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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_4203
_database_code_depnum_ccdc_archive 'CCDC 1503876'
_audit_update_record             
;
2016-09-12 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H17 Cl F6 N7 Ni P'
_chemical_formula_weight         606.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   7.4325(3)
_cell_length_b                   25.4040(9)
_cell_length_c                   12.2332(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.003(3)
_cell_angle_gamma                90.00
_cell_volume                     2306.65(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13892
_cell_measurement_theta_min      3.48
_cell_measurement_theta_max      67.25

_exptl_crystal_description       flat
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    3.638
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7848
_exptl_absorpt_correction_T_max  0.8390
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_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            13892
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.48
_diffrn_reflns_theta_max         67.25
_reflns_number_total             4133
_reflns_number_gt                3310
_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)+(0.0973P)²+2.8416P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4133
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1852
_refine_ls_wR_factor_gt          0.1665
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.80025(9) 0.52820(3) 0.94643(5) 0.0353(2) Uani 1 1 d . . .
P1 P 0.45946(18) 0.68695(5) 0.69869(11) 0.0543(4) Uani 1 1 d . . .
Cl1 Cl 0.81692(16) 0.52631(4) 1.12615(8) 0.0484(3) Uani 1 1 d . . .
F1 F 0.6656(6) 0.6992(3) 0.7120(5) 0.146(2) Uani 1 1 d . . .
F2 F 0.4765(11) 0.63232(19) 0.7594(4) 0.165(3) Uani 1 1 d . . .
F3 F 0.2517(6) 0.6760(2) 0.6809(4) 0.1282(18) Uani 1 1 d . . .
F4 F 0.4385(7) 0.73958(15) 0.6341(4) 0.1066(14) Uani 1 1 d . . .
F5 F 0.4876(7) 0.65785(16) 0.5872(3) 0.1092(15) Uani 1 1 d . . .
F6 F 0.4292(7) 0.71447(18) 0.8119(3) 0.1138(16) Uani 1 1 d . . .
N1 N 0.6883(4) 0.45919(13) 0.9317(3) 0.0380(7) Uani 1 1 d . . .
N2 N 0.7066(5) 0.47971(13) 0.7519(3) 0.0362(7) Uani 1 1 d . . .
N3 N 0.8396(4) 0.55259(13) 0.7147(3) 0.0358(7) Uani 1 1 d . . .
N4 N 0.8938(4) 0.59755(13) 0.9326(3) 0.0376(7) Uani 1 1 d . . .
N5 N 0.9023(5) 0.63147(14) 1.0162(3) 0.0447(8) Uani 1 1 d . . .
N6 N 0.9608(5) 0.67616(14) 0.9748(3) 0.0462(9) Uani 1 1 d . . .
C1 C 0.6418(6) 0.42526(18) 1.0099(4) 0.0464(10) Uani 1 1 d . . .
H1 H 0.6605 0.4346 1.0831 0.056 Uiso 1 1 calc R . .
C2 C 0.5675(7) 0.37732(19) 0.9837(4) 0.0526(11) Uani 1 1 d . . .
H2 H 0.5371 0.3538 1.0381 0.063 Uiso 1 1 calc R . .
C3 C 0.5392(7) 0.36498(18) 0.8758(4) 0.0530(11) Uani 1 1 d . . .
H3 H 0.4882 0.3325 0.8573 0.064 Uiso 1 1 calc R . .
N7 N 0.5821(5) 0.39784(14) 0.7950(3) 0.0459(8) Uani 1 1 d . . .
C5 C 0.6533(5) 0.44254(16) 0.8280(3) 0.0361(8) Uani 1 1 d . . .
C6 C 0.7135(5) 0.48014(16) 0.6381(3) 0.0366(9) Uani 1 1 d . . .
C7 C 0.6556(6) 0.44539(17) 0.5553(3) 0.0430(10) Uani 1 1 d . . .
H7 H 0.6016 0.4134 0.5703 0.052 Uiso 1 1 calc R . .
C8 C 0.6836(6) 0.46154(19) 0.4495(3) 0.0468(10) Uani 1 1 d . . .
H8 H 0.6465 0.4396 0.3917 0.056 Uiso 1 1 calc R . .
C9 C 0.7654(6) 0.50950(19) 0.4260(3) 0.0465(10) Uani 1 1 d . . .
H9 H 0.7807 0.5187 0.3535 0.056 Uiso 1 1 calc R . .
C10 C 0.8242(6) 0.54358(18) 0.5089(3) 0.0418(9) Uani 1 1 d . . .
H10 H 0.8786 0.5756 0.4942 0.050 Uiso 1 1 calc R . .
C11 C 0.7975(5) 0.52745(15) 0.6142(3) 0.0357(8) Uani 1 1 d . . .
C12 C 0.7839(5) 0.52391(15) 0.7962(3) 0.0343(8) Uani 1 1 d . . .
C13 C 0.9516(7) 0.59899(17) 0.7291(4) 0.0478(11) Uani 1 1 d . . .
H13A H 0.9120 0.6253 0.6757 0.057 Uiso 1 1 calc R . .
H13B H 1.0751 0.5898 0.7153 0.057 Uiso 1 1 calc R . .
C14 C 0.9462(6) 0.62196(16) 0.8404(3) 0.0397(9) Uani 1 1 d . . .
C15 C 0.9896(6) 0.67210(17) 0.8687(4) 0.0475(10) Uani 1 1 d . . .
H15 H 1.0311 0.6983 0.8233 0.057 Uiso 1 1 calc R . .
C16 C 0.9822(8) 0.72449(19) 1.0436(4) 0.0594(13) Uani 1 1 d . . .
H16A H 1.1025 0.7258 1.0782 0.071 Uiso 1 1 calc R . .
H16B H 0.8960 0.7242 1.1005 0.071 Uiso 1 1 calc R . .
C17 C 0.9507(6) 0.77175(16) 0.9708(3) 0.0447(10) Uani 1 1 d . . .
C18 C 0.7786(8) 0.7873(2) 0.9423(4) 0.0643(14) Uani 1 1 d . . .
H18 H 0.6833 0.7707 0.9744 0.077 Uiso 1 1 calc R . .
C19 C 0.7427(12) 0.8262(3) 0.8687(6) 0.090(2) Uani 1 1 d . . .
H19 H 0.6243 0.8365 0.8525 0.108 Uiso 1 1 calc R . .
C20 C 0.8771(16) 0.8499(2) 0.8194(6) 0.097(3) Uani 1 1 d . . .
H20 H 0.8522 0.8755 0.7665 0.116 Uiso 1 1 calc R . .
C21 C 1.0554(14) 0.8359(3) 0.8477(6) 0.100(3) Uani 1 1 d . . .
H21 H 1.1493 0.8531 0.8154 0.120 Uiso 1 1 calc R . .
C22 C 1.0934(8) 0.7960(2) 0.9247(5) 0.0678(15) Uani 1 1 d . . .
H22 H 1.2115 0.7862 0.9438 0.081 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C12 1.839(4) . ?
Ni1 N4 1.905(3) . ?
Ni1 N1 1.945(3) . ?
Ni1 Cl1 2.1960(12) . ?
P1 F4 1.556(4) . ?
P1 F1 1.563(4) . ?
P1 F3 1.573(4) . ?
P1 F5 1.575(4) . ?
P1 F2 1.576(5) . ?
P1 F6 1.578(4) . ?
N1 C1 1.346(5) . ?
N1 C5 1.349(5) . ?
N2 C12 1.361(5) . ?
N2 C6 1.395(5) . ?
N2 C5 1.398(5) . ?
N3 C12 1.319(5) . ?
N3 C11 1.406(5) . ?
N3 C13 1.449(5) . ?
N4 N5 1.336(5) . ?
N4 C14 1.361(5) . ?
N5 N6 1.326(5) . ?
N6 C15 1.331(6) . ?
N6 C16 1.492(5) . ?
C1 C2 1.368(7) . ?
C2 C3 1.363(7) . ?
C3 N7 1.345(6) . ?
N7 C5 1.307(5) . ?
C6 C11 1.393(6) . ?
C6 C7 1.394(6) . ?
C7 C8 1.384(6) . ?
C8 C9 1.398(7) . ?
C9 C10 1.387(6) . ?
C10 C11 1.375(6) . ?
C13 C14 1.484(6) . ?
C14 C15 1.354(6) . ?
C16 C17 1.506(6) . ?
C17 C18 1.366(7) . ?
C17 C22 1.373(7) . ?
C18 C19 1.354(9) . ?
C19 C20 1.337(12) . ?
C20 C21 1.398(11) . ?
C21 C22 1.402(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C12 Ni1 N4 88.37(15) . . ?
C12 Ni1 N1 81.28(16) . . ?
N4 Ni1 N1 169.08(15) . . ?
C12 Ni1 Cl1 175.32(12) . . ?
N4 Ni1 Cl1 96.16(11) . . ?
N1 Ni1 Cl1 94.28(11) . . ?
F4 P1 F1 87.3(3) . . ?
F4 P1 F3 90.6(3) . . ?
F1 P1 F3 177.6(3) . . ?
F4 P1 F5 88.7(3) . . ?
F1 P1 F5 90.6(3) . . ?
F3 P1 F5 88.3(3) . . ?
F4 P1 F2 177.4(3) . . ?
F1 P1 F2 94.1(4) . . ?
F3 P1 F2 87.9(4) . . ?
F5 P1 F2 89.1(3) . . ?
F4 P1 F6 92.8(3) . . ?
F1 P1 F6 90.3(3) . . ?
F3 P1 F6 90.9(3) . . ?
F5 P1 F6 178.2(2) . . ?
F2 P1 F6 89.3(3) . . ?
C1 N1 C5 115.0(4) . . ?
C1 N1 Ni1 129.5(3) . . ?
C5 N1 Ni1 115.5(3) . . ?
C12 N2 C6 110.7(3) . . ?
C12 N2 C5 114.9(3) . . ?
C6 N2 C5 134.1(3) . . ?
C12 N3 C11 110.2(3) . . ?
C12 N3 C13 123.9(3) . . ?
C11 N3 C13 125.2(3) . . ?
N5 N4 C14 109.6(3) . . ?
N5 N4 Ni1 122.1(3) . . ?
C14 N4 Ni1 128.0(3) . . ?
N6 N5 N4 105.3(3) . . ?
N5 N6 C15 112.3(3) . . ?
N5 N6 C16 121.1(4) . . ?
C15 N6 C16 126.6(4) . . ?
N1 C1 C2 121.3(4) . . ?
C3 C2 C1 118.1(4) . . ?
N7 C3 C2 122.6(4) . . ?
C5 N7 C3 114.8(4) . . ?
N7 C5 N1 128.1(4) . . ?
N7 C5 N2 120.3(4) . . ?
N1 C5 N2 111.5(3) . . ?
C11 C6 C7 121.2(4) . . ?
C11 C6 N2 104.9(3) . . ?
C7 C6 N2 133.9(4) . . ?
C8 C7 C6 115.8(4) . . ?
C7 C8 C9 122.6(4) . . ?
C10 C9 C8 121.1(4) . . ?
C11 C10 C9 116.3(4) . . ?
C10 C11 C6 122.8(4) . . ?
C10 C11 N3 130.3(4) . . ?
C6 C11 N3 106.8(3) . . ?
N3 C12 N2 107.3(3) . . ?
N3 C12 Ni1 135.7(3) . . ?
N2 C12 Ni1 116.8(3) . . ?
N3 C13 C14 112.9(3) . . ?
C15 C14 N4 106.9(4) . . ?
C15 C14 C13 125.9(4) . . ?
N4 C14 C13 127.1(4) . . ?
N6 C15 C14 105.9(4) . . ?
N6 C16 C17 108.3(4) . . ?
C18 C17 C22 119.9(5) . . ?
C18 C17 C16 119.7(5) . . ?
C22 C17 C16 120.0(5) . . ?
C19 C18 C17 122.0(7) . . ?
C20 C19 C18 120.2(7) . . ?
C19 C20 C21 119.6(6) . . ?
C20 C21 C22 120.4(6) . . ?
C17 C22 C21 117.8(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        67.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.097
####################################################################### 
# 
# 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_080825c
_database_code_depnum_ccdc_archive 'CCDC 1503880'
_audit_update_record             
;
2016-09-12 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H15 Cl F6 N7 Ni P'
_chemical_formula_weight         556.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4549(10)
_cell_length_b                   9.4911(15)
_cell_length_c                   15.3162(19)
_cell_angle_alpha                85.011(2)
_cell_angle_beta                 80.1610(10)
_cell_angle_gamma                77.4800(10)
_cell_volume                     1041.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1911
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      25.00

_exptl_crystal_description       yellow
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_T_max  0.7277
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_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            5239
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3574
_reflns_number_gt                2355
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0935P)²+0.0167P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3574
_refine_ls_number_parameters     335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1696
_refine_ls_wR_factor_gt          0.1399
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.19313(9) 0.96214(7) 0.04393(5) 0.0335(3) Uani 1 1 d . . .
Cl1 Cl 0.1966(2) 1.19189(13) 0.02168(10) 0.0424(4) Uani 1 1 d . . .
F1 F 0.6398(7) 0.4701(5) 0.7100(4) 0.1090(18) Uani 1 1 d . A .
F2 F 0.3941(7) 0.2549(6) 0.6803(4) 0.1167(19) Uani 1 1 d . A .
F3 F 0.6908(17) 0.2731(16) 0.6453(14) 0.124(7) Uani 0.60(3) 1 d P A 1
F4 F 0.483(3) 0.4458(19) 0.6011(9) 0.114(8) Uani 0.60(3) 1 d P A 1
F5 F 0.3308(14) 0.4709(13) 0.7442(14) 0.106(7) Uani 0.60(3) 1 d P A 1
F6 F 0.540(3) 0.2899(19) 0.7851(11) 0.105(7) Uani 0.60(3) 1 d P A 1
F3' F 0.674(3) 0.2279(16) 0.717(2) 0.099(10) Uani 0.40(3) 1 d P A 2
F4' F 0.611(4) 0.349(3) 0.5937(14) 0.118(11) Uani 0.40(3) 1 d P A 2
F5' F 0.384(3) 0.4895(19) 0.671(2) 0.143(11) Uani 0.40(3) 1 d P A 2
F6' F 0.430(4) 0.359(3) 0.7939(16) 0.112(10) Uani 0.40(3) 1 d P A 2
N1 N 0.0478(6) 0.9740(5) 0.1580(3) 0.0363(11) Uani 1 1 d . . .
N2 N -0.0017(6) 1.0965(5) 0.1995(3) 0.0415(12) Uani 1 1 d . . .
N3 N -0.0922(7) 1.0642(6) 0.2777(4) 0.0483(13) Uani 1 1 d . . .
N4 N 0.1271(6) 0.6743(5) 0.1083(3) 0.0374(11) Uani 1 1 d . . .
N5 N 0.2920(6) 0.6934(4) -0.0182(3) 0.0384(12) Uani 1 1 d . . .
N6 N 0.3453(6) 0.9123(4) -0.0687(3) 0.0344(11) Uani 1 1 d . . .
N7 N 0.4771(7) 0.7088(5) -0.1559(4) 0.0518(14) Uani 1 1 d . . .
C1 C -0.1037(8) 0.9249(7) 0.2878(4) 0.0495(16) Uani 1 1 d . . .
H1 H -0.1616 0.8788 0.3373 0.059 Uiso 1 1 calc R . .
C2 C -0.0151(7) 0.8654(6) 0.2122(4) 0.0410(14) Uani 1 1 d . . .
C3 C 0.0063(9) 0.7118(6) 0.1893(4) 0.0497(16) Uani 1 1 d . . .
H3A H 0.0536 0.6486 0.2371 0.060 Uiso 1 1 calc R . .
H3B H -0.1154 0.6943 0.1853 0.060 Uiso 1 1 calc R . .
C4 C 0.1992(7) 0.7653(5) 0.0536(4) 0.0308(12) Uani 1 1 d . . .
C5 C 0.2735(8) 0.5506(6) -0.0072(5) 0.0485(16) Uani 1 1 d . . .
H5 H 0.3224 0.4780 -0.0468 0.058 Uiso 1 1 calc R . .
C6 C 0.1712(8) 0.5394(6) 0.0721(5) 0.0476(16) Uani 1 1 d . . .
H6 H 0.1352 0.4559 0.0987 0.057 Uiso 1 1 calc R . .
C7 C 0.3795(7) 0.7722(6) -0.0866(4) 0.0364(13) Uani 1 1 d . . .
C8 C 0.5551(9) 0.7934(7) -0.2181(5) 0.0551(17) Uani 1 1 d . . .
H8 H 0.6251 0.7537 -0.2697 0.066 Uiso 1 1 calc R . .
C9 C 0.5338(9) 0.9386(7) -0.2072(4) 0.0512(16) Uani 1 1 d . . .
H9 H 0.5906 0.9970 -0.2503 0.061 Uiso 1 1 calc R . .
C10 C 0.4268(8) 0.9956(6) -0.1313(4) 0.0431(15) Uani 1 1 d . . .
H10 H 0.4107 1.0938 -0.1233 0.052 Uiso 1 1 calc R . .
C11 C -0.1534(8) 1.1751(7) 0.3434(5) 0.0584(18) Uani 1 1 d . . .
H11A H -0.2515 1.1486 0.3879 0.070 Uiso 1 1 calc R . .
H11B H -0.2036 1.2667 0.3145 0.070 Uiso 1 1 calc R . .
C12 C 0.0068(8) 1.1919(7) 0.3881(4) 0.0487(15) Uani 1 1 d . . .
C13 C 0.0214(10) 1.3266(8) 0.4072(5) 0.069(2) Uani 1 1 d . . .
H13 H -0.0661 1.4069 0.3922 0.083 Uiso 1 1 calc R . .
C14 C 0.1660(13) 1.3444(10) 0.4488(6) 0.082(3) Uani 1 1 d . . .
H14 H 0.1751 1.4364 0.4616 0.099 Uiso 1 1 calc R . .
C15 C 0.2934(11) 1.2280(11) 0.4706(5) 0.079(2) Uani 1 1 d . . .
H15 H 0.3909 1.2397 0.4980 0.095 Uiso 1 1 calc R . .
C16 C 0.2790(11) 1.0924(10) 0.4522(5) 0.074(2) Uani 1 1 d . . .
H16 H 0.3668 1.0125 0.4676 0.088 Uiso 1 1 calc R . .
C17 C 0.1363(9) 1.0733(7) 0.4113(4) 0.0579(18) Uani 1 1 d . . .
H17 H 0.1271 0.9809 0.3993 0.069 Uiso 1 1 calc R . .
P1 P 0.5155(3) 0.36504(19) 0.69262(15) 0.0591(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
Ni1 C4 1.853(5) . ?
Ni1 N1 1.890(5) . ?
Ni1 N6 1.930(5) . ?
Ni1 Cl1 2.1827(14) . ?
F1 P1 1.567(4) . ?
F2 P1 1.565(4) . ?
F3 P1 1.512(10) . ?
F4 P1 1.569(11) . ?
F5 P1 1.642(11) . ?
F6 P1 1.552(13) . ?
F3' P1 1.622(15) . ?
F4' P1 1.565(18) . ?
F5' P1 1.417(14) . ?
F6' P1 1.57(2) . ?
N1 N2 1.325(6) . ?
N1 C2 1.378(7) . ?
N2 N3 1.317(7) . ?
N3 C1 1.337(8) . ?
N3 C11 1.466(8) . ?
N4 C4 1.287(7) . ?
N4 C6 1.390(7) . ?
N4 C3 1.426(7) . ?
N5 C4 1.349(7) . ?
N5 C5 1.385(7) . ?
N5 C7 1.387(7) . ?
N6 C10 1.339(7) . ?
N6 C7 1.341(7) . ?
N7 C7 1.295(7) . ?
N7 C8 1.330(8) . ?
C1 C2 1.336(8) . ?
C2 C3 1.498(8) . ?
C5 C6 1.328(9) . ?
C8 C9 1.374(9) . ?
C9 C10 1.373(8) . ?
C11 C12 1.517(8) . ?
C12 C13 1.367(9) . ?
C12 C17 1.379(8) . ?
C13 C14 1.389(10) . ?
C14 C15 1.351(11) . ?
C15 C16 1.371(11) . ?
C16 C17 1.375(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
C4 Ni1 N1 87.7(2) . . ?
C4 Ni1 N6 81.9(2) . . ?
N1 Ni1 N6 169.47(17) . . ?
C4 Ni1 Cl1 175.47(18) . . ?
N1 Ni1 Cl1 96.84(14) . . ?
N6 Ni1 Cl1 93.65(13) . . ?
N2 N1 C2 109.5(5) . . ?
N2 N1 Ni1 121.7(4) . . ?
C2 N1 Ni1 128.8(4) . . ?
N3 N2 N1 105.4(4) . . ?
N2 N3 C1 112.3(5) . . ?
N2 N3 C11 119.2(5) . . ?
C1 N3 C11 128.3(6) . . ?
C4 N4 C6 109.5(5) . . ?
C4 N4 C3 124.3(5) . . ?
C6 N4 C3 126.0(5) . . ?
C4 N5 C5 109.6(5) . . ?
C4 N5 C7 117.1(4) . . ?
C5 N5 C7 133.3(5) . . ?
C10 N6 C7 114.4(5) . . ?
C10 N6 Ni1 129.9(4) . . ?
C7 N6 Ni1 115.7(4) . . ?
C7 N7 C8 115.9(5) . . ?
C2 C1 N3 106.0(6) . . ?
C1 C2 N1 106.7(5) . . ?
C1 C2 C3 126.8(6) . . ?
N1 C2 C3 126.4(5) . . ?
N4 C3 C2 114.4(5) . . ?
N4 C4 N5 107.5(5) . . ?
N4 C4 Ni1 137.8(4) . . ?
N5 C4 Ni1 114.5(4) . . ?
C6 C5 N5 105.3(5) . . ?
C5 C6 N4 108.1(5) . . ?
N7 C7 N6 128.9(6) . . ?
N7 C7 N5 120.3(5) . . ?
N6 C7 N5 110.8(5) . . ?
N7 C8 C9 121.0(6) . . ?
C10 C9 C8 118.5(6) . . ?
N6 C10 C9 121.2(6) . . ?
N3 C11 C12 111.0(5) . . ?
C13 C12 C17 119.4(6) . . ?
C13 C12 C11 119.5(6) . . ?
C17 C12 C11 121.1(6) . . ?
C12 C13 C14 120.5(7) . . ?
C15 C14 C13 119.9(7) . . ?
C14 C15 C16 120.0(7) . . ?
C15 C16 C17 120.7(8) . . ?
C16 C17 C12 119.6(7) . . ?
F5' P1 F3 136.3(12) . . ?
F5' P1 F6 129.0(13) . . ?
F3 P1 F6 94.1(8) . . ?
F5' P1 F4' 92.4(12) . . ?
F3 P1 F4' 44.7(9) . . ?
F6 P1 F4' 138.6(12) . . ?
F5' P1 F2 95.1(10) . . ?
F3 P1 F2 92.6(5) . . ?
F6 P1 F2 88.4(6) . . ?
F4' P1 F2 89.4(6) . . ?
F5' P1 F1 87.3(10) . . ?
F3 P1 F1 87.2(5) . . ?
F6 P1 F1 88.3(5) . . ?
F4' P1 F1 92.8(6) . . ?
F2 P1 F1 176.7(3) . . ?
F5' P1 F4 48.5(10) . . ?
F3 P1 F4 88.4(9) . . ?
F6 P1 F4 177.4(10) . . ?
F4' P1 F4 44.0(8) . . ?
F2 P1 F4 91.7(5) . . ?
F1 P1 F4 91.7(5) . . ?
F5' P1 F6' 94.8(13) . . ?
F3 P1 F6' 128.6(11) . . ?
F6 P1 F6' 34.5(8) . . ?
F4' P1 F6' 172.1(12) . . ?
F2 P1 F6' 86.7(9) . . ?
F1 P1 F6' 90.8(9) . . ?
F4 P1 F6' 142.9(12) . . ?
F5' P1 F3' 177.0(11) . . ?
F3 P1 F3' 42.7(7) . . ?
F6 P1 F3' 51.6(8) . . ?
F4' P1 F3' 87.0(12) . . ?
F2 P1 F3' 87.8(5) . . ?
F1 P1 F3' 89.9(5) . . ?
F4 P1 F3' 130.9(11) . . ?
F6' P1 F3' 86.1(11) . . ?
F5' P1 F5 43.0(10) . . ?
F3 P1 F5 177.3(6) . . ?
F6 P1 F5 86.2(8) . . ?
F4' P1 F5 135.1(11) . . ?
F2 P1 F5 90.1(4) . . ?
F1 P1 F5 90.1(4) . . ?
F4 P1 F5 91.2(8) . . ?
F6' P1 F5 51.8(9) . . ?
F3' P1 F5 137.8(11) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.133
####################################################################### 
# 
# 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_exp_4742
_database_code_depnum_ccdc_archive 'CCDC 1503877'
_audit_update_record             
;
2016-09-12 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H32 Cl2 F12 N15 Ni2 P2'
_chemical_formula_weight         1153.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   14.5120(8)
_cell_length_b                   9.4393(3)
_cell_length_c                   34.1126(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.582(5)
_cell_angle_gamma                90.00
_cell_volume                     4663.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4230
_cell_measurement_theta_min      3.0710
_cell_measurement_theta_max      68.9570

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2324
_exptl_absorpt_coefficient_mu    3.567
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6542
_exptl_absorpt_correction_T_max  0.6742
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_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            29345
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         67.25
_reflns_number_total             8374
_reflns_number_gt                4995
_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)+(0.1299P)²+2.9735P] 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     multi-scan
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8374
_refine_ls_number_parameters     622
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0746
_refine_ls_wR_factor_ref         0.2530
_refine_ls_wR_factor_gt          0.2072
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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 0.65251(7) 0.54455(10) 0.02509(3) 0.0555(3) Uani 1 1 d . . .
Ni2 Ni 0.14500(7) 0.46526(10) 0.01618(3) 0.0566(3) Uani 1 1 d . . .
P1 P 0.98880(16) 0.9317(2) 0.14614(6) 0.0813(6) Uani 1 1 d . . .
P2 P 0.52658(14) 0.1453(2) 0.86635(5) 0.0721(5) Uani 1 1 d . . .
Cl1 Cl 0.65636(12) 0.31739(15) 0.01214(5) 0.0666(4) Uani 1 1 d . . .
Cl2 Cl 0.14294(12) 0.23910(16) 0.00211(5) 0.0702(4) Uani 1 1 d . . .
F1 F 0.9187(5) 0.8163(8) 0.1576(2) 0.172(3) Uani 1 1 d . . .
F2 F 1.0168(6) 0.9510(8) 0.18989(19) 0.185(3) Uani 1 1 d . . .
F3 F 1.0610(5) 1.0395(7) 0.1317(2) 0.174(3) Uani 1 1 d . . .
F4 F 0.9647(5) 0.8969(10) 0.10303(19) 0.198(4) Uani 1 1 d . . .
F5 F 1.0670(5) 0.8174(9) 0.1476(3) 0.196(4) Uani 1 1 d . . .
F6 F 0.6067(5) 0.0519(7) 0.8796(3) 0.208(4) Uani 1 1 d . . .
F7 F 0.5965(3) 0.2686(5) 0.85711(15) 0.1048(15) Uani 1 1 d . . .
F8 F 0.4460(4) 0.2377(9) 0.8521(3) 0.215(5) Uani 1 1 d . . .
F9 F 0.4560(3) 0.0239(5) 0.87671(14) 0.0975(14) Uani 1 1 d . . .
F10 F 0.5265(8) 0.0922(11) 0.8243(2) 0.231(5) Uani 1 1 d . . .
F11 F 0.5220(6) 0.2012(8) 0.90753(18) 0.187(4) Uani 1 1 d . . .
F12 F 0.9152(6) 1.0423(8) 0.1441(3) 0.230(5) Uani 1 1 d . . .
N1 N 0.5924(3) 0.5945(5) -0.02566(15) 0.0569(12) Uani 1 1 d . . .
N2 N 0.6137(4) 0.8138(5) 0.00082(16) 0.0643(13) Uani 1 1 d . . .
N3 N 0.6822(4) 0.8313(5) 0.05786(17) 0.0640(13) Uani 1 1 d . . .
N4 N 0.7093(3) 0.5330(5) 0.07662(15) 0.0572(12) Uani 1 1 d . . .
N5 N 0.7264(4) 0.4062(5) 0.09391(16) 0.0642(13) Uani 1 1 d . . .
N6 N 0.7637(4) 0.4371(6) 0.12951(17) 0.0688(14) Uani 1 1 d . . .
N7 N 0.0861(3) 0.5214(5) -0.03442(15) 0.0583(12) Uani 1 1 d . . .
N8 N 0.1057(3) 0.7364(5) -0.00514(16) 0.0617(13) Uani 1 1 d . . .
N9 N 0.1695(4) 0.7469(5) 0.05245(16) 0.0622(13) Uani 1 1 d . . .
N10 N 0.1990(4) 0.4454(5) 0.06825(14) 0.0604(12) Uani 1 1 d . . .
N11 N 0.2108(4) 0.3173(6) 0.08405(16) 0.0668(14) Uani 1 1 d . . .
N12 N 0.2405(4) 0.3412(6) 0.12090(16) 0.0741(15) Uani 1 1 d . . .
C60 C 0.9056(9) 0.1539(13) 0.2583(4) 0.155(5) Uani 1 1 d . . .
N14 N 0.9705(8) 0.0580(11) 0.2813(3) 0.144(4) Uani 1 1 d . . .
N15 N 1.0202(7) -0.0138(11) 0.2998(3) 0.144(4) Uani 1 1 d . . .
C1 C 0.5612(4) 0.5067(7) -0.0543(2) 0.0664(16) Uani 1 1 d . . .
H1 H 0.5666 0.4094 -0.0506 0.080 Uiso 1 1 calc R . .
C2 C 0.5207(5) 0.5581(8) -0.0896(2) 0.0749(19) Uani 1 1 d . . .
H2 H 0.5002 0.4953 -0.1093 0.090 Uiso 1 1 calc R . .
C3 C 0.5110(5) 0.7016(8) -0.0953(2) 0.0784(19) Uani 1 1 d . . .
H3 H 0.4848 0.7365 -0.1190 0.094 Uiso 1 1 calc R . .
C4 C 0.5403(5) 0.7928(7) -0.0658(2) 0.0711(17) Uani 1 1 d . . .
H4 H 0.5336 0.8903 -0.0686 0.085 Uiso 1 1 calc R . .
C5 C 0.5804(4) 0.7341(6) -0.0316(2) 0.0633(16) Uani 1 1 d . . .
C6 C 0.6499(4) 0.7359(6) 0.03157(19) 0.0586(14) Uani 1 1 d . . .
C7 C 0.6238(5) 0.9572(7) 0.0080(2) 0.0737(19) Uani 1 1 d . . .
H7 H 0.6048 1.0314 -0.0085 0.088 Uiso 1 1 calc R . .
C8 C 0.6666(5) 0.9665(7) 0.0438(2) 0.0738(19) Uani 1 1 d . . .
H8 H 0.6831 1.0500 0.0569 0.089 Uiso 1 1 calc R . .
C9 C 0.7325(5) 0.7937(7) 0.0940(2) 0.0762(19) Uani 1 1 d . . .
H9A H 0.7043 0.8408 0.1155 0.091 Uiso 1 1 calc R . .
H9B H 0.7952 0.8289 0.0932 0.091 Uiso 1 1 calc R . .
C10 C 0.7360(4) 0.6383(7) 0.10209(19) 0.0620(15) Uani 1 1 d . . .
C11 C 0.7709(5) 0.5767(8) 0.1357(2) 0.0735(18) Uani 1 1 d . . .
H11 H 0.7947 0.6220 0.1583 0.088 Uiso 1 1 calc R . .
C12 C 0.7936(5) 0.3201(8) 0.1566(2) 0.080(2) Uani 1 1 d . . .
H12A H 0.7969 0.2327 0.1418 0.095 Uiso 1 1 calc R . .
H12B H 0.8549 0.3406 0.1682 0.095 Uiso 1 1 calc R . .
C13 C 0.7296(5) 0.3009(8) 0.1882(2) 0.0705(17) Uani 1 1 d . . .
C14 C 0.6643(6) 0.1983(9) 0.1864(3) 0.091(2) Uani 1 1 d . . .
H14 H 0.6592 0.1395 0.1645 0.109 Uiso 1 1 calc R . .
C15 C 0.6055(7) 0.1784(12) 0.2160(4) 0.124(3) Uani 1 1 d . . .
H15 H 0.5601 0.1088 0.2137 0.148 Uiso 1 1 calc R . .
C16 C 0.6140(9) 0.2597(14) 0.2479(4) 0.135(4) Uani 1 1 d . . .
H16 H 0.5750 0.2438 0.2680 0.162 Uiso 1 1 calc R . .
C17 C 0.6772(10) 0.3640(14) 0.2520(3) 0.141(4) Uani 1 1 d . . .
H17 H 0.6809 0.4210 0.2743 0.169 Uiso 1 1 calc R . .
C18 C 0.7373(7) 0.3845(10) 0.2217(3) 0.107(3) Uani 1 1 d . . .
H18 H 0.7824 0.4544 0.2241 0.129 Uiso 1 1 calc R . .
C19 C 0.0578(4) 0.4383(7) -0.0647(2) 0.0675(17) Uani 1 1 d . . .
H19 H 0.0637 0.3406 -0.0621 0.081 Uiso 1 1 calc R . .
C20 C 0.0202(5) 0.4927(9) -0.0997(2) 0.0765(19) Uani 1 1 d . . .
H20 H 0.0031 0.4326 -0.1205 0.092 Uiso 1 1 calc R . .
C21 C 0.0082(5) 0.6380(8) -0.1035(2) 0.0759(19) Uani 1 1 d . . .
H21 H -0.0179 0.6760 -0.1267 0.091 Uiso 1 1 calc R . .
C22 C 0.0353(5) 0.7256(8) -0.0726(2) 0.0734(18) Uani 1 1 d . . .
H22 H 0.0280 0.8233 -0.0744 0.088 Uiso 1 1 calc R . .
C23 C 0.0737(4) 0.6633(7) -0.03886(19) 0.0621(15) Uani 1 1 d . . .
C24 C 0.1428(4) 0.6567(7) 0.02442(19) 0.0588(14) Uani 1 1 d . . .
C25 C 0.1122(5) 0.8806(7) 0.0040(2) 0.0730(18) Uani 1 1 d . . .
H25 H 0.0928 0.9566 -0.0117 0.088 Uiso 1 1 calc R . .
C26 C 0.1521(5) 0.8856(7) 0.0401(2) 0.0772(19) Uani 1 1 d . . .
H26 H 0.1661 0.9672 0.0545 0.093 Uiso 1 1 calc R . .
C27 C 0.2218(6) 0.7052(8) 0.0879(2) 0.085(2) Uani 1 1 d . . .
H27A H 0.1964 0.7521 0.1101 0.102 Uiso 1 1 calc R . .
H27B H 0.2851 0.7371 0.0865 0.102 Uiso 1 1 calc R . .
C28 C 0.2219(4) 0.5479(7) 0.09491(19) 0.0629(15) Uani 1 1 d . . .
C29 C 0.2498(5) 0.4812(8) 0.1285(2) 0.0748(19) Uani 1 1 d . . .
H29 H 0.2711 0.5229 0.1520 0.090 Uiso 1 1 calc R . .
C30 C 0.2652(6) 0.2167(8) 0.1461(2) 0.090(2) Uani 1 1 d . . .
H30A H 0.3256 0.1823 0.1399 0.108 Uiso 1 1 calc R . .
H30B H 0.2209 0.1415 0.1402 0.108 Uiso 1 1 calc R . .
C31 C 0.2666(6) 0.2510(8) 0.1888(2) 0.079(2) Uani 1 1 d . . .
C32 C 0.1862(6) 0.2480(9) 0.2089(3) 0.094(2) Uani 1 1 d . . .
H32 H 0.1303 0.2223 0.1960 0.112 Uiso 1 1 calc R . .
C33 C 0.1900(9) 0.2840(11) 0.2488(3) 0.117(3) Uani 1 1 d . . .
H33 H 0.1364 0.2853 0.2624 0.140 Uiso 1 1 calc R . .
C34 C 0.2741(10) 0.3174(12) 0.2677(3) 0.121(4) Uani 1 1 d . . .
H34 H 0.2776 0.3409 0.2943 0.145 Uiso 1 1 calc R . .
C35 C 0.3499(9) 0.3160(14) 0.2480(3) 0.139(4) Uani 1 1 d . . .
H35 H 0.4061 0.3372 0.2613 0.167 Uiso 1 1 calc R . .
C36 C 0.3489(7) 0.2849(11) 0.2090(3) 0.119(3) Uani 1 1 d . . .
H36 H 0.4034 0.2865 0.1961 0.142 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C6 1.820(6) . ?
Ni1 N4 1.897(5) . ?
Ni1 N1 1.947(5) . ?
Ni1 Cl1 2.1907(17) . ?
Ni2 C24 1.829(6) . ?
Ni2 N10 1.906(5) . ?
Ni2 N7 1.951(5) . ?
Ni2 Cl2 2.1878(18) . ?
P1 F12 1.492(7) . ?
P1 F4 1.526(6) . ?
P1 F2 1.533(6) . ?
P1 F1 1.556(6) . ?
P1 F3 1.562(6) . ?
P1 F5 1.565(7) . ?
P2 F6 1.505(6) . ?
P2 F11 1.506(5) . ?
P2 F8 1.515(6) . ?
P2 F10 1.520(6) . ?
P2 F7 1.589(5) . ?
P2 F9 1.591(5) . ?
N1 C1 1.339(8) . ?
N1 C5 1.343(7) . ?
N2 C6 1.359(8) . ?
N2 C7 1.382(8) . ?
N2 C5 1.399(8) . ?
N3 C6 1.335(8) . ?
N3 C8 1.378(8) . ?
N3 C9 1.436(8) . ?
N4 N5 1.351(7) . ?
N4 C10 1.360(8) . ?
N5 N6 1.330(7) . ?
N6 C11 1.338(8) . ?
N6 C12 1.487(8) . ?
N7 C19 1.341(8) . ?
N7 C23 1.359(8) . ?
N8 C24 1.343(8) . ?
N8 C23 1.396(8) . ?
N8 C25 1.398(8) . ?
N9 C24 1.320(8) . ?
N9 C26 1.393(8) . ?
N9 C27 1.442(9) . ?
N10 N11 1.331(7) . ?
N10 C28 1.355(8) . ?
N11 N12 1.323(7) . ?
N12 C29 1.352(9) . ?
N12 C30 1.485(9) . ?
C60 N14 1.493(14) . ?
N14 N15 1.150(12) . ?
C1 C2 1.392(9) . ?
C2 C3 1.374(9) . ?
C3 C4 1.372(10) . ?
C4 C5 1.386(9) . ?
C7 C8 1.336(10) . ?
C9 C10 1.494(9) . ?
C10 C11 1.354(9) . ?
C12 C13 1.478(10) . ?
C13 C14 1.353(10) . ?
C13 C18 1.387(10) . ?
C14 C15 1.374(13) . ?
C15 C16 1.331(14) . ?
C16 C17 1.347(15) . ?
C17 C18 1.408(14) . ?
C19 C20 1.378(9) . ?
C20 C21 1.388(11) . ?
C21 C22 1.377(10) . ?
C22 C23 1.379(9) . ?
C25 C26 1.326(10) . ?
C27 C28 1.503(9) . ?
C28 C29 1.346(9) . ?
C30 C31 1.493(10) . ?
C31 C36 1.379(11) . ?
C31 C32 1.391(11) . ?
C32 C33 1.400(12) . ?
C33 C34 1.382(15) . ?
C34 C35 1.326(14) . ?
C35 C36 1.359(13) . ?

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
C6 Ni1 N4 87.4(2) . . ?
C6 Ni1 N1 81.7(2) . . ?
N4 Ni1 N1 169.1(2) . . ?
C6 Ni1 Cl1 175.3(2) . . ?
N4 Ni1 Cl1 96.64(15) . . ?
N1 Ni1 Cl1 94.20(15) . . ?
C24 Ni2 N10 87.9(3) . . ?
C24 Ni2 N7 81.8(3) . . ?
N10 Ni2 N7 169.6(2) . . ?
C24 Ni2 Cl2 175.9(2) . . ?
N10 Ni2 Cl2 96.18(16) . . ?
N7 Ni2 Cl2 94.11(16) . . ?
F12 P1 F4 89.1(6) . . ?
F12 P1 F2 96.2(6) . . ?
F4 P1 F2 174.1(5) . . ?
F12 P1 F1 91.4(5) . . ?
F4 P1 F1 88.7(4) . . ?
F2 P1 F1 88.7(4) . . ?
F12 P1 F3 91.3(5) . . ?
F4 P1 F3 87.4(4) . . ?
F2 P1 F3 94.9(4) . . ?
F1 P1 F3 175.3(5) . . ?
F12 P1 F5 178.8(5) . . ?
F4 P1 F5 90.3(5) . . ?
F2 P1 F5 84.4(5) . . ?
F1 P1 F5 89.6(4) . . ?
F3 P1 F5 87.7(4) . . ?
F6 P2 F11 90.2(6) . . ?
F6 P2 F8 178.7(7) . . ?
F11 P2 F8 91.1(6) . . ?
F6 P2 F10 92.6(6) . . ?
F11 P2 F10 177.1(7) . . ?
F8 P2 F10 86.1(6) . . ?
F6 P2 F7 89.9(3) . . ?
F11 P2 F7 89.7(3) . . ?
F8 P2 F7 90.2(3) . . ?
F10 P2 F7 91.0(4) . . ?
F6 P2 F9 90.4(3) . . ?
F11 P2 F9 88.8(3) . . ?
F8 P2 F9 89.5(3) . . ?
F10 P2 F9 90.6(3) . . ?
F7 P2 F9 178.4(3) . . ?
C1 N1 C5 117.5(6) . . ?
C1 N1 Ni1 127.8(4) . . ?
C5 N1 Ni1 114.7(4) . . ?
C6 N2 C7 111.1(6) . . ?
C6 N2 C5 114.6(5) . . ?
C7 N2 C5 134.1(6) . . ?
C6 N3 C8 110.4(6) . . ?
C6 N3 C9 123.2(5) . . ?
C8 N3 C9 126.2(6) . . ?
N5 N4 C10 109.3(5) . . ?
N5 N4 Ni1 120.9(4) . . ?
C10 N4 Ni1 129.8(4) . . ?
N6 N5 N4 104.9(5) . . ?
N5 N6 C11 112.5(6) . . ?
N5 N6 C12 119.4(6) . . ?
C11 N6 C12 128.1(6) . . ?
C19 N7 C23 117.3(6) . . ?
C19 N7 Ni2 128.3(5) . . ?
C23 N7 Ni2 114.4(4) . . ?
C24 N8 C23 116.0(5) . . ?
C24 N8 C25 111.0(6) . . ?
C23 N8 C25 132.9(6) . . ?
C24 N9 C26 110.3(6) . . ?
C24 N9 C27 123.1(5) . . ?
C26 N9 C27 125.9(6) . . ?
N11 N10 C28 110.9(5) . . ?
N11 N10 Ni2 120.1(4) . . ?
C28 N10 Ni2 128.7(4) . . ?
N12 N11 N10 104.8(5) . . ?
N11 N12 C29 111.8(6) . . ?
N11 N12 C30 117.8(6) . . ?
C29 N12 C30 130.2(6) . . ?
N15 N14 C60 178.3(13) . . ?
N1 C1 C2 121.4(6) . . ?
C3 C2 C1 120.0(7) . . ?
C2 C3 C4 119.3(7) . . ?
C3 C4 C5 117.5(6) . . ?
N1 C5 C4 124.3(6) . . ?
N1 C5 N2 111.9(6) . . ?
C4 C5 N2 123.8(6) . . ?
N3 C6 N2 104.8(5) . . ?
N3 C6 Ni1 137.9(5) . . ?
N2 C6 Ni1 116.9(5) . . ?
C8 C7 N2 105.4(6) . . ?
C7 C8 N3 108.3(6) . . ?
N3 C9 C10 114.3(5) . . ?
C11 C10 N4 107.7(6) . . ?
C11 C10 C9 125.8(6) . . ?
N4 C10 C9 126.4(6) . . ?
N6 C11 C10 105.6(6) . . ?
C13 C12 N6 111.8(6) . . ?
C14 C13 C18 117.6(8) . . ?
C14 C13 C12 121.7(7) . . ?
C18 C13 C12 120.6(7) . . ?
C13 C14 C15 122.1(9) . . ?
C16 C15 C14 119.3(11) . . ?
C15 C16 C17 122.4(11) . . ?
C16 C17 C18 118.2(10) . . ?
C13 C18 C17 120.4(10) . . ?
N7 C19 C20 122.3(7) . . ?
C19 C20 C21 119.3(7) . . ?
C22 C21 C20 119.6(7) . . ?
C23 C22 C21 117.6(7) . . ?
N7 C23 C22 123.9(6) . . ?
N7 C23 N8 111.2(5) . . ?
C22 C23 N8 125.0(6) . . ?
N9 C24 N8 105.5(6) . . ?
N9 C24 Ni2 137.8(5) . . ?
N8 C24 Ni2 116.6(5) . . ?
C26 C25 N8 105.1(6) . . ?
C25 C26 N9 107.9(6) . . ?
N9 C27 C28 113.5(6) . . ?
C29 C28 N10 106.5(6) . . ?
C29 C28 C27 126.5(6) . . ?
N10 C28 C27 126.9(6) . . ?
C28 C29 N12 105.9(6) . . ?
N12 C30 C31 112.4(6) . . ?
C36 C31 C32 119.0(8) . . ?
C36 C31 C30 119.9(9) . . ?
C32 C31 C30 121.1(7) . . ?
C31 C32 C33 119.4(9) . . ?
C34 C33 C32 119.3(10) . . ?
C35 C34 C33 119.8(10) . . ?
C34 C35 C36 122.7(11) . . ?
C35 C36 C31 119.7(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 Ni1 N1 C1 -177.6(5) . . . . ?
N4 Ni1 N1 C1 -172.9(10) . . . . ?
Cl1 Ni1 N1 C1 4.8(5) . . . . ?
C6 Ni1 N1 C5 1.2(5) . . . . ?
N4 Ni1 N1 C5 5.9(13) . . . . ?
Cl1 Ni1 N1 C5 -176.5(4) . . . . ?
C6 Ni1 N4 N5 174.6(5) . . . . ?
N1 Ni1 N4 N5 170.0(9) . . . . ?
Cl1 Ni1 N4 N5 -7.7(4) . . . . ?
C6 Ni1 N4 C10 -3.2(6) . . . . ?
N1 Ni1 N4 C10 -7.8(14) . . . . ?
Cl1 Ni1 N4 C10 174.6(5) . . . . ?
C10 N4 N5 N6 -0.3(7) . . . . ?
Ni1 N4 N5 N6 -178.5(4) . . . . ?
N4 N5 N6 C11 0.1(7) . . . . ?
N4 N5 N6 C12 -178.5(5) . . . . ?
C24 Ni2 N7 C19 180.0(5) . . . . ?
N10 Ni2 N7 C19 -170.3(10) . . . . ?
Cl2 Ni2 N7 C19 0.0(5) . . . . ?
C24 Ni2 N7 C23 0.6(4) . . . . ?
N10 Ni2 N7 C23 10.3(14) . . . . ?
Cl2 Ni2 N7 C23 -179.4(4) . . . . ?
C24 Ni2 N10 N11 172.3(5) . . . . ?
N7 Ni2 N10 N11 162.6(10) . . . . ?
Cl2 Ni2 N10 N11 -7.6(5) . . . . ?
C24 Ni2 N10 C28 -1.1(6) . . . . ?
N7 Ni2 N10 C28 -10.8(15) . . . . ?
Cl2 Ni2 N10 C28 179.0(5) . . . . ?
C28 N10 N11 N12 0.5(7) . . . . ?
Ni2 N10 N11 N12 -174.0(4) . . . . ?
N10 N11 N12 C29 -1.4(7) . . . . ?
N10 N11 N12 C30 -176.7(6) . . . . ?
C5 N1 C1 C2 2.3(9) . . . . ?
Ni1 N1 C1 C2 -179.0(5) . . . . ?
N1 C1 C2 C3 -0.9(11) . . . . ?
C1 C2 C3 C4 -0.9(11) . . . . ?
C2 C3 C4 C5 1.2(11) . . . . ?
C1 N1 C5 C4 -2.0(9) . . . . ?
Ni1 N1 C5 C4 179.1(5) . . . . ?
C1 N1 C5 N2 178.4(5) . . . . ?
Ni1 N1 C5 N2 -0.5(7) . . . . ?
C3 C4 C5 N1 0.2(10) . . . . ?
C3 C4 C5 N2 179.7(6) . . . . ?
C6 N2 C5 N1 -0.9(8) . . . . ?
C7 N2 C5 N1 174.2(7) . . . . ?
C6 N2 C5 C4 179.6(6) . . . . ?
C7 N2 C5 C4 -5.4(12) . . . . ?
C8 N3 C6 N2 -0.1(7) . . . . ?
C9 N3 C6 N2 -175.3(6) . . . . ?
C8 N3 C6 Ni1 172.4(6) . . . . ?
C9 N3 C6 Ni1 -2.8(11) . . . . ?
C7 N2 C6 N3 0.2(7) . . . . ?
C5 N2 C6 N3 176.3(5) . . . . ?
C7 N2 C6 Ni1 -174.2(5) . . . . ?
C5 N2 C6 Ni1 1.9(7) . . . . ?
N4 Ni1 C6 N3 7.3(7) . . . . ?
N1 Ni1 C6 N3 -173.6(7) . . . . ?
Cl1 Ni1 C6 N3 -144(2) . . . . ?
N4 Ni1 C6 N2 179.2(5) . . . . ?
N1 Ni1 C6 N2 -1.7(5) . . . . ?
Cl1 Ni1 C6 N2 28(3) . . . . ?
C6 N2 C7 C8 -0.1(8) . . . . ?
C5 N2 C7 C8 -175.3(7) . . . . ?
N2 C7 C8 N3 0.0(8) . . . . ?
C6 N3 C8 C7 0.1(8) . . . . ?
C9 N3 C8 C7 175.1(7) . . . . ?
C6 N3 C9 C10 -7.1(10) . . . . ?
C8 N3 C9 C10 178.5(6) . . . . ?
N5 N4 C10 C11 0.4(7) . . . . ?
Ni1 N4 C10 C11 178.3(4) . . . . ?
N5 N4 C10 C9 177.4(6) . . . . ?
Ni1 N4 C10 C9 -4.7(10) . . . . ?
N3 C9 C10 C11 -173.0(6) . . . . ?
N3 C9 C10 N4 10.5(10) . . . . ?
N5 N6 C11 C10 0.1(8) . . . . ?
C12 N6 C11 C10 178.6(6) . . . . ?
N4 C10 C11 N6 -0.3(8) . . . . ?
C9 C10 C11 N6 -177.3(6) . . . . ?
N5 N6 C12 C13 -105.7(7) . . . . ?
C11 N6 C12 C13 76.0(9) . . . . ?
N6 C12 C13 C14 99.6(8) . . . . ?
N6 C12 C13 C18 -83.2(9) . . . . ?
C18 C13 C14 C15 1.7(13) . . . . ?
C12 C13 C14 C15 179.0(8) . . . . ?
C13 C14 C15 C16 -1.8(17) . . . . ?
C14 C15 C16 C17 2(2) . . . . ?
C15 C16 C17 C18 -2(2) . . . . ?
C14 C13 C18 C17 -1.6(14) . . . . ?
C12 C13 C18 C17 -178.8(9) . . . . ?
C16 C17 C18 C13 1.5(18) . . . . ?
C23 N7 C19 C20 2.1(9) . . . . ?
Ni2 N7 C19 C20 -177.3(5) . . . . ?
N7 C19 C20 C21 -2.2(10) . . . . ?
C19 C20 C21 C22 1.0(11) . . . . ?
C20 C21 C22 C23 0.0(10) . . . . ?
C19 N7 C23 C22 -0.9(9) . . . . ?
Ni2 N7 C23 C22 178.5(5) . . . . ?
C19 N7 C23 N8 179.7(5) . . . . ?
Ni2 N7 C23 N8 -0.9(6) . . . . ?
C21 C22 C23 N7 -0.1(10) . . . . ?
C21 C22 C23 N8 179.2(6) . . . . ?
C24 N8 C23 N7 0.8(8) . . . . ?
C25 N8 C23 N7 176.6(6) . . . . ?
C24 N8 C23 C22 -178.6(6) . . . . ?
C25 N8 C23 C22 -2.8(11) . . . . ?
C26 N9 C24 N8 -2.1(7) . . . . ?
C27 N9 C24 N8 -173.2(6) . . . . ?
C26 N9 C24 Ni2 176.8(5) . . . . ?
C27 N9 C24 Ni2 5.7(11) . . . . ?
C23 N8 C24 N9 178.8(5) . . . . ?
C25 N8 C24 N9 2.1(7) . . . . ?
C23 N8 C24 Ni2 -0.4(7) . . . . ?
C25 N8 C24 Ni2 -177.1(4) . . . . ?
N10 Ni2 C24 N9 2.8(7) . . . . ?
N7 Ni2 C24 N9 -178.9(7) . . . . ?
Cl2 Ni2 C24 N9 -179(100) . . . . ?
N10 Ni2 C24 N8 -178.3(5) . . . . ?
N7 Ni2 C24 N8 -0.1(5) . . . . ?
Cl2 Ni2 C24 N8 0(3) . . . . ?
C24 N8 C25 C26 -1.3(8) . . . . ?
C23 N8 C25 C26 -177.3(6) . . . . ?
N8 C25 C26 N9 0.0(8) . . . . ?
C24 N9 C26 C25 1.3(8) . . . . ?
C27 N9 C26 C25 172.2(7) . . . . ?
C24 N9 C27 C28 -15.0(10) . . . . ?
C26 N9 C27 C28 175.2(6) . . . . ?
N11 N10 C28 C29 0.6(8) . . . . ?
Ni2 N10 C28 C29 174.5(4) . . . . ?
N11 N10 C28 C27 177.2(7) . . . . ?
Ni2 N10 C28 C27 -8.9(10) . . . . ?
N9 C27 C28 C29 -166.9(7) . . . . ?
N9 C27 C28 N10 17.1(11) . . . . ?
N10 C28 C29 N12 -1.4(8) . . . . ?
C27 C28 C29 N12 -178.1(7) . . . . ?
N11 N12 C29 C28 1.8(8) . . . . ?
C30 N12 C29 C28 176.4(7) . . . . ?
N11 N12 C30 C31 -160.6(7) . . . . ?
C29 N12 C30 C31 25.1(12) . . . . ?
N12 C30 C31 C36 -96.1(9) . . . . ?
N12 C30 C31 C32 84.6(10) . . . . ?
C36 C31 C32 C33 2.1(13) . . . . ?
C30 C31 C32 C33 -178.6(7) . . . . ?
C31 C32 C33 C34 -2.0(14) . . . . ?
C32 C33 C34 C35 0.4(17) . . . . ?
C33 C34 C35 C36 1(2) . . . . ?
C34 C35 C36 C31 -1(2) . . . . ?
C32 C31 C36 C35 -0.7(15) . . . . ?
C30 C31 C36 C35 -180.0(10) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        67.25
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.256
####################################################################### 
# 
# 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_exp_4492
_database_code_depnum_ccdc_archive 'CCDC 1503878'
_audit_update_record             
;
2016-09-12 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H36 F18 N12 Ni2 O P3'
_chemical_formula_weight         1229.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1870(10)
_cell_length_b                   12.8538(11)
_cell_length_c                   19.2945(17)
_cell_angle_alpha                93.155(7)
_cell_angle_beta                 98.282(8)
_cell_angle_gamma                108.215(8)
_cell_volume                     2361.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2109
_cell_measurement_theta_min      3.6250
_cell_measurement_theta_max      51.6140

_exptl_crystal_description       sheet
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1238
_exptl_absorpt_coefficient_mu    3.044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6930
_exptl_absorpt_correction_T_max  0.7306
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_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            14584
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.1423
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.64
_diffrn_reflns_theta_max         67.25
_reflns_number_total             8430
_reflns_number_gt                3636
_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)+(0.1079P)²+0.9525P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8430
_refine_ls_number_parameters     668
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.0901
_refine_ls_wR_factor_ref         0.3038
_refine_ls_wR_factor_gt          0.2089
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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 0.68768(15) 0.66051(11) 0.30556(8) 0.0568(5) Uani 1 1 d . . .
Ni2 Ni 0.63926(15) 0.85758(11) 0.20311(8) 0.0574(5) Uani 1 1 d . . .
P1 P 0.2066(3) 0.1966(2) 0.12463(14) 0.0697(7) Uani 1 1 d . . .
P2 P 0.2038(3) 0.7123(3) 0.11236(16) 0.0815(8) Uani 1 1 d . . .
P3 P 0.3608(3) 0.7466(2) 0.43770(16) 0.0757(8) Uani 1 1 d . . .
F1 F 0.2027(7) 0.0786(5) 0.1476(4) 0.101(2) Uani 1 1 d . . .
F2 F 0.0995(7) 0.2016(6) 0.1769(3) 0.095(2) Uani 1 1 d . . .
F3 F 0.2084(9) 0.3145(6) 0.1031(4) 0.118(3) Uani 1 1 d . . .
F4 F 0.3127(7) 0.1912(6) 0.0730(4) 0.099(2) Uani 1 1 d . . .
F5 F 0.3326(7) 0.2525(6) 0.1865(4) 0.114(2) Uani 1 1 d . . .
F6 F 0.0793(7) 0.1397(7) 0.0630(4) 0.129(3) Uani 1 1 d . . .
F7 F 0.0861(12) 0.6590(10) 0.1525(5) 0.219(6) Uani 1 1 d . . .
F8 F 0.1623(13) 0.8177(9) 0.1205(7) 0.201(5) Uani 1 1 d . . .
F9 F 0.3176(13) 0.7728(9) 0.0714(6) 0.203(5) Uani 1 1 d . . .
F10 F 0.2497(13) 0.6110(8) 0.1028(6) 0.198(5) Uani 1 1 d . . .
F11 F 0.3059(10) 0.7585(9) 0.1829(5) 0.184(4) Uani 1 1 d . . .
F12 F 0.1006(9) 0.6677(10) 0.0429(5) 0.191(5) Uani 1 1 d . . .
F13 F 0.2971(11) 0.6168(6) 0.4204(5) 0.153(4) Uani 1 1 d . . .
F14 F 0.3636(10) 0.7333(6) 0.5174(3) 0.140(3) Uani 1 1 d . . .
F15 F 0.4281(14) 0.8695(6) 0.4566(5) 0.204(6) Uani 1 1 d . . .
F16 F 0.3512(9) 0.7565(7) 0.3558(4) 0.136(3) Uani 1 1 d . . .
F17 F 0.5050(8) 0.7325(10) 0.4374(6) 0.193(5) Uani 1 1 d . . .
F18 F 0.2081(10) 0.7471(11) 0.4330(6) 0.196(5) Uani 1 1 d . . .
N1 N 0.5145(8) 0.5503(6) 0.3135(4) 0.0606(19) Uani 1 1 d . . .
N2 N 0.7472(8) 0.5116(6) 0.3986(4) 0.066(2) Uani 1 1 d . . .
N3 N 0.9123(8) 0.5669(6) 0.3381(4) 0.0591(18) Uani 1 1 d . . .
N4 N 0.8633(8) 0.7619(6) 0.2965(4) 0.062(2) Uani 1 1 d . . .
N5 N 0.8869(8) 0.8692(6) 0.2997(4) 0.067(2) Uani 1 1 d . . .
N6 N 1.0193(9) 0.9138(6) 0.2928(4) 0.068(2) Uani 1 1 d . . .
N7 N 0.5962(8) 0.9672(5) 0.2579(4) 0.064(2) Uani 1 1 d . . .
N8 N 0.6119(8) 1.0261(6) 0.1175(4) 0.0617(19) Uani 1 1 d . . .
N9 N 0.7685(8) 0.9611(7) 0.0905(4) 0.069(2) Uani 1 1 d . . .
N10 N 0.6866(8) 0.7551(6) 0.1463(4) 0.0593(18) Uani 1 1 d . . .
N11 N 0.6242(8) 0.6480(6) 0.1433(4) 0.067(2) Uani 1 1 d . . .
N12 N 0.6755(10) 0.6018(7) 0.0951(5) 0.080(3) Uani 1 1 d . . .
O1 O 0.5930(6) 0.7572(4) 0.2714(3) 0.0612(16) Uani 1 1 d . . .
C1 C 0.4060(9) 0.5348(7) 0.2605(4) 0.055(2) Uani 1 1 d . . .
H1 H 0.4190 0.5770 0.2229 0.066 Uiso 1 1 calc R . .
C2 C 0.2760(11) 0.4580(8) 0.2605(6) 0.074(3) Uani 1 1 d . . .
H2 H 0.2014 0.4519 0.2248 0.089 Uiso 1 1 calc R . .
C3 C 0.2578(12) 0.3910(9) 0.3136(7) 0.090(4) Uani 1 1 d . . .
H3 H 0.1716 0.3379 0.3139 0.108 Uiso 1 1 calc R . .
C4 C 0.3709(12) 0.4040(8) 0.3673(6) 0.080(3) Uani 1 1 d . . .
H4 H 0.3617 0.3585 0.4033 0.096 Uiso 1 1 calc R . .
C5 C 0.4968(10) 0.4851(6) 0.3662(5) 0.059(2) Uani 1 1 d . . .
C6 C 0.6198(11) 0.5054(8) 0.4254(5) 0.075(3) Uani 1 1 d . . .
H6A H 0.6333 0.5738 0.4537 0.090 Uiso 1 1 calc R . .
H6B H 0.5994 0.4463 0.4554 0.090 Uiso 1 1 calc R . .
C7 C 0.8491(12) 0.4630(9) 0.4200(6) 0.088(3) Uani 1 1 d . . .
H7 H 0.8453 0.4144 0.4542 0.106 Uiso 1 1 calc R . .
C8 C 0.9535(12) 0.4982(8) 0.3829(6) 0.079(3) Uani 1 1 d . . .
H8 H 1.0358 0.4802 0.3866 0.095 Uiso 1 1 calc R . .
C9 C 0.7875(10) 0.5743(7) 0.3471(5) 0.059(2) Uani 1 1 d . . .
C10 C 0.9869(11) 0.6221(7) 0.2847(5) 0.070(3) Uani 1 1 d . . .
H10A H 0.9418 0.5846 0.2383 0.084 Uiso 1 1 calc R . .
H10B H 1.0828 0.6214 0.2928 0.084 Uiso 1 1 calc R . .
C11 C 0.9851(9) 0.7376(8) 0.2893(4) 0.060(2) Uani 1 1 d . . .
C12 C 1.0836(11) 0.8349(8) 0.2839(5) 0.074(3) Uani 1 1 d . . .
H12 H 1.1747 0.8462 0.2759 0.089 Uiso 1 1 calc R . .
C13 C 1.0837(12) 1.0335(8) 0.2969(6) 0.083(3) Uani 1 1 d . . .
H13A H 1.0336 1.0620 0.2600 0.099 Uiso 1 1 calc R . .
H13B H 1.1801 1.0510 0.2895 0.099 Uiso 1 1 calc R . .
C14 C 1.0805(10) 1.0872(8) 0.3668(6) 0.067(2) Uani 1 1 d . . .
C15 C 0.9859(13) 1.1422(9) 0.3723(7) 0.093(4) Uani 1 1 d . . .
H15 H 0.9247 1.1450 0.3323 0.112 Uiso 1 1 calc R . .
C16 C 0.9797(17) 1.1939(11) 0.4365(11) 0.124(5) Uani 1 1 d . . .
H16 H 0.9165 1.2320 0.4400 0.149 Uiso 1 1 calc R . .
C17 C 1.067(2) 1.1867(14) 0.4925(9) 0.138(7) Uani 1 1 d . . .
H17 H 1.0600 1.2186 0.5356 0.166 Uiso 1 1 calc R . .
C18 C 1.1651(18) 1.1376(16) 0.4923(9) 0.144(7) Uani 1 1 d . . .
H18 H 1.2265 1.1366 0.5328 0.173 Uiso 1 1 calc R . .
C19 C 1.1680(13) 1.0880(12) 0.4266(8) 0.108(4) Uani 1 1 d . . .
H19 H 1.2348 1.0532 0.4238 0.129 Uiso 1 1 calc R . .
C20 C 0.6273(10) 0.9744(7) 0.3291(5) 0.066(3) Uani 1 1 d . . .
H20 H 0.6738 0.9285 0.3488 0.079 Uiso 1 1 calc R . .
C21 C 0.5942(11) 1.0455(8) 0.3738(6) 0.073(3) Uani 1 1 d . . .
H21 H 0.6207 1.0494 0.4223 0.088 Uiso 1 1 calc R . .
C22 C 0.5210(10) 1.1108(8) 0.3454(6) 0.077(3) Uani 1 1 d . . .
H22 H 0.4923 1.1571 0.3740 0.092 Uiso 1 1 calc R . .
C23 C 0.4911(10) 1.1057(8) 0.2727(6) 0.074(3) Uani 1 1 d . . .
H23 H 0.4430 1.1500 0.2520 0.089 Uiso 1 1 calc R . .
C24 C 0.5324(9) 1.0350(7) 0.2304(5) 0.057(2) Uani 1 1 d . . .
C25 C 0.4950(10) 1.0362(8) 0.1523(5) 0.065(2) Uani 1 1 d . . .
H25A H 0.4102 0.9755 0.1339 0.078 Uiso 1 1 calc R . .
H25B H 0.4776 1.1045 0.1427 0.078 Uiso 1 1 calc R . .
C26 C 0.6597(11) 1.0776(8) 0.0619(5) 0.072(3) Uani 1 1 d . . .
H26 H 0.6292 1.1308 0.0403 0.086 Uiso 1 1 calc R . .
C27 C 0.7599(11) 1.0374(8) 0.0434(5) 0.073(3) Uani 1 1 d . . .
H27 H 0.8111 1.0567 0.0072 0.088 Uiso 1 1 calc R . .
C28 C 0.6754(10) 0.9517(7) 0.1355(5) 0.059(2) Uani 1 1 d . . .
C29 C 0.8608(10) 0.8949(9) 0.0908(5) 0.074(3) Uani 1 1 d . . .
H29A H 0.9395 0.9238 0.1291 0.089 Uiso 1 1 calc R . .
H29B H 0.8971 0.8975 0.0469 0.089 Uiso 1 1 calc R . .
C30 C 0.7791(10) 0.7767(9) 0.0997(5) 0.063(2) Uani 1 1 d . . .
C31 C 0.7733(14) 0.6767(10) 0.0667(6) 0.091(4) Uani 1 1 d . . .
H31 H 0.8246 0.6639 0.0329 0.110 Uiso 1 1 calc R . .
C32 C 0.6243(12) 0.4799(8) 0.0770(6) 0.091(4) Uani 1 1 d . . .
H32A H 0.6318 0.4631 0.0284 0.109 Uiso 1 1 calc R . .
H32B H 0.5262 0.4512 0.0814 0.109 Uiso 1 1 calc R . .
C33 C 0.7066(10) 0.4243(7) 0.1240(5) 0.064(2) Uani 1 1 d . . .
C34 C 0.6635(13) 0.3922(10) 0.1857(6) 0.090(3) Uani 1 1 d . . .
H34 H 0.5858 0.4058 0.1991 0.108 Uiso 1 1 calc R . .
C35 C 0.7404(18) 0.3380(11) 0.2284(7) 0.106(5) Uani 1 1 d . . .
H35 H 0.7149 0.3159 0.2710 0.128 Uiso 1 1 calc R . .
C36 C 0.852(2) 0.3184(11) 0.2062(10) 0.122(6) Uani 1 1 d . . .
H36 H 0.9022 0.2813 0.2336 0.146 Uiso 1 1 calc R . .
C37 C 0.8924(14) 0.3517(11) 0.1456(10) 0.112(5) Uani 1 1 d . . .
H37 H 0.9692 0.3376 0.1314 0.134 Uiso 1 1 calc R . .
C38 C 0.8204(13) 0.4064(9) 0.1045(7) 0.090(3) Uani 1 1 d . . .
H38 H 0.8501 0.4312 0.0632 0.108 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C9 1.863(9) . ?
Ni1 O1 1.889(5) . ?
Ni1 N4 1.894(7) . ?
Ni1 N1 1.919(8) . ?
Ni2 C28 1.825(8) . ?
Ni2 N10 1.887(7) . ?
Ni2 O1 1.900(6) . ?
Ni2 N7 1.911(8) . ?
P1 F5 1.574(6) . ?
P1 F6 1.580(6) . ?
P1 F4 1.585(6) . ?
P1 F3 1.588(7) . ?
P1 F1 1.594(6) . ?
P1 F2 1.602(6) . ?
P2 F7 1.523(8) . ?
P2 F10 1.526(9) . ?
P2 F9 1.530(9) . ?
P2 F12 1.538(8) . ?
P2 F8 1.546(10) . ?
P2 F11 1.550(8) . ?
P3 F15 1.512(8) . ?
P3 F17 1.536(9) . ?
P3 F18 1.547(9) . ?
P3 F14 1.554(7) . ?
P3 F16 1.583(7) . ?
P3 F13 1.586(8) . ?
N1 C5 1.349(11) . ?
N1 C1 1.349(10) . ?
N2 C9 1.344(11) . ?
N2 C7 1.396(12) . ?
N2 C6 1.446(12) . ?
N3 C9 1.339(11) . ?
N3 C8 1.384(11) . ?
N3 C10 1.452(11) . ?
N4 N5 1.320(9) . ?
N4 C11 1.394(11) . ?
N5 N6 1.320(10) . ?
N6 C12 1.384(13) . ?
N6 C13 1.465(11) . ?
N7 C24 1.330(10) . ?
N7 C20 1.355(11) . ?
N8 C28 1.347(11) . ?
N8 C26 1.361(12) . ?
N8 C25 1.485(11) . ?
N9 C28 1.358(11) . ?
N9 C27 1.387(11) . ?
N9 C29 1.452(12) . ?
N10 N11 1.317(10) . ?
N10 C30 1.372(11) . ?
N11 N12 1.329(11) . ?
N12 C31 1.355(15) . ?
N12 C32 1.491(12) . ?
C1 C2 1.383(12) . ?
C2 C3 1.370(15) . ?
C3 C4 1.394(15) . ?
C4 C5 1.381(12) . ?
C5 C6 1.514(12) . ?
C7 C8 1.343(15) . ?
C10 C11 1.488(12) . ?
C11 C12 1.358(12) . ?
C13 C14 1.490(14) . ?
C14 C19 1.349(15) . ?
C14 C15 1.374(15) . ?
C15 C16 1.392(18) . ?
C16 C17 1.33(2) . ?
C17 C18 1.34(2) . ?
C18 C19 1.40(2) . ?
C20 C21 1.373(13) . ?
C21 C22 1.373(14) . ?
C22 C23 1.385(13) . ?
C23 C24 1.387(12) . ?
C24 C25 1.501(12) . ?
C26 C27 1.361(14) . ?
C29 C30 1.520(13) . ?
C30 C31 1.383(14) . ?
C32 C33 1.504(13) . ?
C33 C38 1.349(13) . ?
C33 C34 1.368(14) . ?
C34 C35 1.414(18) . ?
C35 C36 1.36(2) . ?
C36 C37 1.34(2) . ?
C37 C38 1.369(17) . ?

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
C9 Ni1 O1 174.5(3) . . ?
C9 Ni1 N4 86.9(4) . . ?
O1 Ni1 N4 91.4(3) . . ?
C9 Ni1 N1 90.2(4) . . ?
O1 Ni1 N1 91.7(3) . . ?
N4 Ni1 N1 176.3(3) . . ?
C28 Ni2 N10 88.2(4) . . ?
C28 Ni2 O1 177.4(3) . . ?
N10 Ni2 O1 91.9(3) . . ?
C28 Ni2 N7 89.0(4) . . ?
N10 Ni2 N7 177.0(3) . . ?
O1 Ni2 N7 90.9(3) . . ?
F5 P1 F6 179.4(5) . . ?
F5 P1 F4 90.6(4) . . ?
F6 P1 F4 89.8(4) . . ?
F5 P1 F3 90.1(4) . . ?
F6 P1 F3 90.3(5) . . ?
F4 P1 F3 90.8(4) . . ?
F5 P1 F1 89.7(4) . . ?
F6 P1 F1 89.9(4) . . ?
F4 P1 F1 90.6(4) . . ?
F3 P1 F1 178.6(4) . . ?
F5 P1 F2 89.4(4) . . ?
F6 P1 F2 90.2(4) . . ?
F4 P1 F2 179.8(4) . . ?
F3 P1 F2 89.4(4) . . ?
F1 P1 F2 89.2(4) . . ?
F7 P2 F10 95.8(7) . . ?
F7 P2 F9 175.8(8) . . ?
F10 P2 F9 88.3(7) . . ?
F7 P2 F12 89.2(6) . . ?
F10 P2 F12 87.1(6) . . ?
F9 P2 F12 90.1(7) . . ?
F7 P2 F8 86.6(8) . . ?
F10 P2 F8 177.6(8) . . ?
F9 P2 F8 89.3(7) . . ?
F12 P2 F8 93.1(7) . . ?
F7 P2 F11 90.3(6) . . ?
F10 P2 F11 93.9(6) . . ?
F9 P2 F11 90.4(7) . . ?
F12 P2 F11 178.9(6) . . ?
F8 P2 F11 86.0(6) . . ?
F15 P3 F17 91.0(7) . . ?
F15 P3 F18 95.5(7) . . ?
F17 P3 F18 173.2(6) . . ?
F15 P3 F14 88.7(5) . . ?
F17 P3 F14 94.0(6) . . ?
F18 P3 F14 88.2(6) . . ?
F15 P3 F16 93.0(5) . . ?
F17 P3 F16 87.7(6) . . ?
F18 P3 F16 89.9(5) . . ?
F14 P3 F16 177.5(5) . . ?
F15 P3 F13 177.0(7) . . ?
F17 P3 F13 86.6(6) . . ?
F18 P3 F13 87.1(6) . . ?
F14 P3 F13 89.7(4) . . ?
F16 P3 F13 88.6(5) . . ?
C5 N1 C1 118.7(8) . . ?
C5 N1 Ni1 124.5(6) . . ?
C1 N1 Ni1 116.7(6) . . ?
C9 N2 C7 108.6(9) . . ?
C9 N2 C6 121.6(8) . . ?
C7 N2 C6 129.8(9) . . ?
C9 N3 C8 111.5(9) . . ?
C9 N3 C10 121.8(8) . . ?
C8 N3 C10 126.6(9) . . ?
N5 N4 C11 110.6(7) . . ?
N5 N4 Ni1 122.6(7) . . ?
C11 N4 Ni1 126.7(6) . . ?
N6 N5 N4 106.1(8) . . ?
N5 N6 C12 111.8(8) . . ?
N5 N6 C13 121.0(9) . . ?
C12 N6 C13 127.1(9) . . ?
C24 N7 C20 117.5(8) . . ?
C24 N7 Ni2 123.7(7) . . ?
C20 N7 Ni2 118.7(6) . . ?
C28 N8 C26 111.5(9) . . ?
C28 N8 C25 120.5(7) . . ?
C26 N8 C25 127.7(8) . . ?
C28 N9 C27 112.0(8) . . ?
C28 N9 C29 123.1(8) . . ?
C27 N9 C29 124.9(9) . . ?
N11 N10 C30 109.8(8) . . ?
N11 N10 Ni2 122.4(6) . . ?
C30 N10 Ni2 127.7(7) . . ?
N10 N11 N12 106.3(8) . . ?
N11 N12 C31 112.6(9) . . ?
N11 N12 C32 120.5(10) . . ?
C31 N12 C32 126.9(11) . . ?
Ni1 O1 Ni2 128.2(3) . . ?
N1 C1 C2 121.9(9) . . ?
C3 C2 C1 119.5(10) . . ?
C2 C3 C4 118.8(10) . . ?
C5 C4 C3 119.2(10) . . ?
N1 C5 C4 121.7(9) . . ?
N1 C5 C6 117.5(8) . . ?
C4 C5 C6 120.8(9) . . ?
N2 C6 C5 111.5(8) . . ?
C8 C7 N2 108.5(10) . . ?
C7 C8 N3 105.1(10) . . ?
N3 C9 N2 106.3(8) . . ?
N3 C9 Ni1 130.0(7) . . ?
N2 C9 Ni1 123.5(7) . . ?
N3 C10 C11 108.1(8) . . ?
C12 C11 N4 106.2(9) . . ?
C12 C11 C10 132.4(10) . . ?
N4 C11 C10 121.4(8) . . ?
C11 C12 N6 105.2(9) . . ?
N6 C13 C14 110.9(9) . . ?
C19 C14 C15 116.3(12) . . ?
C19 C14 C13 124.2(11) . . ?
C15 C14 C13 119.5(11) . . ?
C14 C15 C16 121.5(14) . . ?
C17 C16 C15 117.4(16) . . ?
C16 C17 C18 125.6(19) . . ?
C17 C18 C19 114.6(15) . . ?
C14 C19 C18 124.5(14) . . ?
N7 C20 C21 123.8(9) . . ?
C20 C21 C22 118.5(10) . . ?
C21 C22 C23 118.0(10) . . ?
C22 C23 C24 120.5(10) . . ?
N7 C24 C23 121.4(9) . . ?
N7 C24 C25 122.5(8) . . ?
C23 C24 C25 116.1(8) . . ?
N8 C25 C24 109.5(7) . . ?
N8 C26 C27 108.0(9) . . ?
C26 C27 N9 104.6(9) . . ?
N8 C28 N9 103.9(8) . . ?
N8 C28 Ni2 127.5(8) . . ?
N9 C28 Ni2 128.6(7) . . ?
N9 C29 C30 109.1(8) . . ?
N10 C30 C31 107.4(10) . . ?
N10 C30 C29 120.2(9) . . ?
C31 C30 C29 132.3(10) . . ?
N12 C31 C30 103.9(11) . . ?
N12 C32 C33 111.9(8) . . ?
C38 C33 C34 121.3(11) . . ?
C38 C33 C32 119.7(11) . . ?
C34 C33 C32 119.0(11) . . ?
C33 C34 C35 118.2(12) . . ?
C36 C35 C34 119.0(13) . . ?
C37 C36 C35 121.2(14) . . ?
C36 C37 C38 120.2(14) . . ?
C33 C38 C37 120.0(13) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        67.25
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.092
####################################################################### 
# 
# 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_130516_130405
_database_code_depnum_ccdc_archive 'CCDC 1503881'
_audit_update_record             
;
2016-09-12 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H37 F12 N15 Ni P2'
_chemical_formula_weight         1124.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
P P 0.1023 0.0942 '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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.6109(6)
_cell_length_b                   12.8032(6)
_cell_length_c                   15.6696(8)
_cell_angle_alpha                89.022(4)
_cell_angle_beta                 75.221(4)
_cell_angle_gamma                81.746(4)
_cell_volume                     2420.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4478
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.7853
_exptl_absorpt_correction_T_max  0.8400
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15107
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.22
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8498
_reflns_number_gt                6232
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1158P)²+3.0598P] 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         8498
_refine_ls_number_parameters     668
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0699
_refine_ls_wR_factor_ref         0.2139
_refine_ls_wR_factor_gt          0.1863
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.97592(4) 0.76618(4) 0.70285(3) 0.0385(2) Uani 1 1 d . . .
P2 P 0.41864(12) 0.61471(11) 0.31579(11) 0.0690(5) Uani 1 1 d . . .
P3 P 0.55717(14) 0.12208(18) 0.22610(12) 0.0857(6) Uani 1 1 d . . .
N10 N 1.1054(3) 0.6428(3) 0.7117(2) 0.0432(8) Uani 1 1 d . . .
N4 N 0.7629(3) 0.6803(3) 0.8024(3) 0.0482(9) Uani 1 1 d . . .
C55 C 0.8507(4) 0.7270(4) 0.7984(3) 0.0443(10) Uani 1 1 d . . .
N3 N 0.9105(3) 0.6849(3) 0.6175(2) 0.0458(9) Uani 1 1 d . . .
N12 N 1.0692(3) 0.9377(3) 0.6052(2) 0.0385(8) Uani 1 1 d . . .
N11 N 1.2044(3) 0.8107(3) 0.5921(2) 0.0404(8) Uani 1 1 d . . .
N2 N 0.9594(3) 0.6686(3) 0.5329(3) 0.0492(9) Uani 1 1 d . . .
N1 N 0.8960(4) 0.6120(3) 0.5011(3) 0.0565(11) Uani 1 1 d . . .
N9 N 1.0920(3) 0.5797(3) 0.7799(3) 0.0475(9) Uani 1 1 d . . .
N5 N 0.8435(3) 0.7603(3) 0.8816(2) 0.0454(9) Uani 1 1 d . . .
N13 N 0.8897(3) 0.9200(3) 0.6782(2) 0.0422(8) Uani 1 1 d . . .
N8 N 1.1932(3) 0.5413(3) 0.7868(3) 0.0527(10) Uani 1 1 d . . .
C21 C 0.9568(4) 0.9843(3) 0.6327(3) 0.0397(9) Uani 1 1 d . . .
N14 N 0.9323(3) 1.0825(3) 0.6108(3) 0.0525(10) Uani 1 1 d . . .
C16 C 1.0947(3) 0.8351(3) 0.6234(3) 0.0387(9) Uani 1 1 d . . .
C30 C 0.7469(4) 0.7345(4) 0.9405(3) 0.0504(12) Uani 1 1 d . . .
N6 N 1.0051(3) 0.8281(3) 0.8252(2) 0.0458(9) Uani 1 1 d . . .
C18 C 1.2507(4) 0.8985(4) 0.5504(3) 0.0440(10) Uani 1 1 d . . .
C10 C 0.8167(4) 0.6383(4) 0.6395(3) 0.0488(11) Uani 1 1 d . . .
C22 C 0.7824(4) 0.9607(4) 0.7032(3) 0.0504(11) Uani 1 1 d . . .
H22 H 0.7312 0.9191 0.7341 0.060 Uiso 1 1 calc R . .
C9 C 0.8078(5) 0.5928(4) 0.5639(4) 0.0620(14) Uani 1 1 d . . .
H9 H 0.7518 0.5559 0.5575 0.074 Uiso 1 1 calc R . .
C17 C 1.1638(4) 0.9808(4) 0.5593(3) 0.0418(10) Uani 1 1 d . . .
C20 C 1.1792(4) 1.0801(4) 0.5260(3) 0.0524(12) Uani 1 1 d . . .
H20 H 1.1212 1.1356 0.5326 0.063 Uiso 1 1 calc R . .
C13 C 1.2151(4) 0.6452(3) 0.6766(3) 0.0447(10) Uani 1 1 d . . .
C23 C 0.7463(4) 1.0618(4) 0.6842(4) 0.0604(14) Uani 1 1 d . . .
H23 H 0.6716 1.0897 0.7016 0.073 Uiso 1 1 calc R . .
C29 C 0.6962(4) 0.6818(4) 0.8896(3) 0.0547(13) Uani 1 1 d . . .
C31 C 0.7003(4) 0.7524(5) 1.0304(3) 0.0652(15) Uani 1 1 d . . .
H31 H 0.7333 0.7896 1.0646 0.078 Uiso 1 1 calc R . .
C14 C 1.2641(4) 0.7059(4) 0.5959(3) 0.0556(13) Uani 1 1 d . . .
H14A H 1.3401 0.7120 0.5950 0.067 Uiso 1 1 calc R . .
H14B H 1.2653 0.6660 0.5435 0.067 Uiso 1 1 calc R . .
C26 C 0.9309(4) 0.8065(4) 0.8981(3) 0.0492(11) Uani 1 1 d . . .
C19 C 1.2874(5) 1.0908(5) 0.4819(4) 0.0631(14) Uani 1 1 d . . .
H19 H 1.3023 1.1555 0.4576 0.076 Uiso 1 1 calc R . .
C44 C 1.2714(4) 0.5801(4) 0.7243(4) 0.0567(13) Uani 1 1 d . . .
H44 H 1.3478 0.5655 0.7157 0.068 Uiso 1 1 calc R . .
C41 C 1.3584(4) 0.9101(4) 0.5073(3) 0.0553(12) Uani 1 1 d . . .
H41 H 1.4168 0.8552 0.5017 0.066 Uiso 1 1 calc R . .
C65 C 1.2001(4) 0.5328(4) 0.9434(4) 0.0556(12) Uani 1 1 d . . .
C43 C 0.8233(5) 1.1210(4) 0.6386(4) 0.0611(14) Uani 1 1 d . . .
H43 H 0.7999 1.1905 0.6263 0.073 Uiso 1 1 calc R . .
C42 C 1.3738(5) 1.0087(5) 0.4730(3) 0.0646(15) Uani 1 1 d . . .
H42 H 1.4448 1.0202 0.4430 0.078 Uiso 1 1 calc R . .
C35 C 0.9269(6) 0.5834(5) 0.4064(4) 0.0759(17) Uani 1 1 d . . .
H35A H 0.8972 0.5196 0.3983 0.091 Uiso 1 1 calc R . .
H35B H 1.0070 0.5685 0.3861 0.091 Uiso 1 1 calc R . .
C39 C 1.0908(4) 0.8690(4) 0.8388(4) 0.0579(13) Uani 1 1 d . . .
H39 H 1.1445 0.8868 0.7902 0.069 Uiso 1 1 calc R . .
C32 C 0.5985(5) 0.6406(5) 0.9258(4) 0.0755(18) Uani 1 1 d . . .
H32 H 0.5642 0.6044 0.8920 0.091 Uiso 1 1 calc R . .
C36 C 0.8852(5) 0.6691(4) 0.3507(3) 0.0633(14) Uani 1 1 d . . .
C34 C 0.6044(5) 0.7132(6) 1.0660(4) 0.083(2) Uani 1 1 d . . .
H34 H 0.5708 0.7243 1.1259 0.100 Uiso 1 1 calc R . .
C45 C 1.2070(5) 0.4717(4) 0.8603(4) 0.0652(14) Uani 1 1 d . . .
H45A H 1.2783 0.4271 0.8431 0.078 Uiso 1 1 calc R . .
H45B H 1.1499 0.4262 0.8722 0.078 Uiso 1 1 calc R . .
C37 C 0.7368(5) 0.6336(5) 0.7280(4) 0.0730(17) Uani 1 1 d . . .
H37A H 0.6647 0.6682 0.7239 0.088 Uiso 1 1 calc R . .
H37B H 0.7302 0.5600 0.7407 0.088 Uiso 1 1 calc R . .
C40 C 1.1029(5) 0.8858(6) 0.9217(4) 0.0804(18) Uani 1 1 d . . .
H40 H 1.1635 0.9137 0.9306 0.096 Uiso 1 1 calc R . .
C33 C 0.5560(5) 0.6578(6) 1.0163(5) 0.090(2) Uani 1 1 d . . .
H33 H 0.4919 0.6303 1.0443 0.108 Uiso 1 1 calc R . .
F16 F 0.5425(3) 0.6174(4) 0.2856(5) 0.150(2) Uani 1 1 d . . .
C60 C 1.1326(4) 0.5083(4) 1.0222(4) 0.0609(14) Uani 1 1 d . . .
H60 H 1.0890 0.4552 1.0241 0.073 Uiso 1 1 calc R . .
C64 C 1.2637(5) 0.6126(5) 0.9419(4) 0.0756(17) Uani 1 1 d . . .
H64 H 1.3097 0.6305 0.8889 0.091 Uiso 1 1 calc R . .
C63 C 1.2591(6) 0.6657(6) 1.0188(5) 0.0867(19) Uani 1 1 d . . .
H63 H 1.3021 0.7192 1.0174 0.104 Uiso 1 1 calc R . .
F5 F 0.3891(7) 0.6942(6) 0.3898(4) 0.202(3) Uani 1 1 d . . .
F2 F 0.4023(5) 0.7127(5) 0.2571(5) 0.187(3) Uani 1 1 d . . .
C48 C 0.7741(7) 0.6890(6) 0.3498(5) 0.087(2) Uani 1 1 d . . .
H48 H 0.7243 0.6476 0.3830 0.104 Uiso 1 1 calc R . .
F4 F 0.4281(5) 0.5078(5) 0.3575(6) 0.205(4) Uani 1 1 d . . .
C62 C 1.1286(5) 0.5619(5) 1.0990(4) 0.0770(17) Uani 1 1 d . . .
H62 H 1.0825 0.5444 1.1522 0.092 Uiso 1 1 calc R . .
F6 F 0.4773(6) 0.1694(6) 0.3126(5) 0.186(3) Uani 1 1 d . . .
F3 F 0.2905(4) 0.6097(5) 0.3376(6) 0.206(4) Uani 1 1 d . . .
C61 C 1.1917(6) 0.6401(6) 1.0974(5) 0.089(2) Uani 1 1 d . . .
H61 H 1.1890 0.6760 1.1492 0.106 Uiso 1 1 calc R . .
C47 C 0.9573(6) 0.7302(5) 0.3006(4) 0.0804(18) Uani 1 1 d . . .
H47 H 1.0319 0.7169 0.2999 0.096 Uiso 1 1 calc R . .
F9 F 0.6396(6) 0.0634(8) 0.1450(4) 0.217(4) Uani 1 1 d . . .
F8 F 0.4610(5) 0.1313(6) 0.1803(5) 0.187(3) Uani 1 1 d . . .
F7 F 0.5238(7) 0.0143(5) 0.2587(6) 0.199(3) Uani 1 1 d . . .
F30 F 0.6512(6) 0.1112(9) 0.2709(5) 0.238(5) Uani 1 1 d . . .
F1 F 0.4342(9) 0.5478(7) 0.2313(5) 0.232(4) Uani 1 1 d . . .
F20 F 0.5781(8) 0.2314(8) 0.1946(7) 0.251(5) Uani 1 1 d . . .
C49 C 0.7371(8) 0.7690(7) 0.3006(6) 0.107(3) Uani 1 1 d . . .
H49 H 0.6627 0.7826 0.3006 0.128 Uiso 1 1 calc R . .
C51 C 0.9213(9) 0.8103(7) 0.2517(5) 0.106(3) Uani 1 1 d . . .
H51 H 0.9713 0.8518 0.2190 0.127 Uiso 1 1 calc R . .
C50 C 0.8131(11) 0.8297(7) 0.2506(5) 0.114(3) Uani 1 1 d . . .
H50 H 0.7895 0.8837 0.2163 0.136 Uiso 1 1 calc R . .
C70 C 1.0218(6) 0.8595(6) 0.9902(4) 0.085(2) Uani 1 1 d . . .
H70 H 1.0283 0.8697 1.0472 0.102 Uiso 1 1 calc R . .
N7 N 0.9331(4) 0.8197(4) 0.9805(3) 0.0693(13) Uani 1 1 d . . .
N17 N 0.1698(7) 0.9506(7) 0.1127(6) 0.126(3) Uani 1 1 d . . .
C74 C 0.2606(9) 0.9474(6) 0.0911(6) 0.099(3) Uani 1 1 d . . .
C76 C 0.3765(9) 0.9468(10) 0.0644(7) 0.156(4) Uani 1 1 d . . .
H76A H 0.3945 1.0107 0.0847 0.234 Uiso 1 1 calc R . .
H76B H 0.4010 0.9420 0.0011 0.234 Uiso 1 1 calc R . .
H76C H 0.4128 0.8872 0.0891 0.234 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C16 1.991(4) . ?
Ni1 C55 1.996(4) . ?
Ni1 N3 2.100(4) . ?
Ni1 N10 2.132(4) . ?
Ni1 N13 2.186(4) . ?
Ni1 N6 2.221(4) . ?
P2 F5 1.493(6) . ?
P2 F4 1.509(5) . ?
P2 F16 1.518(4) . ?
P2 F1 1.544(7) . ?
P2 F2 1.564(5) . ?
P2 F3 1.574(5) . ?
P3 F20 1.513(7) . ?
P3 F30 1.513(6) . ?
P3 F6 1.540(6) . ?
P3 F7 1.541(6) . ?
P3 F9 1.548(7) . ?
P3 F8 1.550(6) . ?
N10 N9 1.319(5) . ?
N10 C13 1.357(6) . ?
N4 C55 1.319(6) . ?
N4 C29 1.409(6) . ?
N4 C37 1.449(7) . ?
C55 N5 1.356(6) . ?
N3 N2 1.318(5) . ?
N3 C10 1.364(6) . ?
N12 C16 1.350(5) . ?
N12 C17 1.408(5) . ?
N12 C21 1.417(5) . ?
N11 C16 1.337(5) . ?
N11 C18 1.414(5) . ?
N11 C14 1.449(6) . ?
N2 N1 1.340(5) . ?
N1 C9 1.333(7) . ?
N1 C35 1.473(7) . ?
N9 N8 1.331(5) . ?
N5 C26 1.403(6) . ?
N5 C30 1.406(6) . ?
N13 C21 1.332(6) . ?
N13 C22 1.339(6) . ?
N8 C44 1.345(6) . ?
N8 C45 1.475(6) . ?
C21 N14 1.312(6) . ?
N14 C43 1.353(7) . ?
C30 C29 1.380(7) . ?
C30 C31 1.391(7) . ?
N6 C39 1.331(6) . ?
N6 C26 1.332(6) . ?
C18 C41 1.383(6) . ?
C18 C17 1.388(6) . ?
C10 C9 1.367(7) . ?
C10 C37 1.498(7) . ?
C22 C23 1.363(7) . ?
C17 C20 1.387(6) . ?
C20 C19 1.388(7) . ?
C13 C44 1.355(7) . ?
C13 C14 1.513(6) . ?
C23 C43 1.366(8) . ?
C29 C32 1.392(7) . ?
C31 C34 1.359(8) . ?
C26 N7 1.313(6) . ?
C19 C42 1.382(8) . ?
C41 C42 1.383(7) . ?
C65 C60 1.370(7) . ?
C65 C64 1.384(8) . ?
C65 C45 1.507(8) . ?
C35 C36 1.509(8) . ?
C39 C40 1.370(8) . ?
C32 C33 1.392(10) . ?
C36 C47 1.369(8) . ?
C36 C48 1.390(9) . ?
C34 C33 1.367(10) . ?
C40 C70 1.355(9) . ?
C60 C62 1.381(9) . ?
C64 C63 1.377(9) . ?
C63 C61 1.371(10) . ?
C48 C49 1.371(10) . ?
C62 C61 1.362(9) . ?
C47 C51 1.364(11) . ?
C49 C50 1.396(13) . ?
C51 C50 1.356(13) . ?
C70 N7 1.337(8) . ?
N17 C74 1.104(11) . ?
C74 C76 1.412(13) . ?

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
C16 Ni1 C55 167.14(18) . . ?
C16 Ni1 N3 104.75(16) . . ?
C55 Ni1 N3 85.54(17) . . ?
C16 Ni1 N10 85.74(16) . . ?
C55 Ni1 N10 100.98(16) . . ?
N3 Ni1 N10 96.39(14) . . ?
C16 Ni1 N13 76.37(16) . . ?
C55 Ni1 N13 95.57(16) . . ?
N3 Ni1 N13 93.65(14) . . ?
N10 Ni1 N13 161.23(14) . . ?
C16 Ni1 N6 93.78(16) . . ?
C55 Ni1 N6 76.19(16) . . ?
N3 Ni1 N6 161.47(15) . . ?
N10 Ni1 N6 84.21(14) . . ?
N13 Ni1 N6 91.26(14) . . ?
F5 P2 F4 106.3(5) . . ?
F5 P2 F16 99.4(4) . . ?
F4 P2 F16 95.5(3) . . ?
F5 P2 F1 168.8(6) . . ?
F4 P2 F1 82.8(5) . . ?
F16 P2 F1 85.9(5) . . ?
F5 P2 F2 84.5(4) . . ?
F4 P2 F2 167.9(5) . . ?
F16 P2 F2 87.9(3) . . ?
F1 P2 F2 85.9(5) . . ?
F5 P2 F3 85.2(5) . . ?
F4 P2 F3 86.0(3) . . ?
F16 P2 F3 174.5(5) . . ?
F1 P2 F3 89.0(5) . . ?
F2 P2 F3 89.6(4) . . ?
F20 P3 F30 92.0(6) . . ?
F20 P3 F6 90.5(5) . . ?
F30 P3 F6 89.3(5) . . ?
F20 P3 F7 174.4(5) . . ?
F30 P3 F7 92.8(6) . . ?
F6 P3 F7 86.6(4) . . ?
F20 P3 F9 95.2(6) . . ?
F30 P3 F9 87.7(4) . . ?
F6 P3 F9 173.7(5) . . ?
F7 P3 F9 88.0(5) . . ?
F20 P3 F8 88.9(5) . . ?
F30 P3 F8 179.1(6) . . ?
F6 P3 F8 91.0(5) . . ?
F7 P3 F8 86.4(4) . . ?
F9 P3 F8 91.9(5) . . ?
N9 N10 C13 109.5(4) . . ?
N9 N10 Ni1 120.0(3) . . ?
C13 N10 Ni1 125.1(3) . . ?
C55 N4 C29 110.8(4) . . ?
C55 N4 C37 125.4(4) . . ?
C29 N4 C37 123.8(4) . . ?
N4 C55 N5 106.8(4) . . ?
N4 C55 Ni1 136.0(4) . . ?
N5 C55 Ni1 117.1(3) . . ?
N2 N3 C10 109.9(4) . . ?
N2 N3 Ni1 123.1(3) . . ?
C10 N3 Ni1 126.9(3) . . ?
C16 N12 C17 111.6(3) . . ?
C16 N12 C21 117.9(3) . . ?
C17 N12 C21 130.4(4) . . ?
C16 N11 C18 110.5(4) . . ?
C16 N11 C14 123.5(4) . . ?
C18 N11 C14 125.8(4) . . ?
N3 N2 N1 106.1(4) . . ?
C9 N1 N2 111.4(4) . . ?
C9 N1 C35 129.2(5) . . ?
N2 N1 C35 119.4(5) . . ?
N10 N9 N8 106.3(4) . . ?
C55 N5 C26 119.1(4) . . ?
C55 N5 C30 110.8(4) . . ?
C26 N5 C30 130.0(4) . . ?
C21 N13 C22 115.2(4) . . ?
C21 N13 Ni1 113.8(3) . . ?
C22 N13 Ni1 131.0(3) . . ?
N9 N8 C44 111.2(4) . . ?
N9 N8 C45 119.8(4) . . ?
C44 N8 C45 128.8(4) . . ?
N14 C21 N13 128.9(4) . . ?
N14 C21 N12 117.3(4) . . ?
N13 C21 N12 113.8(4) . . ?
C21 N14 C43 113.8(4) . . ?
N11 C16 N12 106.4(3) . . ?
N11 C16 Ni1 135.2(3) . . ?
N12 C16 Ni1 117.4(3) . . ?
C29 C30 C31 121.3(5) . . ?
C29 C30 N5 105.1(4) . . ?
C31 C30 N5 133.6(5) . . ?
C39 N6 C26 115.1(4) . . ?
C39 N6 Ni1 131.0(3) . . ?
C26 N6 Ni1 113.1(3) . . ?
C41 C18 C17 122.0(4) . . ?
C41 C18 N11 131.4(4) . . ?
C17 C18 N11 106.6(4) . . ?
N3 C10 C9 106.7(4) . . ?
N3 C10 C37 128.9(4) . . ?
C9 C10 C37 124.4(4) . . ?
N13 C22 C23 121.5(5) . . ?
N1 C9 C10 105.8(4) . . ?
C20 C17 C18 122.4(4) . . ?
C20 C17 N12 132.8(4) . . ?
C18 C17 N12 104.8(4) . . ?
C17 C20 C19 115.2(5) . . ?
C44 C13 N10 107.6(4) . . ?
C44 C13 C14 126.9(4) . . ?
N10 C13 C14 125.4(4) . . ?
C22 C23 C43 117.9(5) . . ?
C30 C29 C32 122.0(5) . . ?
C30 C29 N4 106.6(4) . . ?
C32 C29 N4 131.4(6) . . ?
C34 C31 C30 116.9(6) . . ?
N11 C14 C13 114.0(4) . . ?
N7 C26 N6 128.0(5) . . ?
N7 C26 N5 118.2(4) . . ?
N6 C26 N5 113.8(4) . . ?
C42 C19 C20 122.4(5) . . ?
N8 C44 C13 105.3(4) . . ?
C18 C41 C42 115.7(5) . . ?
C60 C65 C64 118.8(6) . . ?
C60 C65 C45 120.4(5) . . ?
C64 C65 C45 120.8(5) . . ?
N14 C43 C23 122.6(5) . . ?
C19 C42 C41 122.3(5) . . ?
N1 C35 C36 113.0(5) . . ?
N6 C39 C40 122.4(5) . . ?
C29 C32 C33 114.9(6) . . ?
C47 C36 C48 118.7(6) . . ?
C47 C36 C35 119.7(6) . . ?
C48 C36 C35 121.5(6) . . ?
C31 C34 C33 121.9(6) . . ?
N8 C45 C65 112.3(4) . . ?
N4 C37 C10 117.0(4) . . ?
C70 C40 C39 116.4(5) . . ?
C34 C33 C32 122.9(6) . . ?
C65 C60 C62 120.6(5) . . ?
C63 C64 C65 120.1(6) . . ?
C61 C63 C64 120.5(6) . . ?
C49 C48 C36 120.7(7) . . ?
C61 C62 C60 120.4(6) . . ?
C62 C61 C63 119.5(7) . . ?
C51 C47 C36 121.0(8) . . ?
C48 C49 C50 118.9(8) . . ?
C50 C51 C47 120.4(8) . . ?
C51 C50 C49 120.2(8) . . ?
N7 C70 C40 123.7(5) . . ?
C26 N7 C70 114.3(5) . . ?
N17 C74 C76 178.1(10) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.461
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.078
####################################################################### 
# 
# 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_www
_database_code_depnum_ccdc_archive 'CCDC 1503879'
_audit_update_record             
;
2016-09-12 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H47 F18 N13 Ni2 O2 P3'
_chemical_formula_weight         1402.33

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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.201(2)
_cell_length_b                   15.645(3)
_cell_length_c                   19.716(4)
_cell_angle_alpha                89.845(3)
_cell_angle_beta                 81.636(3)
_cell_angle_gamma                71.188(3)
_cell_volume                     2943.5(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3953
_cell_measurement_theta_min      4.48
_cell_measurement_theta_max      41.105

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1422
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8385
_exptl_absorpt_correction_T_max  0.8516
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Eos, Gemini'
_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            23127
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0899
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10135
_reflns_number_gt                6146
_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)+(0.1203P)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         10135
_refine_ls_number_parameters     785
_refine_ls_number_restraints     916
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.0729
_refine_ls_wR_factor_ref         0.2186
_refine_ls_wR_factor_gt          0.1877
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001

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 0.32875(5) 0.22966(3) 0.80747(2) 0.03892(14) Uani 1 1 d . . .
Ni2 Ni 0.25604(5) 0.29877(3) 0.64635(2) 0.03502(13) Uani 1 1 d . . .
O1 O 0.3565(3) 0.27974(18) 0.72125(13) 0.0441(7) Uani 1 1 d . . .
N1 N 0.3633(3) 0.3269(2) 0.85313(16) 0.0424(9) Uani 1 1 d . . .
N2 N 0.3971(4) 0.1767(2) 0.93821(17) 0.0494(10) Uani 1 1 d . . .
N3 N 0.2396(4) 0.1211(2) 0.91195(18) 0.0511(10) Uani 1 1 d . . .
N4 N 0.2828(3) 0.1354(2) 0.76745(17) 0.0461(9) Uani 1 1 d . . .
N5 N 0.3270(4) 0.1069(2) 0.70223(19) 0.0565(11) Uani 1 1 d . . .
N6 N 0.2829(4) 0.0369(3) 0.6939(2) 0.0682(12) Uani 1 1 d . . .
N7 N 0.4264(3) 0.2661(2) 0.58170(16) 0.0386(8) Uani 1 1 d . . .
N8 N 0.1973(3) 0.3661(2) 0.51679(16) 0.0387(8) Uani 1 1 d . . .
N9 N 0.0254(3) 0.3258(2) 0.56928(16) 0.0370(8) Uani 1 1 d . . .
N10 N 0.0856(3) 0.3194(2) 0.70650(16) 0.0385(8) Uani 1 1 d . . .
N11 N 0.0696(3) 0.3420(2) 0.77305(17) 0.0466(9) Uani 1 1 d . . .
N12 N -0.0625(4) 0.3493(2) 0.79818(18) 0.0501(10) Uani 1 1 d . . .
C1 C 0.3051(5) 0.4101(3) 0.8330(2) 0.0576(11) Uani 1 1 d U . .
H1A H 0.2550 0.4173 0.7964 0.069 Uiso 1 1 calc R . .
C2 C 0.3158(5) 0.4862(3) 0.8640(3) 0.0673(12) Uani 1 1 d U . .
H2A H 0.2736 0.5436 0.8490 0.081 Uiso 1 1 calc R . .
C3 C 0.3914(5) 0.4740(3) 0.9180(3) 0.0700(12) Uani 1 1 d U . .
H3A H 0.3996 0.5236 0.9407 0.084 Uiso 1 1 calc R . .
C4 C 0.4534(5) 0.3894(3) 0.9378(3) 0.0671(12) Uani 1 1 d U . .
H4A H 0.5069 0.3806 0.9732 0.080 Uiso 1 1 calc R . .
C5 C 0.4374(5) 0.3170(3) 0.9058(2) 0.0540(10) Uani 1 1 d U . .
C6 C 0.5016(5) 0.2224(3) 0.9290(2) 0.0576(11) Uani 1 1 d U . .
H6A H 0.5800 0.1888 0.8950 0.069 Uiso 1 1 calc R . .
H6B H 0.5362 0.2252 0.9720 0.069 Uiso 1 1 calc R . .
C7 C 0.3173(5) 0.1742(3) 0.8898(2) 0.0507(10) Uani 1 1 d U . .
C8 C 0.2697(5) 0.0896(3) 0.9765(2) 0.0582(11) Uani 1 1 d U . .
C9 C 0.2172(6) 0.0332(3) 1.0189(3) 0.0727(13) Uani 1 1 d U . .
H9 H 0.1514 0.0085 1.0073 0.087 Uiso 1 1 calc R . .
C10 C 0.2700(6) 0.0173(4) 1.0788(3) 0.0815(15) Uani 1 1 d U . .
H10A H 0.2367 -0.0188 1.1096 0.098 Uiso 1 1 calc R . .
C11 C 0.3702(6) 0.0514(4) 1.0969(3) 0.0773(14) Uani 1 1 d U . .
H11A H 0.4021 0.0375 1.1387 0.093 Uiso 1 1 calc R . .
C12 C 0.4229(6) 0.1051(3) 1.0541(2) 0.0701(13) Uani 1 1 d U . .
H12 H 0.4915 0.1278 1.0649 0.084 Uiso 1 1 calc R . .
C13 C 0.3664(5) 0.1240(3) 0.9925(2) 0.0585(11) Uani 1 1 d U . .
C14 C 0.1430(5) 0.1010(3) 0.8725(2) 0.0581(11) Uani 1 1 d U . .
H14A H 0.0559 0.1512 0.8774 0.070 Uiso 1 1 calc R . .
H14B H 0.1222 0.0477 0.8893 0.070 Uiso 1 1 calc R . .
C15 C 0.2078(4) 0.0848(3) 0.7987(2) 0.0524(11) Uani 1 1 d U . .
C16 C 0.2084(5) 0.0224(3) 0.7506(3) 0.0664(12) Uani 1 1 d U . .
H16A H 0.1651 -0.0217 0.7566 0.080 Uiso 1 1 calc R . .
C17 C 0.3214(6) -0.0136(4) 0.6276(3) 0.0804(13) Uani 1 1 d U . .
H17A H 0.2911 -0.0664 0.6320 0.096 Uiso 1 1 calc R . .
H17B H 0.4227 -0.0348 0.6158 0.096 Uiso 1 1 calc R . .
C18 C 0.2592(5) 0.0404(3) 0.5698(3) 0.0691(12) Uani 1 1 d U . .
C19 C 0.1257(6) 0.0461(4) 0.5574(3) 0.0794(12) Uani 1 1 d U . .
H19A H 0.0720 0.0186 0.5860 0.095 Uiso 1 1 calc R . .
C20 C 0.0746(6) 0.0920(4) 0.5033(3) 0.0856(13) Uani 1 1 d U . .
H20A H -0.0159 0.0978 0.4961 0.103 Uiso 1 1 calc R . .
C21 C 0.1541(7) 0.1296(4) 0.4594(3) 0.0898(15) Uani 1 1 d U . .
H21A H 0.1197 0.1570 0.4209 0.108 Uiso 1 1 calc R . .
C22 C 0.2806(6) 0.1277(4) 0.4710(3) 0.0831(14) Uani 1 1 d U . .
H22A H 0.3314 0.1571 0.4425 0.100 Uiso 1 1 calc R . .
C23 C 0.3352(6) 0.0820(4) 0.5254(3) 0.0755(13) Uani 1 1 d U . .
H23A H 0.4247 0.0790 0.5325 0.091 Uiso 1 1 calc R . .
C24 C 0.5326(4) 0.1928(3) 0.5959(2) 0.0450(10) Uani 1 1 d U . .
H24A H 0.5209 0.1653 0.6372 0.054 Uiso 1 1 calc R . .
C25 C 0.6560(4) 0.1580(3) 0.5519(2) 0.0500(11) Uani 1 1 d U . .
H25A H 0.7265 0.1079 0.5633 0.060 Uiso 1 1 calc R . .
C26 C 0.6745(4) 0.1980(3) 0.4909(2) 0.0500(11) Uani 1 1 d U . .
H26A H 0.7576 0.1757 0.4603 0.060 Uiso 1 1 calc R . .
C27 C 0.5680(4) 0.2713(3) 0.4759(2) 0.0468(10) Uani 1 1 d U . .
H27A H 0.5781 0.2993 0.4347 0.056 Uiso 1 1 calc R . .
C28 C 0.4466(4) 0.3035(3) 0.5215(2) 0.0409(9) Uani 1 1 d U . .
C29 C 0.3283(4) 0.3838(3) 0.5058(2) 0.0444(9) Uani 1 1 d U . .
H29A H 0.3215 0.4355 0.5349 0.053 Uiso 1 1 calc R . .
H29B H 0.3478 0.3987 0.4584 0.053 Uiso 1 1 calc R . .
C30 C 0.1538(4) 0.3315(3) 0.5745(2) 0.0407(9) Uani 1 1 d U . .
C31 C -0.0125(4) 0.3588(3) 0.5060(2) 0.0438(9) Uani 1 1 d U . .
C32 C -0.1309(4) 0.3653(3) 0.4774(2) 0.0500(10) Uani 1 1 d U . .
H32A H -0.2041 0.3481 0.5002 0.060 Uiso 1 1 calc R . .
C33 C -0.1334(5) 0.3990(3) 0.4127(3) 0.0612(12) Uani 1 1 d U . .
H33A H -0.2104 0.4042 0.3909 0.073 Uiso 1 1 calc R . .
C34 C -0.0243(5) 0.4253(3) 0.3793(3) 0.0638(12) Uani 1 1 d U . .
H34A H -0.0304 0.4484 0.3360 0.077 Uiso 1 1 calc R . .
C35 C 0.0925(5) 0.4179(3) 0.4089(2) 0.0519(10) Uani 1 1 d U . .
H35A H 0.1661 0.4350 0.3864 0.062 Uiso 1 1 calc R . .
C36 C 0.0954(4) 0.3843(3) 0.4728(2) 0.0436(9) Uani 1 1 d U . .
C37 C -0.0540(4) 0.2892(3) 0.6210(2) 0.0498(10) Uani 1 1 d U . .
H37A H -0.0219 0.2238 0.6149 0.060 Uiso 1 1 calc R . .
H37B H -0.1522 0.3114 0.6156 0.060 Uiso 1 1 calc R . .
C38 C -0.0387(4) 0.3150(3) 0.6909(2) 0.0426(10) Uani 1 1 d U . .
C39 C -0.1323(5) 0.3341(3) 0.7493(2) 0.0552(11) Uani 1 1 d U . .
H39A H -0.2254 0.3362 0.7545 0.066 Uiso 1 1 calc R . .
C40 C -0.1136(5) 0.3762(3) 0.8708(3) 0.0686(12) Uani 1 1 d U . .
H40A H -0.0437 0.3429 0.8981 0.082 Uiso 1 1 calc R . .
H40B H -0.1982 0.3609 0.8849 0.082 Uiso 1 1 calc R . .
C41 C -0.1440(5) 0.4740(4) 0.8838(3) 0.0779(13) Uani 1 1 d DU . .
C42 C -0.0586(7) 0.5059(4) 0.9150(3) 0.0951(14) Uani 1 1 d U . .
H42A H 0.0196 0.4640 0.9288 0.114 Uiso 1 1 calc R . .
C43 C -0.0786(8) 0.5943(5) 0.9275(4) 0.1093(16) Uani 1 1 d U . .
H43A H -0.0166 0.6117 0.9500 0.131 Uiso 1 1 calc R . .
C44 C -0.1800(8) 0.6519(5) 0.9089(4) 0.1156(18) Uani 1 1 d U . .
H44A H -0.1870 0.7123 0.9148 0.139 Uiso 1 1 calc R . .
C45 C -0.2803(9) 0.6339(5) 0.8810(4) 0.1255(19) Uani 1 1 d U . .
H45A H -0.3577 0.6803 0.8710 0.151 Uiso 1 1 calc R . .
C46 C -0.2650(7) 0.5360(5) 0.8659(4) 0.1101(16) Uani 1 1 d DU . .
H46A H -0.3308 0.5187 0.8463 0.132 Uiso 1 1 calc R . .
P1 P 0.81383(16) 0.22738(11) 0.04985(9) 0.0789(5) Uani 1 1 d . . .
F1 F 0.8243(6) 0.1811(4) -0.0199(2) 0.197(2) Uani 1 1 d . . .
F2 F 0.6652(4) 0.2220(5) 0.0672(2) 0.180(2) Uani 1 1 d . . .
F3 F 0.7987(5) 0.2829(3) 0.1185(2) 0.1551(18) Uani 1 1 d . . .
F4 F 0.9629(4) 0.2330(3) 0.0252(3) 0.166(2) Uani 1 1 d . . .
F5 F 0.7598(7) 0.3159(4) 0.0128(3) 0.212(3) Uani 1 1 d . . .
F6 F 0.8656(6) 0.1414(3) 0.0879(4) 0.203(3) Uani 1 1 d . . .
P2 P 0.20460(15) 0.89330(10) 0.25830(7) 0.0674(4) Uani 1 1 d . . .
F7 F 0.0641(4) 0.8784(3) 0.2932(2) 0.1283(15) Uani 1 1 d . . .
F8 F 0.2128(6) 0.9458(3) 0.3232(2) 0.162(2) Uani 1 1 d . . .
F9 F 0.3425(3) 0.9066(2) 0.2208(2) 0.1086(13) Uani 1 1 d . . .
F10 F 0.1952(4) 0.8398(3) 0.19247(17) 0.1078(12) Uani 1 1 d . . .
F11 F 0.2888(4) 0.8017(2) 0.28854(18) 0.1050(11) Uani 1 1 d . . .
F12 F 0.1163(4) 0.9846(2) 0.22872(19) 0.1162(14) Uani 1 1 d . . .
P6 P 0.47587(13) 0.51874(9) 0.33593(7) 0.0619(4) Uani 1 1 d . . .
F13 F 0.5209(5) 0.4197(3) 0.3533(3) 0.159(2) Uani 1 1 d . . .
F14 F 0.3192(3) 0.5225(3) 0.3547(2) 0.1311(15) Uani 1 1 d . . .
F15 F 0.4812(5) 0.5311(4) 0.4135(2) 0.201(2) Uani 1 1 d . . .
F16 F 0.4606(6) 0.5128(6) 0.2628(2) 0.227(3) Uani 1 1 d . . .
F17 F 0.4265(5) 0.6204(3) 0.3278(4) 0.188(2) Uani 1 1 d U . .
F18 F 0.6265(3) 0.5253(3) 0.3242(2) 0.1469(16) Uani 1 1 d . . .
N13 N -0.1328(7) 0.1697(4) 0.3283(3) 0.131(2) Uani 1 1 d . . .
C47 C -0.0557(7) 0.1846(4) 0.2920(3) 0.109(2) Uani 1 1 d DU . .
C48 C 0.0492(8) 0.2024(6) 0.2407(4) 0.163(4) Uani 1 1 d DU . .
H48A H 0.0094 0.2600 0.2219 0.245 Uiso 1 1 calc R . .
H48B H 0.0792 0.1560 0.2047 0.245 Uiso 1 1 calc R . .
H48C H 0.1281 0.2029 0.2617 0.245 Uiso 1 1 calc R . .
C49 C 0.4542(9) 0.2240(7) 0.2936(5) 0.227(5) Uani 1 1 d D . .
H20B H 0.4023 0.1976 0.2682 0.340 Uiso 1 1 d R . .
H20C H 0.5043 0.1800 0.3228 0.340 Uiso 1 1 d R . .
H20D H 0.3907 0.2752 0.3212 0.340 Uiso 1 1 d R . .
O2 O 0.5567(11) 0.2473(8) 0.2411(5) 0.294(6) Uani 1 1 d D . .
H49C H 0.5362 0.3113 0.2478 0.441 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
Ni1 C7 1.845(4) . ?
Ni1 N4 1.891(4) . ?
Ni1 O1 1.892(3) . ?
Ni1 N1 1.922(3) . ?
Ni2 C30 1.855(4) . ?
Ni2 O1 1.887(3) . ?
Ni2 N10 1.891(3) . ?
Ni2 N7 1.921(3) . ?
N1 C1 1.331(5) . ?
N1 C5 1.352(5) . ?
N2 C7 1.350(6) . ?
N2 C13 1.409(6) . ?
N2 C6 1.455(6) . ?
N3 C7 1.353(6) . ?
N3 C8 1.403(6) . ?
N3 C14 1.449(6) . ?
N4 N5 1.327(5) . ?
N4 C15 1.358(6) . ?
N5 N6 1.331(6) . ?
N6 C16 1.320(6) . ?
N6 C17 1.464(6) . ?
N7 C28 1.340(5) . ?
N7 C24 1.361(5) . ?
N8 C30 1.337(5) . ?
N8 C36 1.409(5) . ?
N8 C29 1.437(5) . ?
N9 C30 1.359(5) . ?
N9 C31 1.408(5) . ?
N9 C37 1.442(5) . ?
N10 N11 1.333(4) . ?
N10 C38 1.370(5) . ?
N11 N12 1.334(5) . ?
N12 C39 1.343(6) . ?
N12 C40 1.464(6) . ?
C1 C2 1.383(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.382(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.354(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.364(7) . ?
C4 H4A 0.9300 . ?
C5 C6 1.512(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C8 C13 1.340(7) . ?
C8 C9 1.391(7) . ?
C9 C10 1.356(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.384(9) . ?
C10 H10A 0.9300 . ?
C11 C12 1.365(8) . ?
C11 H11A 0.9300 . ?
C12 C13 1.409(7) . ?
C12 H12 0.9300 . ?
C14 C15 1.494(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.360(7) . ?
C16 H16A 0.9300 . ?
C17 C18 1.508(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C23 1.384(8) . ?
C18 C19 1.393(8) . ?
C19 C20 1.357(8) . ?
C19 H19A 0.9300 . ?
C20 C21 1.361(9) . ?
C20 H20A 0.9300 . ?
C21 C22 1.334(9) . ?
C21 H21A 0.9300 . ?
C22 C23 1.372(8) . ?
C22 H22A 0.9300 . ?
C23 H23A 0.9300 . ?
C24 C25 1.371(5) . ?
C24 H24A 0.9300 . ?
C25 C26 1.371(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.368(6) . ?
C26 H26A 0.9300 . ?
C27 C28 1.368(5) . ?
C27 H27A 0.9300 . ?
C28 C29 1.503(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C31 C36 1.368(6) . ?
C31 C32 1.379(6) . ?
C32 C33 1.378(7) . ?
C32 H32A 0.9300 . ?
C33 C34 1.386(7) . ?
C33 H33A 0.9300 . ?
C34 C35 1.373(7) . ?
C34 H34A 0.9300 . ?
C35 C36 1.364(6) . ?
C35 H35A 0.9300 . ?
C37 C38 1.481(6) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.351(6) . ?
C39 H39A 0.9300 . ?
C40 C41 1.476(7) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.351(9) . ?
C41 C46 1.393(6) . ?
C42 C43 1.349(9) . ?
C42 H42A 0.9300 . ?
C43 C44 1.234(10) . ?
C43 H43A 0.9300 . ?
C44 C45 1.334(12) . ?
C44 H44A 0.9300 . ?
C45 C46 1.515(10) . ?
C45 H45A 0.9300 . ?
C46 H46A 0.9300 . ?
P1 F6 1.518(5) . ?
P1 F1 1.529(5) . ?
P1 F2 1.535(5) . ?
P1 F5 1.541(6) . ?
P1 F4 1.558(5) . ?
P1 F3 1.572(5) . ?
P2 F8 1.549(5) . ?
P2 F9 1.566(4) . ?
P2 F10 1.577(4) . ?
P2 F11 1.581(3) . ?
P2 F7 1.583(4) . ?
P2 F12 1.585(4) . ?
P6 F16 1.479(5) . ?
P6 F17 1.521(4) . ?
P6 F13 1.521(4) . ?
P6 F15 1.553(5) . ?
P6 F18 1.556(4) . ?
P6 F14 1.569(4) . ?
N13 C47 1.068(8) . ?
C47 C48 1.456(7) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 O2 1.493(9) . ?
C49 H20B 0.9598 . ?
C49 H20C 0.9599 . ?
C49 H20D 0.9600 . ?
O2 H49C 0.9598 . ?

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
C7 Ni1 N4 87.70(18) . . ?
C7 Ni1 O1 175.08(15) . . ?
N4 Ni1 O1 91.78(14) . . ?
C7 Ni1 N1 89.76(17) . . ?
N4 Ni1 N1 175.74(14) . . ?
O1 Ni1 N1 91.04(13) . . ?
C30 Ni2 O1 173.40(15) . . ?
C30 Ni2 N10 88.66(15) . . ?
O1 Ni2 N10 90.79(12) . . ?
C30 Ni2 N7 89.58(15) . . ?
O1 Ni2 N7 91.64(12) . . ?
N10 Ni2 N7 173.80(14) . . ?
Ni2 O1 Ni1 132.47(16) . . ?
C1 N1 C5 118.0(4) . . ?
C1 N1 Ni1 117.3(3) . . ?
C5 N1 Ni1 124.6(3) . . ?
C7 N2 C13 108.3(4) . . ?
C7 N2 C6 122.4(4) . . ?
C13 N2 C6 129.2(4) . . ?
C7 N3 C8 109.6(4) . . ?
C7 N3 C14 123.3(4) . . ?
C8 N3 C14 127.2(4) . . ?
N5 N4 C15 109.6(4) . . ?
N5 N4 Ni1 122.7(3) . . ?
C15 N4 Ni1 127.7(3) . . ?
N4 N5 N6 105.8(4) . . ?
C16 N6 N5 111.7(4) . . ?
C16 N6 C17 128.8(5) . . ?
N5 N6 C17 119.5(4) . . ?
C28 N7 C24 116.9(3) . . ?
C28 N7 Ni2 126.4(2) . . ?
C24 N7 Ni2 116.4(3) . . ?
C30 N8 C36 110.3(3) . . ?
C30 N8 C29 122.3(3) . . ?
C36 N8 C29 127.4(3) . . ?
C30 N9 C31 109.1(3) . . ?
C30 N9 C37 123.8(3) . . ?
C31 N9 C37 127.1(3) . . ?
N11 N10 C38 109.1(3) . . ?
N11 N10 Ni2 123.2(3) . . ?
C38 N10 Ni2 127.7(3) . . ?
N10 N11 N12 105.8(3) . . ?
N11 N12 C39 111.9(3) . . ?
N11 N12 C40 118.8(4) . . ?
C39 N12 C40 129.2(4) . . ?
N1 C1 C2 123.0(4) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C3 C2 C1 117.6(5) . . ?
C3 C2 H2A 121.2 . . ?
C1 C2 H2A 121.2 . . ?
C4 C3 C2 119.7(5) . . ?
C4 C3 H3A 120.1 . . ?
C2 C3 H3A 120.1 . . ?
C3 C4 C5 119.9(5) . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
N1 C5 C4 121.7(4) . . ?
N1 C5 C6 117.7(4) . . ?
C4 C5 C6 120.6(4) . . ?
N2 C6 C5 109.8(4) . . ?
N2 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
N2 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 N3 107.4(4) . . ?
N2 C7 Ni1 123.2(3) . . ?
N3 C7 Ni1 129.2(4) . . ?
C13 C8 C9 123.0(5) . . ?
C13 C8 N3 106.5(4) . . ?
C9 C8 N3 130.5(5) . . ?
C10 C9 C8 114.3(6) . . ?
C10 C9 H9 122.8 . . ?
C8 C9 H9 122.8 . . ?
C9 C10 C11 124.2(6) . . ?
C9 C10 H10A 117.9 . . ?
C11 C10 H10A 117.9 . . ?
C12 C11 C10 120.8(5) . . ?
C12 C11 H11A 119.6 . . ?
C10 C11 H11A 119.6 . . ?
C11 C12 C13 115.6(6) . . ?
C11 C12 H12 122.2 . . ?
C13 C12 H12 122.2 . . ?
C8 C13 N2 108.2(4) . . ?
C8 C13 C12 122.0(5) . . ?
N2 C13 C12 129.8(5) . . ?
N3 C14 C15 109.1(4) . . ?
N3 C14 H14A 109.9 . . ?
C15 C14 H14A 109.9 . . ?
N3 C14 H14B 109.9 . . ?
C15 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
N4 C15 C16 106.7(4) . . ?
N4 C15 C14 122.3(4) . . ?
C16 C15 C14 131.0(5) . . ?
N6 C16 C15 106.3(5) . . ?
N6 C16 H16A 126.9 . . ?
C15 C16 H16A 126.9 . . ?
N6 C17 C18 113.9(4) . . ?
N6 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
N6 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C23 C18 C19 117.9(5) . . ?
C23 C18 C17 121.3(5) . . ?
C19 C18 C17 120.8(5) . . ?
C20 C19 C18 119.6(6) . . ?
C20 C19 H19A 120.2 . . ?
C18 C19 H19A 120.2 . . ?
C19 C20 C21 120.9(6) . . ?
C19 C20 H20A 119.6 . . ?
C21 C20 H20A 119.6 . . ?
C22 C21 C20 121.0(6) . . ?
C22 C21 H21A 119.5 . . ?
C20 C21 H21A 119.5 . . ?
C21 C22 C23 119.5(6) . . ?
C21 C22 H22A 120.3 . . ?
C23 C22 H22A 120.3 . . ?
C22 C23 C18 121.1(6) . . ?
C22 C23 H23A 119.5 . . ?
C18 C23 H23A 119.5 . . ?
N7 C24 C25 122.6(4) . . ?
N7 C24 H24A 118.7 . . ?
C25 C24 H24A 118.7 . . ?
C24 C25 C26 119.3(4) . . ?
C24 C25 H25A 120.4 . . ?
C26 C25 H25A 120.4 . . ?
C27 C26 C25 118.5(4) . . ?
C27 C26 H26A 120.7 . . ?
C25 C26 H26A 120.7 . . ?
C26 C27 C28 120.0(4) . . ?
C26 C27 H27A 120.0 . . ?
C28 C27 H27A 120.0 . . ?
N7 C28 C27 122.6(4) . . ?
N7 C28 C29 116.7(3) . . ?
C27 C28 C29 120.7(4) . . ?
N8 C29 C28 111.4(3) . . ?
N8 C29 H29A 109.4 . . ?
C28 C29 H29A 109.4 . . ?
N8 C29 H29B 109.4 . . ?
C28 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
N8 C30 N9 107.4(3) . . ?
N8 C30 Ni2 124.2(3) . . ?
N9 C30 Ni2 128.4(3) . . ?
C36 C31 C32 122.5(4) . . ?
C36 C31 N9 107.0(3) . . ?
C32 C31 N9 130.4(4) . . ?
C33 C32 C31 115.6(4) . . ?
C33 C32 H32A 122.2 . . ?
C31 C32 H32A 122.2 . . ?
C32 C33 C34 121.8(5) . . ?
C32 C33 H33A 119.1 . . ?
C34 C33 H33A 119.1 . . ?
C35 C34 C33 121.4(5) . . ?
C35 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
C36 C35 C34 116.9(4) . . ?
C36 C35 H35A 121.6 . . ?
C34 C35 H35A 121.6 . . ?
C35 C36 C31 121.8(4) . . ?
C35 C36 N8 132.1(4) . . ?
C31 C36 N8 106.2(3) . . ?
N9 C37 C38 111.2(4) . . ?
N9 C37 H37A 109.4 . . ?
C38 C37 H37A 109.4 . . ?
N9 C37 H37B 109.4 . . ?
C38 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
C39 C38 N10 107.7(4) . . ?
C39 C38 C37 130.0(4) . . ?
N10 C38 C37 122.2(3) . . ?
N12 C39 C38 105.5(4) . . ?
N12 C39 H39A 127.3 . . ?
C38 C39 H39A 127.3 . . ?
N12 C40 C41 111.6(4) . . ?
N12 C40 H40A 109.3 . . ?
C41 C40 H40A 109.3 . . ?
N12 C40 H40B 109.3 . . ?
C41 C40 H40B 109.3 . . ?
H40A C40 H40B 108.0 . . ?
C42 C41 C46 118.2(6) . . ?
C42 C41 C40 121.4(5) . . ?
C46 C41 C40 120.3(6) . . ?
C43 C42 C41 124.6(7) . . ?
C43 C42 H42A 117.7 . . ?
C41 C42 H42A 117.7 . . ?
C44 C43 C42 119.5(8) . . ?
C44 C43 H43A 120.3 . . ?
C42 C43 H43A 120.3 . . ?
C43 C44 C45 124.8(9) . . ?
C43 C44 H44A 117.6 . . ?
C45 C44 H44A 117.6 . . ?
C44 C45 C46 118.4(7) . . ?
C44 C45 H45A 120.8 . . ?
C46 C45 H45A 120.8 . . ?
C41 C46 C45 114.2(7) . . ?
C41 C46 H46A 122.9 . . ?
C45 C46 H46A 122.9 . . ?
F6 P1 F1 96.4(4) . . ?
F6 P1 F2 88.2(3) . . ?
F1 P1 F2 87.8(3) . . ?
F6 P1 F5 178.7(4) . . ?
F1 P1 F5 84.8(3) . . ?
F2 P1 F5 91.4(4) . . ?
F6 P1 F4 94.7(3) . . ?
F1 P1 F4 87.5(3) . . ?
F2 P1 F4 174.7(3) . . ?
F5 P1 F4 85.8(3) . . ?
F6 P1 F3 88.5(3) . . ?
F1 P1 F3 175.1(3) . . ?
F2 P1 F3 92.4(3) . . ?
F5 P1 F3 90.3(3) . . ?
F4 P1 F3 92.0(3) . . ?
F8 P2 F9 90.6(3) . . ?
F8 P2 F10 179.6(3) . . ?
F9 P2 F10 89.8(2) . . ?
F8 P2 F11 89.8(2) . . ?
F9 P2 F11 92.1(2) . . ?
F10 P2 F11 90.3(2) . . ?
F8 P2 F7 91.8(3) . . ?
F9 P2 F7 177.6(2) . . ?
F10 P2 F7 87.8(2) . . ?
F11 P2 F7 88.4(2) . . ?
F8 P2 F12 90.4(2) . . ?
F9 P2 F12 89.5(2) . . ?
F10 P2 F12 89.5(2) . . ?
F11 P2 F12 178.4(2) . . ?
F7 P2 F12 90.0(2) . . ?
F16 P6 F17 84.9(4) . . ?
F16 P6 F13 101.6(4) . . ?
F17 P6 F13 173.1(4) . . ?
F16 P6 F15 175.6(3) . . ?
F17 P6 F15 91.8(4) . . ?
F13 P6 F15 81.5(3) . . ?
F16 P6 F18 97.1(3) . . ?
F17 P6 F18 85.7(2) . . ?
F13 P6 F18 95.4(3) . . ?
F15 P6 F18 85.6(3) . . ?
F16 P6 F14 88.0(3) . . ?
F17 P6 F14 89.4(2) . . ?
F13 P6 F14 88.7(3) . . ?
F15 P6 F14 89.1(3) . . ?
F18 P6 F14 172.7(3) . . ?
N13 C47 C48 177.9(9) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O2 C49 H20B 105.5 . . ?
O2 C49 H20C 109.1 . . ?
H20B C49 H20C 109.5 . . ?
O2 C49 H20D 113.7 . . ?
H20B C49 H20D 109.5 . . ?
H20C C49 H20D 109.5 . . ?
C49 O2 H49C 105.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C30 Ni2 O1 Ni1 117.9(12) . . . . ?
N10 Ni2 O1 Ni1 32.8(2) . . . . ?
N7 Ni2 O1 Ni1 -141.5(2) . . . . ?
C7 Ni1 O1 Ni2 126.1(19) . . . . ?
N4 Ni1 O1 Ni2 42.2(2) . . . . ?
N1 Ni1 O1 Ni2 -134.6(2) . . . . ?
C7 Ni1 N1 C1 -142.0(3) . . . . ?
N4 Ni1 N1 C1 -88.7(19) . . . . ?
O1 Ni1 N1 C1 42.8(3) . . . . ?
C7 Ni1 N1 C5 35.2(3) . . . . ?
N4 Ni1 N1 C5 88.5(19) . . . . ?
O1 Ni1 N1 C5 -140.0(3) . . . . ?
C7 Ni1 N4 N5 -150.1(3) . . . . ?
O1 Ni1 N4 N5 25.0(3) . . . . ?
N1 Ni1 N4 N5 156.5(18) . . . . ?
C7 Ni1 N4 C15 27.1(4) . . . . ?
O1 Ni1 N4 C15 -157.8(3) . . . . ?
N1 Ni1 N4 C15 -26(2) . . . . ?
C15 N4 N5 N6 -1.9(4) . . . . ?
Ni1 N4 N5 N6 175.8(3) . . . . ?
N4 N5 N6 C16 2.3(5) . . . . ?
N4 N5 N6 C17 -176.7(4) . . . . ?
C30 Ni2 N7 C28 30.4(4) . . . . ?
O1 Ni2 N7 C28 -143.1(3) . . . . ?
N10 Ni2 N7 C28 103.9(12) . . . . ?
C30 Ni2 N7 C24 -143.6(3) . . . . ?
O1 Ni2 N7 C24 42.9(3) . . . . ?
N10 Ni2 N7 C24 -70.1(13) . . . . ?
C30 Ni2 N10 N11 -153.6(3) . . . . ?
O1 Ni2 N10 N11 19.9(3) . . . . ?
N7 Ni2 N10 N11 132.9(12) . . . . ?
C30 Ni2 N10 C38 25.9(3) . . . . ?
O1 Ni2 N10 C38 -160.6(3) . . . . ?
N7 Ni2 N10 C38 -47.6(14) . . . . ?
C38 N10 N11 N12 1.3(4) . . . . ?
Ni2 N10 N11 N12 -179.1(2) . . . . ?
N10 N11 N12 C39 -1.4(4) . . . . ?
N10 N11 N12 C40 -178.3(3) . . . . ?
C5 N1 C1 C2 -0.8(6) . . . . ?
Ni1 N1 C1 C2 176.6(4) . . . . ?
N1 C1 C2 C3 0.4(7) . . . . ?
C1 C2 C3 C4 1.1(7) . . . . ?
C2 C3 C4 C5 -2.0(8) . . . . ?
C1 N1 C5 C4 -0.2(6) . . . . ?
Ni1 N1 C5 C4 -177.4(3) . . . . ?
C1 N1 C5 C6 179.2(4) . . . . ?
Ni1 N1 C5 C6 2.0(5) . . . . ?
C3 C4 C5 N1 1.6(7) . . . . ?
C3 C4 C5 C6 -177.8(5) . . . . ?
C7 N2 C6 C5 49.9(5) . . . . ?
C13 N2 C6 C5 -135.0(4) . . . . ?
N1 C5 C6 N2 -48.6(5) . . . . ?
C4 C5 C6 N2 130.8(5) . . . . ?
C13 N2 C7 N3 -0.6(4) . . . . ?
C6 N2 C7 N3 175.4(3) . . . . ?
C13 N2 C7 Ni1 -177.1(3) . . . . ?
C6 N2 C7 Ni1 -1.2(5) . . . . ?
C8 N3 C7 N2 0.5(4) . . . . ?
C14 N3 C7 N2 -178.7(3) . . . . ?
C8 N3 C7 Ni1 176.8(3) . . . . ?
C14 N3 C7 Ni1 -2.4(6) . . . . ?
N4 Ni1 C7 N2 147.8(3) . . . . ?
O1 Ni1 C7 N2 64(2) . . . . ?
N1 Ni1 C7 N2 -35.7(3) . . . . ?
N4 Ni1 C7 N3 -28.0(4) . . . . ?
O1 Ni1 C7 N3 -112.0(19) . . . . ?
N1 Ni1 C7 N3 148.6(4) . . . . ?
C7 N3 C8 C13 -0.2(5) . . . . ?
C14 N3 C8 C13 178.9(4) . . . . ?
C7 N3 C8 C9 -179.5(4) . . . . ?
C14 N3 C8 C9 -0.4(7) . . . . ?
C13 C8 C9 C10 1.3(7) . . . . ?
N3 C8 C9 C10 -179.5(4) . . . . ?
C8 C9 C10 C11 -1.5(7) . . . . ?
C9 C10 C11 C12 0.3(8) . . . . ?
C10 C11 C12 C13 1.2(7) . . . . ?
C9 C8 C13 N2 179.2(4) . . . . ?
N3 C8 C13 N2 -0.1(5) . . . . ?
C9 C8 C13 C12 0.2(7) . . . . ?
N3 C8 C13 C12 -179.2(4) . . . . ?
C7 N2 C13 C8 0.4(5) . . . . ?
C6 N2 C13 C8 -175.2(4) . . . . ?
C7 N2 C13 C12 179.4(4) . . . . ?
C6 N2 C13 C12 3.8(7) . . . . ?
C11 C12 C13 C8 -1.4(7) . . . . ?
C11 C12 C13 N2 179.7(4) . . . . ?
C7 N3 C14 C15 40.6(5) . . . . ?
C8 N3 C14 C15 -138.4(4) . . . . ?
N5 N4 C15 C16 0.9(5) . . . . ?
Ni1 N4 C15 C16 -176.6(3) . . . . ?
N5 N4 C15 C14 -179.6(4) . . . . ?
Ni1 N4 C15 C14 2.9(6) . . . . ?
N3 C14 C15 N4 -40.3(5) . . . . ?
N3 C14 C15 C16 139.1(5) . . . . ?
N5 N6 C16 C15 -1.7(5) . . . . ?
C17 N6 C16 C15 177.1(5) . . . . ?
N4 C15 C16 N6 0.5(5) . . . . ?
C14 C15 C16 N6 -179.0(4) . . . . ?
C16 N6 C17 C18 115.6(6) . . . . ?
N5 N6 C17 C18 -65.6(6) . . . . ?
N6 C17 C18 C23 97.1(6) . . . . ?
N6 C17 C18 C19 -86.2(6) . . . . ?
C23 C18 C19 C20 -0.5(7) . . . . ?
C17 C18 C19 C20 -177.2(5) . . . . ?
C18 C19 C20 C21 2.6(8) . . . . ?
C19 C20 C21 C22 -4.6(9) . . . . ?
C20 C21 C22 C23 4.3(9) . . . . ?
C21 C22 C23 C18 -2.2(8) . . . . ?
C19 C18 C23 C22 0.3(8) . . . . ?
C17 C18 C23 C22 177.0(5) . . . . ?
C28 N7 C24 C25 0.5(6) . . . . ?
Ni2 N7 C24 C25 175.1(3) . . . . ?
N7 C24 C25 C26 -0.1(7) . . . . ?
C24 C25 C26 C27 -0.3(7) . . . . ?
C25 C26 C27 C28 0.2(7) . . . . ?
C24 N7 C28 C27 -0.6(6) . . . . ?
Ni2 N7 C28 C27 -174.6(3) . . . . ?
C24 N7 C28 C29 179.4(4) . . . . ?
Ni2 N7 C28 C29 5.4(5) . . . . ?
C26 C27 C28 N7 0.2(7) . . . . ?
C26 C27 C28 C29 -179.8(4) . . . . ?
C30 N8 C29 C28 49.3(5) . . . . ?
C36 N8 C29 C28 -133.4(4) . . . . ?
N7 C28 C29 N8 -49.4(5) . . . . ?
C27 C28 C29 N8 130.6(4) . . . . ?
C36 N8 C30 N9 0.5(4) . . . . ?
C29 N8 C30 N9 178.2(3) . . . . ?
C36 N8 C30 Ni2 -179.6(3) . . . . ?
C29 N8 C30 Ni2 -1.9(5) . . . . ?
C31 N9 C30 N8 -0.4(4) . . . . ?
C37 N9 C30 N8 178.2(3) . . . . ?
C31 N9 C30 Ni2 179.6(3) . . . . ?
C37 N9 C30 Ni2 -1.8(5) . . . . ?
O1 Ni2 C30 N8 68.3(13) . . . . ?
N10 Ni2 C30 N8 153.6(3) . . . . ?
N7 Ni2 C30 N8 -32.4(3) . . . . ?
O1 Ni2 C30 N9 -111.8(12) . . . . ?
N10 Ni2 C30 N9 -26.5(3) . . . . ?
N7 Ni2 C30 N9 147.5(4) . . . . ?
C30 N9 C31 C36 0.3(4) . . . . ?
C37 N9 C31 C36 -178.3(3) . . . . ?
C30 N9 C31 C32 178.9(4) . . . . ?
C37 N9 C31 C32 0.3(7) . . . . ?
C36 C31 C32 C33 0.2(6) . . . . ?
N9 C31 C32 C33 -178.2(4) . . . . ?
C31 C32 C33 C34 -0.6(6) . . . . ?
C32 C33 C34 C35 0.8(7) . . . . ?
C33 C34 C35 C36 -0.6(7) . . . . ?
C34 C35 C36 C31 0.2(6) . . . . ?
C34 C35 C36 N8 178.5(4) . . . . ?
C32 C31 C36 C35 0.0(6) . . . . ?
N9 C31 C36 C35 178.8(4) . . . . ?
C32 C31 C36 N8 -178.7(4) . . . . ?
N9 C31 C36 N8 0.0(4) . . . . ?
C30 N8 C36 C35 -178.9(4) . . . . ?
C29 N8 C36 C35 3.5(7) . . . . ?
C30 N8 C36 C31 -0.3(4) . . . . ?
C29 N8 C36 C31 -177.9(4) . . . . ?
C30 N9 C37 C38 38.1(5) . . . . ?
C31 N9 C37 C38 -143.6(4) . . . . ?
N11 N10 C38 C39 -0.8(4) . . . . ?
Ni2 N10 C38 C39 179.6(3) . . . . ?
N11 N10 C38 C37 -178.5(4) . . . . ?
Ni2 N10 C38 C37 2.0(5) . . . . ?
N9 C37 C38 C39 145.3(4) . . . . ?
N9 C37 C38 N10 -37.6(5) . . . . ?
N11 N12 C39 C38 0.9(5) . . . . ?
C40 N12 C39 C38 177.4(4) . . . . ?
N10 C38 C39 N12 -0.1(5) . . . . ?
C37 C38 C39 N12 177.4(4) . . . . ?
N11 N12 C40 C41 76.4(5) . . . . ?
C39 N12 C40 C41 -99.9(6) . . . . ?
N12 C40 C41 C42 -105.9(6) . . . . ?
N12 C40 C41 C46 76.3(7) . . . . ?
C46 C41 C42 C43 -3.1(10) . . . . ?
C40 C41 C42 C43 179.0(6) . . . . ?
C41 C42 C43 C44 -1.1(12) . . . . ?
C42 C43 C44 C45 5.2(13) . . . . ?
C43 C44 C45 C46 -4.7(13) . . . . ?
C42 C41 C46 C45 3.2(9) . . . . ?
C40 C41 C46 C45 -178.8(5) . . . . ?
C44 C45 C46 C41 0.2(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.092
####################################################################### 
# 
# 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_y
_database_code_depnum_ccdc_archive 'CCDC 1503882'
_audit_update_record             
;
2016-09-12 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_DIFF003_y                   
;
PROBLEM: _diffrn_measurement_device_type is missing
RESPONSE: 'Xcalibur, Eos, Gemini' 
;
# Added during the CSD deposition process: Monday 12 September 2016 07:21 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H21 Cl F6 N7 Ni P'
_chemical_formula_weight         646.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2719(18)
_cell_length_b                   11.226(2)
_cell_length_c                   13.006(2)
_cell_angle_alpha                104.179(3)
_cell_angle_beta                 100.409(3)
_cell_angle_gamma                108.847(3)
_cell_volume                     1319.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2285
_cell_measurement_theta_min      1.68
_cell_measurement_theta_max      25.01

_exptl_crystal_description       yellow
_exptl_crystal_colour            block
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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            7345
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4626
_reflns_number_gt                3555
_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)+(0.0661P)²+1.4957P] 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         4626
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1496
_refine_ls_wR_factor_gt          0.1352
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.027
_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 0.37344(6) 0.03760(5) 0.42519(4) 0.04440(19) Uani 1 1 d . . .
Cl1 Cl 0.20088(14) -0.13963(12) 0.42570(10) 0.0626(3) Uani 1 1 d . . .
C1 C 0.5153(4) 0.1909(4) 0.4340(3) 0.0445(9) Uani 1 1 d . . .
N5 N 0.3486(4) -0.1831(4) 0.2500(3) 0.0532(9) Uani 1 1 d . . .
N4 N 0.4213(4) -0.0536(3) 0.3032(3) 0.0472(8) Uani 1 1 d . . .
N2 N 0.5356(4) 0.3037(3) 0.5158(3) 0.0452(8) Uani 1 1 d . . .
N1 N 0.3457(4) 0.1585(3) 0.5461(3) 0.0477(8) Uani 1 1 d . . .
C3 C 0.4403(5) 0.2867(4) 0.5799(3) 0.0458(10) Uani 1 1 d . . .
N3 N 0.6115(4) 0.2257(3) 0.3806(3) 0.0456(8) Uani 1 1 d . . .
N6 N 0.4069(4) -0.2120(4) 0.1688(3) 0.0571(10) Uani 1 1 d . . .
C13 C 0.5245(5) -0.0041(4) 0.2551(4) 0.0496(10) Uani 1 1 d . . .
C20 C 0.6972(4) 0.3616(4) 0.4269(4) 0.0482(10) Uani 1 1 d . . .
C11 C 0.2439(6) 0.1306(5) 0.5988(4) 0.0660(13) Uani 1 1 d . . .
H11 H 0.1764 0.0440 0.5768 0.079 Uiso 1 1 calc R . .
C21 C 0.6494(4) 0.4132(4) 0.5143(3) 0.0479(10) Uani 1 1 d . . .
C18 C 0.8758(5) 0.5738(5) 0.4624(5) 0.0697(14) Uani 1 1 d . . .
H18 H 0.9524 0.6302 0.4464 0.084 Uiso 1 1 calc R . .
C12 C 0.5140(5) -0.1077(5) 0.1689(4) 0.0615(12) Uani 1 1 d . . .
H12 H 0.5704 -0.1055 0.1204 0.074 Uiso 1 1 calc R . .
C10 C 0.2368(7) 0.2279(6) 0.6854(5) 0.0799(17) Uani 1 1 d . . .
H10 H 0.1650 0.2062 0.7201 0.096 Uiso 1 1 calc R . .
C19 C 0.8104(5) 0.4398(5) 0.3980(4) 0.0627(12) Uani 1 1 d . . .
H19 H 0.8410 0.4046 0.3389 0.075 Uiso 1 1 calc R . .
C9 C 0.4397(5) 0.3863(5) 0.6662(4) 0.0564(11) Uani 1 1 d . . .
H9 H 0.5080 0.4726 0.6883 0.068 Uiso 1 1 calc R . .
C17 C 0.2239(5) -0.3799(4) -0.0057(4) 0.0514(10) Uani 1 1 d . . .
C16 C 0.3479(6) -0.3508(5) 0.0919(4) 0.0649(13) Uani 1 1 d . . .
H16A H 0.3164 -0.4112 0.1326 0.078 Uiso 1 1 calc R . .
H16B H 0.4240 -0.3684 0.0646 0.078 Uiso 1 1 calc R . .
C27 C 0.7152(5) 0.5482(5) 0.5779(4) 0.0608(12) Uani 1 1 d . . .
H27 H 0.6842 0.5849 0.6361 0.073 Uiso 1 1 calc R . .
C24 C -0.0063(6) -0.4497(7) -0.1847(5) 0.0821(17) Uani 1 1 d . . .
H24 H -0.0850 -0.4732 -0.2446 0.099 Uiso 1 1 calc R . .
C22 C 0.1876(6) -0.2827(5) -0.0350(4) 0.0686(14) Uani 1 1 d . . .
H22 H 0.2404 -0.1933 0.0057 0.082 Uiso 1 1 calc R . .
C26 C 0.1438(6) -0.5104(5) -0.0670(4) 0.0650(13) Uani 1 1 d . . .
H26 H 0.1673 -0.5764 -0.0468 0.078 Uiso 1 1 calc R . .
C25 C 0.0302(6) -0.5463(6) -0.1570(4) 0.0741(15) Uani 1 1 d . . .
H25 H -0.0215 -0.6355 -0.1987 0.089 Uiso 1 1 calc R . .
C23 C 0.0717(7) -0.3189(7) -0.1255(5) 0.0839(17) Uani 1 1 d . . .
H23 H 0.0470 -0.2536 -0.1460 0.101 Uiso 1 1 calc R . .
C28 C 0.3347(6) 0.3537(6) 0.7185(4) 0.0718(15) Uani 1 1 d . . .
H28 H 0.3311 0.4186 0.7768 0.086 Uiso 1 1 calc R . .
C29 C 0.8288(6) 0.6231(5) 0.5485(5) 0.0679(14) Uani 1 1 d . . .
H29 H 0.8763 0.7128 0.5900 0.082 Uiso 1 1 calc R . .
C30 C 0.6324(5) 0.1367(4) 0.2906(4) 0.0575(12) Uani 1 1 d . . .
H30A H 0.7280 0.1372 0.3128 0.069 Uiso 1 1 calc R . .
H30B H 0.6263 0.1691 0.2280 0.069 Uiso 1 1 calc R . .
P1 P 0.65684(15) 0.76135(13) 0.89964(11) 0.0627(4) Uani 1 1 d . . .
F5 F 0.6784(5) 0.7514(4) 1.0203(3) 0.1095(13) Uani 1 1 d . . .
F2 F 0.6403(5) 0.7710(5) 0.7803(3) 0.1318(17) Uani 1 1 d . . .
F3 F 0.6873(5) 0.6305(4) 0.8602(3) 0.1260(15) Uani 1 1 d . . .
F4 F 0.6322(7) 0.8912(4) 0.9379(4) 0.154(2) Uani 1 1 d . . .
F6 F 0.8232(4) 0.8401(5) 0.9296(4) 0.1388(17) Uani 1 1 d . . .
F1 F 0.4954(4) 0.6847(6) 0.8684(5) 0.168(2) Uani 1 1 d . . .
C7 C 0.9459(6) 0.0774(6) 0.8397(5) 0.0794(16) Uani 1 1 d . . .
H7A H 0.8538 0.0582 0.7915 0.119 Uiso 1 1 calc R . .
H7B H 1.0049 0.1699 0.8582 0.119 Uiso 1 1 calc R . .
H7C H 0.9339 0.0578 0.9060 0.119 Uiso 1 1 calc R . .
C46 C 1.0140(7) -0.0037(6) 0.7842(5) 0.0765(15) Uani 1 1 d . . .
N7 N 1.0703(7) -0.0633(6) 0.7420(6) 0.113(2) 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
Ni1 C1 1.822(4) . ?
Ni1 N4 1.902(3) . ?
Ni1 N1 1.940(3) . ?
Ni1 Cl1 2.1984(13) . ?
C1 N3 1.320(5) . ?
C1 N2 1.367(5) . ?
N5 N6 1.329(5) . ?
N5 N4 1.330(5) . ?
N4 C13 1.361(6) . ?
N2 C3 1.394(5) . ?
N2 C21 1.404(5) . ?
N1 C11 1.346(6) . ?
N1 C3 1.356(5) . ?
C3 C9 1.379(6) . ?
N3 C20 1.399(5) . ?
N3 C30 1.439(5) . ?
N6 C12 1.322(6) . ?
N6 C16 1.484(6) . ?
C13 C12 1.363(6) . ?
C13 C30 1.505(6) . ?
C20 C19 1.386(6) . ?
C20 C21 1.389(6) . ?
C11 C10 1.395(7) . ?
C21 C27 1.400(6) . ?
C18 C29 1.364(8) . ?
C18 C19 1.393(7) . ?
C10 C28 1.348(8) . ?
C9 C28 1.375(7) . ?
C17 C26 1.368(6) . ?
C17 C22 1.375(6) . ?
C17 C16 1.511(6) . ?
C27 C29 1.378(7) . ?
C24 C25 1.361(8) . ?
C24 C23 1.361(9) . ?
C22 C23 1.384(8) . ?
C26 C25 1.366(7) . ?
P1 F1 1.523(4) . ?
P1 F4 1.538(4) . ?
P1 F2 1.564(4) . ?
P1 F6 1.571(4) . ?
P1 F3 1.582(4) . ?
P1 F5 1.582(4) . ?
C7 C46 1.453(8) . ?
C46 N7 1.126(7) . ?

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
C1 Ni1 N4 88.56(17) . . ?
C1 Ni1 N1 81.69(17) . . ?
N4 Ni1 N1 170.01(15) . . ?
C1 Ni1 Cl1 175.96(14) . . ?
N4 Ni1 Cl1 95.44(11) . . ?
N1 Ni1 Cl1 94.34(11) . . ?
N3 C1 N2 106.7(4) . . ?
N3 C1 Ni1 136.5(3) . . ?
N2 C1 Ni1 116.8(3) . . ?
N6 N5 N4 105.1(4) . . ?
N5 N4 C13 109.9(3) . . ?
N5 N4 Ni1 121.2(3) . . ?
C13 N4 Ni1 128.9(3) . . ?
C1 N2 C3 114.9(3) . . ?
C1 N2 C21 110.8(3) . . ?
C3 N2 C21 134.3(4) . . ?
C11 N1 C3 116.9(4) . . ?
C11 N1 Ni1 127.9(3) . . ?
C3 N1 Ni1 115.2(3) . . ?
N1 C3 C9 123.6(4) . . ?
N1 C3 N2 111.3(4) . . ?
C9 C3 N2 125.1(4) . . ?
C1 N3 C20 110.7(4) . . ?
C1 N3 C30 125.5(4) . . ?
C20 N3 C30 123.6(4) . . ?
C12 N6 N5 112.7(4) . . ?
C12 N6 C16 128.6(4) . . ?
N5 N6 C16 118.7(4) . . ?
N4 C13 C12 106.8(4) . . ?
N4 C13 C30 127.2(4) . . ?
C12 C13 C30 126.0(4) . . ?
C19 C20 C21 122.4(4) . . ?
C19 C20 N3 130.4(4) . . ?
C21 C20 N3 107.2(4) . . ?
N1 C11 C10 121.9(5) . . ?
C20 C21 C27 120.8(4) . . ?
C20 C21 N2 104.5(4) . . ?
C27 C21 N2 134.7(4) . . ?
C29 C18 C19 120.7(5) . . ?
N6 C12 C13 105.6(4) . . ?
C28 C10 C11 119.6(5) . . ?
C20 C19 C18 116.4(5) . . ?
C28 C9 C3 117.8(5) . . ?
C26 C17 C22 118.9(5) . . ?
C26 C17 C16 117.6(4) . . ?
C22 C17 C16 123.5(4) . . ?
N6 C16 C17 114.0(4) . . ?
C29 C27 C21 115.7(5) . . ?
C25 C24 C23 120.5(5) . . ?
C17 C22 C23 119.4(5) . . ?
C25 C26 C17 121.8(5) . . ?
C24 C25 C26 119.0(6) . . ?
C24 C23 C22 120.4(5) . . ?
C10 C28 C9 120.2(5) . . ?
C18 C29 C27 124.0(5) . . ?
N3 C30 C13 113.1(4) . . ?
F1 P1 F4 88.7(3) . . ?
F1 P1 F2 89.1(3) . . ?
F4 P1 F2 89.9(3) . . ?
F1 P1 F6 179.0(3) . . ?
F4 P1 F6 91.5(3) . . ?
F2 P1 F6 89.9(3) . . ?
F1 P1 F3 93.1(3) . . ?
F4 P1 F3 178.1(3) . . ?
F2 P1 F3 89.5(2) . . ?
F6 P1 F3 86.7(3) . . ?
F1 P1 F5 92.4(3) . . ?
F4 P1 F5 91.1(2) . . ?
F2 P1 F5 178.2(2) . . ?
F6 P1 F5 88.6(2) . . ?
F3 P1 F5 89.4(2) . . ?
N7 C46 C7 178.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.072
