# 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_ok

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C150 H126 B12 F50 N36 Ni6'
_chemical_formula_weight         3864.73

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

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P-62c

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

_cell_length_a                   18.058(4)
_cell_length_b                   18.058(4)
_cell_length_c                   14.612(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4126.5(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1956
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_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            25339
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         28.40
_reflns_number_total             3587
_reflns_number_gt                2569
_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)+(0.1176P)²+0.7356P] 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   0.98(3)
_refine_ls_number_reflns         3587
_refine_ls_number_parameters     206
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0594
_refine_ls_wR_factor_ref         0.1834
_refine_ls_wR_factor_gt          0.1617
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
Ni1 Ni 0.30308(5) 0.28662(5) 0.2500 0.0375(2) Uani 1 2 d S . .
N1 N 0.3150(2) 0.2075(2) 0.1543(2) 0.0423(8) Uani 1 1 d . . .
N3 N 0.4343(3) 0.3400(3) 0.2500 0.0375(10) Uani 1 2 d S . .
N4 N 0.3314(2) 0.3833(2) 0.3446(3) 0.0433(9) Uani 1 1 d . . .
N6 N 0.1736(4) 0.2265(4) 0.2500 0.0546(15) Uani 1 2 d S . .
C1 C 0.3957(4) 0.5410(4) 0.4260(4) 0.0708(16) Uani 1 1 d . . .
H1A H 0.4176 0.5945 0.4530 0.085 Uiso 1 1 calc R . .
C2 C 0.3109(4) 0.4915(4) 0.4105(5) 0.0714(18) Uani 1 1 d . . .
H2A H 0.2737 0.5102 0.4286 0.086 Uiso 1 1 calc R . .
C3 C 0.2880(4) 0.1173(4) 0.0254(4) 0.0641(16) Uani 1 1 d . . .
H3A H 0.2525 0.0865 -0.0231 0.077 Uiso 1 1 calc R . .
C4 C 0.3644(5) 0.1189(4) 0.0398(4) 0.0657(16) Uani 1 1 d . . .
H4A H 0.3805 0.0884 0.0014 0.079 Uiso 1 1 calc R . .
C6 C 0.2657(4) 0.1622(3) 0.0840(3) 0.0531(13) Uani 1 1 d . . .
H6A H 0.2143 0.1612 0.0745 0.064 Uiso 1 1 calc R . .
C7 C 0.0078(6) 0.1356(7) 0.2500 0.095(4) Uani 1 2 d S . .
C11 C 0.4160(4) 0.1653(3) 0.1106(4) 0.0537(12) Uani 1 1 d . . .
H11A H 0.4679 0.1675 0.1208 0.064 Uiso 1 1 calc R . .
C14 C 0.1021(4) 0.1878(5) 0.2500 0.0551(18) Uani 1 2 d S . .
C15 C 0.4384(4) 0.2596(4) 0.2500 0.0392(13) Uani 1 2 d S . .
H15A H 0.4975 0.2711 0.2500 0.047 Uiso 1 2 calc SR . .
C16 C 0.4494(4) 0.5100(3) 0.4005(4) 0.0554(13) Uani 1 1 d . . .
H16A H 0.5081 0.5426 0.4101 0.067 Uiso 1 1 calc R . .
C17 C 0.2798(4) 0.4142(4) 0.3684(4) 0.0590(15) Uani 1 1 d . . .
H17A H 0.2216 0.3820 0.3557 0.071 Uiso 1 1 calc R . .
C20 C 0.4143(3) 0.4304(3) 0.3609(3) 0.0443(10) Uani 1 1 d . . .
C22 C 0.3894(3) 0.2089(3) 0.1666(3) 0.0409(9) Uani 1 1 d . . .
C23 C 0.4688(3) 0.3929(3) 0.3337(4) 0.0470(11) Uani 1 1 d . . .
H23A H 0.5268 0.4386 0.3224 0.056 Uiso 1 1 calc R . .
H23B H 0.4703 0.3580 0.3832 0.056 Uiso 1 1 calc R . .
F17 F 0.0651(8) 0.0651(8) 0.0000 0.41(2) Uani 1 2 d S . .
F19 F 0.0000 0.0000 0.073(2) 0.69(6) Uani 1 3 d S . .
B5 B 0.0000 0.0000 0.0000 0.061(4) Uani 1 6 d S . .
F9 F 0.0593(6) 0.3392(7) 0.1762(4) 0.174(4) Uani 1 1 d . . .
F11 F 0.1277(8) 0.4494(9) 0.2500 0.252(9) Uani 1 2 d S . .
F12 F -0.0139(4) 0.3874(4) 0.2500 0.0919(18) Uani 1 2 d S . .
B3 B 0.0509(7) 0.3714(7) 0.2500 0.064(2) Uani 1 2 d S . .
F1 F 0.6217(3) 0.3709(3) 0.1323(3) 0.0946(13) Uani 1 1 d . . .
F4 F 0.6667 0.3333 0.0080(5) 0.0842(19) Uani 1 3 d S . .
B1 B 0.6667 0.3333 0.1033(7) 0.046(2) Uani 1 3 d S . .


_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 N6 2.027(6) . ?
Ni1 N3 2.063(5) . ?
Ni1 N4 2.080(4) . ?
Ni1 N4 2.080(4) 4 ?
Ni1 N1 2.086(4) . ?
Ni1 N1 2.086(4) 4 ?
N1 C6 1.336(6) . ?
N1 C22 1.343(6) . ?
N3 C23 1.484(5) . ?
N3 C23 1.484(5) 4 ?
N3 C15 1.491(8) . ?
N4 C20 1.323(6) . ?
N4 C17 1.349(6) . ?
N6 C14 1.119(9) . ?
C1 C2 1.351(9) . ?
C1 C16 1.392(8) . ?
C1 H1A 0.9300 . ?
C2 C17 1.363(9) . ?
C2 H2A 0.9300 . ?
C3 C6 1.371(8) . ?
C3 C4 1.381(10) . ?
C3 H3A 0.9300 . ?
C4 C11 1.363(9) . ?
C4 H4A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C14 1.479(11) . ?
C11 C22 1.378(7) . ?
C11 H11A 0.9300 . ?
C15 C22 1.515(6) 4 ?
C15 C22 1.515(6) . ?
C15 H15A 0.9800 . ?
C16 C20 1.376(7) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C20 C23 1.499(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
F17 B5 1.176(14) . ?
F17 F19 1.59(2) 8 ?
F17 F19 1.59(2) . ?
F19 B5 1.07(3) . ?
F19 F17 1.59(2) 3 ?
F19 F17 1.59(2) 5 ?
B5 F19 1.07(3) 8 ?
B5 F17 1.176(14) 3 ?
B5 F17 1.176(14) 5 ?
F9 B3 1.269(8) . ?
F11 B3 1.398(17) . ?
F12 B3 1.339(12) . ?
B3 F9 1.269(8) 4 ?
F1 B1 1.359(5) . ?
F4 B1 1.392(13) . ?
B1 F1 1.359(5) 3_655 ?
B1 F1 1.360(5) 5_665 ?

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
N6 Ni1 N3 176.2(2) . . ?
N6 Ni1 N4 100.56(17) . . ?
N3 Ni1 N4 82.24(14) . . ?
N6 Ni1 N4 100.56(17) . 4 ?
N3 Ni1 N4 82.23(14) . 4 ?
N4 Ni1 N4 83.3(2) . 4 ?
N6 Ni1 N1 96.85(17) . . ?
N3 Ni1 N1 80.37(15) . . ?
N4 Ni1 N1 162.59(15) . . ?
N4 Ni1 N1 93.62(15) 4 . ?
N6 Ni1 N1 96.85(17) . 4 ?
N3 Ni1 N1 80.37(15) . 4 ?
N4 Ni1 N1 93.62(15) . 4 ?
N4 Ni1 N1 162.59(15) 4 4 ?
N1 Ni1 N1 84.2(2) . 4 ?
C6 N1 C22 117.9(4) . . ?
C6 N1 Ni1 132.0(4) . . ?
C22 N1 Ni1 110.0(3) . . ?
C23 N3 C23 111.0(5) . 4 ?
C23 N3 C15 114.7(3) . . ?
C23 N3 C15 114.7(3) 4 . ?
C23 N3 Ni1 108.4(3) . . ?
C23 N3 Ni1 108.4(3) 4 . ?
C15 N3 Ni1 98.6(3) . . ?
C20 N4 C17 118.8(4) . . ?
C20 N4 Ni1 112.6(3) . . ?
C17 N4 Ni1 126.0(4) . . ?
C14 N6 Ni1 174.9(6) . . ?
C2 C1 C16 118.4(5) . . ?
C2 C1 H1A 120.8 . . ?
C16 C1 H1A 120.8 . . ?
C1 C2 C17 120.3(5) . . ?
C1 C2 H2A 119.8 . . ?
C17 C2 H2A 119.8 . . ?
C6 C3 C4 118.5(5) . . ?
C6 C3 H3A 120.8 . . ?
C4 C3 H3A 120.8 . . ?
C11 C4 C3 119.8(5) . . ?
C11 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
N1 C6 C3 122.7(6) . . ?
N1 C6 H6A 118.7 . . ?
C3 C6 H6A 118.7 . . ?
C4 C11 C22 118.4(5) . . ?
C4 C11 H11A 120.8 . . ?
C22 C11 H11A 120.8 . . ?
N6 C14 C7 179.3(9) . . ?
N3 C15 C22 106.8(3) . 4 ?
N3 C15 C22 106.8(3) . . ?
C22 C15 C22 107.1(5) 4 . ?
N3 C15 H15A 111.9 . . ?
C22 C15 H15A 111.9 4 . ?
C22 C15 H15A 111.9 . . ?
C20 C16 C1 118.9(5) . . ?
C20 C16 H16A 120.5 . . ?
C1 C16 H16A 120.5 . . ?
N4 C17 C2 121.5(6) . . ?
N4 C17 H17A 119.2 . . ?
C2 C17 H17A 119.2 . . ?
N4 C20 C16 122.0(5) . . ?
N4 C20 C23 116.7(4) . . ?
C16 C20 C23 121.3(5) . . ?
N1 C22 C11 122.7(5) . . ?
N1 C22 C15 113.4(4) . . ?
C11 C22 C15 123.9(4) . . ?
N3 C23 C20 110.5(4) . . ?
N3 C23 H23A 109.6 . . ?
C20 C23 H23A 109.6 . . ?
N3 C23 H23B 109.6 . . ?
C20 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
B5 F17 F19 42.3(9) . 8 ?
B5 F17 F19 42.3(9) . . ?
F19 F17 F19 84.6(18) 8 . ?
B5 F19 F17 47.7(9) . . ?
B5 F19 F17 47.7(9) . 3 ?
F17 F19 F17 79.7(14) . 3 ?
B5 F19 F17 47.7(9) . 5 ?
F17 F19 F17 79.7(14) . 5 ?
F17 F19 F17 79.7(14) 3 5 ?
F19 B5 F19 179.998(1) . 8 ?
F19 B5 F17 90.0 . . ?
F19 B5 F17 89.999(1) 8 . ?
F19 B5 F17 90.0 . 3 ?
F19 B5 F17 90.002(1) 8 3 ?
F17 B5 F17 120.0 . 3 ?
F19 B5 F17 90.0 . 5 ?
F19 B5 F17 90.0 8 5 ?
F17 B5 F17 120.0 . 5 ?
F17 B5 F17 120.0 3 5 ?
F9 B3 F9 116.4(10) . 4 ?
F9 B3 F12 114.6(6) . . ?
F9 B3 F12 114.6(6) 4 . ?
F9 B3 F11 100.1(8) . . ?
F9 B3 F11 100.1(8) 4 . ?
F12 B3 F11 108.4(10) . . ?
F1 B1 F1 110.7(5) 3_655 . ?
F1 B1 F1 110.7(5) 3_655 5_665 ?
F1 B1 F1 110.7(5) . 5_665 ?
F1 B1 F4 108.2(5) 3_655 . ?
F1 B1 F4 108.2(5) . . ?
F1 B1 F4 108.2(5) 5_665 . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.40
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.073
_database_code_depnum_ccdc_archive 'CCDC 989005'
#######################################################################
#
#                 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_ok

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H29 B2 F8 N6 Ni O0'
_chemical_formula_weight         693.91

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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.0812(5)
_cell_length_b                   23.7229(11)
_cell_length_c                   13.0438(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.471(2)
_cell_angle_gamma                90.00
_cell_volume                     3145.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1420
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_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            12472
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5536
_reflns_number_gt                4462
_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)+(0.1476P)²+1.7181P] 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         5536
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0682
_refine_ls_wR_factor_ref         0.2223
_refine_ls_wR_factor_gt          0.2118
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_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
Ni Ni 0.33985(5) 0.87753(2) 0.13940(4) 0.0421(2) Uani 1 1 d . . .
N1 N 0.3730(3) 0.83856(13) 0.0087(3) 0.0459(7) Uani 1 1 d . . .
N4 N 0.2363(3) 0.80783(13) 0.1716(3) 0.0448(7) Uani 1 1 d . . .
N6 N 0.1813(3) 0.92056(15) 0.0253(3) 0.0524(8) Uani 1 1 d . . .
N5 N 0.2840(3) 0.91135(14) 0.2670(3) 0.0498(8) Uani 1 1 d . . .
N2 N 0.4847(3) 0.93891(15) 0.1771(3) 0.0538(8) Uani 1 1 d . . .
N3 N 0.5092(4) 0.83052(18) 0.2327(3) 0.0658(11) Uani 1 1 d . . .
C5 C 0.4854(4) 0.80913(18) 0.0409(4) 0.0568(10) Uani 1 1 d . . .
C16 C 0.1846(5) 0.88414(18) 0.2766(4) 0.0561(11) Uani 1 1 d . . .
C1 C 0.2917(4) 0.83758(17) -0.1001(3) 0.0524(10) Uani 1 1 d . . .
H1A H 0.2131 0.8576 -0.1228 0.063 Uiso 1 1 calc R . .
C28 C 0.0942(5) 0.9394(2) -0.0464(4) 0.0618(12) Uani 1 1 d . . .
C22 C 0.0907(5) 0.72198(18) 0.0917(4) 0.0553(11) Uani 1 1 d . . .
C14 C 0.3401(6) 0.7800(2) 0.2674(5) 0.0837(17) Uani 1 1 d . . .
H14A H 0.3457 0.7992 0.3349 0.100 Uiso 1 1 calc R . .
H14B H 0.3118 0.7417 0.2714 0.100 Uiso 1 1 calc R . .
C17 C 0.1232(5) 0.9029(2) 0.3439(4) 0.0696(13) Uani 1 1 d . . .
H17A H 0.0549 0.8824 0.3499 0.083 Uiso 1 1 calc R . .
C23 C -0.0449(5) 0.7278(2) 0.0591(4) 0.0629(12) Uani 1 1 d . . .
H23A H -0.0852 0.7618 0.0292 0.075 Uiso 1 1 calc R . .
C21 C 0.1714(5) 0.76914(19) 0.0751(3) 0.0589(11) Uani 1 1 d . . .
H21A H 0.2392 0.7528 0.0550 0.071 Uiso 1 1 calc R . .
H21B H 0.1149 0.7915 0.0120 0.071 Uiso 1 1 calc R . .
C12 C 0.4769(5) 0.9890(2) 0.1280(4) 0.0648(12) Uani 1 1 d . . .
H12A H 0.4013 0.9981 0.0658 0.078 Uiso 1 1 calc R . .
C20 C 0.3257(5) 0.95923(19) 0.3251(4) 0.0623(11) Uani 1 1 d . . .
H20A H 0.3966 0.9783 0.3204 0.075 Uiso 1 1 calc R . .
C18 C 0.1651(5) 0.9527(2) 0.4020(4) 0.0694(13) Uani 1 1 d . . .
H18A H 0.1250 0.9666 0.4473 0.083 Uiso 1 1 calc R . .
C15 C 0.1356(5) 0.8320(2) 0.2061(5) 0.0698(14) Uani 1 1 d . . .
H15A H 0.1105 0.8041 0.2483 0.084 Uiso 1 1 calc R . .
H15B H 0.0579 0.8414 0.1401 0.084 Uiso 1 1 calc R . .
C8 C 0.5935(5) 0.9254(2) 0.2691(4) 0.0684(13) Uani 1 1 d . . .
C2 C 0.3192(6) 0.8085(2) -0.1789(4) 0.0708(13) Uani 1 1 d . . .
H2A H 0.2618 0.8098 -0.2538 0.085 Uiso 1 1 calc R . .
C11 C 0.5789(7) 1.0278(3) 0.1679(6) 0.093(2) Uani 1 1 d . . .
H11A H 0.5718 1.0629 0.1343 0.111 Uiso 1 1 calc R . .
C6 C 0.5766(4) 0.8140(2) 0.1609(5) 0.0731(14) Uani 1 1 d . . .
H6A H 0.6198 0.7780 0.1863 0.088 Uiso 1 1 calc R . .
H6B H 0.6440 0.8416 0.1681 0.088 Uiso 1 1 calc R . .
C27 C 0.1454(6) 0.6707(2) 0.1339(6) 0.0904(19) Uani 1 1 d . . .
H27A H 0.2350 0.6649 0.1544 0.108 Uiso 1 1 calc R . .
C19 C 0.2666(5) 0.9810(2) 0.3916(4) 0.0692(13) Uani 1 1 d . . .
H19A H 0.2959 1.0149 0.4292 0.083 Uiso 1 1 calc R . .
C7 C 0.5910(6) 0.8691(3) 0.3195(4) 0.0814(17) Uani 1 1 d . . .
H7A H 0.6798 0.8543 0.3545 0.098 Uiso 1 1 calc R . .
H7B H 0.5560 0.8729 0.3765 0.098 Uiso 1 1 calc R . .
C24 C -0.1201(5) 0.6838(2) 0.0704(4) 0.0718(14) Uani 1 1 d . . .
H24A H -0.2104 0.6884 0.0477 0.086 Uiso 1 1 calc R . .
C13 C 0.4634(6) 0.7778(3) 0.2687(6) 0.104(2) Uani 1 1 d . . .
H13A H 0.4664 0.7473 0.2202 0.125 Uiso 1 1 calc R . .
H13B H 0.5247 0.7686 0.3439 0.125 Uiso 1 1 calc R . .
C4 C 0.5157(6) 0.7777(3) -0.0352(6) 0.0904(18) Uani 1 1 d . . .
H4A H 0.5927 0.7565 -0.0115 0.109 Uiso 1 1 calc R . .
C25 C -0.0632(8) 0.6339(3) 0.1145(6) 0.090(2) Uani 1 1 d . . .
H25A H -0.1137 0.6044 0.1230 0.108 Uiso 1 1 calc R . .
C29 C -0.0177(7) 0.9629(3) -0.1392(5) 0.103(2) Uani 1 1 d . . .
C9 C 0.6989(5) 0.9615(3) 0.3095(6) 0.092(2) Uani 1 1 d . . .
H9A H 0.7745 0.9512 0.3705 0.111 Uiso 1 1 calc R . .
C3 C 0.4309(7) 0.7781(3) -0.1460(6) 0.098(2) Uani 1 1 d . . .
H3A H 0.4506 0.7574 -0.1980 0.117 Uiso 1 1 calc R . .
C26 C 0.0686(9) 0.6277(2) 0.1460(8) 0.107(3) Uani 1 1 d . . .
H26A H 0.1079 0.5936 0.1766 0.129 Uiso 1 1 calc R . .
C10 C 0.6921(7) 1.0126(4) 0.2596(8) 0.111(3) Uani 1 1 d . . .
H10A H 0.7629 1.0374 0.2869 0.134 Uiso 1 1 calc R . .
F4 F -0.4040(6) 0.6400(3) 0.0772(6) 0.186(3) Uani 1 1 d . . .
F3 F -0.4977(6) 0.6418(3) 0.1952(5) 0.167(2) Uani 1 1 d . . .
B1 B -0.5141(6) 0.6257(2) 0.0885(5) 0.0633(14) Uani 1 1 d . . .
F8 F 0.1715(6) 1.1445(4) -0.1274(7) 0.203(4) Uani 1 1 d . . .
F2 F -0.6028(7) 0.6574(4) 0.0183(8) 0.241(4) Uani 1 1 d . . .
F7 F 0.3300(6) 1.0970(3) -0.0061(8) 0.227(4) Uani 1 1 d . . .
F1 F -0.5473(12) 0.5758(3) 0.0671(7) 0.280(5) Uani 1 1 d . . .
F6 F 0.1319(10) 1.0710(4) -0.0485(11) 0.295(6) Uani 1 1 d . . .
F5 F 0.1885(11) 1.1437(4) 0.0384(7) 0.249(5) Uani 1 1 d . . .
B2 B 0.2061(11) 1.1092(4) -0.0349(17) 0.144(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N6 2.064(3) . ?
Ni N2 2.076(3) . ?
Ni N1 2.096(3) . ?
Ni N3 2.104(4) . ?
Ni N5 2.149(3) . ?
Ni N4 2.147(3) . ?
N1 C5 1.341(5) . ?
N1 C1 1.345(5) . ?
N4 C15 1.476(6) . ?
N4 C14 1.474(6) . ?
N4 C21 1.491(5) . ?
N6 C28 1.134(6) . ?
N5 C16 1.325(6) . ?
N5 C20 1.341(5) . ?
N2 C12 1.336(6) . ?
N2 C8 1.357(6) . ?
N3 C7 1.458(7) . ?
N3 C6 1.465(7) . ?
N3 C13 1.494(7) . ?
C5 C4 1.385(8) . ?
C5 C6 1.492(7) . ?
C16 C17 1.381(6) . ?
C16 C15 1.508(6) . ?
C1 C2 1.369(6) . ?
C1 H1A 0.9300 . ?
C28 C29 1.455(7) . ?
C22 C27 1.373(7) . ?
C22 C23 1.396(7) . ?
C22 C21 1.501(6) . ?
C14 C13 1.361(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C17 C18 1.381(7) . ?
C17 H17A 0.9300 . ?
C23 C24 1.378(7) . ?
C23 H23A 0.9300 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C12 C11 1.388(7) . ?
C12 H12A 0.9300 . ?
C20 C19 1.379(7) . ?
C20 H20A 0.9300 . ?
C18 C19 1.362(7) . ?
C18 H18A 0.9300 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C8 C9 1.373(8) . ?
C8 C7 1.493(8) . ?
C2 C3 1.348(8) . ?
C2 H2A 0.9300 . ?
C11 C10 1.392(10) . ?
C11 H11A 0.9300 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C27 C26 1.377(9) . ?
C27 H27A 0.9300 . ?
C19 H19A 0.9300 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C24 C25 1.358(9) . ?
C24 H24A 0.9300 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C4 C3 1.375(9) . ?
C4 H4A 0.9300 . ?
C25 C26 1.358(11) . ?
C25 H25A 0.9300 . ?
C9 C10 1.364(11) . ?
C9 H9A 0.9300 . ?
C3 H3A 0.9300 . ?
C26 H26A 0.9300 . ?
C10 H10A 0.9300 . ?
F4 B1 1.329(8) . ?
F3 B1 1.384(8) . ?
B1 F1 1.237(8) . ?
B1 F2 1.286(8) . ?
F8 B2 1.390(16) . ?
F7 B2 1.303(11) . ?
F6 B2 1.190(11) . ?
F5 B2 1.331(16) . ?

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
N6 Ni N2 100.36(14) . . ?
N6 Ni N1 90.35(13) . . ?
N2 Ni N1 97.62(13) . . ?
N6 Ni N3 170.42(15) . . ?
N2 Ni N3 78.89(15) . . ?
N1 Ni N3 80.32(15) . . ?
N6 Ni N5 87.08(13) . . ?
N2 Ni N5 89.35(13) . . ?
N1 Ni N5 172.91(12) . . ?
N3 Ni N5 102.44(15) . . ?
N6 Ni N4 98.87(13) . . ?
N2 Ni N4 156.44(13) . . ?
N1 Ni N4 95.74(12) . . ?
N3 Ni N4 84.36(14) . . ?
N5 Ni N4 78.16(12) . . ?
C5 N1 C1 118.0(4) . . ?
C5 N1 Ni 114.7(3) . . ?
C1 N1 Ni 127.2(3) . . ?
C15 N4 C14 110.2(4) . . ?
C15 N4 C21 109.1(3) . . ?
C14 N4 C21 113.0(4) . . ?
C15 N4 Ni 106.8(3) . . ?
C14 N4 Ni 102.3(3) . . ?
C21 N4 Ni 115.1(2) . . ?
C28 N6 Ni 171.8(3) . . ?
C16 N5 C20 118.1(4) . . ?
C16 N5 Ni 113.5(3) . . ?
C20 N5 Ni 127.8(3) . . ?
C12 N2 C8 119.9(4) . . ?
C12 N2 Ni 127.8(3) . . ?
C8 N2 Ni 112.0(3) . . ?
C7 N3 C6 110.3(4) . . ?
C7 N3 C13 117.8(5) . . ?
C6 N3 C13 107.4(5) . . ?
C7 N3 Ni 104.6(3) . . ?
C6 N3 Ni 109.7(3) . . ?
C13 N3 Ni 106.8(3) . . ?
N1 C5 C4 121.1(5) . . ?
N1 C5 C6 116.4(4) . . ?
C4 C5 C6 122.5(5) . . ?
N5 C16 C17 122.8(4) . . ?
N5 C16 C15 117.0(4) . . ?
C17 C16 C15 120.2(4) . . ?
N1 C1 C2 123.0(4) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
N6 C28 C29 179.2(5) . . ?
C27 C22 C23 117.3(4) . . ?
C27 C22 C21 121.7(5) . . ?
C23 C22 C21 120.9(4) . . ?
C13 C14 N4 117.9(5) . . ?
C13 C14 H14A 107.8 . . ?
N4 C14 H14A 107.8 . . ?
C13 C14 H14B 107.8 . . ?
N4 C14 H14B 107.8 . . ?
H14A C14 H14B 107.2 . . ?
C18 C17 C16 118.8(5) . . ?
C18 C17 H17A 120.6 . . ?
C16 C17 H17A 120.6 . . ?
C24 C23 C22 121.1(5) . . ?
C24 C23 H23A 119.5 . . ?
C22 C23 H23A 119.5 . . ?
N4 C21 C22 116.9(3) . . ?
N4 C21 H21A 108.1 . . ?
C22 C21 H21A 108.1 . . ?
N4 C21 H21B 108.1 . . ?
C22 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
N2 C12 C11 121.5(5) . . ?
N2 C12 H12A 119.3 . . ?
C11 C12 H12A 119.3 . . ?
N5 C20 C19 122.0(5) . . ?
N5 C20 H20A 119.0 . . ?
C19 C20 H20A 119.0 . . ?
C19 C18 C17 118.5(4) . . ?
C19 C18 H18A 120.7 . . ?
C17 C18 H18A 120.7 . . ?
N4 C15 C16 111.8(4) . . ?
N4 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
N4 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
N2 C8 C9 120.8(6) . . ?
N2 C8 C7 115.8(4) . . ?
C9 C8 C7 123.4(5) . . ?
C3 C2 C1 118.8(5) . . ?
C3 C2 H2A 120.6 . . ?
C1 C2 H2A 120.6 . . ?
C10 C11 C12 118.1(6) . . ?
C10 C11 H11A 120.9 . . ?
C12 C11 H11A 120.9 . . ?
N3 C6 C5 112.8(4) . . ?
N3 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
N3 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
C26 C27 C22 120.5(6) . . ?
C26 C27 H27A 119.7 . . ?
C22 C27 H27A 119.7 . . ?
C18 C19 C20 119.7(4) . . ?
C18 C19 H19A 120.2 . . ?
C20 C19 H19A 120.2 . . ?
N3 C7 C8 109.6(4) . . ?
N3 C7 H7A 109.8 . . ?
C8 C7 H7A 109.8 . . ?
N3 C7 H7B 109.8 . . ?
C8 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
C25 C24 C23 120.4(6) . . ?
C25 C24 H24A 119.8 . . ?
C23 C24 H24A 119.8 . . ?
C14 C13 N3 115.4(5) . . ?
C14 C13 H13A 108.4 . . ?
N3 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
N3 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C3 C4 C5 119.4(5) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C24 C25 C26 119.0(5) . . ?
C24 C25 H25A 120.5 . . ?
C26 C25 H25A 120.5 . . ?
C10 C9 C8 119.7(6) . . ?
C10 C9 H9A 120.2 . . ?
C8 C9 H9A 120.2 . . ?
C2 C3 C4 119.6(5) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C27 C26 C25 121.6(6) . . ?
C27 C26 H26A 119.2 . . ?
C25 C26 H26A 119.2 . . ?
C9 C10 C11 119.9(5) . . ?
C9 C10 H10A 120.0 . . ?
C11 C10 H10A 120.0 . . ?
F1 B1 F2 108.9(8) . . ?
F1 B1 F4 115.0(8) . . ?
F2 B1 F4 104.3(7) . . ?
F1 B1 F3 113.5(7) . . ?
F2 B1 F3 108.1(7) . . ?
F4 B1 F3 106.4(6) . . ?
F6 B2 F7 117.3(10) . . ?
F6 B2 F5 106.6(12) . . ?
F7 B2 F5 111.6(15) . . ?
F6 B2 F8 113.2(16) . . ?
F7 B2 F8 106.2(9) . . ?
F5 B2 F8 100.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.083
_database_code_depnum_ccdc_archive 'CCDC 989006'
#######################################################################
#
#                 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_ok

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H29 B2 F8 N5 Ni O2'
_chemical_formula_weight         687.88

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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   10.5139(12)
_cell_length_b                   14.6832(17)
_cell_length_c                   40.182(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6203.3(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2816
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_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            39721
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         27.51
_reflns_number_total             7120
_reflns_number_gt                4761
_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)+(0.0860P)²+6.9086P] 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         7120
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1905
_refine_ls_wR_factor_gt          0.1695
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
Ni Ni 0.06390(4) 0.04255(3) 0.383857(10) 0.05013(17) Uani 1 1 d . . .
N1 N 0.0738(3) -0.0913(2) 0.40039(7) 0.0539(7) Uani 1 1 d . . .
N2 N -0.1273(3) 0.0071(2) 0.37580(7) 0.0565(8) Uani 1 1 d . . .
N5 N 0.0490(3) 0.1731(2) 0.36420(7) 0.0557(8) Uani 1 1 d . . .
N3 N -0.0147(3) 0.0805(2) 0.42987(7) 0.0567(8) Uani 1 1 d . . .
C10 C 0.1924(4) -0.0567(3) 0.32568(9) 0.0601(10) Uani 1 1 d . . .
H10A H 0.1763 -0.1093 0.3396 0.072 Uiso 1 1 calc R . .
H10B H 0.2715 -0.0296 0.3332 0.072 Uiso 1 1 calc R . .
C9 C 0.0172(4) 0.2481(3) 0.38130(10) 0.0641(10) Uani 1 1 d . . .
H9A H 0.0051 0.2434 0.4042 0.077 Uiso 1 1 calc R . .
N4 N 0.0883(3) 0.0105(2) 0.33140(7) 0.0544(7) Uani 1 1 d . . .
C8 C 0.2915(4) -0.0439(3) 0.26844(9) 0.0657(10) Uani 1 1 d . . .
H8A H 0.3307 0.0099 0.2751 0.079 Uiso 1 1 calc R . .
C7 C -0.0367(4) -0.0280(3) 0.32142(10) 0.0684(11) Uani 1 1 d . . .
H7A H -0.0375 -0.0928 0.3261 0.082 Uiso 1 1 calc R . .
H7B H -0.0478 -0.0203 0.2976 0.082 Uiso 1 1 calc R . .
C6 C -0.1515(4) -0.0878(3) 0.38713(11) 0.0701(11) Uani 1 1 d . . .
H6A H -0.1775 -0.1241 0.3681 0.084 Uiso 1 1 calc R . .
H6B H -0.2213 -0.0873 0.4029 0.084 Uiso 1 1 calc R . .
C5 C 0.0459(5) 0.0942(3) 0.45901(10) 0.0686(11) Uani 1 1 d . . .
H5A H 0.1343 0.0925 0.4595 0.082 Uiso 1 1 calc R . .
C4 C 0.1767(4) -0.1324(3) 0.41338(9) 0.0627(10) Uani 1 1 d . . .
H4A H 0.2557 -0.1047 0.4108 0.075 Uiso 1 1 calc R . .
C3 C 0.0666(3) 0.1809(3) 0.33125(9) 0.0576(9) Uani 1 1 d . . .
C2 C 0.2115(3) -0.0898(3) 0.29029(9) 0.0569(9) Uani 1 1 d . . .
C1 C -0.1423(4) 0.0827(3) 0.42956(9) 0.0592(10) Uani 1 1 d . . .
C24 C 0.0512(4) 0.2624(3) 0.31482(10) 0.0654(11) Uani 1 1 d . . .
H24A H 0.0631 0.2660 0.2919 0.078 Uiso 1 1 calc R . .
C23 C 0.1541(4) -0.1691(3) 0.27969(10) 0.0678(11) Uani 1 1 d . . .
H23A H 0.1000 -0.2003 0.2940 0.081 Uiso 1 1 calc R . .
C22 C -0.0514(5) -0.2135(3) 0.42023(13) 0.0808(13) Uani 1 1 d . . .
H22A H -0.1312 -0.2401 0.4226 0.097 Uiso 1 1 calc R . .
C21 C -0.2130(5) 0.0967(3) 0.45808(11) 0.0757(13) Uani 1 1 d . . .
H21A H -0.3014 0.0967 0.4573 0.091 Uiso 1 1 calc R . .
C20 C 0.0532(6) -0.2542(4) 0.43358(16) 0.0980(18) Uani 1 1 d . . .
H20A H 0.0454 -0.3091 0.4449 0.118 Uiso 1 1 calc R . .
C19 C 0.1700(6) -0.2138(3) 0.43025(11) 0.0793(13) Uani 1 1 d . . .
H19A H 0.2426 -0.2406 0.4391 0.095 Uiso 1 1 calc R . .
C18 C 0.0182(4) 0.3381(3) 0.33281(12) 0.0701(11) Uani 1 1 d . . .
H18A H 0.0068 0.3937 0.3221 0.084 Uiso 1 1 calc R . .
C17 C -0.1468(4) 0.0173(3) 0.33954(9) 0.0676(11) Uani 1 1 d . . .
H17A H -0.1507 0.0813 0.3337 0.081 Uiso 1 1 calc R . .
H17B H -0.2264 -0.0110 0.3331 0.081 Uiso 1 1 calc R . .
C16 C -0.0379(4) -0.1325(3) 0.40323(9) 0.0587(10) Uani 1 1 d . . .
C15 C -0.2025(4) 0.0719(3) 0.39572(10) 0.0654(10) Uani 1 1 d . . .
H15A H -0.2889 0.0497 0.3981 0.078 Uiso 1 1 calc R . .
H15B H -0.2056 0.1305 0.3845 0.078 Uiso 1 1 calc R . .
C14 C -0.1506(7) 0.1109(4) 0.48771(11) 0.0907(16) Uani 1 1 d . . .
H14A H -0.1965 0.1204 0.5072 0.109 Uiso 1 1 calc R . .
C13 C 0.2557(5) -0.1572(4) 0.22652(10) 0.0804(14) Uani 1 1 d . . .
H13A H 0.2709 -0.1798 0.2053 0.096 Uiso 1 1 calc R . .
C12 C 0.1760(4) -0.2030(4) 0.24781(11) 0.0774(13) Uani 1 1 d . . .
H12A H 0.1367 -0.2565 0.2410 0.093 Uiso 1 1 calc R . .
C11 C -0.0201(7) 0.1107(3) 0.48829(10) 0.0865(15) Uani 1 1 d . . .
H11A H 0.0235 0.1215 0.5080 0.104 Uiso 1 1 calc R . .
C25 C 0.1153(4) 0.0973(3) 0.31372(9) 0.0658(11) Uani 1 1 d . . .
H25A H 0.0775 0.0945 0.2917 0.079 Uiso 1 1 calc R . .
H25B H 0.2066 0.1031 0.3109 0.079 Uiso 1 1 calc R . .
C30 C 0.3128(5) -0.0778(4) 0.23681(10) 0.0783(13) Uani 1 1 d . . .
H30A H 0.3663 -0.0465 0.2224 0.094 Uiso 1 1 calc R . .
C31 C 0.0018(4) 0.3317(3) 0.36650(11) 0.0642(10) Uani 1 1 d . . .
H31A H -0.0192 0.3827 0.3791 0.077 Uiso 1 1 calc R . .
O1 O 0.2539(3) 0.0680(2) 0.39404(7) 0.0682(8) Uani 1 1 d . . .
H1 H 0.3032 0.1009 0.3824 0.082 Uiso 1 1 d R . .
H2 H 0.2873 0.0558 0.4128 0.082 Uiso 1 1 d R . .
O2 O 0.3578(5) 0.0279(3) 0.45350(10) 0.1147(14) Uani 1 1 d . . .
F4 F -0.3997(4) 0.2013(3) 0.33939(10) 0.1234(12) Uani 1 1 d . . .
F3 F -0.6051(3) 0.1734(3) 0.34816(9) 0.1196(12) Uani 1 1 d . . .
F2 F -0.4647(4) 0.0636(3) 0.35449(15) 0.168(2) Uani 1 1 d . . .
F1 F -0.5088(5) 0.1176(4) 0.30433(10) 0.1636(19) Uani 1 1 d . . .
F8 F -0.4116(5) -0.0617(3) 0.44539(15) 0.172(2) Uani 1 1 d . . .
F7 F -0.3509(5) -0.1987(4) 0.44392(12) 0.1645(17) Uani 1 1 d . . .
B1 B -0.4914(6) 0.1398(4) 0.33669(14) 0.0740(14) Uani 1 1 d . . .
F5 F -0.5182(6) -0.1635(4) 0.4716(2) 0.240(4) Uani 1 1 d . . .
B2 B -0.4033(8) -0.1372(5) 0.46461(19) 0.0949(19) Uani 1 1 d . . .
F6 F -0.3298(8) -0.1275(6) 0.48953(15) 0.271(4) Uani 1 1 d . . .
H3 H 0.4235 0.0002 0.4460 0.325 Uiso 1 1 d R . .
H4 H 0.3628 0.0581 0.4715 0.325 Uiso 1 1 d 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 O1 2.073(3) . ?
Ni N1 2.077(3) . ?
Ni N5 2.079(3) . ?
Ni N3 2.100(3) . ?
Ni N2 2.102(3) . ?
Ni N4 2.175(3) . ?
N1 C16 1.327(5) . ?
N1 C4 1.344(5) . ?
N2 C15 1.474(5) . ?
N2 C17 1.479(5) . ?
N2 C6 1.487(6) . ?
N5 C9 1.341(5) . ?
N5 C3 1.342(5) . ?
N3 C1 1.342(6) . ?
N3 C5 1.348(5) . ?
C10 N4 1.492(5) . ?
C10 C2 1.516(5) . ?
C9 C31 1.374(6) . ?
N4 C7 1.486(5) . ?
N4 C25 1.486(5) . ?
C8 C30 1.383(6) . ?
C8 C2 1.390(6) . ?
C7 C17 1.521(6) . ?
C6 C16 1.508(6) . ?
C5 C11 1.388(6) . ?
C4 C19 1.375(6) . ?
C3 C24 1.375(6) . ?
C3 C25 1.506(6) . ?
C2 C23 1.378(6) . ?
C1 C21 1.381(5) . ?
C1 C15 1.508(6) . ?
C24 C18 1.371(6) . ?
C23 C12 1.393(6) . ?
C22 C20 1.361(7) . ?
C22 C16 1.379(6) . ?
C21 C14 1.375(7) . ?
C20 C19 1.371(7) . ?
C18 C31 1.368(6) . ?
C14 C11 1.372(8) . ?
C13 C12 1.372(7) . ?
C13 C30 1.376(7) . ?
F4 B1 1.325(6) . ?
F3 B1 1.373(7) . ?
F2 B1 1.358(7) . ?
F1 B1 1.353(7) . ?
F8 B2 1.353(8) . ?
F7 B2 1.345(8) . ?
F5 B2 1.299(9) . ?
B2 F6 1.273(9) . ?

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
O1 Ni N1 93.38(12) . . ?
O1 Ni N5 88.93(12) . . ?
N1 Ni N5 176.02(12) . . ?
O1 Ni N3 99.07(13) . . ?
N1 Ni N3 89.38(12) . . ?
N5 Ni N3 93.45(12) . . ?
O1 Ni N2 175.39(12) . . ?
N1 Ni N2 82.12(13) . . ?
N5 Ni N2 95.61(13) . . ?
N3 Ni N2 79.91(13) . . ?
O1 Ni N4 96.71(11) . . ?
N1 Ni N4 95.71(12) . . ?
N5 Ni N4 80.80(12) . . ?
N3 Ni N4 163.10(12) . . ?
N2 Ni N4 84.83(11) . . ?
C16 N1 C4 118.3(4) . . ?
C16 N1 Ni 114.5(3) . . ?
C4 N1 Ni 126.1(3) . . ?
C15 N2 C17 113.3(3) . . ?
C15 N2 C6 110.3(3) . . ?
C17 N2 C6 111.9(3) . . ?
C15 N2 Ni 105.6(3) . . ?
C17 N2 Ni 105.0(2) . . ?
C6 N2 Ni 110.4(2) . . ?
C9 N5 C3 118.0(3) . . ?
C9 N5 Ni 125.6(2) . . ?
C3 N5 Ni 116.3(3) . . ?
C1 N3 C5 118.5(4) . . ?
C1 N3 Ni 113.1(2) . . ?
C5 N3 Ni 128.2(3) . . ?
N4 C10 C2 117.0(3) . . ?
N5 C9 C31 122.8(4) . . ?
C7 N4 C25 111.5(3) . . ?
C7 N4 C10 110.8(3) . . ?
C25 N4 C10 110.7(3) . . ?
C7 N4 Ni 103.9(2) . . ?
C25 N4 Ni 107.5(2) . . ?
C10 N4 Ni 112.3(2) . . ?
C30 C8 C2 120.2(4) . . ?
N4 C7 C17 112.2(3) . . ?
N2 C6 C16 113.8(3) . . ?
N3 C5 C11 121.7(5) . . ?
N1 C4 C19 122.7(4) . . ?
N5 C3 C24 122.1(4) . . ?
N5 C3 C25 116.0(3) . . ?
C24 C3 C25 121.6(4) . . ?
C23 C2 C8 118.6(4) . . ?
C23 C2 C10 120.2(4) . . ?
C8 C2 C10 121.1(4) . . ?
N3 C1 C21 122.2(4) . . ?
N3 C1 C15 115.2(3) . . ?
C21 C1 C15 122.6(4) . . ?
C18 C24 C3 118.8(4) . . ?
C2 C23 C12 120.9(4) . . ?
C20 C22 C16 119.4(5) . . ?
C14 C21 C1 119.0(5) . . ?
C22 C20 C19 119.7(5) . . ?
C20 C19 C4 118.1(5) . . ?
C24 C18 C31 119.9(4) . . ?
N2 C17 C7 108.8(3) . . ?
N1 C16 C22 121.8(4) . . ?
N1 C16 C6 117.7(4) . . ?
C22 C16 C6 120.4(4) . . ?
N2 C15 C1 109.4(3) . . ?
C11 C14 C21 119.4(4) . . ?
C12 C13 C30 119.6(4) . . ?
C13 C12 C23 119.9(5) . . ?
C14 C11 C5 119.1(5) . . ?
N4 C25 C3 114.2(3) . . ?
C13 C30 C8 120.7(4) . . ?
C18 C31 C9 118.3(4) . . ?
F4 B1 F1 110.0(5) . . ?
F4 B1 F2 111.6(5) . . ?
F1 B1 F2 109.6(6) . . ?
F4 B1 F3 111.2(5) . . ?
F1 B1 F3 107.0(5) . . ?
F2 B1 F3 107.4(5) . . ?
F6 B2 F5 115.3(8) . . ?
F6 B2 F7 108.2(7) . . ?
F5 B2 F7 108.3(7) . . ?
F6 B2 F8 113.4(8) . . ?
F5 B2 F8 107.9(7) . . ?
F7 B2 F8 102.9(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.062
_database_code_depnum_ccdc_archive 'CCDC 989007'
#######################################################################
#
#                 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_ok

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H46 B2 F8 N8 Ni'
_chemical_formula_weight         907.21

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'
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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.3663(12)
_cell_length_b                   28.640(4)
_cell_length_c                   16.685(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.340(7)
_cell_angle_gamma                90.00
_cell_volume                     4728.5(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1880
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_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            30791
_diffrn_reflns_av_R_equivalents  0.0984
_diffrn_reflns_av_sigmaI/netI    0.1240
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         27.68
_reflns_number_total             10980
_reflns_number_gt                5387
_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)+(0.2000P)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         10980
_refine_ls_number_parameters     534
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1911
_refine_ls_R_factor_gt           0.1197
_refine_ls_wR_factor_ref         0.3766
_refine_ls_wR_factor_gt          0.3284
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.003
_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 0.16772(8) 0.11877(3) 0.85573(5) 0.0466(3) Uani 1 1 d . . .
N3 N -0.0203(5) 0.1095(2) 0.7691(3) 0.0556(13) Uani 1 1 d . . .
N2 N 0.0650(5) 0.18461(17) 0.8686(3) 0.0488(11) Uani 1 1 d . . .
N1 N 0.3443(5) 0.15442(17) 0.9278(3) 0.0474(11) Uani 1 1 d . . .
C17 C 0.4309(6) 0.1245(2) 0.9956(4) 0.0506(14) Uani 1 1 d . . .
H17A H 0.4652 0.0990 0.9696 0.061 Uiso 1 1 calc R . .
H17B H 0.3743 0.1109 1.0266 0.061 Uiso 1 1 calc R . .
N6 N 0.2649(5) 0.12836(18) 0.7529(3) 0.0501(12) Uani 1 1 d . . .
C16 C 0.2484(7) 0.0830(2) 0.7089(4) 0.0584(16) Uani 1 1 d . . .
H16A H 0.3127 0.0808 0.6771 0.070 Uiso 1 1 calc R . .
H16B H 0.1582 0.0809 0.6699 0.070 Uiso 1 1 calc R . .
C15 C 0.4088(6) 0.1351(2) 0.8013(4) 0.0542(15) Uani 1 1 d . . .
H15A H 0.4591 0.1456 0.7640 0.065 Uiso 1 1 calc R . .
H15B H 0.4472 0.1057 0.8261 0.065 Uiso 1 1 calc R . .
C14 C 0.5495(6) 0.1481(2) 1.0578(4) 0.0536(15) Uani 1 1 d . . .
C13 C 0.2830(6) 0.1696(2) 0.6186(4) 0.0533(15) Uani 1 1 d . . .
C12 C 0.2172(6) 0.1666(2) 0.6894(3) 0.0513(14) Uani 1 1 d . . .
H12A H 0.1506 0.1876 0.6928 0.062 Uiso 1 1 calc R . .
N5 N 0.1136(5) 0.09168(19) 0.9589(4) 0.0595(14) Uani 1 1 d . . .
C10 C 0.0789(7) 0.0799(2) 1.0118(5) 0.0640(18) Uani 1 1 d . . .
N4 N 0.2466(5) 0.05182(17) 0.8443(3) 0.0551(13) Uani 1 1 d . . .
C9 C -0.0915(6) 0.1492(2) 0.7439(4) 0.0547(15) Uani 1 1 d . . .
C8 C -0.2351(7) 0.2271(3) 0.8874(4) 0.0615(17) Uani 1 1 d . . .
H8A H -0.2739 0.2037 0.8492 0.074 Uiso 1 1 calc R . .
C7 C -0.0190(6) 0.1811(2) 0.9291(4) 0.0540(15) Uani 1 1 d . . .
H7A H 0.0412 0.1741 0.9845 0.065 Uiso 1 1 calc R . .
H7B H -0.0805 0.1550 0.9121 0.065 Uiso 1 1 calc R . .
C6 C 0.2941(7) 0.1965(2) 0.9634(4) 0.0538(15) Uani 1 1 d . . .
H6A H 0.3668 0.2190 0.9819 0.065 Uiso 1 1 calc R . .
H6B H 0.2668 0.1872 1.0119 0.065 Uiso 1 1 calc R . .
C5 C 0.1751(6) 0.2192(2) 0.8990(4) 0.0565(15) Uani 1 1 d . . .
H5A H 0.1428 0.2455 0.9243 0.068 Uiso 1 1 calc R . .
H5B H 0.2035 0.2307 0.8522 0.068 Uiso 1 1 calc R . .
C4 C -0.0213(6) 0.1939(2) 0.7836(4) 0.0559(15) Uani 1 1 d . . .
H4A H 0.0329 0.2061 0.7500 0.067 Uiso 1 1 calc R . .
H4B H -0.0884 0.2171 0.7852 0.067 Uiso 1 1 calc R . .
C3 C -0.1007(7) 0.2239(2) 0.9358(4) 0.0562(15) Uani 1 1 d . . .
C2 C 0.3941(7) 0.1977(2) 0.6270(4) 0.0628(17) Uani 1 1 d . . .
H2A H 0.4301 0.2150 0.6757 0.075 Uiso 1 1 calc R . .
C1 C 0.4206(6) 0.1706(2) 0.8691(4) 0.0518(14) Uani 1 1 d . . .
H1A H 0.5150 0.1751 0.9001 0.062 Uiso 1 1 calc R . .
H1B H 0.3843 0.2002 0.8442 0.062 Uiso 1 1 calc R . .
C31 C 0.2709(7) 0.0431(2) 0.7710(4) 0.0604(16) Uani 1 1 d . . .
C30 C -0.3111(8) 0.2654(3) 0.8967(5) 0.071(2) Uani 1 1 d . . .
H30A H -0.4014 0.2671 0.8648 0.085 Uiso 1 1 calc R . .
C29 C -0.0465(8) 0.2588(3) 0.9926(5) 0.073(2) Uani 1 1 d . . .
H29A H 0.0431 0.2567 1.0256 0.087 Uiso 1 1 calc R . .
C28 C 0.2726(7) 0.0175(2) 0.9012(4) 0.0599(16) Uani 1 1 d . . .
H28A H 0.2612 0.0233 0.9535 0.072 Uiso 1 1 calc R . .
C27 C 0.6728(7) 0.1502(2) 1.0440(4) 0.0631(17) Uani 1 1 d . . .
H27A H 0.6826 0.1363 0.9957 0.076 Uiso 1 1 calc R . .
C26 C 0.2311(8) 0.1457(3) 0.5447(4) 0.076(2) Uani 1 1 d . . .
H26A H 0.1549 0.1271 0.5378 0.092 Uiso 1 1 calc R . .
C25 C 0.3144(8) 0.0000(3) 0.7527(5) 0.076(2) Uani 1 1 d . . .
H25A H 0.3285 -0.0051 0.7009 0.091 Uiso 1 1 calc R . .
F3 F 0.3242(7) 0.2893(3) 0.7588(4) 0.142(3) Uani 1 1 d . . .
C24 C 0.3365(9) -0.0350(3) 0.8099(6) 0.081(2) Uani 1 1 d . . .
H24A H 0.3651 -0.0642 0.7977 0.097 Uiso 1 1 calc R . .
C23 C -0.2151(8) 0.1496(3) 0.6853(5) 0.080(2) Uani 1 1 d . . .
H23A H -0.2629 0.1774 0.6708 0.096 Uiso 1 1 calc R . .
C22 C 0.4525(8) 0.1999(3) 0.5607(5) 0.077(2) Uani 1 1 d . . .
H22A H 0.5276 0.2188 0.5662 0.092 Uiso 1 1 calc R . .
B1 B 0.2062(11) 0.3098(3) 0.7170(6) 0.075(2) Uani 1 1 d . . .
C21 C 0.3163(9) -0.0266(3) 0.8853(6) 0.081(2) Uani 1 1 d . . .
H21A H 0.3313 -0.0499 0.9258 0.098 Uiso 1 1 calc R . .
C20 C -0.0762(8) 0.0697(3) 0.7346(5) 0.072(2) Uani 1 1 d . . .
H20A H -0.0296 0.0420 0.7521 0.086 Uiso 1 1 calc R . .
C19 C -0.1238(9) 0.2971(3) 1.0013(6) 0.085(2) Uani 1 1 d . . .
H19A H -0.0860 0.3203 1.0403 0.102 Uiso 1 1 calc R . .
C18 C 0.2898(10) 0.1486(4) 0.4797(5) 0.089(3) Uani 1 1 d . . .
H18A H 0.2518 0.1323 0.4300 0.107 Uiso 1 1 calc R . .
C50 C 0.4005(10) 0.1746(3) 0.4883(5) 0.082(2) Uani 1 1 d . . .
H50A H 0.4416 0.1756 0.4458 0.098 Uiso 1 1 calc R . .
C41 C -0.2568(9) 0.3008(3) 0.9519(6) 0.081(2) Uani 1 1 d . . .
H41A H -0.3084 0.3267 0.9559 0.097 Uiso 1 1 calc R . .
C49 C 0.5350(9) 0.1675(4) 1.1276(5) 0.093(3) Uani 1 1 d . . .
H49A H 0.4515 0.1662 1.1376 0.112 Uiso 1 1 calc R . .
C48 C 0.7836(10) 0.1719(4) 1.0980(6) 0.095(3) Uani 1 1 d . . .
H48A H 0.8659 0.1726 1.0865 0.114 Uiso 1 1 calc R . .
F2 F 0.1075(9) 0.2776(3) 0.6980(7) 0.207(5) Uani 1 1 d . . .
C47 C -0.2001(9) 0.0676(4) 0.6740(6) 0.096(3) Uani 1 1 d . . .
H47A H -0.2367 0.0393 0.6510 0.115 Uiso 1 1 calc R . .
C46 C -0.2674(9) 0.1088(4) 0.6486(6) 0.098(3) Uani 1 1 d . . .
H46A H -0.3493 0.1088 0.6060 0.118 Uiso 1 1 calc R . .
F1 F 0.1619(15) 0.3371(4) 0.7638(6) 0.246(6) Uani 1 1 d . . .
C44 C 0.7697(14) 0.1926(4) 1.1693(8) 0.125(5) Uani 1 1 d . . .
H44A H 0.8423 0.2081 1.2061 0.150 Uiso 1 1 calc R . .
C43 C 0.6449(16) 0.1900(5) 1.1864(7) 0.151(6) Uani 1 1 d . . .
H43A H 0.6347 0.2028 1.2354 0.182 Uiso 1 1 calc R . .
F5 F 0.3979(7) -0.0452(3) 1.0869(4) 0.127(2) Uani 1 1 d . . .
F4 F 0.2031(9) 0.3290(3) 0.6445(5) 0.167(3) Uani 1 1 d . . .
F6 F 0.1962(10) -0.0259(4) 1.1030(11) 0.291(8) Uani 1 1 d . . .
F7 F 0.2662(9) -0.0946(3) 1.1317(6) 0.164(3) Uani 1 1 d . . .
F8 F 0.3718(9) -0.0385(3) 1.2098(5) 0.174(4) Uani 1 1 d . . .
B2 B 0.3007(13) -0.0468(5) 1.1290(8) 0.099(3) Uani 1 1 d . . .
C45 C 0.0292(11) 0.0664(3) 1.0826(6) 0.101(3) Uani 1 1 d . . .
C202 C 0.437(2) -0.0823(8) 0.6244(15) 0.226(9) Uiso 1 1 d . . .
C203 C 0.594(3) -0.0685(9) 0.6928(16) 0.250(10) Uiso 1 1 d . . .
C201 C -0.009(2) 0.0769(8) 0.3230(12) 0.179(7) Uiso 1 1 d . . .
C200 C -0.0756(19) 0.1212(6) 0.3347(11) 0.165(6) Uiso 1 1 d . . .
N7 N 0.053(3) 0.0451(9) 0.3190(15) 0.268(10) Uiso 1 1 d . . .
C205 C 0.0000 0.0000 0.5000 0.79(10) Uiso 1 2 d S . .
N9 N 0.061(7) -0.061(2) 0.474(5) 0.66(4) Uiso 1 1 d . . .
C204 C -0.236(8) -0.011(2) 0.438(5) 0.60(4) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3 2.068(5) . ?
Ni1 N5 2.111(6) . ?
Ni1 N4 2.115(5) . ?
Ni1 N1 2.127(5) . ?
Ni1 N2 2.207(5) . ?
Ni1 N6 2.250(5) . ?
N3 C20 1.330(9) . ?
N3 C9 1.352(8) . ?
N2 C4 1.457(8) . ?
N2 C5 1.483(8) . ?
N2 C7 1.521(8) . ?
N1 C17 1.489(7) . ?
N1 C1 1.503(7) . ?
N1 C6 1.504(8) . ?
C17 C14 1.511(9) . ?
N6 C16 1.476(8) . ?
N6 C15 1.483(8) . ?
N6 C12 1.503(7) . ?
C16 C31 1.513(9) . ?
C15 C1 1.497(9) . ?
C14 C49 1.339(10) . ?
C14 C27 1.366(9) . ?
C13 C26 1.373(10) . ?
C13 C2 1.378(10) . ?
C13 C12 1.532(8) . ?
N5 C10 1.100(8) . ?
C10 C45 1.475(10) . ?
N4 C28 1.335(8) . ?
N4 C31 1.345(9) . ?
C9 C23 1.361(10) . ?
C9 C4 1.522(10) . ?
C8 C30 1.386(10) . ?
C8 C3 1.390(9) . ?
C7 C3 1.511(9) . ?
C6 C5 1.519(9) . ?
C3 C29 1.377(10) . ?
C2 C22 1.412(10) . ?
C31 C25 1.381(10) . ?
C30 C41 1.372(11) . ?
C29 C19 1.393(11) . ?
C28 C21 1.394(10) . ?
C27 C48 1.379(11) . ?
C26 C18 1.396(11) . ?
C25 C24 1.354(11) . ?
F3 B1 1.349(12) . ?
C24 C21 1.358(12) . ?
C23 C46 1.354(13) . ?
C22 C50 1.374(12) . ?
B1 F1 1.284(12) . ?
B1 F4 1.320(11) . ?
B1 F2 1.343(12) . ?
C20 C47 1.379(11) . ?
C19 C41 1.384(12) . ?
C18 C50 1.340(12) . ?
C49 C43 1.418(16) . ?
C48 C44 1.374(16) . ?
C47 C46 1.373(14) . ?
C44 C43 1.41(2) . ?
F5 B2 1.391(14) . ?
F6 B2 1.200(14) . ?
F7 B2 1.418(16) . ?
F8 B2 1.350(14) . ?
C202 C203 1.74(3) . ?
C201 N7 1.13(3) . ?
C201 C200 1.48(2) . ?
C205 N9 1.96(7) . ?
C205 N9 1.96(7) 3_556 ?
C205 C204 2.38(8) . ?
C205 C204 2.38(8) 3_556 ?
N9 C204 2.85(9) 3_556 ?
C204 N9 2.85(9) 3_556 ?

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 N5 95.6(2) . . ?
N3 Ni1 N4 97.5(2) . . ?
N5 Ni1 N4 86.8(2) . . ?
N3 Ni1 N1 158.3(2) . . ?
N5 Ni1 N1 96.2(2) . . ?
N4 Ni1 N1 101.3(2) . . ?
N3 Ni1 N2 78.2(2) . . ?
N5 Ni1 N2 89.0(2) . . ?
N4 Ni1 N2 173.6(2) . . ?
N1 Ni1 N2 83.91(18) . . ?
N3 Ni1 N6 91.47(19) . . ?
N5 Ni1 N6 162.7(2) . . ?
N4 Ni1 N6 76.7(2) . . ?
N1 Ni1 N6 82.36(18) . . ?
N2 Ni1 N6 107.96(18) . . ?
C20 N3 C9 117.3(6) . . ?
C20 N3 Ni1 127.7(5) . . ?
C9 N3 Ni1 115.0(4) . . ?
C4 N2 C5 113.5(5) . . ?
C4 N2 C7 110.5(5) . . ?
C5 N2 C7 110.6(5) . . ?
C4 N2 Ni1 103.6(4) . . ?
C5 N2 Ni1 105.1(4) . . ?
C7 N2 Ni1 113.4(3) . . ?
C17 N1 C1 111.0(5) . . ?
C17 N1 C6 111.2(4) . . ?
C1 N1 C6 108.8(5) . . ?
C17 N1 Ni1 112.0(4) . . ?
C1 N1 Ni1 108.1(3) . . ?
C6 N1 Ni1 105.5(3) . . ?
N1 C17 C14 116.5(5) . . ?
C16 N6 C15 109.5(5) . . ?
C16 N6 C12 109.1(5) . . ?
C15 N6 C12 110.8(5) . . ?
C16 N6 Ni1 105.1(4) . . ?
C15 N6 Ni1 101.9(3) . . ?
C12 N6 Ni1 119.9(4) . . ?
N6 C16 C31 110.7(5) . . ?
N6 C15 C1 110.0(5) . . ?
C49 C14 C27 118.8(7) . . ?
C49 C14 C17 120.2(7) . . ?
C27 C14 C17 121.0(6) . . ?
C26 C13 C2 118.4(6) . . ?
C26 C13 C12 121.3(6) . . ?
C2 C13 C12 120.3(6) . . ?
N6 C12 C13 117.1(5) . . ?
C10 N5 Ni1 175.1(6) . . ?
N5 C10 C45 177.2(8) . . ?
C28 N4 C31 117.2(6) . . ?
C28 N4 Ni1 127.2(5) . . ?
C31 N4 Ni1 115.6(4) . . ?
N3 C9 C23 122.7(7) . . ?
N3 C9 C4 115.1(5) . . ?
C23 C9 C4 122.1(7) . . ?
C30 C8 C3 119.5(7) . . ?
N2 C7 C3 116.1(5) . . ?
N1 C6 C5 111.6(5) . . ?
N2 C5 C6 109.6(5) . . ?
N2 C4 C9 110.3(5) . . ?
C29 C3 C8 119.0(7) . . ?
C29 C3 C7 121.1(6) . . ?
C8 C3 C7 119.9(6) . . ?
C13 C2 C22 119.2(7) . . ?
N1 C1 C15 110.0(5) . . ?
N4 C31 C25 122.0(7) . . ?
N4 C31 C16 116.8(6) . . ?
C25 C31 C16 121.2(7) . . ?
C8 C30 C41 121.8(7) . . ?
C19 C29 C3 121.0(7) . . ?
N4 C28 C21 122.7(7) . . ?
C14 C27 C48 123.3(8) . . ?
C13 C26 C18 121.6(8) . . ?
C24 C25 C31 120.3(8) . . ?
C25 C24 C21 118.8(7) . . ?
C9 C23 C46 118.8(8) . . ?
C50 C22 C2 121.2(8) . . ?
F1 B1 F4 112.8(10) . . ?
F1 B1 F2 100.2(11) . . ?
F4 B1 F2 105.1(9) . . ?
F1 B1 F3 112.6(9) . . ?
F4 B1 F3 115.3(9) . . ?
F2 B1 F3 109.5(8) . . ?
C24 C21 C28 119.1(7) . . ?
N3 C20 C47 123.0(8) . . ?
C41 C19 C29 119.9(8) . . ?
C50 C18 C26 120.5(8) . . ?
C18 C50 C22 119.2(7) . . ?
C19 C41 C30 118.8(7) . . ?
C14 C49 C43 121.1(10) . . ?
C27 C48 C44 118.6(10) . . ?
C46 C47 C20 117.8(9) . . ?
C23 C46 C47 120.2(8) . . ?
C43 C44 C48 119.5(10) . . ?
C44 C43 C49 118.8(10) . . ?
F6 B2 F8 116.0(14) . . ?
F6 B2 F5 120.9(14) . . ?
F8 B2 F5 103.7(10) . . ?
F6 B2 F7 106.5(12) . . ?
F8 B2 F7 101.9(11) . . ?
F5 B2 F7 105.9(10) . . ?
N7 C201 C200 173(3) . . ?
N9 C205 N9 179.998(12) . 3_556 ?
N9 C205 C204 98(2) . . ?
N9 C205 C204 82(2) 3_556 . ?
N9 C205 C204 82(2) . 3_556 ?
N9 C205 C204 98(2) 3_556 3_556 ?
C204 C205 C204 179.999(3) . 3_556 ?
C204 N9 C205 56(2) 3_556 . ?
N9 C204 C205 42.8(19) 3_556 . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.68
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.120
_database_code_depnum_ccdc_archive 'CCDC 989008'
