# 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_I-4_BF4_-50
_database_code_depnum_ccdc_archive 'CCDC 1033454'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H117.71 B8 F32 N28 Ni4 O17.35'
_chemical_formula_iupac          ?
_chemical_formula_weight         2294.40
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   15.754(2)
_cell_length_b                   15.754(2)
_cell_length_c                   19.585(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4860.8(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8071
_cell_measurement_theta_min      2.5858
_cell_measurement_theta_max      30.0780
_cell_measurement_temperature    223

_exptl_crystal_description       prismatic
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2361

_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.90

_exptl_special_details           
;
;

_diffrn_ambient_temperature      223

_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Tourbo X-ray Source'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayered conforcal mirror'

_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            17913
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         30.18
_diffrn_reflns_theta_full        30.18
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
;

_reflns_number_total             7017
_reflns_number_gt                5781
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0620
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1742
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.102
_refine_ls_number_reflns         7017
_refine_ls_number_parameters     354
_refine_ls_number_restraints     196
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1099P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.466
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Flack x determined using 2364 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.101(11)

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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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'

_computing_data_collection       'Bruker SMART APEXII ULTRA'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.7231(11) 1.0825(7) 0.8073(11) 0.158(10) Uani d . . . 1.0 . .
H H1A 0.7531 1.132 0.7906 0.237 Uiso calc U . R 1.0 . .
H H1B 0.6845 1.0993 0.8435 0.237 Uiso calc U . R 1.0 . .
H H1C 0.691 1.057 0.7703 0.237 Uiso calc U . R 1.0 . .
C C2 0.7868(7) 1.0181(5) 0.8350(6) 0.085(3) Uani d . . . 1.0 . .
C C3 0.8171(6) 0.9008(5) 0.9171(4) 0.069(2) Uani d . . . 1.0 . .
H H3A 0.8175 0.9082 0.9668 0.083 Uiso calc U . R 1.0 . .
H H3B 0.8753 0.9095 0.9007 0.083 Uiso calc U . R 1.0 . .
C C4 0.7904(5) 0.8093(4) 0.9008(4) 0.0514(16) Uani d . . . 1.0 . .
C C5 0.8527(5) 0.7524(5) 0.9404(4) 0.0585(18) Uani d . . . 1.0 . .
H H5A 0.9104 0.7741 0.9341 0.07 Uiso calc U . R 1.0 . .
H H5B 0.8393 0.7556 0.9892 0.07 Uiso calc U . R 1.0 . .
C C6 0.6976(5) 0.7950(4) 0.9233(4) 0.0538(17) Uani d . . . 1.0 . .
H H6A 0.6867 0.8286 0.9645 0.065 Uiso calc U . R 1.0 . .
H H6B 0.6598 0.816 0.8873 0.065 Uiso calc U . R 1.0 . .
C C7 0.7971(4) 0.7870(4) 0.8253(3) 0.0402(11) Uani d . . . 1.0 . .
C C8 0.8495(3) 0.8229(4) 0.7108(3) 0.0394(11) Uani d . . . 1.0 . .
H H8A 0.8298 0.8744 0.6877 0.047 Uiso calc U . R 1.0 . .
H H8B 0.8116 0.7764 0.6976 0.047 Uiso calc U . R 1.0 . .
C C9 0.9403(3) 0.8023(3) 0.6861(3) 0.0314(9) Uani d . . . 1.0 . .
C C10 1.0014(4) 0.8703(3) 0.7148(3) 0.0382(11) Uani d . . . 1.0 . .
H H10A 0.9738 0.9259 0.7117 0.046 Uiso calc U . R 1.0 . .
H H10B 1.0115 0.8585 0.7632 0.046 Uiso calc U . R 1.0 . .
C C11 0.9345(3) 0.8073(3) 0.6070(3) 0.0363(10) Uani d . . . 1.0 . .
H H11A 0.8848 0.7749 0.592 0.044 Uiso calc U . R 1.0 . .
H H11B 0.9253 0.8667 0.5939 0.044 Uiso calc U . R 1.0 . .
C C12 0.9713(3) 0.7147(3) 0.7067(3) 0.0337(10) Uani d . . . 1.0 . .
N N1 0.7627(6) 0.9654(4) 0.8871(5) 0.090(3) Uani d . . . 1.0 . .
H H1 0.7115 0.9709 0.9033 0.108 Uiso calc U . R 1.0 . .
N N2 0.8501(3) 0.6621(4) 0.9186(3) 0.0473(11) Uani d . . . 1.0 . .
H H2A 0.859 0.6293 0.9555 0.057 Uiso calc U . R 1.0 . .
H H2B 0.8934 0.653 0.8895 0.057 Uiso calc U . R 1.0 . .
N N3 0.6766(3) 0.7054(3) 0.9374(3) 0.0425(11) Uani d . . . 1.0 . .
H H3C 0.62 0.6984 0.9341 0.051 Uiso calc U . R 1.0 . .
H H3D 0.6919 0.6928 0.9805 0.051 Uiso calc U . R 1.0 . .
N N4 0.8435(3) 0.8356(3) 0.7846(3) 0.0418(10) Uani d . . . 1.0 . .
H H4 0.8718 0.8773 0.8028 0.05 Uiso calc U . R 1.0 . .
N N5 1.0838(3) 0.8748(3) 0.6796(2) 0.0371(9) Uani d . . . 1.0 . .
H H5C 1.124 0.8882 0.7104 0.045 Uiso calc U . R 1.0 . .
H H5D 1.0817 0.9172 0.6488 0.045 Uiso calc U . R 1.0 . .
N N6 1.0097(3) 0.7752(3) 0.5707(2) 0.0383(9) Uani d . . . 1.0 . .
H H6C 1.0206 0.8102 0.5354 0.046 Uiso calc U . R 1.0 . .
H H6D 0.997 0.724 0.5532 0.046 Uiso calc U . R 1.0 . .
N N7 0.9205(3) 0.6603(3) 0.7363(3) 0.0424(11) Uani d . . . 1.0 . .
H H7A 0.9391 0.6102 0.7476 0.051 Uiso calc U . R 1.0 . .
H H7B 0.8681 0.6741 0.7446 0.051 Uiso calc U . R 1.0 . .
Ni Ni1 0.73652(4) 0.62119(4) 0.87082(3) 0.03292(19) Uani d . . . 1.0 . .
O O1 0.8577(4) 1.0099(3) 0.8083(4) 0.0772(19) Uani d . . . 1.0 . .
O O2 0.7616(3) 0.7212(2) 0.8035(2) 0.0391(8) Uani d . . . 1.0 . .
O O3 1.0469(2) 0.6948(2) 0.6946(2) 0.0419(9) Uani d . . . 1.0 . .
B B1 1.0 0 0.5 0.040(2) Uani d T P S 1.0 . .
B B2 0.2876(5) 0.0520(6) 0.5970(5) 0.061(2) Uani d . . . 1.0 . .
F F1 0.9426(4) 0.0435(4) 0.5372(4) 0.106(3) Uani d . . . 1.0 . .
F F2 0.3174(5) 0.0571(5) 0.6613(4) 0.108(2) Uani d . . . 1.0 . .
F F3 0.2728(4) 0.1301(4) 0.5700(3) 0.0875(16) Uani d . . . 1.0 . .
F F4 0.3427(4) 0.0095(5) 0.5520(4) 0.103(2) Uani d . . . 1.0 . .
F F5 0.2127(3) 0.0071(4) 0.5983(4) 0.0919(19) Uani d . . . 1.0 . .
O O4SA 1.0 0.5 0.75 0.058(5) Uani d TU P S 0.65(3) A 1
B B3C 0.799(2) 0.613(2) 0.6181(17) 0.132(6) Uani d U P D 0.228(10) B 1
F F6C 0.873(3) 0.642(3) 0.578(2) 0.127(7) Uani d U P D 0.228(10) B 1
F F7C 0.752(3) 0.550(3) 0.579(2) 0.148(7) Uiso d U P D 0.228(10) B 1
F F8C 0.743(3) 0.652(3) 0.670(2) 0.150(10) Uiso d U P D 0.228(10) B 1
O O3SA 0.9086(11) 0.5060(10) 0.4482(10) 0.189(7) Uani d U . . 1.0 C 1
O O4SB 1.0 0.5 0.6886(16) 0.066(9) Uani d TU P S 0.35(3) A 2
F F6B 0.9157(11) 0.6010(11) 0.5822(9) 0.122(5) Uani d U P D 0.522(10) B 2
F F9B 0.8161(11) 0.5252(8) 0.6393(7) 0.160(4) Uani d U P D 0.75 B 2
B B3B 0.8322(12) 0.5736(12) 0.5816(8) 0.121(5) Uani d U P D 0.522(10) B 2
F F8B 0.7819(13) 0.6453(11) 0.5833(9) 0.145(5) Uani d U P D 0.522(10) B 2
F F7B 0.8194(10) 0.5283(8) 0.5217(6) 0.114(5) Uani d U P D 0.522(10) B 2


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.527(19) ?
C1 H1A . 0.97 ?
C1 H1B . 0.97 ?
C1 H1C . 0.97 ?
C2 O1 . 1.241(11) ?
C2 N1 . 1.368(12) ?
C3 N1 . 1.456(14) ?
C3 C4 . 1.534(9) ?
C3 H3A . 0.98 ?
C3 H3B . 0.98 ?
C4 C7 . 1.525(9) ?
C4 C5 . 1.539(12) ?
C4 C6 . 1.543(9) ?
C5 N2 . 1.486(9) ?
C5 H5A . 0.98 ?
C5 H5B . 0.98 ?
C6 N3 . 1.477(8) ?
C6 H6A . 0.98 ?
C6 H6B . 0.98 ?
C7 O2 . 1.252(7) ?
C7 N4 . 1.325(7) ?
C8 N4 . 1.463(8) ?
C8 C9 . 1.545(7) ?
C8 H8A . 0.98 ?
C8 H8B . 0.98 ?
C9 C12 . 1.518(7) ?
C9 C10 . 1.547(7) ?
C9 C11 . 1.554(8) ?
C10 N5 . 1.472(7) ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C11 N6 . 1.472(7) ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C12 O3 . 1.253(7) ?
C12 N7 . 1.309(7) ?
N1 H1 . 0.87 ?
N2 Ni1 . 2.119(5) ?
N2 H2A . 0.9 ?
N2 H2B . 0.9 ?
N3 Ni1 . 2.086(4) ?
N3 H3C . 0.9 ?
N3 H3D . 0.9 ?
N4 H4 . 0.87 ?
N5 Ni1 7_566 2.096(5) ?
N5 H5C . 0.9 ?
N5 H5D . 0.9 ?
N6 Ni1 7_566 2.104(5) ?
N6 H6C . 0.9 ?
N6 H6D . 0.9 ?
N7 H7A . 0.87 ?
N7 H7B . 0.87 ?
Ni1 O3 8_646 2.046(4) ?
Ni1 O2 . 2.092(4) ?
Ni1 N5 8_646 2.096(5) ?
Ni1 N6 8_646 2.104(5) ?
O3 Ni1 7_566 2.046(4) ?
B1 F1 4_646 1.348(5) ?
B1 F1 3_666 1.348(5) ?
B1 F1 2_755 1.348(5) ?
B1 F1 . 1.348(5) ?
B2 F2 . 1.347(10) ?
B2 F3 . 1.360(12) ?
B2 F5 . 1.376(10) ?
B2 F4 . 1.407(12) ?
B3C F7C . 1.45(3) ?
B3C F8C . 1.48(3) ?
B3C F6C . 1.48(3) ?
F6B B3B . 1.385(16) ?
F9B B3B . 1.385(15) ?
B3B F8B . 1.381(16) ?
B3B F7B . 1.388(15) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
O1 C2 N1 . . 120.1(9) ?
O1 C2 C1 . . 120.7(9) ?
N1 C2 C1 . . 119.0(9) ?
N1 C3 C4 . . 114.3(8) ?
N1 C3 H3A . . 108.7 ?
C4 C3 H3A . . 108.7 ?
N1 C3 H3B . . 108.7 ?
C4 C3 H3B . . 108.7 ?
H3A C3 H3B . . 107.6 ?
C7 C4 C3 . . 113.5(6) ?
C7 C4 C5 . . 108.1(5) ?
C3 C4 C5 . . 105.5(7) ?
C7 C4 C6 . . 107.9(6) ?
C3 C4 C6 . . 109.8(6) ?
C5 C4 C6 . . 112.1(6) ?
N2 C5 C4 . . 113.3(6) ?
N2 C5 H5A . . 108.9 ?
C4 C5 H5A . . 108.9 ?
N2 C5 H5B . . 108.9 ?
C4 C5 H5B . . 108.9 ?
H5A C5 H5B . . 107.7 ?
N3 C6 C4 . . 113.9(5) ?
N3 C6 H6A . . 108.8 ?
C4 C6 H6A . . 108.8 ?
N3 C6 H6B . . 108.8 ?
C4 C6 H6B . . 108.8 ?
H6A C6 H6B . . 107.7 ?
O2 C7 N4 . . 121.3(5) ?
O2 C7 C4 . . 119.4(5) ?
N4 C7 C4 . . 119.2(5) ?
N4 C8 C9 . . 113.5(5) ?
N4 C8 H8A . . 108.9 ?
C9 C8 H8A . . 108.9 ?
N4 C8 H8B . . 108.9 ?
C9 C8 H8B . . 108.9 ?
H8A C8 H8B . . 107.7 ?
C12 C9 C8 . . 114.0(4) ?
C12 C9 C10 . . 109.4(4) ?
C8 C9 C10 . . 108.5(4) ?
C12 C9 C11 . . 109.3(4) ?
C8 C9 C11 . . 104.3(4) ?
C10 C9 C11 . . 111.3(4) ?
N5 C10 C9 . . 114.3(4) ?
N5 C10 H10A . . 108.7 ?
C9 C10 H10A . . 108.7 ?
N5 C10 H10B . . 108.7 ?
C9 C10 H10B . . 108.7 ?
H10A C10 H10B . . 107.6 ?
N6 C11 C9 . . 114.6(4) ?
N6 C11 H11A . . 108.6 ?
C9 C11 H11A . . 108.6 ?
N6 C11 H11B . . 108.6 ?
C9 C11 H11B . . 108.6 ?
H11A C11 H11B . . 107.6 ?
O3 C12 N7 . . 120.1(5) ?
O3 C12 C9 . . 118.9(4) ?
N7 C12 C9 . . 121.0(5) ?
C2 N1 C3 . . 124.2(8) ?
C2 N1 H1 . . 117.9 ?
C3 N1 H1 . . 117.9 ?
C5 N2 Ni1 . . 116.2(5) ?
C5 N2 H2A . . 108.2 ?
Ni1 N2 H2A . . 108.2 ?
C5 N2 H2B . . 108.2 ?
Ni1 N2 H2B . . 108.2 ?
H2A N2 H2B . . 107.4 ?
C6 N3 Ni1 . . 112.9(3) ?
C6 N3 H3C . . 109.0 ?
Ni1 N3 H3C . . 109.0 ?
C6 N3 H3D . . 109.0 ?
Ni1 N3 H3D . . 109.0 ?
H3C N3 H3D . . 107.8 ?
C7 N4 C8 . . 123.4(5) ?
C7 N4 H4 . . 118.3 ?
C8 N4 H4 . . 118.3 ?
C10 N5 Ni1 . 7_566 115.4(3) ?
C10 N5 H5C . . 108.4 ?
Ni1 N5 H5C 7_566 . 108.4 ?
C10 N5 H5D . . 108.4 ?
Ni1 N5 H5D 7_566 . 108.4 ?
H5C N5 H5D . . 107.5 ?
C11 N6 Ni1 . 7_566 116.1(4) ?
C11 N6 H6C . . 108.3 ?
Ni1 N6 H6C 7_566 . 108.3 ?
C11 N6 H6D . . 108.3 ?
Ni1 N6 H6D 7_566 . 108.3 ?
H6C N6 H6D . . 107.4 ?
C12 N7 H7A . . 120.0 ?
C12 N7 H7B . . 120.0 ?
H7A N7 H7B . . 120.0 ?
O3 Ni1 N3 8_646 . 174.32(18) ?
O3 Ni1 O2 8_646 . 86.35(16) ?
N3 Ni1 O2 . . 90.04(18) ?
O3 Ni1 N5 8_646 8_646 89.22(18) ?
N3 Ni1 N5 . 8_646 95.4(2) ?
O2 Ni1 N5 . 8_646 94.15(18) ?
O3 Ni1 N6 8_646 8_646 84.82(18) ?
N3 Ni1 N6 . 8_646 98.7(2) ?
O2 Ni1 N6 . 8_646 171.08(17) ?
N5 Ni1 N6 8_646 8_646 87.03(19) ?
O3 Ni1 N2 8_646 . 90.2(2) ?
N3 Ni1 N2 . . 85.0(2) ?
O2 Ni1 N2 . . 83.7(2) ?
N5 Ni1 N2 8_646 . 177.8(2) ?
N6 Ni1 N2 8_646 . 95.0(2) ?
C7 O2 Ni1 . . 119.5(4) ?
C12 O3 Ni1 . 7_566 122.0(3) ?
F1 B1 F1 4_646 3_666 114.6(8) ?
F1 B1 F1 4_646 2_755 107.0(4) ?
F1 B1 F1 3_666 2_755 107.0(4) ?
F1 B1 F1 4_646 . 107.0(4) ?
F1 B1 F1 3_666 . 107.0(4) ?
F1 B1 F1 2_755 . 114.6(8) ?
F2 B2 F3 . . 111.7(8) ?
F2 B2 F5 . . 108.3(9) ?
F3 B2 F5 . . 109.0(7) ?
F2 B2 F4 . . 113.5(8) ?
F3 B2 F4 . . 106.9(8) ?
F5 B2 F4 . . 107.2(7) ?
F7C B3C F8C . . 110.(2) ?
F7C B3C F6C . . 110.(2) ?
F8C B3C F6C . . 135.(4) ?
F8B B3B F9B . . 109.0(13) ?
F8B B3B F6B . . 106.8(18) ?
F9B B3B F6B . . 109.8(13) ?
F8B B3B F7B . . 110.9(14) ?
F9B B3B F7B . . 112.3(15) ?
F6B B3B F7B . . 107.7(13) ?

####################################################################### 
# 
# 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_I-4_BF4_-80
_database_code_depnum_ccdc_archive 'CCDC 1033455'
_audit_update_record             
;
2014-11-10 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H127.61 B8 F32 N28 Ni4 O22.30'
_chemical_formula_iupac          ?
_chemical_formula_weight         2383.58
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   15.7784(6)
_cell_length_b                   15.7784(6)
_cell_length_c                   19.7467(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4916.1(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    863
_cell_measurement_theta_min      1.5982
_cell_measurement_theta_max      29.5621
_cell_measurement_temperature    193

_exptl_crystal_description       prismatic
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2460

_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.90

_exptl_special_details           
;
;

_diffrn_ambient_temperature      193

_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Tourbo X-ray Source'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayered conforcal mirror'

_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            18856
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         30.15
_diffrn_reflns_theta_full        30.15
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
;

_reflns_number_total             7075
_reflns_number_gt                6677
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1125
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.087
_refine_ls_number_reflns         7075
_refine_ls_number_parameters     401
_refine_ls_number_restraints     302
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0843P)²] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.447
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;
Flack x determined using 3031 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(4)

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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 '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'

_computing_data_collection       'Bruker SMART APEXII ULTRA'
_computing_cell_refinement       'APEX2 v2014.5-0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.7211(6) 1.0787(4) 0.8024(6) 0.106(3) Uani d . . . 1.0 . .
H H1A 0.7496 1.1325 0.7925 0.159 Uiso calc U . R 1.0 . .
H H1B 0.6766 1.0882 0.8362 0.159 Uiso calc U . R 1.0 . .
H H1C 0.6957 1.0562 0.7608 0.159 Uiso calc U . R 1.0 . .
C C2 0.7840(4) 1.0168(2) 0.8294(3) 0.0642(15) Uani d . . . 1.0 . .
C C3 0.8121(4) 0.9030(2) 0.9128(3) 0.0589(13) Uani d . . . 1.0 . .
H H3A 0.8098 0.9121 0.9624 0.071 Uiso calc U . R 1.0 . .
H H3B 0.8714 0.9124 0.8982 0.071 Uiso calc U . R 1.0 . .
C C4 0.7880(3) 0.8098(2) 0.89769(19) 0.0397(7) Uani d . . . 1.0 . .
C C5 0.8512(3) 0.7538(2) 0.9378(2) 0.0443(8) Uani d . . . 1.0 . .
H H5A 0.9092 0.7762 0.9314 0.053 Uiso calc U . R 1.0 . .
H H5B 0.8375 0.7575 0.9867 0.053 Uiso calc U . R 1.0 . .
C C6 0.6955(3) 0.7946(2) 0.9212(2) 0.0460(9) Uani d . . . 1.0 . .
H H6A 0.6849 0.8283 0.9627 0.055 Uiso calc U . R 1.0 . .
H H6B 0.6564 0.8154 0.8857 0.055 Uiso calc U . R 1.0 . .
C C7 0.7945(2) 0.78612(19) 0.82259(18) 0.0335(6) Uani d . . . 1.0 . .
C C8 0.8478(2) 0.8210(2) 0.70887(16) 0.0326(6) Uani d . . . 1.0 . .
H H8A 0.8271 0.8722 0.6851 0.039 Uiso calc U . R 1.0 . .
H H8B 0.8104 0.7732 0.6961 0.039 Uiso calc U . R 1.0 . .
C C9 0.93844(17) 0.80152(18) 0.68468(15) 0.0262(5) Uani d . . . 1.0 . .
C C10 0.9987(2) 0.8708(2) 0.71253(18) 0.0347(6) Uani d . . . 1.0 . .
H H10A 0.9702 0.9265 0.7084 0.042 Uiso calc U . R 1.0 . .
H H10B 1.0083 0.86 0.7613 0.042 Uiso calc U . R 1.0 . .
C C11 0.93360(18) 0.8055(2) 0.60661(16) 0.0301(5) Uani d . . . 1.0 . .
H H11A 0.8838 0.7725 0.5914 0.036 Uiso calc U . R 1.0 . .
H H11B 0.9245 0.8652 0.5929 0.036 Uiso calc U . R 1.0 . .
C C12 0.97074(17) 0.71483(17) 0.70704(14) 0.0244(5) Uani d . . . 1.0 . .
N N1 0.7588(3) 0.9652(2) 0.8804(3) 0.0740(16) Uani d . . . 1.0 . .
H H1 0.7062 0.9699 0.8947 0.089 Uiso calc U . R 1.0 . .
N N2 0.84936(19) 0.66308(19) 0.91673(16) 0.0368(6) Uani d . . . 1.0 . .
H H2A 0.8588 0.6305 0.954 0.044 Uiso calc U . R 1.0 . .
H H2B 0.8931 0.654 0.8876 0.044 Uiso calc U . R 1.0 . .
N N3 0.67573(19) 0.70477(17) 0.93547(15) 0.0342(6) Uani d . . . 1.0 . .
H H3C 0.6187 0.697 0.9325 0.041 Uiso calc U . R 1.0 . .
H H3D 0.6916 0.6925 0.9787 0.041 Uiso calc U . R 1.0 . .
N N4 0.84107(19) 0.83491(17) 0.78215(15) 0.0350(6) Uani d . . . 1.0 . .
H H4 0.8691 0.8775 0.8002 0.042 Uiso calc U . R 1.0 . .
N N5 1.08163(17) 0.87578(17) 0.67838(14) 0.0308(5) Uani d . . . 1.0 . .
H H5C 1.1215 0.8904 0.7096 0.037 Uiso calc U . R 1.0 . .
H H5D 1.0795 0.9179 0.647 0.037 Uiso calc U . R 1.0 . .
N N6 1.00977(16) 0.77293(16) 0.57144(13) 0.0277(5) Uani d . . . 1.0 . .
H H6C 1.0207 0.8072 0.5354 0.033 Uiso calc U . R 1.0 . .
H H6D 0.9976 0.7205 0.5549 0.033 Uiso calc U . R 1.0 . .
N N7 0.91996(17) 0.65999(17) 0.73681(15) 0.0320(5) Uani d . . . 1.0 . .
H H7A 0.9393 0.61 0.7491 0.038 Uiso calc U . R 1.0 . .
H H7B 0.8667 0.6734 0.7444 0.038 Uiso calc U . R 1.0 . .
Ni Ni1 0.73590(2) 0.62069(2) 0.86968(2) 0.02492(11) Uani d . . . 1.0 . .
O O1 0.8553(3) 1.01155(18) 0.8047(2) 0.0588(9) Uani d . . . 1.0 . .
O O2 0.75919(15) 0.72039(14) 0.80182(12) 0.0320(4) Uani d . . . 1.0 . .
O O3 1.04700(13) 0.69593(14) 0.69608(12) 0.0309(4) Uani d . . . 1.0 . .
B B1 1.0 0 0.5 0.0344(13) Uani d T P S 1.0 . .
B B2 0.2870(3) 0.0535(3) 0.5950(2) 0.0479(10) Uani d . . . 1.0 . .
F F1 0.9438(3) 0.0474(3) 0.5357(2) 0.1023(17) Uani d . . . 1.0 . .
F F2 0.3169(3) 0.0575(2) 0.65879(18) 0.0743(9) Uani d . . . 1.0 . .
F F3 0.2737(3) 0.1324(3) 0.5687(2) 0.0841(11) Uani d . . . 1.0 . .
F F4 0.3436(2) 0.0119(3) 0.5522(2) 0.0969(14) Uani d . . . 1.0 . .
F F5 0.2110(2) 0.0104(2) 0.5952(2) 0.0833(12) Uani d . . . 1.0 . .
O O4SA 1.0 0.5 0.75 0.053(3) Uani d TU P S 0.695(17) A 1
B B3A 1.0 0.5 0.6124(6) 0.028(3) Uani d TU P DS 0.279(7) B 1
F F7A 0.9948(6) 0.5712(5) 0.5695(5) 0.055(3) Uani d U P D 0.279(7) B 1
F F6A 0.9280(6) 0.4954(6) 0.6489(5) 0.068(3) Uani d U P D 0.279(7) B 1
B B3C 0.7988(15) 0.6054(14) 0.6057(13) 0.091(5) Uani d U P D 0.205(6) C 1
F F6C 0.8757(15) 0.6246(17) 0.5752(13) 0.103(6) Uani d U P D 0.205(6) C 1
F F7C 0.7518(16) 0.5631(17) 0.5608(12) 0.112(6) Uani d U P D 0.205(6) C 1
F F8C 0.7496(19) 0.6499(18) 0.6477(16) 0.141(8) Uani d U P D 0.205(6) C 1
O O3SA 0.8962(8) 0.5031(5) 0.4490(6) 0.187(5) Uani d U . . 1.0 D 1
O O4SB 1.0 0.5 0.6848(7) 0.040(4) Uani d TU P S 0.305(17) A 2
F F6B 0.9158(7) 0.6054(7) 0.5790(7) 0.090(3) Uani d U P D 0.406(6) E 2
F F9B 0.8142(7) 0.5265(5) 0.6352(5) 0.126(3) Uani d U P D 0.610(4) E 2
B B3B 0.8311(9) 0.5764(9) 0.5787(7) 0.091(4) Uani d U P D 0.406(6) E 2
F F8B 0.7753(7) 0.6422(7) 0.5835(7) 0.101(3) Uani d U P D 0.406(6) E 2
F F7B 0.8241(9) 0.5278(6) 0.5209(6) 0.106(4) Uani d U P D 0.406(6) E 2
O O1S 0.6131(4) 0.5416(5) 0.6037(3) 0.1084(19) Uani d . . . 1.0 . .
O O2S 0.5 0.5 0.5 0.104(3) Uani d T P S 1.0 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.492(10) ?
C1 H1A . 0.98 ?
C1 H1B . 0.98 ?
C1 H1C . 0.98 ?
C2 O1 . 1.228(6) ?
C2 N1 . 1.354(6) ?
C3 N1 . 1.442(8) ?
C3 C4 . 1.547(5) ?
C3 H3A . 0.99 ?
C3 H3B . 0.99 ?
C4 C7 . 1.533(5) ?
C4 C5 . 1.550(6) ?
C4 C6 . 1.552(5) ?
C5 N2 . 1.491(5) ?
C5 H5A . 0.99 ?
C5 H5B . 0.99 ?
C6 N3 . 1.478(4) ?
C6 H6A . 0.99 ?
C6 H6B . 0.99 ?
C7 O2 . 1.247(4) ?
C7 N4 . 1.330(4) ?
C8 N4 . 1.467(4) ?
C8 C9 . 1.539(4) ?
C8 H8A . 0.99 ?
C8 H8B . 0.99 ?
C9 C12 . 1.525(4) ?
C9 C11 . 1.545(4) ?
C9 C10 . 1.549(4) ?
C10 N5 . 1.474(4) ?
C10 H10A . 0.99 ?
C10 H10B . 0.99 ?
C11 N6 . 1.480(4) ?
C11 H11A . 0.99 ?
C11 H11B . 0.99 ?
C12 O3 . 1.258(3) ?
C12 N7 . 1.318(3) ?
N1 H1 . 0.88 ?
N2 Ni1 . 2.125(3) ?
N2 H2A . 0.91 ?
N2 H2B . 0.91 ?
N3 Ni1 . 2.085(3) ?
N3 H3C . 0.91 ?
N3 H3D . 0.91 ?
N4 H4 . 0.88 ?
N5 Ni1 7_566 2.094(3) ?
N5 H5C . 0.91 ?
N5 H5D . 0.91 ?
N6 Ni1 7_566 2.106(3) ?
N6 H6C . 0.91 ?
N6 H6D . 0.91 ?
N7 H7A . 0.88 ?
N7 H7B . 0.88 ?
Ni1 O3 8_646 2.048(2) ?
Ni1 N5 8_646 2.094(3) ?
Ni1 O2 . 2.099(2) ?
Ni1 N6 8_646 2.106(3) ?
O3 Ni1 7_566 2.048(2) ?
B1 F1 4_646 1.358(3) ?
B1 F1 3_666 1.358(3) ?
B1 F1 2_755 1.358(3) ?
B1 F1 . 1.358(3) ?
B2 F2 . 1.347(5) ?
B2 F3 . 1.364(7) ?
B2 F5 . 1.379(6) ?
B2 F4 . 1.395(6) ?
B3A F6A 2_765 1.347(10) ?
B3A F6A . 1.347(10) ?
B3A F7A 2_765 1.409(10) ?
B3A F7A . 1.409(10) ?
B3C F7C . 1.33(2) ?
B3C F8C . 1.34(2) ?
B3C F6C . 1.39(2) ?
F6B B3B . 1.412(14) ?
F9B B3B . 1.391(13) ?
B3B F8B . 1.364(14) ?
B3B F7B . 1.380(14) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
O1 C2 N1 . . 121.5(5) ?
O1 C2 C1 . . 120.8(5) ?
N1 C2 C1 . . 117.7(5) ?
N1 C3 C4 . . 114.7(5) ?
N1 C3 H3A . . 108.6 ?
C4 C3 H3A . . 108.6 ?
N1 C3 H3B . . 108.6 ?
C4 C3 H3B . . 108.6 ?
H3A C3 H3B . . 107.6 ?
C7 C4 C3 . . 113.7(3) ?
C7 C4 C5 . . 108.2(3) ?
C3 C4 C5 . . 106.6(4) ?
C7 C4 C6 . . 108.3(3) ?
C3 C4 C6 . . 108.7(3) ?
C5 C4 C6 . . 111.3(3) ?
N2 C5 C4 . . 113.1(3) ?
N2 C5 H5A . . 109.0 ?
C4 C5 H5A . . 109.0 ?
N2 C5 H5B . . 109.0 ?
C4 C5 H5B . . 109.0 ?
H5A C5 H5B . . 107.8 ?
N3 C6 C4 . . 113.8(3) ?
N3 C6 H6A . . 108.8 ?
C4 C6 H6A . . 108.8 ?
N3 C6 H6B . . 108.8 ?
C4 C6 H6B . . 108.8 ?
H6A C6 H6B . . 107.7 ?
O2 C7 N4 . . 122.0(3) ?
O2 C7 C4 . . 119.4(3) ?
N4 C7 C4 . . 118.4(3) ?
N4 C8 C9 . . 113.8(3) ?
N4 C8 H8A . . 108.8 ?
C9 C8 H8A . . 108.8 ?
N4 C8 H8B . . 108.8 ?
C9 C8 H8B . . 108.8 ?
H8A C8 H8B . . 107.7 ?
C12 C9 C8 . . 113.6(2) ?
C12 C9 C11 . . 110.0(2) ?
C8 C9 C11 . . 104.8(2) ?
C12 C9 C10 . . 109.0(2) ?
C8 C9 C10 . . 108.6(3) ?
C11 C9 C10 . . 110.8(2) ?
N5 C10 C9 . . 114.8(3) ?
N5 C10 H10A . . 108.6 ?
C9 C10 H10A . . 108.6 ?
N5 C10 H10B . . 108.6 ?
C9 C10 H10B . . 108.6 ?
H10A C10 H10B . . 107.5 ?
N6 C11 C9 . . 114.4(2) ?
N6 C11 H11A . . 108.6 ?
C9 C11 H11A . . 108.6 ?
N6 C11 H11B . . 108.6 ?
C9 C11 H11B . . 108.6 ?
H11A C11 H11B . . 107.6 ?
O3 C12 N7 . . 120.2(3) ?
O3 C12 C9 . . 118.8(2) ?
N7 C12 C9 . . 121.0(3) ?
C2 N1 C3 . . 124.6(4) ?
C2 N1 H1 . . 117.7 ?
C3 N1 H1 . . 117.7 ?
C5 N2 Ni1 . . 116.1(2) ?
C5 N2 H2A . . 108.3 ?
Ni1 N2 H2A . . 108.3 ?
C5 N2 H2B . . 108.3 ?
Ni1 N2 H2B . . 108.3 ?
H2A N2 H2B . . 107.4 ?
C6 N3 Ni1 . . 113.29(19) ?
C6 N3 H3C . . 108.9 ?
Ni1 N3 H3C . . 108.9 ?
C6 N3 H3D . . 108.9 ?
Ni1 N3 H3D . . 108.9 ?
H3C N3 H3D . . 107.7 ?
C7 N4 C8 . . 123.1(3) ?
C7 N4 H4 . . 118.5 ?
C8 N4 H4 . . 118.5 ?
C10 N5 Ni1 . 7_566 115.07(19) ?
C10 N5 H5C . . 108.5 ?
Ni1 N5 H5C 7_566 . 108.5 ?
C10 N5 H5D . . 108.5 ?
Ni1 N5 H5D 7_566 . 108.5 ?
H5C N5 H5D . . 107.5 ?
C11 N6 Ni1 . 7_566 116.0(2) ?
C11 N6 H6C . . 108.3 ?
Ni1 N6 H6C 7_566 . 108.3 ?
C11 N6 H6D . . 108.3 ?
Ni1 N6 H6D 7_566 . 108.3 ?
H6C N6 H6D . . 107.4 ?
C12 N7 H7A . . 120.0 ?
C12 N7 H7B . . 120.0 ?
H7A N7 H7B . . 120.0 ?
O3 Ni1 N3 8_646 . 174.36(10) ?
O3 Ni1 N5 8_646 8_646 89.28(10) ?
N3 Ni1 N5 . 8_646 94.96(12) ?
O3 Ni1 O2 8_646 . 85.91(9) ?
N3 Ni1 O2 . . 90.04(10) ?
N5 Ni1 O2 8_646 . 94.50(11) ?
O3 Ni1 N6 8_646 8_646 85.01(9) ?
N3 Ni1 N6 . 8_646 98.89(11) ?
N5 Ni1 N6 8_646 8_646 87.13(11) ?
O2 Ni1 N6 . 8_646 170.76(9) ?
O3 Ni1 N2 8_646 . 90.77(11) ?
N3 Ni1 N2 . . 84.89(12) ?
N5 Ni1 N2 8_646 . 178.51(12) ?
O2 Ni1 N2 . . 84.02(11) ?
N6 Ni1 N2 8_646 . 94.36(11) ?
C7 O2 Ni1 . . 119.4(2) ?
C12 O3 Ni1 . 7_566 121.83(18) ?
F1 B1 F1 4_646 3_666 117.5(5) ?
F1 B1 F1 4_646 2_755 105.6(2) ?
F1 B1 F1 3_666 2_755 105.6(2) ?
F1 B1 F1 4_646 . 105.6(2) ?
F1 B1 F1 3_666 . 105.6(2) ?
F1 B1 F1 2_755 . 117.5(5) ?
F2 B2 F3 . . 111.5(4) ?
F2 B2 F5 . . 109.0(5) ?
F3 B2 F5 . . 108.5(4) ?
F2 B2 F4 . . 111.4(4) ?
F3 B2 F4 . . 107.3(5) ?
F5 B2 F4 . . 109.1(4) ?
F6A B3A F6A 2_765 . 115.3(12) ?
F6A B3A F7A 2_765 2_765 108.4(6) ?
F6A B3A F7A . 2_765 109.1(5) ?
F6A B3A F7A 2_765 . 109.1(5) ?
F6A B3A F7A . . 108.4(6) ?
F7A B3A F7A 2_765 . 106.1(11) ?
F7C B3C F8C . . 110.6(18) ?
F7C B3C F6C . . 107.9(18) ?
F8C B3C F6C . . 132.(3) ?
F8B B3B F7B . . 115.4(12) ?
F8B B3B F9B . . 104.6(11) ?
F7B B3B F9B . . 109.4(12) ?
F8B B3B F6B . . 111.4(12) ?
F7B B3B F6B . . 105.0(11) ?
F9B B3B F6B . . 111.1(11) ?

