# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_added_by_encifer

#data_Ni(OETPP)Br2
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C60 H60 Br2 N4 Ni'
_chemical_formula_sum            'C60 H60 Br2 N4 Ni'
_chemical_melting_point          ?

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            blue

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1055.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I -4 3 d'
_symmetry_int_tables_number      220
_chemical_absolute_configuration ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'z, x, y'
'y, z, x'
'-z, -x+1/2, y'
'-y+1/2, z, -x'
'z, -x, -y+1/2'
'-y, -z+1/2, x'
'-z+1/2, x, -y'
'y, -z, -x+1/2'
'y+1/4, x+1/4, z+1/4'
'-y+3/4, -x+1/4, z+1/4'
'-y+1/4, x+1/4, -z+3/4'
'y+1/4, -x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'z+1/4, y+1/4, x+1/4'
'-x+3/4, -z+1/4, y+1/4'
'z+1/4, -y+3/4, -x+1/4'
'-x+1/4, z+1/4, -y+3/4'
'-z+3/4, -y+1/4, x+1/4'
'x+1/4, -z+3/4, -y+1/4'
'-z+1/4, y+1/4, -x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-z+1/2, -x+1, y+1/2'
'-y+1, z+1/2, -x+1/2'
'z+1/2, -x+1/2, -y+1'
'-y+1/2, -z+1, x+1/2'
'-z+1, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1'
'y+3/4, x+3/4, z+3/4'
'-y+5/4, -x+3/4, z+3/4'
'-y+3/4, x+3/4, -z+5/4'
'y+3/4, -x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'z+3/4, y+3/4, x+3/4'
'-x+5/4, -z+3/4, y+3/4'
'z+3/4, -y+5/4, -x+3/4'
'-x+3/4, z+3/4, -y+5/4'
'-z+5/4, -y+3/4, x+3/4'
'x+3/4, -z+5/4, -y+3/4'
'-z+3/4, y+3/4, -x+5/4'

_cell_length_a                   25.945
_cell_length_b                   25.945
_cell_length_c                   25.945
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     17464.7
_cell_formula_units_Z            12
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2021
_cell_measurement_theta_min      2.9295
_cell_measurement_theta_max      29.1871
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6552
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8564
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.2126
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         29.27
_reflns_number_total             2825
_reflns_number_gt                1061
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
;
_computing_cell_refinement       
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
;
_computing_data_reduction        
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) 
(compiled Jun 10 2008,16:49:55) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1450P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_number_reflns         2825
_refine_ls_number_parameters     117
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1731
_refine_ls_R_factor_gt           0.1010
_refine_ls_wR_factor_ref         0.2819
_refine_ls_wR_factor_gt          0.2663
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_restrained_S_all      0.976
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br Br 0.47797(7) 0.0000 0.2500 0.0634(7) Uani 1 2 d S . .
Ni Ni 0.3750 0.0000 0.2500 0.0378(8) Uani 1 4 d S . .
N N 0.3771(3) -0.0697(3) 0.2808(3) 0.0162(14) Uani 1 1 d . . .
C1 C 0.3974(4) -0.1126(3) 0.2541(4) 0.021(2) Uani 1 1 d . . .
C2 C 0.4282(4) -0.1451(4) 0.2908(4) 0.031(3) Uani 1 1 d . . .
C3 C 0.4194(4) -0.1245(3) 0.3375(3) 0.017(2) Uani 1 1 d . . .
C4 C 0.3871(3) -0.0778(3) 0.3315(3) 0.0162(14) Uani 1 1 d . . .
C5 C 0.3648(4) -0.0461(4) 0.3703(4) 0.030(3) Uani 1 1 d . . .
C6 C 0.3562(6) -0.0676(5) 0.4243(5) 0.0574(17) Uani 1 1 d . . .
C7 C 0.3217(6) -0.1170(5) 0.4235(5) 0.0574(17) Uani 1 1 d . . .
H7A H 0.3091 -0.1313 0.3922 0.069 Uiso 1 1 calc R . .
C8 C 0.3103(6) -0.1392(5) 0.4728(5) 0.0574(17) Uani 1 1 d . . .
H8A H 0.2884 -0.1683 0.4763 0.069 Uiso 1 1 calc R . .
C9 C 0.3320(6) -0.1170(5) 0.5128(5) 0.0574(17) Uani 1 1 d . . .
H9A H 0.3244 -0.1321 0.5453 0.069 Uiso 1 1 calc R . .
C10 C 0.3628(6) -0.0766(5) 0.5142(5) 0.0574(17) Uani 1 1 d . . .
H10A H 0.3763 -0.0654 0.5463 0.069 Uiso 1 1 calc R . .
C11 C 0.3767(6) -0.0487(5) 0.4667(5) 0.0574(17) Uani 1 1 d . . .
H11A H 0.3986 -0.0194 0.4667 0.069 Uiso 1 1 calc R . .
C12 C 0.4667(4) -0.1854(3) 0.2767(4) 0.023(2) Uani 1 1 d . . .
H12A H 0.4773 -0.2040 0.3082 0.027 Uiso 1 1 calc R . .
H12B H 0.4504 -0.2105 0.2531 0.027 Uiso 1 1 calc R . .
C13 C 0.5124(4) -0.1632(5) 0.2518(5) 0.045(3) Uani 1 1 d . . .
H13A H 0.5366 -0.1908 0.2430 0.068 Uiso 1 1 calc R . .
H13B H 0.5291 -0.1389 0.2754 0.068 Uiso 1 1 calc R . .
H13C H 0.5020 -0.1450 0.2203 0.068 Uiso 1 1 calc R . .
C14 C 0.4464(5) -0.1392(5) 0.3875(4) 0.043(3) Uani 1 1 d . . .
H14A H 0.4591 -0.1751 0.3851 0.051 Uiso 1 1 calc R . .
H14B H 0.4215 -0.1375 0.4164 0.051 Uiso 1 1 calc R . .
C15 C 0.4915(5) -0.1032(6) 0.3985(5) 0.064(4) Uani 1 1 d . . .
H15A H 0.5083 -0.1135 0.4307 0.096 Uiso 1 1 calc R . .
H15B H 0.4788 -0.0678 0.4018 0.096 Uiso 1 1 calc R . .
H15C H 0.5164 -0.1051 0.3701 0.096 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
Br Ni 2.6716(18) . ?
Ni N 1.977(7) 45_544 ?
Ni N 1.977(7) 19 ?
Ni N 1.977(7) 3 ?
Ni N 1.977(7) . ?
Ni Br 2.6716(18) 19 ?
N C4 1.356(11) . ?
N C1 1.414(12) . ?
C1 C5 1.355(14) 19 ?
C1 C2 1.502(14) . ?
C2 C3 1.343(14) . ?
C2 C12 1.490(14) . ?
C3 C4 1.482(13) . ?
C3 C14 1.525(13) . ?
C4 C5 1.422(14) . ?
C5 C1 1.355(14) 45_544 ?
C5 C6 1.524(16) . ?
C6 C11 1.316(18) . ?
C6 C7 1.563(19) . ?
C7 C8 1.435(18) . ?
C7 H7A 0.9500 . ?
C8 C9 1.316(19) . ?
C8 H8A 0.9500 . ?
C9 C10 1.32(2) . ?
C9 H9A 0.9500 . ?
C10 C11 1.475(18) . ?
C10 H10A 0.9500 . ?
C11 H11A 0.9500 . ?
C12 C13 1.469(15) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.525(18) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 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
N Ni N 176.8(5) 45_544 19 ?
N Ni N 90.044(13) 45_544 3 ?
N Ni N 90.044(13) 19 3 ?
N Ni N 90.042(13) 45_544 . ?
N Ni N 90.046(13) 19 . ?
N Ni N 176.8(5) 3 . ?
N Ni Br 88.4(2) 45_544 19 ?
N Ni Br 88.4(2) 19 19 ?
N Ni Br 91.6(2) 3 19 ?
N Ni Br 91.6(2) . 19 ?
N Ni Br 91.6(2) 45_544 . ?
N Ni Br 91.6(2) 19 . ?
N Ni Br 88.4(2) 3 . ?
N Ni Br 88.4(2) . . ?
Br Ni Br 180.0 19 . ?
C4 N C1 106.4(7) . . ?
C4 N Ni 122.6(6) . . ?
C1 N Ni 122.1(6) . . ?
C5 C1 N 120.1(9) 19 . ?
C5 C1 C2 130.6(9) 19 . ?
N C1 C2 109.2(8) . . ?
C3 C2 C12 127.8(10) . . ?
C3 C2 C1 105.0(9) . . ?
C12 C2 C1 126.5(9) . . ?
C2 C3 C4 109.1(8) . . ?
C2 C3 C14 126.2(9) . . ?
C4 C3 C14 123.6(9) . . ?
N C4 C5 121.3(8) . . ?
N C4 C3 109.6(8) . . ?
C5 C4 C3 128.9(8) . . ?
C1 C5 C4 123.1(9) 45_544 . ?
C1 C5 C6 116.9(10) 45_544 . ?
C4 C5 C6 119.9(9) . . ?
C11 C6 C5 125.1(13) . . ?
C11 C6 C7 123.2(12) . . ?
C5 C6 C7 111.7(12) . . ?
C8 C7 C6 115.8(13) . . ?
C8 C7 H7A 122.1 . . ?
C6 C7 H7A 122.1 . . ?
C9 C8 C7 116.1(14) . . ?
C9 C8 H8A 122.0 . . ?
C7 C8 H8A 121.9 . . ?
C8 C9 C10 129.0(14) . . ?
C8 C9 H9A 115.5 . . ?
C10 C9 H9A 115.5 . . ?
C9 C10 C11 121.0(14) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 H10A 119.5 . . ?
C6 C11 C10 114.7(13) . . ?
C6 C11 H11A 122.6 . . ?
C10 C11 H11A 122.6 . . ?
C13 C12 C2 112.0(8) . . ?
C13 C12 H12A 109.2 . . ?
C2 C12 H12A 109.2 . . ?
C13 C12 H12B 109.2 . . ?
C2 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C3 C14 C15 111.0(10) . . ?
C3 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C3 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.902
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.099
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.182

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 -0.058 -0.058 -0.058 260 63 ' '
2 -0.058 0.058 0.558 260 63 ' '
3 0.000 0.250 0.875 13 3 ' '
4 0.058 0.442 0.558 260 63 ' '
5 0.058 0.558 0.942 260 63 ' '
6 0.000 0.750 0.625 13 3 ' '
7 0.192 0.192 0.192 260 63 ' '
8 0.192 0.808 0.308 260 63 ' '
9 0.125 0.500 0.250 13 3 ' '
10 0.308 0.192 0.808 260 63 ' '
11 0.308 0.808 0.692 260 63 ' '
12 0.250 0.125 0.500 13 3 ' '
13 0.250 0.875 0.000 13 3 ' '
14 0.442 0.442 0.442 260 63 ' '
15 0.442 0.558 0.058 260 63 ' '
16 0.375 0.500 0.750 13 3 ' '
17 0.558 0.058 0.442 260 63 ' '
18 0.558 0.942 0.058 260 63 ' '
19 0.500 0.250 0.125 13 3 ' '
20 0.500 0.750 0.375 13 3 ' '
21 0.692 0.308 0.808 260 63 ' '
22 0.692 0.692 0.692 260 63 ' '
23 0.625 0.000 0.750 13 3 ' '
24 0.808 0.308 0.192 260 63 ' '
25 0.808 0.692 0.308 260 63 ' '
26 0.750 0.375 0.500 13 3 ' '
27 0.750 0.625 0.000 13 3 ' '
28 0.875 0.000 0.250 13 3 ' '
_platon_squeeze_details          
;
;

_database_code_depnum_ccdc_archive 'CCDC 1001656'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rjc20m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            rjc20m
_chemical_melting_point          ?
_chemical_formula_moiety         'C64 H68 Br2 N4 Ni'
_chemical_formula_sum            'C64 H68 Br2 N4 Ni'
_chemical_formula_weight         1111.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'I -4 3 d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'y+1/4, x+1/4, z+1/4'
'-y+1/4, -x+3/4, z+3/4'
'y+3/4, -x+1/4, -z+3/4'
'-y+3/4, x+3/4, -z+1/4'
'x+1/4, z+1/4, y+1/4'
'-x+3/4, z+3/4, -y+1/4'
'-x+1/4, -z+3/4, y+3/4'
'x+3/4, -z+1/4, -y+3/4'
'z+1/4, y+1/4, x+1/4'
'z+3/4, -y+1/4, -x+3/4'
'-z+3/4, y+3/4, -x+1/4'
'-z+1/4, -y+3/4, x+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'y+3/4, x+3/4, z+3/4'
'-y+3/4, -x+5/4, z+5/4'
'y+5/4, -x+3/4, -z+5/4'
'-y+5/4, x+5/4, -z+3/4'
'x+3/4, z+3/4, y+3/4'
'-x+5/4, z+5/4, -y+3/4'
'-x+3/4, -z+5/4, y+5/4'
'x+5/4, -z+3/4, -y+5/4'
'z+3/4, y+3/4, x+3/4'
'z+5/4, -y+3/4, -x+5/4'
'-z+5/4, y+5/4, -x+3/4'
'-z+3/4, -y+5/4, x+5/4'

_cell_length_a                   26.4497(10)
_cell_length_b                   26.4497(10)
_cell_length_c                   26.4497(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     18503.9(12)
_cell_formula_units_Z            12
_cell_measurement_temperature    150
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       cubic
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6936
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49512
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         25.99
_reflns_number_total             1613
_reflns_number_gt                1247
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1100P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         1613
_refine_ls_number_parameters     161
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1342
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_restrained_S_all      0.898
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 1.0000 0.2500 0.8750 0.0609(4) Uani 1 4 d S . .
Br Br 1.0000 0.2500 0.97649(3) 0.0830(4) Uani 1 2 d S . .
N N 0.96977(16) 0.31920(15) 0.87222(17) 0.0498(9) Uani 1 1 d . . .
C1 C 0.9960(2) 0.35995(18) 0.85241(19) 0.0513(11) Uani 1 1 d . . .
C2 C 0.92118(18) 0.32714(18) 0.86300(19) 0.0486(12) Uani 1 1 d . . .
C3 C 0.9604(2) 0.39216(19) 0.8237(2) 0.0513(12) Uani 1 1 d . . .
C4 C 0.9137(2) 0.3719(2) 0.8308(2) 0.0555(13) Uani 1 1 d . . .
C5 C 0.88156(19) 0.29579(19) 0.8860(2) 0.0512(11) Uani 1 1 d . . .
C6 C 0.9736(3) 0.4338(2) 0.7873(2) 0.0650(15) Uani 1 1 d . . .
H6A H 0.9965 0.4575 0.8035 0.078 Uiso 1 1 calc R . .
H6B H 0.9431 0.4520 0.7779 0.078 Uiso 1 1 calc R . .
C7 C 0.9990(4) 0.4115(3) 0.7391(2) 0.100(2) Uani 1 1 d . . .
H7A H 1.0079 0.4385 0.7165 0.149 Uiso 1 1 calc R . .
H7B H 0.9758 0.3890 0.7225 0.149 Uiso 1 1 calc R . .
H7C H 1.0289 0.3932 0.7485 0.149 Uiso 1 1 calc R . .
C8 C 0.8665(2) 0.3888(2) 0.8041(3) 0.0694(17) Uani 1 1 d . . .
H8A H 0.8391 0.3907 0.8284 0.083 Uiso 1 1 calc R . .
H8B H 0.8719 0.4224 0.7905 0.083 Uiso 1 1 calc R . .
C9 C 0.8518(5) 0.3552(6) 0.7634(5) 0.156(5) Uani 1 1 d . . .
H9A H 0.8215 0.3677 0.7478 0.234 Uiso 1 1 calc R . .
H9B H 0.8459 0.3220 0.7766 0.234 Uiso 1 1 calc R . .
H9C H 0.8784 0.3538 0.7387 0.234 Uiso 1 1 calc R . .
C10 C 0.8326(2) 0.3207(2) 0.8960(2) 0.0566(13) Uani 1 1 d . . .
C11 C 0.7881(2) 0.3029(2) 0.8742(3) 0.0628(14) Uani 1 1 d . . .
H11A H 0.7889 0.2752 0.8525 0.075 Uiso 1 1 calc R . .
C12 C 0.7430(2) 0.3265(3) 0.8849(3) 0.0775(18) Uani 1 1 d . . .
H12A H 0.7133 0.3137 0.8711 0.093 Uiso 1 1 calc R . .
C13 C 0.7407(2) 0.3691(3) 0.9158(3) 0.0744(18) Uani 1 1 d . . .
C14 C 0.7840(3) 0.3872(3) 0.9358(3) 0.082(2) Uani 1 1 d . . .
H14A H 0.7829 0.4156 0.9565 0.099 Uiso 1 1 calc R . .
C15 C 0.8306(2) 0.3642(2) 0.9262(2) 0.0613(14) Uani 1 1 d . . .
H15A H 0.8601 0.3776 0.9397 0.074 Uiso 1 1 calc R . .
C16 C 0.6915(3) 0.3961(4) 0.9257(4) 0.107(3) Uani 1 1 d . . .
H16A H 0.6975 0.4251 0.9466 0.160 Uiso 1 1 calc R . .
H16B H 0.6685 0.3736 0.9426 0.160 Uiso 1 1 calc R . .
H16C H 0.6770 0.4067 0.8941 0.160 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
Ni N 1.999(4) 15_566 ?
Ni N 1.999(4) 40_536 ?
Ni N 1.999(4) 26_654 ?
Ni N 1.999(4) . ?
Ni Br 2.6844(8) 15_566 ?
Ni Br 2.6845(8) . ?
N C2 1.325(7) . ?
N C1 1.385(7) . ?
C1 C5 1.371(7) 15_566 ?
C1 C3 1.478(7) . ?
C2 C5 1.468(8) . ?
C2 C4 1.472(7) . ?
C3 C4 1.359(8) . ?
C3 C6 1.504(8) . ?
C4 C8 1.502(8) . ?
C5 C1 1.371(7) 40_536 ?
C5 C10 1.477(8) . ?
C6 C7 1.559(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.448(14) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.393(8) . ?
C10 C15 1.400(8) . ?
C11 C12 1.375(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.395(11) . ?
C12 H12A 0.9300 . ?
C13 C14 1.349(11) . ?
C13 C16 1.507(9) . ?
C14 C15 1.397(9) . ?
C14 H14A 0.9300 . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?

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
N Ni N 175.8(3) 15_566 40_536 ?
N Ni N 90.078(10) 15_566 26_654 ?
N Ni N 90.077(10) 40_536 26_654 ?
N Ni N 90.076(10) 15_566 . ?
N Ni N 90.079(10) 40_536 . ?
N Ni N 175.8(3) 26_654 . ?
N Ni Br 92.11(13) 15_566 15_566 ?
N Ni Br 92.11(13) 40_536 15_566 ?
N Ni Br 87.89(13) 26_654 15_566 ?
N Ni Br 87.89(13) . 15_566 ?
N Ni Br 87.89(13) 15_566 . ?
N Ni Br 87.89(13) 40_536 . ?
N Ni Br 92.11(13) 26_654 . ?
N Ni Br 92.11(13) . . ?
Br Ni Br 180.0 15_566 . ?
C2 N C1 107.0(4) . . ?
C2 N Ni 122.7(3) . . ?
C1 N Ni 121.8(3) . . ?
C5 C1 N 121.6(4) 15_566 . ?
C5 C1 C3 129.2(5) 15_566 . ?
N C1 C3 108.9(4) . . ?
N C2 C5 121.8(4) . . ?
N C2 C4 111.4(4) . . ?
C5 C2 C4 126.7(4) . . ?
C4 C3 C1 106.3(5) . . ?
C4 C3 C6 125.9(5) . . ?
C1 C3 C6 127.1(5) . . ?
C3 C4 C2 105.9(4) . . ?
C3 C4 C8 125.0(5) . . ?
C2 C4 C8 128.5(5) . . ?
C1 C5 C2 121.2(4) 40_536 . ?
C1 C5 C10 122.2(5) 40_536 . ?
C2 C5 C10 116.6(4) . . ?
C3 C6 C7 110.3(5) . . ?
C3 C6 H6A 109.6 . . ?
C7 C6 H6A 109.6 . . ?
C3 C6 H6B 109.6 . . ?
C7 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C4 113.0(7) . . ?
C9 C8 H8A 109.0 . . ?
C4 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C4 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
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 C15 118.8(5) . . ?
C11 C10 C5 121.0(5) . . ?
C15 C10 C5 120.1(5) . . ?
C12 C11 C10 119.6(6) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.2 . . ?
C11 C12 C13 121.7(6) . . ?
C11 C12 H12A 119.1 . . ?
C13 C12 H12A 119.1 . . ?
C14 C13 C12 118.5(6) . . ?
C14 C13 C16 120.0(7) . . ?
C12 C13 C16 121.4(7) . . ?
C13 C14 C15 121.6(7) . . ?
C13 C14 H14A 119.2 . . ?
C15 C14 H14A 119.2 . . ?
C14 C15 C10 119.6(6) . . ?
C14 C15 H15A 120.2 . . ?
C10 C15 H15A 120.2 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.061

# SQUEEZE RESULTS (APPEND TO CIF) 
# 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 0.041 0.041 0.041 197 4 ' '
2 0.459 0.041 -0.041 197 4 ' '
3 0.041 -0.041 0.459 197 4 ' '
4 0.459 -0.041 0.541 197 4 ' '
5 0.709 0.209 0.291 197 4 ' '
6 0.791 0.209 0.709 197 4 ' '
7 0.291 0.291 0.291 197 4 ' '
8 0.209 0.291 0.709 197 4 ' '
9 0.541 0.459 -0.041 197 4 ' '
10 0.959 0.459 0.041 197 4 ' '
11 0.959 0.541 0.459 197 4 ' '
12 0.541 0.541 0.541 197 4 ' '
13 0.291 0.709 0.209 197 4 ' '
14 0.209 0.709 0.791 197 4 ' '
15 0.709 0.791 0.209 197 4 ' '
16 0.791 0.791 0.791 197 4 ' '
_platon_squeeze_details          
; 
;
_database_code_depnum_ccdc_archive 'CCDC 1021469'
