(3) 0.6887(5) 0.47802(18) 0.0393(14) Uani 1 1 d . . .
H26 H 0.1831 0.6243 0.4905 0.047 Uiso 1 1 calc R . .
C25 C 0.1506(3) 0.7853(5) 0.50014(16) 0.0340(13) Uani 1 1 d . . .
C27 C 0.1398(3) 0.6792(5) 0.43912(16) 0.0315(12) Uani 1 1 d . . .
C8 C -0.0761(3) 0.6101(5) 0.27875(16) 0.0296(12) Uani 1 1 d . . .
H8 H -0.0620 0.6325 0.2547 0.036 Uiso 1 1 calc R . .
C5 C -0.1201(3) 0.5396(5) 0.34986(16) 0.0304(12) Uani 1 1 d . . .
C38 C 0.0267(4) 1.1626(5) 0.45446(17) 0.0418(15) Uani 1 1 d . . .
H38 H -0.0198 1.1354 0.4535 0.050 Uiso 1 1 calc R . .
C30 C 0.0597(3) 0.9782(5) 0.42050(17) 0.0320(12) Uani 1 1 d . . .
H30 H 0.0757 0.9820 0.3943 0.038 Uiso 1 1 calc R . .
C18 C 0.0939(3) 0.7280(5) 0.23866(18) 0.0366(14) Uani 1 1 d . . .
C31 C -0.0178(3) 0.9533(5) 0.41502(16) 0.0282(12) Uani 1 1 d . . .
C28 C 0.1721(4) 0.7866(6) 0.54280(18) 0.0494(17) Uani 1 1 d . . .
H28A H 0.1842 0.8653 0.5510 0.074 Uiso 1 1 calc R . .
H28B H 0.2126 0.7363 0.5487 0.074 Uiso 1 1 calc R . .
H28C H 0.1334 0.7590 0.5564 0.074 Uiso 1 1 calc R . .
C6 C -0.1572(3) 0.5045(5) 0.31440(17) 0.0363(14) Uani 1 1 d . . .
H6 H -0.1974 0.4574 0.3143 0.044 Uiso 1 1 calc R . .
C37 C 0.0761(3) 1.0959(5) 0.43949(17) 0.0359(14) Uani 1 1 d . . .
C23 C 0.0992(3) 0.8792(5) 0.44143(15) 0.0269(11) Uani 1 1 d . . .
C16 C 0.0177(5) 0.7980(6) 0.18355(19) 0.055(2) Uani 1 1 d . . .
F1 F -0.2282(2) 0.8859(5) 0.39938(15) 0.0809(15) Uani 1 1 d . . .
C13 C 0.0509(3) 0.7839(5) 0.26253(16) 0.0307(12) Uani 1 1 d . . .
C42 C 0.1440(4) 1.1380(6) 0.4401(2) 0.0529(18) Uani 1 1 d . . .
H42 H 0.1792 1.0932 0.4301 0.063 Uiso 1 1 calc R . .
C14 C -0.0057(3) 0.8514(5) 0.24811(18) 0.0358(13) Uani 1 1 d . . .
C32 C -0.0574(3) 0.9791(5) 0.38067(17) 0.0384(14) Uani 1 1 d . . .
H32 H -0.0350 1.0124 0.3605 0.046 Uiso 1 1 calc R . .
C29 C 0.1519(4) 0.5708(5) 0.41692(18) 0.0438(16) Uani 1 1 d . . .
H29A H 0.1083 0.5273 0.4126 0.066 Uiso 1 1 calc R . .
H29B H 0.1874 0.5236 0.4316 0.066 Uiso 1 1 calc R . .
H29C H 0.1679 0.5914 0.3922 0.066 Uiso 1 1 calc R . .
C21 C 0.1574(3) 0.6607(6) 0.2545(2) 0.0528(19) Uani 1 1 d . . .
H21A H 0.1930 0.7139 0.2662 0.079 Uiso 1 1 calc R . .
H21B H 0.1760 0.6184 0.2336 0.079 Uiso 1 1 calc R . .
H21C H 0.1445 0.6063 0.2739 0.079 Uiso 1 1 calc R . .
C15 C -0.0202(4) 0.8562(6) 0.20817(18) 0.0488(18) Uani 1 1 d . . .
H15 H -0.0582 0.9023 0.1977 0.059 Uiso 1 1 calc R . .
C33 C -0.1282(4) 0.9582(6) 0.3748(2) 0.0537(18) Uani 1 1 d . . .
H33 H -0.1547 0.9772 0.3513 0.064 Uiso 1 1 calc R . .
C2 C -0.0336(3) 0.6167(5) 0.41690(19) 0.0406(15) Uani 1 1 d . . .
H2 H -0.0054 0.6413 0.4393 0.049 Uiso 1 1 calc R . .
C3 C -0.0937(4) 0.5476(6) 0.41933(18) 0.0451(17) Uani 1 1 d . . .
H3 H -0.1061 0.5274 0.4440 0.054 Uiso 1 1 calc R . .
C7 C -0.1346(3) 0.5390(5) 0.28052(19) 0.0349(13) Uani 1 1 d . . .
H7 H -0.1595 0.5138 0.2572 0.042 Uiso 1 1 calc R . .
C4 C -0.1350(3) 0.5083(5) 0.38705(19) 0.0427(16) Uani 1 1 d . . .
H4 H -0.1737 0.4599 0.3901 0.051 Uiso 1 1 calc R . .
C34 C -0.1586(3) 0.9086(6) 0.4047(2) 0.0477(17) Uani 1 1 d . . .
C17 C 0.0755(4) 0.7363(6) 0.19839(18) 0.0452(17) Uani 1 1 d . . .
H17 H 0.1035 0.6989 0.1814 0.054 Uiso 1 1 calc R . .
C35 C -0.1224(4) 0.8796(6) 0.4387(2) 0.0503(17) Uani 1 1 d . . .
H35 H -0.1453 0.8447 0.4585 0.060 Uiso 1 1 calc R . .
C20 C -0.0020(5) 0.8035(7) 0.1401(2) 0.079(3) Uani 1 1 d . . .
H20A H -0.0198 0.8804 0.1330 0.118 Uiso 1 1 calc R . .
H20B H -0.0380 0.7460 0.1326 0.118 Uiso 1 1 calc R . .
H20C H 0.0393 0.7875 0.1269 0.118 Uiso 1 1 calc R . .
C19 C -0.0469(4) 0.9192(6) 0.2745(2) 0.0517(18) Uani 1 1 d . . .
H19A H -0.0660 0.8667 0.2927 0.078 Uiso 1 1 calc R . .
H19B H -0.0851 0.9594 0.2594 0.078 Uiso 1 1 calc R . .
H19C H -0.0164 0.9755 0.2887 0.078 Uiso 1 1 calc R . .
F2 F 0.1275(4) 1.4121(4) 0.48787(14) 0.119(3) Uani 1 1 d . . .
C40 C 0.1103(6) 1.3074(7) 0.4711(2) 0.075(3) Uani 1 1 d . . .
C39 C 0.0439(5) 1.2709(6) 0.4712(2) 0.063(2) Uani 1 1 d . . .
H39 H 0.0100 1.3163 0.4820 0.076 Uiso 1 1 calc R . .
C36 C -0.0512(3) 0.9022(6) 0.44410(19) 0.0423(15) Uani 1 1 d . . .
H36 H -0.0252 0.8826 0.4677 0.051 Uiso 1 1 calc R . .
C41 C 0.1597(6) 1.2485(7) 0.4557(2) 0.074(3) Uani 1 1 d . . .
H41 H 0.2049 1.2804 0.4552 0.089 Uiso 1 1 calc R . .
Br3 Br 0.36163(4) 1.02544(6) 0.17072(2) 0.04700(19) Uani 1 1 d . . .
Br4 Br 0.24670(3) 0.72885(6) 0.14674(2) 0.04592(19) Uani 1 1 d . . .
Ni2 Ni 0.35216(4) 0.82642(7) 0.15986(2) 0.03208(19) Uani 1 1 d . . .
N4 N 0.4301(2) 0.7636(4) 0.19646(13) 0.0286(10) Uani 1 1 d . . .
N3 N 0.4103(2) 0.7647(4) 0.11953(13) 0.0279(10) Uani 1 1 d . . .
C54 C 0.4775(3) 0.7153(4) 0.17856(16) 0.0269(11) Uani 1 1 d . . .
C53 C 0.4661(3) 0.7147(5) 0.13544(15) 0.0285(12) Uani 1 1 d . . .
C51 C 0.5432(3) 0.6544(5) 0.18945(16) 0.0284(12) Uani 1 1 d . . .
C52 C 0.5691(3) 0.6208(5) 0.15480(17) 0.0322(13) Uani 1 1 d . . .
C72 C 0.4314(3) 0.9699(5) 0.07745(15) 0.0311(13) Uani 1 1 d . . .
H72 H 0.4149 0.9701 0.1036 0.037 Uiso 1 1 calc R . .
C50 C 0.5795(3) 0.6227(5) 0.22406(17) 0.0345(13) Uani 1 1 d . . .
H50 H 0.5632 0.6434 0.2478 0.041 Uiso 1 1 calc R . .
C73 C 0.5098(3) 0.9571(5) 0.08367(18) 0.0369(14) Uani 1 1 d . . .
C75 C 0.6171(4) 0.9709(7) 0.1256(2) 0.0548(19) Uani 1 1 d . . .
H75 H 0.6409 0.9892 0.1500 0.066 Uiso 1 1 calc R . .
C60 C 0.3995(3) 0.7180(5) 0.26093(16) 0.0322(13) Uani 1 1 d . . .
C49 C 0.6420(3) 0.5579(6) 0.22291(19) 0.0438(16) Uani 1 1 d . . .
H49 H 0.6674 0.5352 0.2464 0.053 Uiso 1 1 calc R . .
F3 F 0.7228(2) 0.9127(5) 0.10213(16) 0.0794(15) Uani 1 1 d . . .
C55 C 0.4425(3) 0.7765(4) 0.23770(16) 0.0269(11) Uani 1 1 d . . .
C47 C 0.6303(3) 0.5588(6) 0.1529(2) 0.0450(16) Uani 1 1 d . . .
C46 C 0.6490(4) 0.5361(6) 0.11559(19) 0.0497(18) Uani 1 1 d . . .
H46 H 0.6918 0.4978 0.1129 0.060 Uiso 1 1 calc R . .
C69 C 0.3684(3) 0.6583(5) 0.06080(17) 0.0373(14) Uani 1 1 d . . .
C43 C 0.5259(3) 0.6559(5) 0.12076(16) 0.0317(12) Uani 1 1 d . . .
C59 C 0.4135(4) 0.7296(5) 0.30084(19) 0.0426(16) Uani 1 1 d . . .
H59 H 0.3849 0.6897 0.3169 0.051 Uiso 1 1 calc R . .
C64 C 0.3935(3) 0.7623(5) 0.07819(15) 0.0281(12) Uani 1 1 d . . .
C65 C 0.4001(3) 0.8622(5) 0.05716(17) 0.0354(13) Uani 1 1 d . . .
C79 C 0.4046(4) 1.0807(5) 0.05817(18) 0.0440(16) Uani 1 1 d . . .
C48 C 0.6667(3) 0.5272(6) 0.1888(2) 0.0460(17) Uani 1 1 d . . .
H48 H 0.7087 0.4843 0.1893 0.055 Uiso 1 1 calc R . .
C78 C 0.5483(4) 0.9177(6) 0.05505(19) 0.0442(16) Uani 1 1 d . . .
H78 H 0.5246 0.9013 0.0305 0.053 Uiso 1 1 calc R . .
C67 C 0.3583(3) 0.7576(6) -0.00075(19) 0.0434(16) Uani 1 1 d . . .
C80 C 0.4474(5) 1.1630(6) 0.0449(2) 0.060(2) Uani 1 1 d . . .
H80 H 0.4964 1.1518 0.0477 0.072 Uiso 1 1 calc R . .
C74 C 0.5464(3) 0.9851(6) 0.11862(19) 0.0413(15) Uani 1 1 d . . .
H74 H 0.5215 1.0151 0.1384 0.050 Uiso 1 1 calc R . .
C44 C 0.5451(4) 0.6291(6) 0.08496(17) 0.0423(16) Uani 1 1 d . . .
H44 H 0.5173 0.6514 0.0622 0.051 Uiso 1 1 calc R . .
C58 C 0.4664(4) 0.7959(6) 0.31745(19) 0.0520(19) Uani 1 1 d . . .
C76 C 0.6526(4) 0.9297(6) 0.0966(2) 0.0536(19) Uani 1 1 d . . .
C68 C 0.3512(3) 0.6601(5) 0.02108(16) 0.0362(14) Uani 1 1 d . . .
H68 H 0.3340 0.5917 0.0086 0.043 Uiso 1 1 calc R . .
C57 C 0.5056(4) 0.8573(6) 0.2935(2) 0.0502(18) Uani 1 1 d . . .
H57 H 0.5413 0.9064 0.3050 0.060 Uiso 1 1 calc R . .
C63 C 0.3402(3) 0.6464(6) 0.2433(2) 0.0492(17) Uani 1 1 d . . .
H63A H 0.3013 0.6967 0.2339 0.074 Uiso 1 1 calc R . .
H63B H 0.3251 0.5936 0.2626 0.074 Uiso 1 1 calc R . .
H63C H 0.3552 0.6021 0.2218 0.074 Uiso 1 1 calc R . .
F4 F 0.3204(4) 1.3749(4) 0.00650(15) 0.129(3) Uani 1 1 d . . .
C56 C 0.4957(4) 0.8514(5) 0.25347(18) 0.0392(14) Uani 1 1 d . . .
C71 C 0.3598(4) 0.5502(5) 0.08378(19) 0.0476(17) Uani 1 1 d . . .
H71A H 0.4051 0.5123 0.0893 0.071 Uiso 1 1 calc R . .
H71B H 0.3274 0.4979 0.0690 0.071 Uiso 1 1 calc R . .
H71C H 0.3414 0.5702 0.1079 0.071 Uiso 1 1 calc R . .
C66 C 0.3815(3) 0.8581(5) 0.01761(17) 0.0352(13) Uani 1 1 d . . .
H66 H 0.3848 0.9262 0.0029 0.042 Uiso 1 1 calc R . .
C61 C 0.5387(4) 0.9199(6) 0.2287(2) 0.0502(18) Uani 1 1 d . . .
H61A H 0.5742 0.8701 0.2192 0.075 Uiso 1 1 calc R . .
H61B H 0.5616 0.9831 0.2437 0.075 Uiso 1 1 calc R . .
H61C H 0.5087 0.9515 0.2069 0.075 Uiso 1 1 calc R . .
C77 C 0.6191(4) 0.9012(6) 0.0607(2) 0.0550(19) Uani 1 1 d . . .
H77 H 0.6442 0.8717 0.0409 0.066 Uiso 1 1 calc R . .
C70 C 0.3399(4) 0.7532(7) -0.04432(19) 0.056(2) Uani 1 1 d . . .
H70A H 0.3722 0.7014 -0.0556 0.084 Uiso 1 1 calc R . .
H70B H 0.3435 0.8306 -0.0550 0.084 Uiso 1 1 calc R . .
H70C H 0.2921 0.7248 -0.0501 0.084 Uiso 1 1 calc R . .
C45 C 0.6078(4) 0.5673(7) 0.0836(2) 0.057(2) Uani 1 1 d . . .
H45 H 0.6216 0.5467 0.0593 0.068 Uiso 1 1 calc R . .
C82 C 0.3492(8) 1.2802(7) 0.0245(3) 0.088(4) Uani 1 1 d . . .
C83 C 0.3058(7) 1.2042(9) 0.0386(2) 0.098(4) Uani 1 1 d . . .
H83 H 0.2573 1.2202 0.0374 0.118 Uiso 1 1 calc R . .
C84 C 0.3325(5) 1.1005(7) 0.0553(2) 0.063(2) Uani 1 1 d . . .
H84 H 0.3021 1.0450 0.0644 0.076 Uiso 1 1 calc R . .
C81 C 0.4189(7) 1.2644(7) 0.0269(2) 0.083(3) Uani 1 1 d . . .
H81 H 0.4482 1.3200 0.0168 0.100 Uiso 1 1 calc R . .
C62 C 0.4831(5) 0.8057(7) 0.3610(2) 0.078(3) Uani 1 1 d . . .
H62A H 0.4424 0.7825 0.3736 0.117 Uiso 1 1 calc R . .
H62B H 0.4952 0.8856 0.3678 0.117 Uiso 1 1 calc R . .
H62C H 0.5226 0.7555 0.3695 0.117 Uiso 1 1 calc R . .


_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 2.3458(10) . ?
Br2 Ni1 2.3352(11) . ?
Ni1 N2 2.023(4) . ?
Ni1 N1 2.038(5) . ?
N1 C11 1.286(7) . ?
N1 C22 1.438(7) . ?
N2 C12 1.298(6) . ?
N2 C13 1.437(7) . ?
C24 C25 1.389(8) . ?
C24 C23 1.404(7) . ?
C9 C8 1.368(7) . ?
C9 C10 1.424(7) . ?
C9 C12 1.455(7) . ?
C12 C11 1.515(7) . ?
C22 C27 1.394(8) . ?
C22 C23 1.407(8) . ?
C1 C2 1.396(8) . ?
C1 C10 1.419(8) . ?
C1 C11 1.452(7) . ?
C10 C5 1.395(7) . ?
C26 C27 1.384(8) . ?
C26 C25 1.388(8) . ?
C25 C28 1.509(8) . ?
C27 C29 1.510(8) . ?
C8 C7 1.406(7) . ?
C5 C4 1.412(8) . ?
C5 C6 1.427(8) . ?
C38 C37 1.375(8) . ?
C38 C39 1.412(9) . ?
C30 C31 1.515(8) . ?
C30 C23 1.525(8) . ?
C30 C37 1.539(8) . ?
C18 C13 1.399(8) . ?
C18 C17 1.422(8) . ?
C18 C21 1.509(9) . ?
C31 C32 1.389(8) . ?
C31 C36 1.394(8) . ?
C6 C7 1.367(8) . ?
C37 C42 1.397(9) . ?
C16 C15 1.367(10) . ?
C16 C17 1.381(11) . ?
C16 C20 1.532(9) . ?
F1 C34 1.361(7) . ?
C13 C14 1.395(8) . ?
C42 C41 1.416(10) . ?
C14 C15 1.399(8) . ?
C14 C19 1.504(9) . ?
C32 C33 1.381(9) . ?
C33 C34 1.378(10) . ?
C2 C3 1.419(8) . ?
C3 C4 1.391(9) . ?
C34 C35 1.361(10) . ?
C35 C36 1.392(9) . ?
F2 C40 1.375(8) . ?
C40 C41 1.333(14) . ?
C40 C39 1.349(13) . ?
Br3 Ni2 2.3470(11) . ?
Br4 Ni2 2.3323(11) . ?
Ni2 N4 2.009(5) . ?
Ni2 N3 2.026(5) . ?
N4 C54 1.290(7) . ?
N4 C55 1.448(7) . ?
N3 C53 1.297(7) . ?
N3 C64 1.451(7) . ?
C54 C51 1.466(7) . ?
C54 C53 1.504(7) . ?
C53 C43 1.479(7) . ?
C51 C50 1.385(8) . ?
C51 C52 1.416(7) . ?
C52 C47 1.390(8) . ?
C52 C43 1.441(8) . ?
C72 C73 1.513(8) . ?
C72 C79 1.519(8) . ?
C72 C65 1.532(8) . ?
C50 C49 1.426(8) . ?
C73 C74 1.386(9) . ?
C73 C78 1.386(9) . ?
C75 C74 1.370(9) . ?
C75 C76 1.372(10) . ?
C60 C55 1.398(7) . ?
C60 C59 1.403(8) . ?
C60 C63 1.495(9) . ?
C49 C48 1.380(9) . ?
F3 C76 1.362(8) . ?
C55 C56 1.414(8) . ?
C47 C46 1.419(9) . ?
C47 C48 1.422(9) . ?
C46 C45 1.353(10) . ?
C69 C68 1.397(8) . ?
C69 C64 1.416(8) . ?
C69 C71 1.510(8) . ?
C43 C44 1.380(7) . ?
C59 C58 1.359(10) . ?
C64 C65 1.388(8) . ?
C65 C66 1.395(8) . ?
C79 C80 1.376(10) . ?
C79 C84 1.403(10) . ?
C78 C77 1.374(9) . ?
C67 C68 1.382(9) . ?
C67 C66 1.385(9) . ?
C67 C70 1.532(9) . ?
C80 C81 1.419(11) . ?
C44 C45 1.412(9) . ?
C58 C57 1.386(10) . ?
C58 C62 1.531(9) . ?
C76 C77 1.391(11) . ?
C57 C56 1.397(9) . ?
F4 C82 1.357(9) . ?
C56 C61 1.492(9) . ?
C82 C83 1.347(15) . ?
C82 C81 1.351(15) . ?
C83 C84 1.412(11) . ?

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 N1 83.33(18) . . ?
N2 Ni1 Br2 119.70(13) . . ?
N1 Ni1 Br2 102.29(13) . . ?
N2 Ni1 Br1 103.68(13) . . ?
N1 Ni1 Br1 116.72(13) . . ?
Br2 Ni1 Br1 124.26(4) . . ?
C11 N1 C22 122.1(5) . . ?
C11 N1 Ni1 110.9(4) . . ?
C22 N1 Ni1 126.4(3) . . ?
C12 N2 C13 119.1(4) . . ?
C12 N2 Ni1 111.1(4) . . ?
C13 N2 Ni1 129.5(3) . . ?
C25 C24 C23 122.2(6) . . ?
C8 C9 C10 118.6(5) . . ?
C8 C9 C12 135.7(5) . . ?
C10 C9 C12 105.6(4) . . ?
N2 C12 C9 135.3(5) . . ?
N2 C12 C11 117.1(5) . . ?
C9 C12 C11 107.5(4) . . ?
C27 C22 C23 122.5(5) . . ?
C27 C22 N1 119.6(5) . . ?
C23 C22 N1 117.8(5) . . ?
C2 C1 C10 119.5(5) . . ?
C2 C1 C11 134.2(6) . . ?
C10 C1 C11 106.2(5) . . ?
N1 C11 C1 135.6(5) . . ?
N1 C11 C12 117.4(5) . . ?
C1 C11 C12 107.0(4) . . ?
C5 C10 C1 123.5(5) . . ?
C5 C10 C9 122.9(5) . . ?
C1 C10 C9 113.6(5) . . ?
C27 C26 C25 124.9(6) . . ?
C26 C25 C24 116.6(5) . . ?
C26 C25 C28 121.4(6) . . ?
C24 C25 C28 121.9(6) . . ?
C26 C27 C22 116.1(5) . . ?
C26 C27 C29 122.0(5) . . ?
C22 C27 C29 121.8(5) . . ?
C9 C8 C7 119.2(5) . . ?
C10 C5 C4 116.4(5) . . ?
C10 C5 C6 116.8(5) . . ?
C4 C5 C6 126.7(5) . . ?
C37 C38 C39 121.2(7) . . ?
C31 C30 C23 110.8(5) . . ?
C31 C30 C37 112.4(5) . . ?
C23 C30 C37 113.1(5) . . ?
C13 C18 C17 117.4(6) . . ?
C13 C18 C21 122.1(6) . . ?
C17 C18 C21 120.5(6) . . ?
C32 C31 C36 118.1(6) . . ?
C32 C31 C30 121.0(5) . . ?
C36 C31 C30 120.9(5) . . ?
C7 C6 C5 119.8(5) . . ?
C38 C37 C42 118.9(6) . . ?
C38 C37 C30 123.1(6) . . ?
C42 C37 C30 117.9(6) . . ?
C24 C23 C22 117.5(5) . . ?
C24 C23 C30 123.1(5) . . ?
C22 C23 C30 119.0(5) . . ?
C15 C16 C17 118.9(6) . . ?
C15 C16 C20 120.9(8) . . ?
C17 C16 C20 120.1(8) . . ?
C14 C13 C18 122.4(6) . . ?
C14 C13 N2 119.2(5) . . ?
C18 C13 N2 118.5(5) . . ?
C37 C42 C41 119.0(8) . . ?
C13 C14 C15 116.8(6) . . ?
C13 C14 C19 121.0(6) . . ?
C15 C14 C19 122.1(6) . . ?
C33 C32 C31 122.4(6) . . ?
C16 C15 C14 123.2(7) . . ?
C34 C33 C32 117.1(7) . . ?
C1 C2 C3 117.2(6) . . ?
C4 C3 C2 122.6(6) . . ?
C6 C7 C8 122.8(6) . . ?
C3 C4 C5 120.7(5) . . ?
F1 C34 C35 118.6(7) . . ?
F1 C34 C33 118.1(7) . . ?
C35 C34 C33 123.3(6) . . ?
C16 C17 C18 121.1(6) . . ?
C34 C35 C36 118.7(6) . . ?
C41 C40 C39 123.9(7) . . ?
C41 C40 F2 118.5(9) . . ?
C39 C40 F2 117.6(10) . . ?
C40 C39 C38 117.5(8) . . ?
C35 C36 C31 120.5(6) . . ?
C40 C41 C42 119.4(8) . . ?
N4 Ni2 N3 83.35(19) . . ?
N4 Ni2 Br4 121.91(13) . . ?
N3 Ni2 Br4 103.07(13) . . ?
N4 Ni2 Br3 102.36(13) . . ?
N3 Ni2 Br3 114.98(13) . . ?
Br4 Ni2 Br3 124.20(4) . . ?
C54 N4 C55 118.7(5) . . ?
C54 N4 Ni2 111.7(4) . . ?
C55 N4 Ni2 129.3(3) . . ?
C53 N3 C64 120.6(5) . . ?
C53 N3 Ni2 110.8(4) . . ?
C64 N3 Ni2 128.4(3) . . ?
N4 C54 C51 136.1(5) . . ?
N4 C54 C53 117.0(5) . . ?
C51 C54 C53 106.9(4) . . ?
N3 C53 C43 134.5(5) . . ?
N3 C53 C54 117.2(5) . . ?
C43 C53 C54 108.3(5) . . ?
C50 C51 C52 119.1(5) . . ?
C50 C51 C54 134.4(5) . . ?
C52 C51 C54 106.5(5) . . ?
C47 C52 C51 124.2(6) . . ?
C47 C52 C43 121.9(5) . . ?
C51 C52 C43 113.9(5) . . ?
C73 C72 C79 115.9(5) . . ?
C73 C72 C65 109.1(4) . . ?
C79 C72 C65 112.7(5) . . ?
C51 C50 C49 117.8(5) . . ?
C74 C73 C78 117.1(6) . . ?
C74 C73 C72 120.8(6) . . ?
C78 C73 C72 122.1(6) . . ?
C74 C75 C76 118.4(7) . . ?
C55 C60 C59 118.0(6) . . ?
C55 C60 C63 120.3(5) . . ?
C59 C60 C63 121.7(5) . . ?
C48 C49 C50 122.1(6) . . ?
C60 C55 C56 121.5(6) . . ?
C60 C55 N4 119.0(5) . . ?
C56 C55 N4 119.4(5) . . ?
C52 C47 C46 116.1(6) . . ?
C52 C47 C48 115.8(6) . . ?
C46 C47 C48 128.1(6) . . ?
C45 C46 C47 121.9(6) . . ?
C68 C69 C64 116.8(5) . . ?
C68 C69 C71 121.1(6) . . ?
C64 C69 C71 122.1(5) . . ?
C44 C43 C52 120.1(5) . . ?
C44 C43 C53 135.5(6) . . ?
C52 C43 C53 104.4(5) . . ?
C58 C59 C60 122.6(6) . . ?
C65 C64 C69 122.1(5) . . ?
C65 C64 N3 119.4(5) . . ?
C69 C64 N3 118.5(5) . . ?
C64 C65 C66 118.1(6) . . ?
C64 C65 C72 119.3(5) . . ?
C66 C65 C72 122.5(5) . . ?
C80 C79 C84 119.1(7) . . ?
C80 C79 C72 123.4(7) . . ?
C84 C79 C72 117.4(6) . . ?
C49 C48 C47 121.0(6) . . ?
C77 C78 C73 122.8(7) . . ?
C68 C67 C66 118.7(6) . . ?
C68 C67 C70 119.9(6) . . ?
C66 C67 C70 121.4(6) . . ?
C79 C80 C81 120.6(9) . . ?
C75 C74 C73 122.3(7) . . ?
C43 C44 C45 117.2(6) . . ?
C59 C58 C57 117.7(6) . . ?
C59 C58 C62 122.7(7) . . ?
C57 C58 C62 119.6(8) . . ?
F3 C76 C75 120.8(7) . . ?
F3 C76 C77 117.1(7) . . ?
C75 C76 C77 122.1(7) . . ?
C67 C68 C69 122.5(6) . . ?
C58 C57 C56 123.9(7) . . ?
C57 C56 C55 116.1(6) . . ?
C57 C56 C61 122.2(6) . . ?
C55 C56 C61 121.7(6) . . ?
C67 C66 C65 121.8(6) . . ?
C78 C77 C76 117.3(7) . . ?
C46 C45 C44 122.7(6) . . ?
C83 C82 C81 122.8(9) . . ?
C83 C82 F4 117.5(12) . . ?
C81 C82 F4 119.7(11) . . ?
C82 C83 C84 119.8(10) . . ?
C79 C84 C83 119.1(9) . . ?
C82 C81 C80 118.5(9) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.129
# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.745 -0.174 0.253 195 94 ' '
2 0.500 0.000 0.500 19 8 ' '
3 0.255 0.174 0.747 195 94 ' '
4 0.255 0.326 0.247 194 95 ' '
5 0.500 0.500 0.000 19 8 ' '
6 0.745 0.674 0.753 195 94 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

#==END

