# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_p1
_database_code_depnum_ccdc_archive 'CCDC 1434422'
_audit_update_record             
;
2015-10-30 deposited with the CCDC.
2016-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H78 Cl12 N28 Ni8 O6'
_chemical_formula_weight         2134.54

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_H-M_alt        'P 4/m n c'
_space_group_name_Hall           '-P 4 2n'

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

_cell_length_a                   11.786(2)
_cell_length_b                   11.786
_cell_length_c                   29.019(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4031.3(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       NEEDLE
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2172
_exptl_absorpt_coefficient_mu    2.289
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8381
_exptl_absorpt_correction_T_max  0.8942
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18247
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.40
_diffrn_reflns_theta_max         24.99
_reflns_number_total             1816
_reflns_number_gt                1457
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0405P)²+8.7494P] 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         1816
_refine_ls_number_parameters     145
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.036
_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
Ni1 Ni 0.56571(4) 0.33240(4) 0.448656(15) 0.02424(17) Uani 1 1 d . . .
Cl1 Cl 0.95919(12) 0.30839(14) 0.32305(6) 0.0857(5) Uani 1 1 d . . .
Cl2 Cl 0.74362(15) -0.11603(12) 0.5000 0.0551(5) Uani 1 2 d S . .
O1 O 0.6556(3) 0.4310(3) 0.5000 0.0243(8) Uani 1 2 d S . .
H1 H 0.714(5) 0.409(4) 0.5000 0.021(16) Uiso 1 2 d S . .
O2 O 0.5000 0.5000 0.43078(17) 0.0266(11) Uani 1 4 d S . .
H2 H 0.5000 0.5000 0.4076 0.032 Uiso 1 4 d SR . .
N1 N 0.6981(3) 0.3503(3) 0.40368(10) 0.0312(7) Uani 1 1 d . . .
N2 N 0.7414(3) 0.4574(3) 0.40338(11) 0.0319(7) Uani 1 1 d . . .
N3 N 0.6190(3) 0.1840(2) 0.47668(10) 0.0313(7) Uani 1 1 d . . .
C1 C 0.7648(4) 0.2859(4) 0.37664(14) 0.0423(10) Uani 1 1 d . . .
H1A H 0.7543 0.2090 0.3707 0.051 Uiso 1 1 calc R . .
C2 C 0.8500(3) 0.3509(4) 0.35931(16) 0.0438(11) Uani 1 1 d . . .
C3 C 0.8329(3) 0.4580(4) 0.37625(14) 0.0407(10) Uani 1 1 d . . .
H3 H 0.8778 0.5209 0.3699 0.049 Uiso 1 1 calc R . .
C4 C 0.6586(3) 0.0835(3) 0.46224(15) 0.0377(9) Uani 1 1 d . . .
H4 H 0.6671 0.0617 0.4316 0.045 Uiso 1 1 calc R . .
C5 C 0.6847(5) 0.0181(4) 0.5000 0.0350(13) Uani 1 2 d S . .
N5 N 0.5000 0.5000 0.2739(5) 0.159(4) Uani 1 4 d SU . .
H5 H 0.5000 0.5000 0.2438 0.191 Uiso 1 4 d SR . .
C8 C 0.373(2) 0.536(2) 0.2814(6) 0.162(4) Uani 0.50 1 d PU . .
H8A H 0.3477 0.5229 0.3124 0.195 Uiso 0.50 1 d PR . .
H8B H 0.3229 0.5002 0.2598 0.195 Uiso 0.50 1 d PR . .
C8A C 0.435(3) 0.586(2) 0.3024(6) 0.166(4) Uani 0.50 1 d PU . .
H8AA H 0.4864 0.6195 0.3242 0.199 Uiso 0.50 1 d PR . .
H8C H 0.3742 0.5507 0.3189 0.199 Uiso 0.50 1 d PR . .
C9 C 0.3887(10) 0.6823(10) 0.2706(3) 0.173(4) Uani 1 1 d U . .
H9B H 0.3185 0.7231 0.2732 0.260 Uiso 1 1 d R . .
H8AB H 0.4425 0.7126 0.2922 0.260 Uiso 1 1 d R . .
H9A H 0.4179 0.6901 0.2399 0.260 Uiso 1 1 d R . .
N4 N 0.5000 0.5000 0.1728(5) 0.108(4) Uani 1 4 d S . .
C6 C 0.5000 0.5000 0.1334(5) 0.085(4) Uani 1 4 d S . .
C7 C 0.5000 0.5000 0.0842(5) 0.128(6) Uani 1 4 d S . .
H7A H 0.4235 0.4858 0.0745 0.153 Uiso 0.25 1 d PR . .
H7C H 0.5463 0.4407 0.0715 0.153 Uiso 0.25 1 d PR . .
H7B H 0.5218 0.5720 0.0715 0.153 Uiso 0.25 1 d PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.028(3) 7_565 ?
Ni1 N3 2.029(3) . ?
Ni1 N1 2.045(3) . ?
Ni1 O1 2.166(2) . ?
Ni1 O1 2.182(2) 10_566 ?
Ni1 O2 2.1842(12) . ?
Ni1 Ni1 2.9799(11) 12_556 ?
Cl1 C2 1.736(4) . ?
Cl2 C5 1.726(5) . ?
O1 Ni1 2.166(2) 12_556 ?
O1 Ni1 2.182(2) 2_655 ?
O1 Ni1 2.182(2) 15_656 ?
O2 Ni1 2.1842(13) 7_565 ?
O2 Ni1 2.1842(12) 4_665 ?
O2 Ni1 2.1842(13) 2_655 ?
N1 C1 1.345(5) . ?
N1 N2 1.361(4) . ?
N2 C3 1.336(5) . ?
N2 Ni1 2.028(3) 2_655 ?
N3 C4 1.340(5) . ?
N3 N3 1.353(6) 12_556 ?
C1 C2 1.359(6) . ?
C2 C3 1.370(6) . ?
C4 C5 1.375(5) . ?
C5 C4 1.375(5) 12_556 ?
N5 C8A 1.51(2) 2_655 ?
N5 C8A 1.51(2) . ?
N5 C8A 1.51(2) 7_565 ?
N5 C8A 1.51(2) 4_665 ?
N5 C8 1.58(2) 2_655 ?
N5 C8 1.58(2) 7_565 ?
N5 C8 1.58(2) . ?
N5 C8 1.58(2) 4_665 ?
C8 C8A 1.12(3) . ?
C8 C8A 1.42(3) 2_655 ?
C8 C9 1.76(3) . ?
C8 C9 1.88(3) 2_655 ?
C8A C8 1.42(3) 7_565 ?
C8A C9 1.562(19) . ?
C8A C8A 1.79(3) 2_655 ?
C8A C8A 1.79(3) 7_565 ?
C9 C8 1.88(3) 7_565 ?
N4 C6 1.143(15) . ?
C6 C7 1.429(19) . ?

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 94.88(12) 7_565 . ?
N2 Ni1 N1 96.38(12) 7_565 . ?
N3 Ni1 N1 96.22(12) . . ?
N2 Ni1 O1 169.60(13) 7_565 . ?
N3 Ni1 O1 92.02(12) . . ?
N1 Ni1 O1 90.59(12) . . ?
N2 Ni1 O1 90.68(12) 7_565 10_566 ?
N3 Ni1 O1 90.42(12) . 10_566 ?
N1 Ni1 O1 169.85(13) . 10_566 ?
O1 Ni1 O1 81.48(15) . 10_566 ?
N2 Ni1 O2 90.61(12) 7_565 . ?
N3 Ni1 O2 169.98(15) . . ?
N1 Ni1 O2 91.48(12) . . ?
O1 Ni1 O2 81.48(13) . . ?
O1 Ni1 O2 81.12(13) 10_566 . ?
N2 Ni1 Ni1 130.38(9) 7_565 12_556 ?
N3 Ni1 Ni1 66.37(9) . 12_556 ?
N1 Ni1 Ni1 129.65(9) . 12_556 ?
O1 Ni1 Ni1 46.55(6) . 12_556 ?
O1 Ni1 Ni1 46.94(6) 10_566 12_556 ?
O2 Ni1 Ni1 103.74(12) . 12_556 ?
Ni1 O1 Ni1 86.91(12) . 12_556 ?
Ni1 O1 Ni1 87.27(5) . 2_655 ?
Ni1 O1 Ni1 153.06(19) 12_556 2_655 ?
Ni1 O1 Ni1 153.06(19) . 15_656 ?
Ni1 O1 Ni1 87.27(5) 12_556 15_656 ?
Ni1 O1 Ni1 86.12(12) 2_655 15_656 ?
Ni1 O2 Ni1 86.77(6) 7_565 4_665 ?
Ni1 O2 Ni1 86.77(6) 7_565 . ?
Ni1 O2 Ni1 152.5(2) 4_665 . ?
Ni1 O2 Ni1 152.5(2) 7_565 2_655 ?
Ni1 O2 Ni1 86.77(6) 4_665 2_655 ?
Ni1 O2 Ni1 86.77(6) . 2_655 ?
C1 N1 N2 107.5(3) . . ?
C1 N1 Ni1 139.5(3) . . ?
N2 N1 Ni1 112.7(2) . . ?
C3 N2 N1 108.1(3) . . ?
C3 N2 Ni1 136.5(3) . 2_655 ?
N1 N2 Ni1 114.8(2) . 2_655 ?
C4 N3 N3 108.2(2) . 12_556 ?
C4 N3 Ni1 138.1(3) . . ?
N3 N3 Ni1 113.63(9) 12_556 . ?
N1 C1 C2 109.2(4) . . ?
C1 C2 C3 106.1(4) . . ?
C1 C2 Cl1 127.5(3) . . ?
C3 C2 Cl1 126.3(3) . . ?
N2 C3 C2 109.0(4) . . ?
N3 C4 C5 108.9(4) . . ?
C4 C5 C4 105.7(5) 12_556 . ?
C4 C5 Cl2 127.1(2) 12_556 . ?
C4 C5 Cl2 127.1(2) . . ?
C8A N5 C8A 72.7(8) 2_655 . ?
C8A N5 C8A 114.0(17) 2_655 7_565 ?
C8A N5 C8A 72.7(8) . 7_565 ?
C8A N5 C8A 72.7(8) 2_655 4_665 ?
C8A N5 C8A 114.0(17) . 4_665 ?
C8A N5 C8A 72.7(8) 7_565 4_665 ?
C8A N5 C8 115.2(15) . 2_655 ?
C8A N5 C8 125.9(15) 7_565 2_655 ?
C8A N5 C8 54.8(14) 4_665 2_655 ?
C8A N5 C8 125.9(15) 2_655 7_565 ?
C8A N5 C8 54.8(14) . 7_565 ?
C8A N5 C8 115.2(15) 4_665 7_565 ?
C8 N5 C8 164.1(19) 2_655 7_565 ?
C8A N5 C8 54.8(14) 2_655 . ?
C8A N5 C8 115.2(15) 7_565 . ?
C8A N5 C8 125.9(15) 4_665 . ?
C8 N5 C8 88.9(3) 2_655 . ?
C8 N5 C8 88.9(3) 7_565 . ?
C8A N5 C8 115.2(15) 2_655 4_665 ?
C8A N5 C8 125.9(15) . 4_665 ?
C8A N5 C8 54.8(14) 7_565 4_665 ?
C8 N5 C8 88.9(3) 2_655 4_665 ?
C8 N5 C8 88.9(3) 7_565 4_665 ?
C8 N5 C8 164.1(19) . 4_665 ?
C8A C8 C8A 89(2) . 2_655 ?
C8A C8 N5 65.8(18) . . ?
C8A C8 N5 60.4(15) 2_655 . ?
C8A C8 C9 61.0(15) . . ?
C8A C8 C9 149.1(19) 2_655 . ?
N5 C8 C9 98.0(13) . . ?
C8A C8 C9 143(2) . 2_655 ?
C8A C8 C9 54.2(10) 2_655 2_655 ?
N5 C8 C9 93.1(13) . 2_655 ?
C9 C8 C9 155.6(14) . 2_655 ?
C8 C8A C8 120(3) . 7_565 ?
C8 C8A N5 71.7(18) . . ?
C8 C8A N5 64.8(14) 7_565 . ?
C8 C8A C9 80(2) . . ?
C8 C8A C9 78.1(19) 7_565 . ?
N5 C8A C9 110.0(13) . . ?
C8 C8A C8A 52(2) . 2_655 ?
C8 C8A C8A 117.1(15) 7_565 2_655 ?
N5 C8A C8A 53.6(4) . 2_655 ?
C9 C8A C8A 132(2) . 2_655 ?
C8 C8A C8A 125.3(19) . 7_565 ?
N5 C8A C8A 53.6(4) . 7_565 ?
C9 C8A C8A 117(3) . 7_565 ?
C8A C8A C8A 90.000(8) 2_655 7_565 ?
C8A C9 C8 47.6(14) . 7_565 ?
C8 C9 C8 74.5(15) . 7_565 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.074
####################################################################### 
# 
# 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_p2
_database_code_depnum_ccdc_archive 'CCDC 1434423'
_audit_update_record             
;
2015-10-30 deposited with the CCDC.
2016-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H62 Br12 N26 Ni8 O6'
_chemical_formula_weight         2527.84

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

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

_cell_length_a                   21.043(6)
_cell_length_b                   22.205(7)
_cell_length_c                   17.844(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8338(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4896
_exptl_absorpt_coefficient_mu    7.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5180
_exptl_absorpt_correction_T_max  0.5825
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'bruker apex ii'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40524
_diffrn_reflns_av_R_equivalents  0.1408
_diffrn_reflns_av_sigmaI/netI    0.1353
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7313
_reflns_number_gt                3563
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1264P)²+3.5939P] 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         7313
_refine_ls_number_parameters     419
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.1730
_refine_ls_R_factor_gt           0.0898
_refine_ls_wR_factor_ref         0.2527
_refine_ls_wR_factor_gt          0.2218
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.016
_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 0.5000 0.68280(11) 0.2500 0.0875(10) Uani 1 2 d S . .
Br2 Br 0.62381(9) 0.50296(8) 0.60493(9) 0.0573(5) Uani 1 1 d . . .
Br3 Br 0.61594(13) 0.14350(14) 0.60906(14) 0.1207(11) Uani 1 1 d . . .
Br4 Br 0.5000 -0.03342(15) 0.2500 0.306(6) Uani 1 2 d S . .
Br5 Br 0.80313(10) 0.12477(10) 0.17771(12) 0.0839(7) Uani 1 1 d . . .
Br6 Br 0.70757(11) 0.35482(16) -0.11580(12) 0.1216(11) Uani 1 1 d . . .
Br7 Br 0.83303(9) 0.48752(11) 0.25577(18) 0.1143(11) Uani 1 1 d . . .
Ni1 Ni 0.55863(8) 0.42016(8) 0.29571(9) 0.0303(5) Uani 1 1 d . . .
Ni2 Ni 0.50476(8) 0.32413(8) 0.39440(10) 0.0336(5) Uani 1 1 d . . .
Ni3 Ni 0.55892(8) 0.22859(8) 0.29612(11) 0.0388(5) Uani 1 1 d . . .
Ni4 Ni 0.61276(8) 0.32446(8) 0.19826(10) 0.0331(5) Uani 1 1 d . . .
O1 O 0.5797(4) 0.3232(4) 0.3123(5) 0.039(2) Uani 1 1 d . . .
H1 H 0.6136 0.3231 0.3382 0.046 Uiso 1 1 d R . .
O2 O 0.5366(4) 0.3872(3) 0.1847(4) 0.023(2) Uani 1 1 d . . .
H2 H 0.5526 0.4140 0.1565 0.028 Uiso 1 1 d R . .
O3 O 0.5359(4) 0.2603(4) 0.1842(5) 0.039(2) Uani 1 1 d . . .
H3 H 0.5521 0.2336 0.1559 0.047 Uiso 1 1 d R . .
N1 N 0.5266(5) 0.5046(5) 0.2704(6) 0.029(3) Uani 1 1 d . . .
N2 N 0.5698(5) 0.4378(6) 0.4058(7) 0.043(3) Uani 1 1 d . . .
N3 N 0.5500(5) 0.3904(6) 0.4514(6) 0.042(3) Uani 1 1 d . . .
N4 N 0.5457(6) 0.2547(6) 0.4500(7) 0.051(4) Uani 1 1 d . . .
N5 N 0.5762(6) 0.2156(5) 0.4057(7) 0.042(3) Uani 1 1 d . . .
N6 N 0.6459(5) 0.2089(6) 0.2566(6) 0.041(3) Uani 1 1 d . . .
N7 N 0.6711(5) 0.2555(5) 0.2158(6) 0.032(3) Uani 1 1 d . . .
N8 N 0.6307(6) 0.3291(5) 0.0864(7) 0.049(3) Uani 1 1 d . . .
N9 N 0.5757(5) 0.3279(5) 0.0454(6) 0.038(3) Uani 1 1 d . . .
N10 N 0.6759(6) 0.3889(5) 0.2289(6) 0.039(3) Uani 1 1 d . . .
N11 N 0.6517(5) 0.4342(5) 0.2689(6) 0.029(3) Uani 1 1 d . . .
N13 N 0.5237(6) 0.1454(6) 0.2736(9) 0.071(3) Uani 1 1 d U . .
C1 C 0.5000 0.5973(10) 0.2500 0.051(6) Uani 1 2 d S . .
C2 C 0.5459(7) 0.5626(6) 0.2823(8) 0.040(4) Uani 1 1 d . . .
H2A H 0.5832 0.5758 0.3074 0.048 Uiso 1 1 calc R . .
C3 C 0.5974(7) 0.4769(7) 0.4462(8) 0.040(4) Uani 1 1 d . . .
H3A H 0.6183 0.5120 0.4282 0.048 Uiso 1 1 calc R . .
C4 C 0.5919(7) 0.4599(7) 0.5219(7) 0.045(4) Uani 1 1 d . . .
C5 C 0.5634(7) 0.4038(8) 0.5226(9) 0.050(4) Uani 1 1 d . . .
H5 H 0.5549 0.3796 0.5654 0.060 Uiso 1 1 calc R . .
C6 C 0.5540(7) 0.2370(7) 0.5236(9) 0.050(4) Uani 1 1 d . . .
H6 H 0.5368 0.2575 0.5657 0.060 Uiso 1 1 calc R . .
C7 C 0.5883(8) 0.1886(8) 0.5275(12) 0.070(6) Uani 1 1 d . . .
C8 C 0.6033(9) 0.1719(9) 0.4456(12) 0.075(6) Uani 1 1 d . . .
H8 H 0.6265 0.1381 0.4276 0.090 Uiso 1 1 calc R . .
C10 C 0.5387(8) 0.0878(7) 0.2971(12) 0.071(3) Uani 1 1 d U . .
H10 H 0.5675 0.0756 0.3352 0.086 Uiso 1 1 calc R . .
C11 C 0.5000 0.0515(11) 0.2500 0.071(3) Uani 1 2 d SU . .
C12 C 0.6829(8) 0.1607(7) 0.2526(9) 0.052(5) Uani 1 1 d . . .
H12 H 0.6747 0.1231 0.2760 0.063 Uiso 1 1 calc R . .
C13 C 0.7368(7) 0.1743(7) 0.2075(8) 0.042(4) Uani 1 1 d . . .
C14 C 0.7254(7) 0.2349(6) 0.1839(8) 0.046(4) Uani 1 1 d . . .
H14 H 0.7518 0.2572 0.1508 0.055 Uiso 1 1 calc R . .
C15 C 0.6791(8) 0.3384(7) 0.0425(9) 0.053(5) Uani 1 1 d . . .
H15 H 0.7222 0.3414 0.0579 0.064 Uiso 1 1 calc R . .
C16 C 0.6568(8) 0.3433(10) -0.0316(9) 0.075(6) Uani 1 1 d . . .
C17 C 0.5927(8) 0.3379(8) -0.0257(9) 0.065(5) Uani 1 1 d . . .
H17 H 0.5639 0.3409 -0.0665 0.077 Uiso 1 1 calc R . .
C18 C 0.7358(6) 0.4008(7) 0.2182(8) 0.045(4) Uani 1 1 d . . .
H18 H 0.7638 0.3764 0.1895 0.053 Uiso 1 1 calc R . .
C19 C 0.7530(8) 0.4524(9) 0.2533(10) 0.067(5) Uani 1 1 d . . .
C20 C 0.6969(7) 0.4729(7) 0.2833(8) 0.035(3) Uani 1 1 d . . .
H20 H 0.6917 0.5095 0.3102 0.042 Uiso 1 1 calc R . .
N12 N 0.8021(17) 0.3790(17) 0.506(2) 0.467(14) Uiso 1 1 d DU . .
H12A H 0.7860 0.3647 0.5513 0.560 Uiso 1 1 calc R . .
C21 C 0.9086(18) 0.3388(19) 0.541(3) 0.32(3) Uiso 1 1 d DU . .
H21A H 0.9539 0.3463 0.5328 0.485 Uiso 1 1 calc R . .
H21B H 0.8949 0.3041 0.5116 0.485 Uiso 1 1 calc R . .
H21C H 0.9014 0.3305 0.5947 0.485 Uiso 1 1 calc R . .
C22 C 0.872(2) 0.3922(17) 0.519(3) 0.467(14) Uiso 1 1 d DU . .
H22A H 0.8903 0.4091 0.4727 0.560 Uiso 1 1 calc R . .
H22B H 0.8756 0.4232 0.5589 0.560 Uiso 1 1 calc R . .
C23 C 0.7901(18) 0.331(2) 0.449(3) 0.467(14) Uiso 1 1 d DU . .
H23A H 0.8121 0.2932 0.4632 0.560 Uiso 1 1 calc R . .
H23B H 0.8052 0.3438 0.3991 0.560 Uiso 1 1 calc R . .
C24 C 0.7187(17) 0.3220(15) 0.449(2) 0.222(17) Uiso 1 1 d DU . .
H24A H 0.7036 0.3174 0.5007 0.333 Uiso 1 1 calc R . .
H24B H 0.7081 0.2858 0.4202 0.333 Uiso 1 1 calc R . .
H24C H 0.6982 0.3571 0.4262 0.333 Uiso 1 1 calc R . .
C25 C 0.766(2) 0.4363(18) 0.489(4) 0.467(14) Uiso 1 1 d DU . .
H25A H 0.7555 0.4362 0.4346 0.560 Uiso 1 1 calc R . .
H25B H 0.7260 0.4359 0.5169 0.560 Uiso 1 1 calc R . .
C26 C 0.800(2) 0.493(2) 0.506(3) 0.34(3) Uiso 1 1 d DU . .
H26A H 0.7691 0.5254 0.5142 0.511 Uiso 1 1 calc R . .
H26B H 0.8277 0.5041 0.4635 0.511 Uiso 1 1 calc R . .
H26C H 0.8261 0.4879 0.5508 0.511 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 C1 1.90(2) . ?
Br2 C4 1.887(14) . ?
Br3 C7 1.859(17) . ?
Br4 C11 1.89(2) . ?
Br5 C13 1.855(15) . ?
Br6 C16 1.860(15) . ?
Br7 C19 1.857(16) . ?
Ni1 N2 2.018(12) . ?
Ni1 N11 2.040(11) . ?
Ni1 N1 2.042(10) . ?
Ni1 O2 2.161(8) 4_655 ?
Ni1 O2 2.163(8) . ?
Ni1 O1 2.219(9) . ?
Ni1 Ni1 2.958(3) 4_655 ?
Ni1 Ni4 2.973(2) . ?
Ni1 Ni2 2.989(2) . ?
Ni2 N9 2.007(11) 4_655 ?
Ni2 N3 2.026(11) . ?
Ni2 N4 2.027(12) . ?
Ni2 O1 2.152(9) . ?
Ni2 O3 2.169(9) 4_655 ?
Ni2 O2 2.169(8) 4_655 ?
Ni2 Ni4 2.975(3) 4_655 ?
Ni2 Ni3 2.979(3) . ?
Ni3 N5 2.009(12) . ?
Ni3 N6 2.009(11) . ?
Ni3 N13 2.030(13) . ?
Ni3 O3 2.145(9) 4_655 ?
Ni3 O1 2.165(9) . ?
Ni3 O3 2.173(9) . ?
Ni3 Ni3 2.976(4) 4_655 ?
Ni3 Ni4 2.977(3) . ?
Ni4 N7 1.989(11) . ?
Ni4 N10 2.027(12) . ?
Ni4 N8 2.034(13) . ?
Ni4 O2 2.138(8) . ?
Ni4 O1 2.151(9) . ?
Ni4 O3 2.170(9) . ?
Ni4 Ni2 2.975(3) 4_655 ?
O1 H1 0.8498 . ?
O2 Ni1 2.161(8) 4_655 ?
O2 Ni2 2.169(8) 4_655 ?
O2 H2 0.8495 . ?
O3 Ni3 2.145(9) 4_655 ?
O3 Ni2 2.169(9) 4_655 ?
O3 H3 0.8500 . ?
N1 N1 1.334(19) 4_655 ?
N1 C2 1.368(17) . ?
N2 C3 1.267(16) . ?
N2 N3 1.395(16) . ?
N3 C5 1.335(18) . ?
N4 N5 1.338(16) . ?
N4 C6 1.381(18) . ?
N5 C8 1.33(2) . ?
N6 C12 1.324(18) . ?
N6 N7 1.373(15) . ?
N7 C14 1.355(17) . ?
N8 C15 1.300(18) . ?
N8 N9 1.369(16) . ?
N9 C17 1.337(19) . ?
N9 Ni2 2.007(11) 4_655 ?
N10 C18 1.303(16) . ?
N10 N11 1.335(15) . ?
N11 C20 1.307(16) . ?
N13 N13 1.31(3) 4_655 ?
N13 C10 1.38(2) . ?
C1 C2 1.364(17) 4_655 ?
C1 C2 1.364(17) . ?
C2 H2A 0.9500 . ?
C3 C4 1.408(18) . ?
C3 H3A 0.9500 . ?
C4 C5 1.38(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.30(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.54(3) . ?
C8 H8 0.9500 . ?
C10 C11 1.42(2) . ?
C10 H10 0.9500 . ?
C11 C10 1.42(2) 4_655 ?
C12 C13 1.42(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.431(19) . ?
C14 H14 0.9500 . ?
C15 C16 1.41(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.36(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.35(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.37(2) . ?
C20 H20 0.9500 . ?
N12 C23 1.49(2) . ?
N12 C25 1.511(19) . ?
N12 C22 1.514(19) . ?
N12 H12A 0.9300 . ?
C21 C22 1.471(19) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.516(19) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.48(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 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 N11 95.0(4) . . ?
N2 Ni1 N1 94.3(5) . . ?
N11 Ni1 N1 97.2(4) . . ?
N2 Ni1 O2 90.9(4) . 4_655 ?
N11 Ni1 O2 168.4(4) . 4_655 ?
N1 Ni1 O2 92.3(4) . 4_655 ?
N2 Ni1 O2 169.5(4) . . ?
N11 Ni1 O2 92.5(4) . . ?
N1 Ni1 O2 92.1(3) . . ?
O2 Ni1 O2 80.5(3) 4_655 . ?
N2 Ni1 O1 92.0(4) . . ?
N11 Ni1 O1 89.3(4) . . ?
N1 Ni1 O1 170.5(4) . . ?
O2 Ni1 O1 80.5(3) 4_655 . ?
O2 Ni1 O1 80.6(3) . . ?
N2 Ni1 Ni1 129.4(3) . 4_655 ?
N11 Ni1 Ni1 132.2(3) . 4_655 ?
N1 Ni1 Ni1 66.6(3) . 4_655 ?
O2 Ni1 Ni1 46.9(2) 4_655 4_655 ?
O2 Ni1 Ni1 46.8(2) . 4_655 ?
O1 Ni1 Ni1 103.9(2) . 4_655 ?
N2 Ni1 Ni4 131.6(3) . . ?
N11 Ni1 Ni4 66.7(3) . . ?
N1 Ni1 Ni4 130.8(3) . . ?
O2 Ni1 Ni4 102.0(2) 4_655 . ?
O2 Ni1 Ni4 45.9(2) . . ?
O1 Ni1 Ni4 46.2(2) . . ?
Ni1 Ni1 Ni4 89.83(6) 4_655 . ?
N2 Ni1 Ni2 67.0(4) . . ?
N11 Ni1 Ni2 127.7(3) . . ?
N1 Ni1 Ni2 131.3(3) . . ?
O2 Ni1 Ni2 46.5(2) 4_655 . ?
O2 Ni1 Ni2 102.5(2) . . ?
O1 Ni1 Ni2 45.9(2) . . ?
Ni1 Ni1 Ni2 90.49(7) 4_655 . ?
Ni4 Ni1 Ni2 88.85(7) . . ?
N9 Ni2 N3 95.6(5) 4_655 . ?
N9 Ni2 N4 97.4(5) 4_655 . ?
N3 Ni2 N4 96.1(5) . . ?
N9 Ni2 O1 169.3(4) 4_655 . ?
N3 Ni2 O1 90.3(4) . . ?
N4 Ni2 O1 90.8(4) . . ?
N9 Ni2 O3 92.3(4) 4_655 4_655 ?
N3 Ni2 O3 169.8(4) . 4_655 ?
N4 Ni2 O3 89.3(4) . 4_655 ?
O1 Ni2 O3 80.9(3) . 4_655 ?
N9 Ni2 O2 89.0(4) 4_655 4_655 ?
N3 Ni2 O2 92.6(4) . 4_655 ?
N4 Ni2 O2 168.5(5) . 4_655 ?
O1 Ni2 O2 81.8(3) . 4_655 ?
O3 Ni2 O2 81.0(3) 4_655 4_655 ?
N9 Ni2 Ni4 66.2(3) 4_655 4_655 ?
N3 Ni2 Ni4 131.9(3) . 4_655 ?
N4 Ni2 Ni4 128.9(4) . 4_655 ?
O1 Ni2 Ni4 103.3(3) . 4_655 ?
O3 Ni2 Ni4 46.7(2) 4_655 4_655 ?
O2 Ni2 Ni4 45.9(2) 4_655 4_655 ?
N9 Ni2 Ni3 131.8(3) 4_655 . ?
N3 Ni2 Ni3 129.3(3) . . ?
N4 Ni2 Ni3 65.4(4) . . ?
O1 Ni2 Ni3 46.5(2) . . ?
O3 Ni2 Ni3 46.0(2) 4_655 . ?
O2 Ni2 Ni3 103.3(2) 4_655 . ?
Ni4 Ni2 Ni3 89.57(7) 4_655 . ?
N9 Ni2 Ni1 127.3(3) 4_655 . ?
N3 Ni2 Ni1 66.4(3) . . ?
N4 Ni2 Ni1 132.1(3) . . ?
O1 Ni2 Ni1 47.8(2) . . ?
O3 Ni2 Ni1 103.6(2) 4_655 . ?
O2 Ni2 Ni1 46.2(2) 4_655 . ?
Ni4 Ni2 Ni1 89.20(7) 4_655 . ?
Ni3 Ni2 Ni1 90.92(7) . . ?
N5 Ni3 N6 98.3(5) . . ?
N5 Ni3 N13 97.4(6) . . ?
N6 Ni3 N13 93.7(5) . . ?
N5 Ni3 O3 93.2(4) . 4_655 ?
N6 Ni3 O3 167.5(4) . 4_655 ?
N13 Ni3 O3 89.5(4) . 4_655 ?
N5 Ni3 O1 88.4(4) . . ?
N6 Ni3 O1 94.3(4) . . ?
N13 Ni3 O1 169.3(4) . . ?
O3 Ni3 O1 81.2(3) 4_655 . ?
N5 Ni3 O3 168.9(4) . . ?
N6 Ni3 O3 87.2(4) . . ?
N13 Ni3 O3 91.8(5) . . ?
O3 Ni3 O3 80.6(4) 4_655 . ?
O1 Ni3 O3 81.5(3) . . ?
N5 Ni3 Ni3 133.6(4) . 4_655 ?
N6 Ni3 Ni3 124.4(3) . 4_655 ?
N13 Ni3 Ni3 65.6(4) . 4_655 ?
O3 Ni3 Ni3 46.8(2) 4_655 4_655 ?
O1 Ni3 Ni3 104.0(2) . 4_655 ?
O3 Ni3 Ni3 46.0(2) . 4_655 ?
N5 Ni3 Ni4 127.2(4) . . ?
N6 Ni3 Ni4 66.6(4) . . ?
N13 Ni3 Ni4 132.3(5) . . ?
O3 Ni3 Ni4 102.4(2) 4_655 . ?
O1 Ni3 Ni4 46.2(2) . . ?
O3 Ni3 Ni4 46.7(2) . . ?
Ni3 Ni3 Ni4 89.58(7) 4_655 . ?
N5 Ni3 Ni2 66.3(4) . . ?
N6 Ni3 Ni2 135.2(4) . . ?
N13 Ni3 Ni2 128.7(4) . . ?
O3 Ni3 Ni2 46.7(2) 4_655 . ?
O1 Ni3 Ni2 46.2(2) . . ?
O3 Ni3 Ni2 103.0(2) . . ?
Ni3 Ni3 Ni2 90.39(7) 4_655 . ?
Ni4 Ni3 Ni2 88.95(7) . . ?
N7 Ni4 N10 95.6(5) . . ?
N7 Ni4 N8 94.5(5) . . ?
N10 Ni4 N8 96.1(5) . . ?
N7 Ni4 O2 169.5(4) . . ?
N10 Ni4 O2 93.6(4) . . ?
N8 Ni4 O2 89.7(4) . . ?
N7 Ni4 O1 92.3(4) . . ?
N10 Ni4 O1 88.1(4) . . ?
N8 Ni4 O1 171.6(4) . . ?
O2 Ni4 O1 82.7(3) . . ?
N7 Ni4 O3 88.5(4) . . ?
N10 Ni4 O3 169.4(4) . . ?
N8 Ni4 O3 93.3(5) . . ?
O2 Ni4 O3 81.7(3) . . ?
O1 Ni4 O3 81.9(3) . . ?
N7 Ni4 Ni1 134.1(3) . . ?
N10 Ni4 Ni1 65.7(3) . . ?
N8 Ni4 Ni1 127.5(3) . . ?
O2 Ni4 Ni1 46.6(2) . . ?
O1 Ni4 Ni1 48.1(2) . . ?
O3 Ni4 Ni1 104.5(2) . . ?
N7 Ni4 Ni2 126.8(3) . 4_655 ?
N10 Ni4 Ni2 134.1(3) . 4_655 ?
N8 Ni4 Ni2 67.0(4) . 4_655 ?
O2 Ni4 Ni2 46.8(2) . 4_655 ?
O1 Ni4 Ni2 104.9(2) . 4_655 ?
O3 Ni4 Ni2 46.7(2) . 4_655 ?
Ni1 Ni4 Ni2 90.48(7) . 4_655 ?
N7 Ni4 Ni3 65.9(3) . . ?
N10 Ni4 Ni3 126.6(3) . . ?
N8 Ni4 Ni3 133.0(4) . . ?
O2 Ni4 Ni3 104.3(2) . . ?
O1 Ni4 Ni3 46.6(2) . . ?
O3 Ni4 Ni3 46.8(2) . . ?
Ni1 Ni4 Ni3 91.28(7) . . ?
Ni2 Ni4 Ni3 90.46(7) 4_655 . ?
Ni4 O1 Ni2 151.7(5) . . ?
Ni4 O1 Ni3 87.2(3) . . ?
Ni2 O1 Ni3 87.3(3) . . ?
Ni4 O1 Ni1 85.7(3) . . ?
Ni2 O1 Ni1 86.3(3) . . ?
Ni3 O1 Ni1 152.1(5) . . ?
Ni4 O1 H1 104.0 . . ?
Ni2 O1 H1 104.2 . . ?
Ni3 O1 H1 103.9 . . ?
Ni1 O1 H1 104.0 . . ?
Ni4 O2 Ni1 153.8(4) . 4_655 ?
Ni4 O2 Ni1 87.4(3) . . ?
Ni1 O2 Ni1 86.3(3) 4_655 . ?
Ni4 O2 Ni2 87.4(3) . 4_655 ?
Ni1 O2 Ni2 87.3(3) 4_655 4_655 ?
Ni1 O2 Ni2 154.2(4) . 4_655 ?
Ni4 O2 H2 103.1 . . ?
Ni1 O2 H2 103.1 4_655 . ?
Ni1 O2 H2 102.7 . . ?
Ni2 O2 H2 103.1 4_655 . ?
Ni3 O3 Ni2 87.4(3) 4_655 4_655 ?
Ni3 O3 Ni4 152.9(5) 4_655 . ?
Ni2 O3 Ni4 86.6(3) 4_655 . ?
Ni3 O3 Ni3 87.1(3) 4_655 . ?
Ni2 O3 Ni3 153.4(5) 4_655 . ?
Ni4 O3 Ni3 86.6(3) . . ?
Ni3 O3 H3 103.9 4_655 . ?
Ni2 O3 H3 103.3 4_655 . ?
Ni4 O3 H3 103.2 . . ?
Ni3 O3 H3 103.3 . . ?
N1 N1 C2 109.5(7) 4_655 . ?
N1 N1 Ni1 113.4(3) 4_655 . ?
C2 N1 Ni1 137.0(9) . . ?
C3 N2 N3 108.8(12) . . ?
C3 N2 Ni1 137.7(11) . . ?
N3 N2 Ni1 112.7(9) . . ?
C5 N3 N2 108.8(12) . . ?
C5 N3 Ni2 137.7(11) . . ?
N2 N3 Ni2 113.3(8) . . ?
N5 N4 C6 108.5(12) . . ?
N5 N4 Ni2 114.0(9) . . ?
C6 N4 Ni2 137.3(12) . . ?
C8 N5 N4 111.2(14) . . ?
C8 N5 Ni3 134.6(13) . . ?
N4 N5 Ni3 113.3(9) . . ?
C12 N6 N7 110.6(12) . . ?
C12 N6 Ni3 136.9(12) . . ?
N7 N6 Ni3 112.0(8) . . ?
C14 N7 N6 107.1(11) . . ?
C14 N7 Ni4 135.6(10) . . ?
N6 N7 Ni4 115.2(8) . . ?
C15 N8 N9 110.1(13) . . ?
C15 N8 Ni4 138.1(12) . . ?
N9 N8 Ni4 111.4(9) . . ?
C17 N9 N8 106.1(12) . . ?
C17 N9 Ni2 137.8(11) . 4_655 ?
N8 N9 Ni2 115.4(9) . 4_655 ?
C18 N10 N11 107.1(12) . . ?
C18 N10 Ni4 137.5(10) . . ?
N11 N10 Ni4 115.3(9) . . ?
C20 N11 N10 108.9(11) . . ?
C20 N11 Ni1 138.8(10) . . ?
N10 N11 Ni1 112.1(8) . . ?
N13 N13 C10 111.7(10) 4_655 . ?
N13 N13 Ni3 114.0(4) 4_655 . ?
C10 N13 Ni3 134.3(12) . . ?
C2 C1 C2 111(2) 4_655 . ?
C2 C1 Br1 124.4(10) 4_655 . ?
C2 C1 Br1 124.4(10) . . ?
C1 C2 N1 104.8(14) . . ?
C1 C2 H2A 127.6 . . ?
N1 C2 H2A 127.6 . . ?
N2 C3 C4 108.9(14) . . ?
N2 C3 H3A 125.5 . . ?
C4 C3 H3A 125.5 . . ?
C5 C4 C3 106.6(13) . . ?
C5 C4 Br2 127.2(11) . . ?
C3 C4 Br2 126.0(13) . . ?
N3 C5 C4 106.5(14) . . ?
N3 C5 H5 126.7 . . ?
C4 C5 H5 126.7 . . ?
C7 C6 N4 110.9(17) . . ?
C7 C6 H6 124.5 . . ?
N4 C6 H6 124.5 . . ?
C6 C7 C8 105.2(16) . . ?
C6 C7 Br3 131.5(17) . . ?
C8 C7 Br3 123.3(13) . . ?
N5 C8 C7 104.1(16) . . ?
N5 C8 H8 127.9 . . ?
C7 C8 H8 127.9 . . ?
N13 C10 C11 102.4(17) . . ?
N13 C10 H10 128.8 . . ?
C11 C10 H10 128.8 . . ?
C10 C11 C10 111(2) 4_655 . ?
C10 C11 Br4 124.6(11) 4_655 . ?
C10 C11 Br4 124.6(11) . . ?
N6 C12 C13 109.2(14) . . ?
N6 C12 H12 125.4 . . ?
C13 C12 H12 125.4 . . ?
C12 C13 C14 103.4(13) . . ?
C12 C13 Br5 129.6(12) . . ?
C14 C13 Br5 126.8(12) . . ?
N7 C14 C13 109.6(13) . . ?
N7 C14 H14 125.2 . . ?
C13 C14 H14 125.2 . . ?
N8 C15 C16 108.5(15) . . ?
N8 C15 H15 125.7 . . ?
C16 C15 H15 125.7 . . ?
C17 C16 C15 104.5(14) . . ?
C17 C16 Br6 130.2(14) . . ?
C15 C16 Br6 125.4(12) . . ?
N9 C17 C16 110.8(15) . . ?
N9 C17 H17 124.6 . . ?
C16 C17 H17 124.6 . . ?
N10 C18 C19 111.2(13) . . ?
N10 C18 H18 124.4 . . ?
C19 C18 H18 124.4 . . ?
C18 C19 C20 103.4(14) . . ?
C18 C19 Br7 127.5(14) . . ?
C20 C19 Br7 129.1(14) . . ?
N11 C20 C19 109.3(14) . . ?
N11 C20 H20 125.4 . . ?
C19 C20 H20 125.4 . . ?
C23 N12 C25 112(2) . . ?
C23 N12 C22 114(2) . . ?
C25 N12 C22 110.4(19) . . ?
C23 N12 H12A 106.6 . . ?
C25 N12 H12A 106.6 . . ?
C22 N12 H12A 106.6 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C21 C22 N12 113.2(19) . . ?
C21 C22 H22A 108.9 . . ?
N12 C22 H22A 108.9 . . ?
C21 C22 H22B 108.9 . . ?
N12 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
N12 C23 C24 105(3) . . ?
N12 C23 H23A 110.7 . . ?
C24 C23 H23A 110.7 . . ?
N12 C23 H23B 110.7 . . ?
C24 C23 H23B 110.7 . . ?
H23A C23 H23B 108.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N12 116(3) . . ?
C26 C25 H25A 108.3 . . ?
N12 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
N12 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.185

# 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 0.000 0.500 0.000 92 46 ' '
2 0.500 0.000 0.000 92 46 ' '
3 0.000 0.306 0.252 147 59 ' '
4 0.500 0.806 0.252 147 57 ' '
5 0.000 0.502 0.502 90 45 ' '
6 0.500 1.002 0.502 90 46 ' '
7 0.000 0.696 0.750 146 59 ' '
8 0.500 0.196 0.750 146 60 ' '
_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_p3
_database_code_depnum_ccdc_archive 'CCDC 1434424'
_audit_update_record             
;
2015-10-30 deposited with the CCDC.
2016-04-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H30 I12 N24 Ni8 O6'
_chemical_formula_weight         2887.32

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'

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                   11.998(7)
_cell_length_b                   26.923(16)
_cell_length_c                   19.114(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.81(3)
_cell_angle_gamma                90.00
_cell_volume                     5511(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2644
_exptl_absorpt_coefficient_mu    4.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7643
_exptl_absorpt_correction_T_max  0.7977
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'bruker apex ii'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24580
_diffrn_reflns_av_R_equivalents  0.2261
_diffrn_reflns_av_sigmaI/netI    0.2821
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9581
_reflns_number_gt                2970
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0869P)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_number_reflns         9581
_refine_ls_number_parameters     388
_refine_ls_number_restraints     181
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.0997
_refine_ls_wR_factor_ref         0.2408
_refine_ls_wR_factor_gt          0.2155
_refine_ls_goodness_of_fit_ref   0.710
_refine_ls_restrained_S_all      0.707
_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
I1 I 0.44484(15) 0.22036(7) -0.01897(11) 0.0796(5) Uani 1 1 d . . .
I2 I 0.74384(13) -0.04826(7) 0.17074(9) 0.0723(5) Uani 1 1 d . . .
I3 I 0.30058(15) -0.27582(6) 0.08285(9) 0.0687(5) Uani 1 1 d . . .
I4 I 0.25332(18) -0.14009(8) -0.27680(11) 0.0901(6) Uani 1 1 d . . .
I5 I -0.50795(18) -0.11194(8) -0.42061(10) 0.0915(6) Uani 1 1 d . . .
I6 I -0.12169(18) 0.13691(8) -0.40733(9) 0.0895(6) Uani 1 1 d . . .
Ni1 Ni 0.2189(2) 0.04108(10) 0.07565(14) 0.0494(7) Uani 1 1 d . . .
Ni2 Ni 0.1671(2) -0.05607(11) -0.00463(15) 0.0519(7) Uani 1 1 d . . .
Ni3 Ni -0.0038(2) -0.08363(10) 0.06520(14) 0.0505(7) Uani 1 1 d . . .
Ni4 Ni -0.0485(2) -0.01559(10) -0.14583(14) 0.0500(7) Uani 1 1 d . . .
O1 O 0.1130(13) 0.0185(5) -0.0499(8) 0.061(4) Uani 1 1 d . . .
H1 H 0.1616 0.0256 -0.0699 0.074 Uiso 1 1 d R . .
O2 O 0.1368(13) -0.0300(5) 0.0906(8) 0.060(4) Uani 1 1 d . . .
H2 H 0.1979 -0.0427 0.1299 0.072 Uiso 1 1 d R . .
O3 O -0.0312(11) -0.0658(5) -0.0509(7) 0.051(3) Uani 1 1 d . . .
H3 H -0.0429 -0.0941 -0.0726 0.062 Uiso 1 1 d R . .
N1 N 0.1571(17) 0.1232(7) -0.0287(11) 0.070(4) Uani 1 1 d U . .
N2 N 0.2636(16) 0.1037(7) 0.0350(11) 0.062(4) Uani 1 1 d U . .
N3 N 0.3727(14) 0.0044(7) 0.0897(10) 0.055(3) Uani 1 1 d U . .
N4 N 0.3521(14) -0.0387(7) 0.0498(9) 0.052(3) Uani 1 1 d U . .
N5 N 0.1875(17) -0.1280(7) 0.0344(11) 0.066(4) Uani 1 1 d U . .
N6 N 0.1125(17) -0.1396(8) 0.0665(11) 0.066(4) Uani 1 1 d U . .
N7 N -0.2885(14) -0.0595(6) -0.1905(9) 0.050(3) Uani 1 1 d U . .
N8 N -0.2110(14) -0.0469(6) -0.2232(8) 0.049(3) Uani 1 1 d U . .
N9 N 0.1622(15) -0.0750(6) -0.1054(10) 0.056(3) Uani 1 1 d U . .
N10 N 0.0650(16) -0.0591(7) -0.1686(10) 0.062(4) Uani 1 1 d U . .
N11 N -0.0596(13) 0.0427(6) -0.2169(8) 0.040(3) Uani 1 1 d U . .
N12 N -0.0339(14) 0.0848(6) -0.1794(9) 0.049(3) Uani 1 1 d U . .
C1 C 0.202(2) 0.1657(9) -0.0541(13) 0.060(4) Uani 1 1 d U . .
H1A H 0.1541 0.1871 -0.0966 0.072 Uiso 1 1 calc R . .
C2 C 0.3302(18) 0.1695(8) -0.0043(12) 0.055(4) Uani 1 1 d U . .
C3 C 0.3587(18) 0.1299(8) 0.0503(13) 0.057(4) Uani 1 1 d U . .
H3A H 0.4388 0.1240 0.0927 0.069 Uiso 1 1 calc R . .
C4 C 0.5010(19) 0.0094(7) 0.1370(12) 0.065(4) Uani 1 1 d DU . .
H4 H 0.5430 0.0347 0.1742 0.078 Uiso 1 1 calc R . .
C5 C 0.5549(18) -0.0321(8) 0.1168(12) 0.057(4) Uani 1 1 d U . .
C6 C 0.4551(18) -0.0606(8) 0.0571(11) 0.062(4) Uani 1 1 d DU . .
H6 H 0.4621 -0.0888 0.0294 0.074 Uiso 1 1 calc R . .
C7 C 0.254(2) -0.1662(9) 0.0407(13) 0.068(4) Uani 1 1 d U . .
H7 H 0.3174 -0.1648 0.0242 0.082 Uiso 1 1 calc R . .
C8 C 0.234(2) -0.2077(9) 0.0702(13) 0.067(4) Uani 1 1 d U . .
C9 C 0.127(2) -0.1863(9) 0.0917(13) 0.066(4) Uani 1 1 d U . .
H9 H 0.0846 -0.2031 0.1165 0.080 Uiso 1 1 calc R . .
C10 C 0.2370(19) -0.1025(8) -0.1332(12) 0.055(4) Uani 1 1 d U . .
H10 H 0.3120 -0.1195 -0.1003 0.066 Uiso 1 1 calc R . .
C11 C 0.189(2) -0.1011(8) -0.2085(13) 0.058(4) Uani 1 1 d U . .
C12 C 0.076(2) -0.0758(9) -0.2371(13) 0.062(4) Uani 1 1 d U . .
H12 H 0.0176 -0.0707 -0.2904 0.074 Uiso 1 1 calc R . .
C13 C -0.2718(18) -0.0597(8) -0.3005(11) 0.056(4) Uani 1 1 d U . .
H13 H -0.2442 -0.0524 -0.3388 0.068 Uiso 1 1 calc R . .
C14 C -0.3835(18) -0.0858(8) -0.3147(11) 0.051(4) Uani 1 1 d U . .
C15 C -0.3866(18) -0.0833(8) -0.2415(10) 0.050(4) Uani 1 1 d U . .
H15 H -0.4506 -0.0968 -0.2311 0.060 Uiso 1 1 calc R . .
C16 C -0.0862(18) 0.0480(8) -0.2902(12) 0.053(4) Uani 1 1 d U . .
H16 H -0.1095 0.0218 -0.3274 0.064 Uiso 1 1 calc R . .
C17 C -0.0755(18) 0.0980(8) -0.3062(11) 0.051(4) Uani 1 1 d U . .
C18 C -0.0463(19) 0.1235(9) -0.2266(13) 0.064(4) Uani 1 1 d U . .
H18 H -0.0390 0.1579 -0.2144 0.077 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
I1 C2 2.049(18) . ?
I2 C5 2.070(19) . ?
I3 C8 1.97(3) . ?
I4 C11 2.074(19) . ?
I5 C14 2.024(18) . ?
I6 C17 2.04(2) . ?
Ni1 N3 2.002(15) . ?
Ni1 N7 2.026(15) 3 ?
Ni1 N2 2.028(17) . ?
Ni1 O3 2.185(13) 3 ?
Ni1 O2 2.229(13) . ?
Ni1 O1 2.234(14) . ?
Ni1 Ni2 2.953(4) . ?
Ni1 Ni4 2.987(3) 3 ?
Ni1 Ni3 2.992(4) 3 ?
Ni2 N9 1.967(16) . ?
Ni2 N4 2.036(16) . ?
Ni2 N5 2.05(2) . ?
Ni2 O2 2.130(15) . ?
Ni2 O3 2.147(12) . ?
Ni2 O1 2.167(14) . ?
Ni2 Ni4 2.978(4) . ?
Ni3 N1 1.960(19) 3 ?
Ni3 N12 2.020(15) 3 ?
Ni3 N6 2.046(19) . ?
Ni3 O2 2.104(13) . ?
Ni3 O1 2.128(15) 3 ?
Ni3 O3 2.147(12) . ?
Ni3 Ni1 2.992(4) 3 ?
Ni4 N10 1.988(18) . ?
Ni4 N8 2.024(15) . ?
Ni4 N11 2.041(15) . ?
Ni4 O2 2.179(15) 3 ?
Ni4 O1 2.181(15) . ?
Ni4 O3 2.195(13) . ?
Ni4 Ni1 2.987(3) 3 ?
O1 Ni3 2.128(15) 3 ?
O1 H1 0.8502 . ?
O2 Ni4 2.179(15) 3 ?
O2 H2 0.8497 . ?
O3 Ni1 2.185(13) 3 ?
O3 H3 0.8502 . ?
N1 N2 1.41(2) . ?
N1 C1 1.44(3) . ?
N1 Ni3 1.960(19) 3 ?
N2 C3 1.26(2) . ?
N3 N4 1.35(2) . ?
N3 C4 1.40(2) . ?
N4 C6 1.32(2) . ?
N5 C7 1.27(3) . ?
N5 N6 1.33(2) . ?
N6 C9 1.33(3) . ?
N7 C15 1.31(2) . ?
N7 N8 1.376(19) . ?
N7 Ni1 2.026(15) 3 ?
N8 C13 1.36(2) . ?
N9 N10 1.32(2) . ?
N9 C10 1.44(2) . ?
N10 C12 1.44(3) . ?
N11 C16 1.30(2) . ?
N11 N12 1.30(2) . ?
N12 C18 1.34(3) . ?
N12 Ni3 2.020(15) 3 ?
C1 C2 1.40(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.42(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.43(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.45(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.32(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.62(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.29(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.40(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.43(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.42(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.40(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.56(3) . ?
C18 H18 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 N7 94.1(7) . 3 ?
N3 Ni1 N2 94.3(7) . . ?
N7 Ni1 N2 99.2(7) 3 . ?
N3 Ni1 O3 167.6(7) . 3 ?
N7 Ni1 O3 92.4(5) 3 3 ?
N2 Ni1 O3 95.1(6) . 3 ?
N3 Ni1 O2 89.6(6) . . ?
N7 Ni1 O2 93.5(6) 3 . ?
N2 Ni1 O2 166.4(7) . . ?
O3 Ni1 O2 79.4(5) 3 . ?
N3 Ni1 O1 93.0(6) . . ?
N7 Ni1 O1 170.7(5) 3 . ?
N2 Ni1 O1 86.3(6) . . ?
O3 Ni1 O1 79.6(5) 3 . ?
O2 Ni1 O1 80.5(5) . . ?
N3 Ni1 Ni2 66.3(5) . . ?
N7 Ni1 Ni2 131.8(5) 3 . ?
N2 Ni1 Ni2 124.6(5) . . ?
O3 Ni1 Ni2 101.7(4) 3 . ?
O2 Ni1 Ni2 46.0(4) . . ?
O1 Ni1 Ni2 46.9(4) . . ?
N3 Ni1 Ni4 127.1(5) . 3 ?
N7 Ni1 Ni4 66.5(4) 3 3 ?
N2 Ni1 Ni4 135.7(5) . 3 ?
O3 Ni1 Ni4 47.2(3) 3 3 ?
O2 Ni1 Ni4 46.6(4) . 3 ?
O1 Ni1 Ni4 104.3(3) . 3 ?
Ni2 Ni1 Ni4 90.21(10) . 3 ?
N3 Ni1 Ni3 132.7(5) . 3 ?
N7 Ni1 Ni3 130.4(5) 3 3 ?
N2 Ni1 Ni3 66.8(5) . 3 ?
O3 Ni1 Ni3 45.8(3) 3 3 ?
O2 Ni1 Ni3 101.1(4) . 3 ?
O1 Ni1 Ni3 45.2(4) . 3 ?
Ni2 Ni1 Ni3 88.72(11) . 3 ?
Ni4 Ni1 Ni3 90.29(10) 3 3 ?
N9 Ni2 N4 96.0(7) . . ?
N9 Ni2 N5 93.3(7) . . ?
N4 Ni2 N5 96.2(7) . . ?
N9 Ni2 O2 168.8(6) . . ?
N4 Ni2 O2 93.1(6) . . ?
N5 Ni2 O2 92.2(6) . . ?
N9 Ni2 O3 91.5(6) . . ?
N4 Ni2 O3 171.2(6) . . ?
N5 Ni2 O3 87.9(6) . . ?
O2 Ni2 O3 78.9(5) . . ?
N9 Ni2 O1 88.7(6) . . ?
N4 Ni2 O1 93.0(6) . . ?
N5 Ni2 O1 170.4(6) . . ?
O2 Ni2 O1 84.3(5) . . ?
O3 Ni2 O1 82.6(5) . . ?
N9 Ni2 Ni1 130.1(5) . . ?
N4 Ni2 Ni1 66.8(5) . . ?
N5 Ni2 Ni1 133.2(5) . . ?
O2 Ni2 Ni1 48.8(4) . . ?
O3 Ni2 Ni1 104.8(4) . . ?
O1 Ni2 Ni1 48.8(4) . . ?
N9 Ni2 Ni4 65.0(5) . . ?
N4 Ni2 Ni4 132.9(5) . . ?
N5 Ni2 Ni4 126.0(5) . . ?
O2 Ni2 Ni4 103.9(4) . . ?
O3 Ni2 Ni4 47.4(3) . . ?
O1 Ni2 Ni4 47.0(4) . . ?
Ni1 Ni2 Ni4 92.29(11) . . ?
N1 Ni3 N12 95.3(7) 3 3 ?
N1 Ni3 N6 97.5(8) 3 . ?
N12 Ni3 N6 99.0(7) 3 . ?
N1 Ni3 O2 168.6(7) 3 . ?
N12 Ni3 O2 89.7(6) 3 . ?
N6 Ni3 O2 91.8(7) . . ?
N1 Ni3 O1 88.7(7) 3 3 ?
N12 Ni3 O1 89.1(6) 3 3 ?
N6 Ni3 O1 169.2(6) . 3 ?
O2 Ni3 O1 81.1(5) . 3 ?
N1 Ni3 O3 94.2(7) 3 . ?
N12 Ni3 O3 167.4(6) 3 . ?
N6 Ni3 O3 87.9(6) . . ?
O2 Ni3 O3 79.5(5) . . ?
O1 Ni3 O3 82.9(5) 3 . ?
N1 Ni3 Ni1 66.3(6) 3 3 ?
N12 Ni3 Ni1 131.3(5) 3 3 ?
N6 Ni3 Ni1 126.8(5) . 3 ?
O2 Ni3 Ni1 102.8(4) . 3 ?
O1 Ni3 Ni1 48.2(4) 3 3 ?
O3 Ni3 Ni1 46.9(3) . 3 ?
N10 Ni4 N8 97.1(7) . . ?
N10 Ni4 N11 98.8(6) . . ?
N8 Ni4 N11 94.7(6) . . ?
N10 Ni4 O2 165.6(6) . 3 ?
N8 Ni4 O2 94.0(6) . 3 ?
N11 Ni4 O2 89.4(5) . 3 ?
N10 Ni4 O1 89.7(6) . . ?
N8 Ni4 O1 170.9(5) . . ?
N11 Ni4 O1 90.1(5) . . ?
O2 Ni4 O1 78.3(5) 3 . ?
N10 Ni4 O3 90.0(6) . . ?
N8 Ni4 O3 92.7(5) . . ?
N11 Ni4 O3 167.7(5) . . ?
O2 Ni4 O3 80.3(5) 3 . ?
O1 Ni4 O3 81.2(4) . . ?
N10 Ni4 Ni2 65.3(5) . . ?
N8 Ni4 Ni2 131.8(5) . . ?
N11 Ni4 Ni2 130.8(4) . . ?
O2 Ni4 Ni2 100.4(4) 3 . ?
O1 Ni4 Ni2 46.6(4) . . ?
O3 Ni4 Ni2 46.0(3) . . ?
N10 Ni4 Ni1 129.6(6) . 3 ?
N8 Ni4 Ni1 66.6(4) . 3 ?
N11 Ni4 Ni1 128.6(4) . 3 ?
O2 Ni4 Ni1 48.1(3) 3 3 ?
O1 Ni4 Ni1 104.4(3) . 3 ?
O3 Ni4 Ni1 46.9(3) . 3 ?
Ni2 Ni4 Ni1 89.97(10) . 3 ?
Ni3 O1 Ni2 150.8(6) 3 . ?
Ni3 O1 Ni4 88.5(5) 3 . ?
Ni2 O1 Ni4 86.4(5) . . ?
Ni3 O1 Ni1 86.6(5) 3 . ?
Ni2 O1 Ni1 84.3(5) . . ?
Ni4 O1 Ni1 151.2(6) . . ?
Ni3 O1 H1 105.0 3 . ?
Ni2 O1 H1 104.2 . . ?
Ni4 O1 H1 104.3 . . ?
Ni1 O1 H1 104.4 . . ?
Ni3 O2 Ni2 90.3(5) . . ?
Ni3 O2 Ni4 89.1(5) . 3 ?
Ni2 O2 Ni4 155.1(7) . 3 ?
Ni3 O2 Ni1 156.1(7) . . ?
Ni2 O2 Ni1 85.3(5) . . ?
Ni4 O2 Ni1 85.3(5) 3 . ?
Ni3 O2 H2 102.1 . . ?
Ni2 O2 H2 102.1 . . ?
Ni4 O2 H2 102.4 3 . ?
Ni1 O2 H2 101.8 . . ?
Ni3 O3 Ni2 88.7(4) . . ?
Ni3 O3 Ni1 87.4(5) . 3 ?
Ni2 O3 Ni1 153.4(7) . 3 ?
Ni3 O3 Ni4 154.9(7) . . ?
Ni2 O3 Ni4 86.6(5) . . ?
Ni1 O3 Ni4 86.0(5) 3 . ?
Ni3 O3 H3 102.5 . . ?
Ni2 O3 H3 102.6 . . ?
Ni1 O3 H3 103.9 3 . ?
Ni4 O3 H3 102.6 . . ?
N2 N1 C1 104.7(16) . . ?
N2 N1 Ni3 116.4(13) . 3 ?
C1 N1 Ni3 138.3(15) . 3 ?
C3 N2 N1 111.5(17) . . ?
C3 N2 Ni1 138.2(16) . . ?
N1 N2 Ni1 110.3(12) . . ?
N4 N3 C4 108.5(15) . . ?
N4 N3 Ni1 115.2(12) . . ?
C4 N3 Ni1 136.0(14) . . ?
C6 N4 N3 113.7(16) . . ?
C6 N4 Ni2 134.7(14) . . ?
N3 N4 Ni2 111.5(11) . . ?
C7 N5 N6 107(2) . . ?
C7 N5 Ni2 139.9(16) . . ?
N6 N5 Ni2 113.2(14) . . ?
C9 N6 N5 112.6(19) . . ?
C9 N6 Ni3 132.6(15) . . ?
N5 N6 Ni3 114.8(15) . . ?
C15 N7 N8 110.2(15) . . ?
C15 N7 Ni1 136.1(13) . 3 ?
N8 N7 Ni1 113.5(11) . 3 ?
C13 N8 N7 106.8(14) . . ?
C13 N8 Ni4 139.9(13) . . ?
N7 N8 Ni4 113.3(11) . . ?
N10 N9 C10 105.7(16) . . ?
N10 N9 Ni2 116.0(12) . . ?
C10 N9 Ni2 138.4(13) . . ?
N9 N10 C12 109.1(17) . . ?
N9 N10 Ni4 113.7(13) . . ?
C12 N10 Ni4 137.0(15) . . ?
C16 N11 N12 112.4(16) . . ?
C16 N11 Ni4 135.6(14) . . ?
N12 N11 Ni4 112.0(10) . . ?
N11 N12 C18 112.3(16) . . ?
N11 N12 Ni3 117.6(12) . 3 ?
C18 N12 Ni3 129.9(14) . 3 ?
C2 C1 N1 107.0(18) . . ?
C2 C1 H1A 126.5 . . ?
N1 C1 H1A 126.5 . . ?
C1 C2 C3 105.7(17) . . ?
C1 C2 I1 123.7(14) . . ?
C3 C2 I1 130.4(15) . . ?
N2 C3 C2 110.9(19) . . ?
N2 C3 H3A 124.5 . . ?
C2 C3 H3A 124.5 . . ?
N3 C4 C5 104.5(16) . . ?
N3 C4 H4 127.7 . . ?
C5 C4 H4 127.7 . . ?
C4 C5 C6 108.3(15) . . ?
C4 C5 I2 123.9(16) . . ?
C6 C5 I2 127.8(16) . . ?
N4 C6 C5 104.4(16) . . ?
N4 C6 H6 127.8 . . ?
C5 C6 H6 127.8 . . ?
N5 C7 C8 120(2) . . ?
N5 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 97(2) . . ?
C7 C8 I3 134.2(18) . . ?
C9 C8 I3 128.6(16) . . ?
N6 C9 C8 103.4(18) . . ?
N6 C9 H9 128.3 . . ?
C8 C9 H9 128.3 . . ?
C11 C10 N9 111.1(18) . . ?
C11 C10 H10 124.4 . . ?
N9 C10 H10 124.4 . . ?
C10 C11 C12 108.5(17) . . ?
C10 C11 I4 125.7(16) . . ?
C12 C11 I4 125.0(16) . . ?
C11 C12 N10 105.4(18) . . ?
C11 C12 H12 127.3 . . ?
N10 C12 H12 127.3 . . ?
N8 C13 C14 109.2(16) . . ?
N8 C13 H13 125.4 . . ?
C14 C13 H13 125.4 . . ?
C15 C14 C13 103.2(16) . . ?
C15 C14 I5 131.9(14) . . ?
C13 C14 I5 124.6(13) . . ?
N7 C15 C14 110.2(17) . . ?
N7 C15 H15 124.9 . . ?
C14 C15 H15 124.9 . . ?
N11 C16 C17 109.9(18) . . ?
N11 C16 H16 125.1 . . ?
C17 C16 H16 125.1 . . ?
C16 C17 C18 102.3(17) . . ?
C16 C17 I6 133.5(15) . . ?
C18 C17 I6 122.9(15) . . ?
N12 C18 C17 102.8(18) . . ?
N12 C18 H18 128.6 . . ?
C17 C18 H18 128.6 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.446
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.235

# 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 -0.005 -0.008 0.438 2716 1576 ' '
_platon_squeeze_details          ?

