# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1839747'
_audit_update_record             
;
2018-05-04 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            C30H28F12N8NiP2
_chemical_formula_weight         849.23

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'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.7258(12)
_cell_length_b                   18.871(2)
_cell_length_c                   16.3402(17)
_cell_angle_alpha                90
_cell_angle_beta                 93.244(2)
_cell_angle_gamma                90
_cell_volume                     3302.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3210
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      23.46

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_F_000             2178
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.791
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28993
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.650
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7386
_reflns_number_gt                4635
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0840P)²+4.6482P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7386
_refine_ls_number_parameters     483
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0643
_refine_ls_wR_factor_ref         0.1909
_refine_ls_wR_factor_gt          0.1639
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.057
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C30 C 0.0682(14) 0.0666(6) 0.5630(11) 0.204(7) Uani 1 1 d . U . . .
H30A H -0.0137 0.0490 0.5476 0.307 Uiso 1 1 calc R U . . .
H30B H 0.0984 0.0941 0.5188 0.307 Uiso 1 1 calc R U . . .
H30C H 0.0645 0.0960 0.6108 0.307 Uiso 1 1 calc R U . . .
C3 C 0.1324(4) 0.5001(3) 0.4408(3) 0.0349(11) Uani 1 1 d . . . . .
H3 H 0.0802 0.4691 0.4109 0.042 Uiso 1 1 calc R U . . .
C10 C 0.5241(5) 0.3189(3) 0.6160(3) 0.0376(11) Uani 1 1 d . . . . .
H10 H 0.5106 0.2716 0.6022 0.045 Uiso 1 1 calc R U . . .
C11 C 0.6213(5) 0.3361(3) 0.6717(3) 0.0398(12) Uani 1 1 d . . . . .
H11 H 0.6714 0.3001 0.6945 0.048 Uiso 1 1 calc R U . . .
C12 C 0.6453(5) 0.4053(3) 0.6942(3) 0.0386(12) Uani 1 1 d . . . . .
H12 H 0.7107 0.4170 0.7316 0.046 Uiso 1 1 calc R U . . .
C15 C 0.6886(5) 0.7466(3) 0.7422(3) 0.0391(12) Uani 1 1 d . . . . .
H15A H 0.7705 0.7286 0.7308 0.047 Uiso 1 1 calc R U . . .
H15B H 0.6898 0.7626 0.7987 0.047 Uiso 1 1 calc R U . . .
C16 C 0.6486(5) 0.8056(3) 0.6835(3) 0.0379(11) Uani 1 1 d . . . . .
H16 H 0.6173 0.8461 0.7125 0.046 Uiso 1 1 calc R U . . .
H16A H 0.7171 0.8206 0.6513 0.046 Uiso 1 1 calc R U . . .
C20 C 0.5404(5) 0.8651(3) 0.5294(3) 0.0391(11) Uani 1 1 d . . . . .
H20 H 0.6211 0.8788 0.5461 0.047 Uiso 1 1 calc R U . . .
C23 C 0.2994(5) 0.8252(3) 0.4789(3) 0.0382(11) Uani 1 1 d . . . . .
H23 H 0.2193 0.8112 0.4610 0.046 Uiso 1 1 calc R U . . .
C24 C 0.0823(4) 0.8341(3) 0.6988(3) 0.0370(11) Uani 1 1 d . . . . .
H24 H 0.0514 0.8802 0.6994 0.044 Uiso 1 1 calc R U . . .
C26 C 0.0847(5) 0.7166(3) 0.7458(3) 0.0428(12) Uani 1 1 d . . . . .
H26 H 0.0562 0.6821 0.7808 0.051 Uiso 1 1 calc R U . . .
C2 C 0.1078(4) 0.5717(3) 0.4401(3) 0.0360(11) Uani 1 1 d . . . . .
H2 H 0.0398 0.5898 0.4089 0.043 Uiso 1 1 calc R U . . .
C25 C 0.0383(5) 0.7855(3) 0.7502(3) 0.0427(12) Uani 1 1 d . . . . .
H25 H -0.0210 0.7974 0.7872 0.051 Uiso 1 1 calc R U . . .
C21 C 0.4755(6) 0.9013(3) 0.4667(3) 0.0470(13) Uani 1 1 d . . . . .
H21 H 0.5126 0.9397 0.4419 0.056 Uiso 1 1 calc R U . . .
C13 C 0.6545(5) 0.5668(3) 0.7272(3) 0.0448(13) Uani 1 1 d . . . . .
H13B H 0.7236 0.5856 0.6982 0.054 Uiso 1 1 calc R U . . .
H13A H 0.6881 0.5330 0.7674 0.054 Uiso 1 1 calc R U . . .
C22 C 0.3565(6) 0.8809(3) 0.4411(3) 0.0458(13) Uani 1 1 d . . . . .
H22 H 0.3144 0.9047 0.3980 0.055 Uiso 1 1 calc R U . . .
C29 C 0.1517(10) 0.0078(4) 0.5807(5) 0.090(3) Uani 1 1 d . . . . .
C5 C 0.3083(4) 0.5224(2) 0.5312(3) 0.0272(9) Uani 1 1 d . . . . .
C8 C 0.4698(4) 0.4394(2) 0.6028(3) 0.0288(10) Uani 1 1 d . . . . .
C6 C 0.4757(4) 0.5605(2) 0.6220(3) 0.0286(10) Uani 1 1 d . . . . .
C19 C 0.3619(4) 0.7897(2) 0.5441(3) 0.0299(10) Uani 1 1 d . . . . .
C28 C 0.2176(4) 0.7502(2) 0.6396(3) 0.0281(10) Uani 1 1 d . . . . .
C17 C 0.5193(4) 0.7063(2) 0.6582(3) 0.0275(9) Uani 1 1 d . . . . .
C9 C 0.4463(4) 0.3702(2) 0.5801(3) 0.0326(10) Uani 1 1 d . . . . .
H9 H 0.3813 0.3585 0.5425 0.039 Uiso 1 1 calc R U . . .
C1 C 0.1857(4) 0.6162(3) 0.4864(3) 0.0326(10) Uani 1 1 d . U . . .
H1 H 0.1690 0.6645 0.4857 0.039 Uiso 1 1 calc R U . . .
C18 C 0.4848(4) 0.8088(2) 0.5668(3) 0.0311(10) Uani 1 1 d . . . . .
C4 C 0.2352(4) 0.4746(2) 0.4863(3) 0.0325(10) Uani 1 1 d . . . . .
H4 H 0.2546 0.4266 0.4867 0.039 Uiso 1 1 calc R U . . .
C7 C 0.5678(4) 0.4567(2) 0.6587(3) 0.0310(10) Uani 1 1 d . . . . .
C27 C 0.1704(4) 0.6994(2) 0.6916(3) 0.0335(10) Uani 1 1 d . . . . .
H27 H 0.1984 0.6528 0.6890 0.040 Uiso 1 1 calc R U . . .
C14 C 0.5918(5) 0.6265(2) 0.7709(3) 0.0377(11) Uani 1 1 d . . . . .
H14A H 0.5064 0.6131 0.7800 0.045 Uiso 1 1 calc R U . . .
H14B H 0.6349 0.6337 0.8240 0.045 Uiso 1 1 calc R U . . .
F1 F 0.1483(4) 0.56376(16) 0.8025(2) 0.0606(9) Uani 1 1 d . . . . .
F8 F 0.1429(3) 0.32090(19) 0.5700(2) 0.0608(9) Uani 1 1 d . . . . .
F3 F 0.1640(4) 0.45095(18) 0.8445(2) 0.0654(10) Uani 1 1 d . . . . .
F4 F 0.1597(4) 0.52764(19) 0.67138(19) 0.0662(10) Uani 1 1 d . . . . .
F5 F 0.0143(3) 0.4838(2) 0.7486(2) 0.0679(10) Uani 1 1 d . . . . .
F7 F 0.1173(3) 0.1923(2) 0.4456(2) 0.0825(13) Uani 1 1 d . . . . .
F6 F 0.1752(4) 0.41518(19) 0.7149(2) 0.0837(13) Uani 1 1 d . . . . .
F2 F 0.3103(3) 0.4967(2) 0.7675(3) 0.0813(12) Uani 1 1 d . . . . .
F9 F 0.2388(4) 0.2886(2) 0.4560(3) 0.0877(14) Uani 1 1 d . . . . .
F10 F 0.2278(5) 0.2145(2) 0.5611(3) 0.1049(18) Uani 1 1 d . . . . .
F11 F 0.0149(4) 0.2304(3) 0.5517(3) 0.1130(19) Uani 1 1 d . . . . .
F12 F 0.0379(5) 0.3042(3) 0.4492(3) 0.119(2) Uani 1 1 d . . . . .
N1 N 0.2848(3) 0.59258(19) 0.5325(2) 0.0273(8) Uani 1 1 d . . . . .
N6 N 0.3058(3) 0.73386(19) 0.5876(2) 0.0283(8) Uani 1 1 d . . . . .
N2 N 0.4149(3) 0.50516(18) 0.5811(2) 0.0278(8) Uani 1 1 d . . . . .
N4 N 0.5912(3) 0.69296(19) 0.7252(2) 0.0302(8) Uani 1 1 d . . . . .
N3 N 0.5679(4) 0.53006(19) 0.6687(2) 0.0311(9) Uani 1 1 d . . . . .
N5 N 0.5487(4) 0.7718(2) 0.6314(2) 0.0319(9) Uani 1 1 d . . . . .
N7 N 0.1717(4) 0.8169(2) 0.6459(3) 0.0328(9) Uani 1 1 d . . . . .
N8 N 0.2279(7) -0.0343(4) 0.6027(4) 0.086(2) Uani 1 1 d . . . . .
Ni1 Ni 0.40001(5) 0.64905(3) 0.60220(3) 0.02629(17) Uani 1 1 d . . . . .
P1 P 0.16362(14) 0.48926(7) 0.75802(8) 0.0404(3) Uani 1 1 d . . . . .
P2 P 0.13006(13) 0.25668(9) 0.50760(9) 0.0522(4) Uani 1 1 d . . . . .
H7N H 0.196(4) 0.850(2) 0.612(3) 0.016(11) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C30 C29 1.445(14) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C3 C2 1.377(7) . ?
C3 C4 1.381(6) . ?
C3 H3 0.9300 . ?
C10 C11 1.383(7) . ?
C10 C9 1.387(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(7) . ?
C11 H11 0.9300 . ?
C12 C7 1.383(6) . ?
C12 H12 0.9300 . ?
C15 N4 1.471(6) . ?
C15 C16 1.515(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N5 1.475(6) . ?
C16 H16 0.9700 . ?
C16 H16A 0.9700 . ?
C20 C18 1.380(7) . ?
C20 C21 1.385(7) . ?
C20 H20 0.9300 . ?
C23 C22 1.381(7) . ?
C23 C19 1.397(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.347(7) . ?
C24 N7 1.366(6) . ?
C24 H24 0.9300 . ?
C26 C27 1.352(7) . ?
C26 C25 1.395(7) . ?
C26 H26 0.9300 . ?
C2 C1 1.380(6) . ?
C2 H2 0.9300 . ?
C25 H25 0.9300 . ?
C21 C22 1.376(8) . ?
C21 H21 0.9300 . ?
C13 N3 1.468(6) . ?
C13 C14 1.512(7) . ?
C13 H13B 0.9700 . ?
C13 H13A 0.9700 . ?
C22 H22 0.9300 . ?
C29 N8 1.181(10) . ?
C5 N1 1.349(5) . ?
C5 C4 1.378(6) . ?
C5 N2 1.404(5) . ?
C8 C9 1.377(6) . ?
C8 C7 1.392(6) . ?
C8 N2 1.410(5) . ?
C6 N3 1.344(5) . ?
C6 N2 1.383(6) . ?
C6 Ni1 1.878(4) . ?
C19 C18 1.396(6) . ?
C19 N6 1.423(6) . ?
C28 N6 1.342(6) . ?
C28 N7 1.358(6) . ?
C28 C27 1.395(6) . ?
C17 N4 1.327(6) . ?
C17 N5 1.354(6) . ?
C17 Ni1 1.873(4) . ?
C9 H9 0.9300 . ?
C1 N1 1.343(5) . ?
C1 H1 0.9300 . ?
C18 N5 1.411(6) . ?
C4 H4 0.9300 . ?
C7 N3 1.395(6) . ?
C27 H27 0.9300 . ?
C14 N4 1.458(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
F1 P1 1.596(3) . ?
F8 P2 1.584(3) . ?
F3 P1 1.587(3) . ?
F4 P1 1.589(3) . ?
F5 P1 1.603(4) . ?
F7 P2 1.583(3) . ?
F6 P1 1.573(4) . ?
F2 P1 1.578(4) . ?
F9 P2 1.596(4) . ?
F10 P2 1.547(4) . ?
F11 P2 1.547(4) . ?
F12 P2 1.607(5) . ?
N1 Ni1 1.949(4) . ?
N6 Ni1 1.900(4) . ?
N7 H7N 0.89(4) . ?

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
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C11 C10 C9 121.9(5) . . ?
C11 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C12 C11 C10 121.4(5) . . ?
C12 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C11 C12 C7 116.9(5) . . ?
C11 C12 H12 121.5 . . ?
C7 C12 H12 121.5 . . ?
N4 C15 C16 102.3(4) . . ?
N4 C15 H15A 111.3 . . ?
C16 C15 H15A 111.3 . . ?
N4 C15 H15B 111.3 . . ?
C16 C15 H15B 111.3 . . ?
H15A C15 H15B 109.2 . . ?
N5 C16 C15 102.6(4) . . ?
N5 C16 H16 111.2 . . ?
C15 C16 H16 111.2 . . ?
N5 C16 H16A 111.2 . . ?
C15 C16 H16A 111.2 . . ?
H16 C16 H16A 109.2 . . ?
C18 C20 C21 119.8(5) . . ?
C18 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C23 C19 120.0(5) . . ?
C22 C23 H23 120.0 . . ?
C19 C23 H23 120.0 . . ?
C25 C24 N7 121.0(5) . . ?
C25 C24 H24 119.5 . . ?
N7 C24 H24 119.5 . . ?
C27 C26 C25 121.0(5) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C3 C2 C1 118.8(4) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C24 C25 C26 117.7(5) . . ?
C24 C25 H25 121.2 . . ?
C26 C25 H25 121.2 . . ?
C22 C21 C20 120.4(5) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
N3 C13 C14 112.2(4) . . ?
N3 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
N3 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
H13B C13 H13A 107.9 . . ?
C21 C22 C23 120.3(5) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
N8 C29 C30 171.1(12) . . ?
N1 C5 C4 123.3(4) . . ?
N1 C5 N2 111.4(4) . . ?
C4 C5 N2 125.3(4) . . ?
C9 C8 C7 121.2(4) . . ?
C9 C8 N2 134.4(4) . . ?
C7 C8 N2 104.4(4) . . ?
N3 C6 N2 105.3(4) . . ?
N3 C6 Ni1 140.8(3) . . ?
N2 C6 Ni1 113.7(3) . . ?
C18 C19 C23 119.0(4) . . ?
C18 C19 N6 118.5(4) . . ?
C23 C19 N6 122.5(4) . . ?
N6 C28 N7 122.2(4) . . ?
N6 C28 C27 121.4(4) . . ?
N7 C28 C27 116.4(4) . . ?
N4 C17 N5 107.7(4) . . ?
N4 C17 Ni1 130.0(3) . . ?
N5 C17 Ni1 122.3(3) . . ?
C8 C9 C10 116.9(4) . . ?
C8 C9 H9 121.6 . . ?
C10 C9 H9 121.6 . . ?
N1 C1 C2 122.8(4) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C20 C18 C19 120.4(4) . . ?
C20 C18 N5 120.6(4) . . ?
C19 C18 N5 118.9(4) . . ?
C5 C4 C3 118.1(4) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
C12 C7 C8 121.7(4) . . ?
C12 C7 N3 130.5(4) . . ?
C8 C7 N3 107.7(4) . . ?
C26 C27 C28 121.2(4) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
N4 C14 C13 112.9(4) . . ?
N4 C14 H14A 109.0 . . ?
C13 C14 H14A 109.0 . . ?
N4 C14 H14B 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C1 N1 C5 117.3(4) . . ?
C1 N1 Ni1 127.0(3) . . ?
C5 N1 Ni1 115.7(3) . . ?
C28 N6 C19 118.6(4) . . ?
C28 N6 Ni1 120.2(3) . . ?
C19 N6 Ni1 116.7(3) . . ?
C6 N2 C5 116.9(3) . . ?
C6 N2 C8 111.4(4) . . ?
C5 N2 C8 131.6(4) . . ?
C17 N4 C14 124.8(4) . . ?
C17 N4 C15 113.5(4) . . ?
C14 N4 C15 120.8(4) . . ?
C6 N3 C7 111.2(4) . . ?
C6 N3 C13 125.9(4) . . ?
C7 N3 C13 122.8(4) . . ?
C17 N5 C18 125.5(4) . . ?
C17 N5 C16 112.6(4) . . ?
C18 N5 C16 121.6(4) . . ?
C28 N7 C24 122.7(4) . . ?
C28 N7 H7N 119(3) . . ?
C24 N7 H7N 118(3) . . ?
C17 Ni1 C6 98.76(19) . . ?
C17 Ni1 N6 85.38(17) . . ?
C6 Ni1 N6 173.01(18) . . ?
C17 Ni1 N1 173.45(17) . . ?
C6 Ni1 N1 82.38(17) . . ?
N6 Ni1 N1 94.15(15) . . ?
F6 P1 F2 91.1(2) . . ?
F6 P1 F3 89.8(2) . . ?
F2 P1 F3 90.1(2) . . ?
F6 P1 F4 90.3(2) . . ?
F2 P1 F4 91.3(2) . . ?
F3 P1 F4 178.6(2) . . ?
F6 P1 F1 178.5(3) . . ?
F2 P1 F1 90.3(2) . . ?
F3 P1 F1 89.46(19) . . ?
F4 P1 F1 90.37(19) . . ?
F6 P1 F5 90.2(2) . . ?
F2 P1 F5 178.6(2) . . ?
F3 P1 F5 90.5(2) . . ?
F4 P1 F5 88.1(2) . . ?
F1 P1 F5 88.4(2) . . ?
F11 P2 F10 96.0(3) . . ?
F11 P2 F7 90.6(2) . . ?
F10 P2 F7 89.9(2) . . ?
F11 P2 F8 89.3(2) . . ?
F10 P2 F8 89.9(2) . . ?
F7 P2 F8 179.8(3) . . ?
F11 P2 F9 173.9(3) . . ?
F10 P2 F9 90.0(3) . . ?
F7 P2 F9 89.5(2) . . ?
F8 P2 F9 90.6(2) . . ?
F11 P2 F12 88.6(3) . . ?
F10 P2 F12 175.3(3) . . ?
F7 P2 F12 91.1(3) . . ?
F8 P2 F12 89.1(2) . . ?
F9 P2 F12 85.4(3) . . ?

_refine_diff_density_max         1.528
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1839765'
_audit_update_record             
;
2018-05-04 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            C30H28F12N8NiP2
_chemical_formula_weight         849.23

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.1990(7)
_cell_length_b                   15.1982(9)
_cell_length_c                   19.6380(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3342.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9967
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_F_000             2178
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.781
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29210
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.259
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7682
_reflns_number_gt                7141
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0232P)²+1.9330P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.048(13)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7682
_refine_ls_number_parameters     484
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0742
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.65673(4) 0.71098(3) 0.28162(2) 0.01718(9) Uani 1 1 d . . . . .
P2 P 0.34847(9) 0.42142(5) 0.06189(4) 0.02145(17) Uani 1 1 d . . . . .
P1 P 0.66166(9) 0.41675(6) 0.31015(4) 0.02541(18) Uani 1 1 d . . . . .
F12 F 0.24434(18) 0.36934(15) 0.09994(12) 0.0337(5) Uani 1 1 d . . . . .
F9 F 0.4531(2) 0.47335(14) 0.02377(14) 0.0405(6) Uani 1 1 d . . . . .
F2 F 0.7412(2) 0.4331(2) 0.37549(13) 0.0524(7) Uani 1 1 d . . . . .
N2 N 0.7377(2) 0.66362(17) 0.40762(14) 0.0175(6) Uani 1 1 d . . . . .
F1 F 0.5949(3) 0.33662(18) 0.34640(14) 0.0555(7) Uani 1 1 d . . . . .
F7 F 0.4288(3) 0.4133(2) 0.12842(15) 0.0653(9) Uani 1 1 d . . . . .
N1 N 0.8226(2) 0.70911(17) 0.30841(13) 0.0174(5) Uani 1 1 d . . . . .
N6 N 0.7183(2) 0.80588(17) 0.14730(13) 0.0193(5) Uani 1 1 d . . . . .
F5 F 0.5805(3) 0.40046(18) 0.24432(14) 0.0563(8) Uani 1 1 d . . . . .
F4 F 0.7271(3) 0.49637(19) 0.27302(16) 0.0652(9) Uani 1 1 d . . . . .
N3 N 0.5452(2) 0.65191(18) 0.40937(15) 0.0202(6) Uani 1 1 d . . . . .
F11 F 0.4021(3) 0.33143(16) 0.03561(19) 0.0832(13) Uani 1 1 d . . . . .
F8 F 0.3004(3) 0.51239(16) 0.08974(16) 0.0612(8) Uani 1 1 d . . . . .
N5 N 0.6081(2) 0.68959(17) 0.14334(14) 0.0207(6) Uani 1 1 d . . . . .
F10 F 0.2700(3) 0.4304(2) -0.00409(14) 0.0752(11) Uani 1 1 d . . . . .
N7 N 0.8894(3) 0.89167(19) 0.13882(16) 0.0254(6) Uani 1 1 d . . . . .
F6 F 0.7569(3) 0.3513(2) 0.28063(19) 0.0737(9) Uani 1 1 d . . . . .
C17 C 0.6687(3) 0.74180(19) 0.18639(16) 0.0188(6) Uani 1 1 d . . . . .
C6 C 0.6369(3) 0.67317(19) 0.37010(16) 0.0180(6) Uani 1 1 d . . . . .
N4 N 0.4857(2) 0.7080(2) 0.26626(15) 0.0246(6) Uani 1 1 d . . . . .
C28 C 0.7912(3) 0.8757(2) 0.17413(17) 0.0195(6) Uani 1 1 d . . . . .
C7 C 0.5846(3) 0.6290(2) 0.47446(18) 0.0207(7) Uani 1 1 d . . . . .
C5 C 0.8437(3) 0.68392(19) 0.37335(15) 0.0188(6) Uani 1 1 d . . . . .
C16 C 0.5459(3) 0.6113(2) 0.1686(2) 0.0272(8) Uani 1 1 d . . . . .
H16A H 0.6028 0.5725 0.1906 0.033 Uiso 1 1 calc R U . . .
H16B H 0.5110 0.5799 0.1305 0.033 Uiso 1 1 calc R U . . .
F3 F 0.5646(3) 0.4818(2) 0.3393(2) 0.0796(12) Uani 1 1 d . . . . .
C27 C 0.7581(3) 0.9172(2) 0.23379(18) 0.0247(7) Uani 1 1 d . . . . .
H27 H 0.6855 0.9056 0.2549 0.030 Uiso 1 1 calc R U . . .
C26 C 0.8390(4) 0.9771(2) 0.26059(18) 0.0313(8) Uani 1 1 d . . . . .
H26 H 0.8225 1.0057 0.3014 0.038 Uiso 1 1 calc R U . . .
C1 C 0.9175(3) 0.7303(2) 0.27006(17) 0.0216(7) Uani 1 1 d . . . . .
H1 H 0.9053 0.7467 0.2250 0.026 Uiso 1 1 calc R U . . .
C13 C 0.4234(3) 0.6490(2) 0.38294(19) 0.0255(7) Uani 1 1 d . . . . .
H13A H 0.3674 0.6604 0.4196 0.031 Uiso 1 1 calc R U . . .
H13B H 0.4069 0.5908 0.3650 0.031 Uiso 1 1 calc R U . . .
C18 C 0.6204(3) 0.7167(2) 0.07633(16) 0.0207(6) Uani 1 1 d . . . . .
C12 C 0.5212(3) 0.6054(2) 0.53203(19) 0.0269(8) Uani 1 1 d . . . . .
H12 H 0.4384 0.6002 0.5318 0.032 Uiso 1 1 calc R U . . .
C19 C 0.6926(3) 0.7919(2) 0.07828(16) 0.0210(6) Uani 1 1 d . . . . .
C8 C 0.7095(3) 0.6368(2) 0.47457(17) 0.0204(7) Uani 1 1 d . . . . .
C3 C 1.0514(3) 0.7018(3) 0.3610(2) 0.0295(8) Uani 1 1 d . . . . .
H3 H 1.1284 0.6999 0.3786 0.035 Uiso 1 1 calc R U . . .
C21 C 0.6810(3) 0.8042(2) -0.04088(18) 0.0317(9) Uani 1 1 d . . . . .
H21 H 0.7008 0.8325 -0.0813 0.038 Uiso 1 1 calc R U . . .
C20 C 0.7235(3) 0.8376(2) 0.01985(18) 0.0275(7) Uani 1 1 d . . . . .
H20 H 0.7704 0.8880 0.0214 0.033 Uiso 1 1 calc R U . . .
C15 C 0.4479(3) 0.6357(2) 0.2190(2) 0.0296(8) Uani 1 1 d . . . . .
H15A H 0.3774 0.6542 0.1942 0.035 Uiso 1 1 calc R U . . .
H15B H 0.4268 0.5841 0.2456 0.035 Uiso 1 1 calc R U . . .
C24 C 0.9645(3) 0.9514(2) 0.1650(2) 0.0327(9) Uani 1 1 d . . . . .
H24 H 1.0334 0.9649 0.1408 0.039 Uiso 1 1 calc R U . . .
C4 C 0.9562(3) 0.6777(2) 0.4012(2) 0.0263(7) Uani 1 1 d . . . . .
H4 H 0.9675 0.6578 0.4455 0.032 Uiso 1 1 calc R U . . .
C10 C 0.7117(4) 0.5968(2) 0.5904(2) 0.0316(8) Uani 1 1 d . . . . .
H10 H 0.7531 0.5853 0.6305 0.038 Uiso 1 1 calc R U . . .
C30 C 0.8879(4) 0.6161(3) 0.0082(2) 0.0412(10) Uani 1 1 d . . . . .
H30A H 0.8308 0.5717 -0.0039 0.062 Uiso 1 1 calc R U . . .
H30B H 0.9642 0.6017 -0.0112 0.062 Uiso 1 1 calc R U . . .
H30C H 0.8619 0.6721 -0.0090 0.062 Uiso 1 1 calc R U . . .
C23 C 0.5766(3) 0.6839(2) 0.01511(19) 0.0280(8) Uani 1 1 d . . . . .
H23 H 0.5280 0.6342 0.0136 0.034 Uiso 1 1 calc R U . . .
C11 C 0.5883(4) 0.5898(2) 0.59041(19) 0.0321(9) Uani 1 1 d . . . . .
H11 H 0.5493 0.5743 0.6305 0.039 Uiso 1 1 calc R U . . .
C9 C 0.7755(3) 0.6204(2) 0.53246(18) 0.0274(8) Uani 1 1 d . . . . .
H9 H 0.8583 0.6249 0.5327 0.033 Uiso 1 1 calc R U . . .
C14 C 0.4064(3) 0.7171(3) 0.32686(18) 0.0282(7) Uani 1 1 d . . . . .
H14A H 0.3241 0.7144 0.3115 0.034 Uiso 1 1 calc R U . . .
H14B H 0.4189 0.7751 0.3464 0.034 Uiso 1 1 calc R U . . .
C2 C 1.0335(3) 0.7286(2) 0.29529(19) 0.0269(8) Uani 1 1 d . . . . .
H2 H 1.0975 0.7454 0.2681 0.032 Uiso 1 1 calc R U . . .
C22 C 0.6086(4) 0.7284(2) -0.04329(18) 0.0325(8) Uani 1 1 d . . . . .
H22 H 0.5818 0.7080 -0.0852 0.039 Uiso 1 1 calc R U . . .
N8 N 0.9064(5) 0.6228(3) 0.1387(2) 0.0606(12) Uani 1 1 d . . . . .
C25 C 0.9448(3) 0.9939(2) 0.2261(2) 0.0321(8) Uani 1 1 d . . . . .
H25 H 1.0009 1.0328 0.2437 0.039 Uiso 1 1 calc R U . . .
C29 C 0.8985(4) 0.6206(3) 0.0821(2) 0.0395(10) Uani 1 1 d . . . . .
H4N H 0.476(4) 0.756(3) 0.240(2) 0.038(12) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C6 1.844(3) . ?
Ni1 N1 1.931(2) . ?
Ni1 C17 1.933(3) . ?
Ni1 N4 1.939(3) . ?
P2 F10 1.572(3) . ?
P2 F11 1.580(3) . ?
P2 F8 1.581(3) . ?
P2 F7 1.591(3) . ?
P2 F12 1.595(2) . ?
P2 F9 1.599(2) . ?
P1 F6 1.569(3) . ?
P1 F3 1.577(3) . ?
P1 F2 1.582(3) . ?
P1 F4 1.592(3) . ?
P1 F1 1.597(3) . ?
P1 F5 1.600(3) . ?
N2 C6 1.356(4) . ?
N2 C5 1.400(4) . ?
N2 C8 1.412(4) . ?
N1 C1 1.342(4) . ?
N1 C5 1.352(4) . ?
N6 C17 1.358(4) . ?
N6 C19 1.402(4) . ?
N6 C28 1.439(4) . ?
N3 C6 1.324(4) . ?
N3 C7 1.396(4) . ?
N3 C13 1.461(4) . ?
N5 C17 1.344(4) . ?
N5 C18 1.386(4) . ?
N5 C16 1.465(4) . ?
N7 C28 1.323(4) . ?
N7 C24 1.340(5) . ?
N4 C14 1.492(4) . ?
N4 C15 1.499(5) . ?
N4 H4N 0.90(4) . ?
C28 C27 1.381(5) . ?
C7 C12 1.383(5) . ?
C7 C8 1.404(5) . ?
C5 C4 1.377(5) . ?
C16 C15 1.524(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C27 C26 1.388(5) . ?
C27 H27 0.9300 . ?
C26 C25 1.388(6) . ?
C26 H26 0.9300 . ?
C1 C2 1.390(5) . ?
C1 H1 0.9300 . ?
C13 C14 1.524(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C18 C23 1.391(5) . ?
C18 C19 1.401(4) . ?
C12 C11 1.391(6) . ?
C12 H12 0.9300 . ?
C19 C20 1.385(5) . ?
C8 C9 1.379(5) . ?
C3 C2 1.368(5) . ?
C3 C4 1.377(5) . ?
C3 H3 0.9300 . ?
C21 C20 1.380(5) . ?
C21 C22 1.409(5) . ?
C21 H21 0.9300 . ?
C20 H20 0.9300 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C24 C25 1.380(6) . ?
C24 H24 0.9300 . ?
C4 H4 0.9300 . ?
C10 C11 1.386(6) . ?
C10 C9 1.392(5) . ?
C10 H10 0.9300 . ?
C30 C29 1.458(6) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C23 C22 1.380(5) . ?
C23 H23 0.9300 . ?
C11 H11 0.9300 . ?
C9 H9 0.9300 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C2 H2 0.9300 . ?
C22 H22 0.9300 . ?
N8 C29 1.116(6) . ?
C25 H25 0.9300 . ?

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 N1 81.64(12) . . ?
C6 Ni1 C17 174.86(13) . . ?
N1 Ni1 C17 101.55(12) . . ?
C6 Ni1 N4 91.15(13) . . ?
N1 Ni1 N4 172.80(12) . . ?
C17 Ni1 N4 85.63(13) . . ?
F10 P2 F11 91.1(2) . . ?
F10 P2 F8 91.1(2) . . ?
F11 P2 F8 177.4(2) . . ?
F10 P2 F7 179.32(17) . . ?
F11 P2 F7 89.2(2) . . ?
F8 P2 F7 88.62(19) . . ?
F10 P2 F12 91.17(14) . . ?
F11 P2 F12 90.08(14) . . ?
F8 P2 F12 91.33(14) . . ?
F7 P2 F12 89.44(14) . . ?
F10 P2 F9 88.90(15) . . ?
F11 P2 F9 89.76(14) . . ?
F8 P2 F9 88.83(14) . . ?
F7 P2 F9 90.48(15) . . ?
F12 P2 F9 179.83(15) . . ?
F6 P1 F3 179.3(2) . . ?
F6 P1 F2 90.91(18) . . ?
F3 P1 F2 89.73(18) . . ?
F6 P1 F4 89.97(19) . . ?
F3 P1 F4 90.41(19) . . ?
F2 P1 F4 89.60(15) . . ?
F6 P1 F1 89.98(18) . . ?
F3 P1 F1 89.63(19) . . ?
F2 P1 F1 91.23(15) . . ?
F4 P1 F1 179.17(16) . . ?
F6 P1 F5 89.42(18) . . ?
F3 P1 F5 89.94(18) . . ?
F2 P1 F5 179.64(18) . . ?
F4 P1 F5 90.53(16) . . ?
F1 P1 F5 88.64(15) . . ?
C6 N2 C5 114.9(3) . . ?
C6 N2 C8 110.5(3) . . ?
C5 N2 C8 134.5(3) . . ?
C1 N1 C5 117.3(3) . . ?
C1 N1 Ni1 127.3(2) . . ?
C5 N1 Ni1 115.4(2) . . ?
C17 N6 C19 110.7(3) . . ?
C17 N6 C28 123.6(3) . . ?
C19 N6 C28 125.6(3) . . ?
C6 N3 C7 110.4(3) . . ?
C6 N3 C13 121.7(3) . . ?
C7 N3 C13 127.8(3) . . ?
C17 N5 C18 111.8(3) . . ?
C17 N5 C16 120.5(3) . . ?
C18 N5 C16 127.6(3) . . ?
C28 N7 C24 116.4(3) . . ?
N5 C17 N6 105.9(3) . . ?
N5 C17 Ni1 115.5(2) . . ?
N6 C17 Ni1 138.5(2) . . ?
N3 C6 N2 107.6(3) . . ?
N3 C6 Ni1 135.9(3) . . ?
N2 C6 Ni1 116.4(2) . . ?
C14 N4 C15 113.2(3) . . ?
C14 N4 Ni1 117.5(2) . . ?
C15 N4 Ni1 113.1(2) . . ?
C14 N4 H4N 108(3) . . ?
C15 N4 H4N 102(3) . . ?
Ni1 N4 H4N 101(3) . . ?
N7 C28 C27 125.8(3) . . ?
N7 C28 N6 114.5(3) . . ?
C27 C28 N6 119.7(3) . . ?
C12 C7 N3 130.6(3) . . ?
C12 C7 C8 122.2(3) . . ?
N3 C7 C8 107.2(3) . . ?
N1 C5 C4 123.7(3) . . ?
N1 C5 N2 111.5(3) . . ?
C4 C5 N2 124.8(3) . . ?
N5 C16 C15 111.5(3) . . ?
N5 C16 H16A 109.3 . . ?
C15 C16 H16A 109.3 . . ?
N5 C16 H16B 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C28 C27 C26 116.5(3) . . ?
C28 C27 H27 121.8 . . ?
C26 C27 H27 121.8 . . ?
C27 C26 C25 119.5(3) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
N3 C13 C14 110.7(3) . . ?
N3 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
N5 C18 C23 132.8(3) . . ?
N5 C18 C19 105.9(3) . . ?
C23 C18 C19 121.3(3) . . ?
C7 C12 C11 116.2(3) . . ?
C7 C12 H12 121.9 . . ?
C11 C12 H12 121.9 . . ?
C20 C19 C18 122.0(3) . . ?
C20 C19 N6 132.4(3) . . ?
C18 C19 N6 105.6(3) . . ?
C9 C8 C7 121.4(3) . . ?
C9 C8 N2 134.4(3) . . ?
C7 C8 N2 104.2(3) . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C20 C21 C22 121.8(3) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 H21 119.1 . . ?
C21 C20 C19 116.5(3) . . ?
C21 C20 H20 121.8 . . ?
C19 C20 H20 121.8 . . ?
N4 C15 C16 112.1(3) . . ?
N4 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
N4 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
N7 C24 C25 123.4(3) . . ?
N7 C24 H24 118.3 . . ?
C25 C24 H24 118.3 . . ?
C3 C4 C5 117.5(3) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
C11 C10 C9 122.1(4) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C22 C23 C18 116.8(3) . . ?
C22 C23 H23 121.6 . . ?
C18 C23 H23 121.6 . . ?
C10 C11 C12 121.7(4) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C8 C9 C10 116.5(3) . . ?
C8 C9 H9 121.8 . . ?
C10 C9 H9 121.8 . . ?
N4 C14 C13 116.0(3) . . ?
N4 C14 H14A 108.3 . . ?
C13 C14 H14A 108.3 . . ?
N4 C14 H14B 108.3 . . ?
C13 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C23 C22 C21 121.5(3) . . ?
C23 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C24 C25 C26 118.3(3) . . ?
C24 C25 H25 120.8 . . ?
C26 C25 H25 120.8 . . ?
N8 C29 C30 179.0(5) . . ?

_refine_diff_density_max         0.512
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1839764'
_audit_update_record             
;
2018-05-04 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H24 F6 N7 Ni P'
_chemical_formula_weight         662.22

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.3433(11)
_cell_length_b                   28.320(4)
_cell_length_c                   11.5936(17)
_cell_angle_alpha                90
_cell_angle_beta                 90.533(4)
_cell_angle_gamma                90
_cell_volume                     2739.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6312
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.57

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_F_000             1352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.842
_shelx_estimated_absorpt_T_min   0.830
_shelx_estimated_absorpt_T_max   0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8300
_exptl_absorpt_correction_T_max  0.8633
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19776
_diffrn_reflns_av_unetI/netI     0.1036
_diffrn_reflns_av_R_equivalents  0.1285
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.270
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5382
_reflns_number_gt                4022
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0368P)²+2.4143P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5382
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1293
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.09187(5) 0.09588(2) 0.16611(4) 0.01707(14) Uani 1 1 d . . . . .
F1 F 0.5268(2) 0.18781(8) 0.76219(18) 0.0272(5) Uani 1 1 d . . . . .
F2 F 0.9052(2) 0.16746(8) 0.7768(2) 0.0350(6) Uani 1 1 d . . . . .
F3 F 0.7021(2) 0.16244(9) 0.90081(18) 0.0365(6) Uani 1 1 d . . . . .
F4 F 0.7454(3) 0.23117(8) 0.8059(2) 0.0462(7) Uani 1 1 d . . . . .
F5 F 0.7312(3) 0.19144(12) 0.6366(2) 0.0613(9) Uani 1 1 d . . . . .
F6 F 0.6840(3) 0.12386(8) 0.7322(2) 0.0515(8) Uani 1 1 d . . . . .
N1 N 0.0464(3) 0.03202(10) 0.2234(3) 0.0192(7) Uani 1 1 d . . . . .
N2 N 0.1782(3) 0.01294(10) 0.0588(2) 0.0184(7) Uani 1 1 d . . . . .
N3 N 0.2855(3) 0.06868(10) -0.0440(2) 0.0181(6) Uani 1 1 d . . . . .
N4 N 0.2051(3) 0.17421(10) 0.0306(3) 0.0190(7) Uani 1 1 d . . . . .
N5 N -0.0326(3) 0.18465(10) 0.1013(2) 0.0175(6) Uani 1 1 d . . . . .
N6 N 0.0004(4) 0.12719(11) 0.2936(2) 0.0242(7) Uani 1 1 d . . . . .
N7 N 0.2299(4) 0.10117(12) 0.3814(3) 0.0298(8) Uani 1 1 d . . . . .
P1 P 0.71635(11) 0.17787(4) 0.76810(8) 0.0217(2) Uani 1 1 d . . . . .
C1 C -0.0356(4) 0.02143(14) 0.3193(3) 0.0260(9) Uani 1 1 d . . . . .
H1 H -0.0756 0.0458 0.3644 0.031 Uiso 1 1 calc R U . . .
C2 C -0.0619(4) -0.02470(14) 0.3526(3) 0.0290(9) Uani 1 1 d . . . . .
H2 H -0.1178 -0.0311 0.4198 0.035 Uiso 1 1 calc R U . . .
C3 C -0.0051(5) -0.06111(14) 0.2859(4) 0.0327(10) Uani 1 1 d . . . . .
H3 H -0.0204 -0.0923 0.3083 0.039 Uiso 1 1 calc R U . . .
C4 C 0.0757(4) -0.05062(14) 0.1844(3) 0.0269(9) Uani 1 1 d . . . . .
H4 H 0.1132 -0.0745 0.1366 0.032 Uiso 1 1 calc R U . . .
C5 C 0.0983(4) -0.00373(13) 0.1568(3) 0.0204(8) Uani 1 1 d . . . . .
C6 C 0.1917(4) 0.06150(13) 0.0477(3) 0.0201(8) Uani 1 1 d . . . . .
C7 C 0.2882(4) -0.05796(13) -0.0568(3) 0.0267(9) Uani 1 1 d . . . . .
H7 H 0.2418 -0.0823 -0.0150 0.032 Uiso 1 1 calc R U . . .
C8 C 0.3848(4) -0.06685(15) -0.1504(3) 0.0309(10) Uani 1 1 d . . . . .
H8 H 0.4016 -0.0980 -0.1727 0.037 Uiso 1 1 calc R U . . .
C9 C 0.4580(5) -0.03085(15) -0.2125(4) 0.0312(10) Uani 1 1 d . . . . .
H9 H 0.5258 -0.0385 -0.2729 0.037 Uiso 1 1 calc R U . . .
C10 C 0.4314(4) 0.01627(14) -0.1859(3) 0.0257(9) Uani 1 1 d . . . . .
H10 H 0.4774 0.0405 -0.2284 0.031 Uiso 1 1 calc R U . . .
C11 C 0.3326(4) 0.02530(13) -0.0926(3) 0.0214(8) Uani 1 1 d . . . . .
C12 C 0.2636(4) -0.01048(13) -0.0277(3) 0.0213(8) Uani 1 1 d . . . . .
C13 C 0.3414(5) 0.11408(13) -0.0898(3) 0.0252(8) Uani 1 1 d . . . . .
H13A H 0.2673 0.1247 -0.1494 0.030 Uiso 1 1 calc R U . . .
H13B H 0.4452 0.1096 -0.1251 0.030 Uiso 1 1 calc R U . . .
C14 C 0.3555(4) 0.15197(13) 0.0018(3) 0.0212(8) Uani 1 1 d . . . . .
H14A H 0.4013 0.1381 0.0711 0.025 Uiso 1 1 calc R U . . .
H14B H 0.4291 0.1760 -0.0248 0.025 Uiso 1 1 calc R U . . .
C15 C 0.1552(4) 0.21896(13) -0.0238(3) 0.0251(9) Uani 1 1 d . . . . .
H15A H 0.1441 0.2156 -0.1067 0.030 Uiso 1 1 calc R U . . .
H15B H 0.2310 0.2441 -0.0069 0.030 Uiso 1 1 calc R U . . .
C16 C -0.0068(4) 0.22839(12) 0.0324(3) 0.0223(8) Uani 1 1 d . . . . .
H16A H -0.0024 0.2561 0.0814 0.027 Uiso 1 1 calc R U . . .
H16B H -0.0907 0.2325 -0.0252 0.027 Uiso 1 1 calc R U . . .
C17 C 0.0940(4) 0.15522(12) 0.0962(3) 0.0163(7) Uani 1 1 d . . . . .
C18 C -0.1607(4) 0.18152(13) 0.1796(3) 0.0211(8) Uani 1 1 d . . . . .
C19 C -0.1394(4) 0.15448(13) 0.2813(3) 0.0242(9) Uani 1 1 d . . . . .
C20 C -0.3018(4) 0.20618(14) 0.1588(3) 0.0284(9) Uani 1 1 d . . . . .
H20 H -0.3143 0.2237 0.0915 0.034 Uiso 1 1 calc R U . . .
C21 C -0.4241(5) 0.20459(15) 0.2389(4) 0.0366(11) Uani 1 1 d . . . . .
H21 H -0.5193 0.2208 0.2249 0.044 Uiso 1 1 calc R U . . .
C22 C -0.4046(5) 0.17898(15) 0.3396(4) 0.0388(11) Uani 1 1 d . . . . .
H22 H -0.4859 0.1785 0.3939 0.047 Uiso 1 1 calc R U . . .
C23 C -0.2645(5) 0.15405(14) 0.3599(3) 0.0320(10) Uani 1 1 d . . . . .
H23 H -0.2536 0.1366 0.4276 0.038 Uiso 1 1 calc R U . . .
C24 C 0.3356(5) 0.10170(16) 0.4703(4) 0.0362(11) Uani 1 1 d . . . . .
H24 H 0.4230 0.0814 0.4665 0.043 Uiso 1 1 calc R U . . .
C25 C 0.3232(5) 0.13005(16) 0.5655(3) 0.0360(11) Uani 1 1 d . . . . .
H25 H 0.3992 0.1289 0.6246 0.043 Uiso 1 1 calc R U . . .
C26 C 0.1935(6) 0.16035(15) 0.5706(3) 0.0385(12) Uani 1 1 d . . . . .
H26 H 0.1819 0.1804 0.6336 0.046 Uiso 1 1 calc R U . . .
C27 C 0.0809(5) 0.16089(14) 0.4821(3) 0.0338(10) Uani 1 1 d . . . . .
H27 H -0.0065 0.1812 0.4848 0.041 Uiso 1 1 calc R U . . .
C28 C 0.1012(5) 0.13008(14) 0.3879(3) 0.0270(9) 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 C17 1.866(3) . ?
Ni1 C6 1.884(4) . ?
Ni1 N6 1.890(3) . ?
Ni1 N1 1.965(3) . ?
F1 P1 1.607(2) . ?
F2 P1 1.605(2) . ?
F3 P1 1.605(2) . ?
F4 P1 1.589(3) . ?
F5 P1 1.579(2) . ?
F6 P1 1.607(3) . ?
N1 C1 1.345(5) . ?
N1 C5 1.346(5) . ?
N2 C6 1.386(4) . ?
N2 C12 1.402(5) . ?
N2 C5 1.405(5) . ?
N3 C6 1.341(5) . ?
N3 C11 1.409(4) . ?
N3 C13 1.468(4) . ?
N4 C17 1.319(4) . ?
N4 C14 1.446(4) . ?
N4 C15 1.474(4) . ?
N5 C17 1.348(4) . ?
N5 C18 1.411(5) . ?
N5 C16 1.491(4) . ?
N6 C28 1.376(4) . ?
N6 C19 1.405(5) . ?
N7 C24 1.350(5) . ?
N7 C28 1.353(5) . ?
C1 C2 1.380(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.376(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.394(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.379(5) . ?
C4 H4 0.9300 . ?
C7 C8 1.381(6) . ?
C7 C12 1.402(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.392(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.388(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.390(5) . ?
C13 C14 1.513(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.530(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C18 C20 1.388(5) . ?
C18 C19 1.416(5) . ?
C19 C23 1.392(5) . ?
C20 C21 1.386(6) . ?
C20 H20 0.9300 . ?
C21 C22 1.383(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.384(6) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.370(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.383(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.385(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.409(5) . ?
C27 H27 0.9300 . ?

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
C17 Ni1 C6 98.21(15) . . ?
C17 Ni1 N6 85.56(14) . . ?
C6 Ni1 N6 175.39(13) . . ?
C17 Ni1 N1 168.10(12) . . ?
C6 Ni1 N1 81.86(14) . . ?
N6 Ni1 N1 95.00(13) . . ?
C1 N1 C5 118.3(3) . . ?
C1 N1 Ni1 125.9(3) . . ?
C5 N1 Ni1 115.8(2) . . ?
C6 N2 C12 111.1(3) . . ?
C6 N2 C5 116.6(3) . . ?
C12 N2 C5 131.9(3) . . ?
C6 N3 C11 110.6(3) . . ?
C6 N3 C13 127.5(3) . . ?
C11 N3 C13 121.9(3) . . ?
C17 N4 C14 124.9(3) . . ?
C17 N4 C15 113.6(3) . . ?
C14 N4 C15 121.2(3) . . ?
C17 N5 C18 126.0(3) . . ?
C17 N5 C16 111.9(3) . . ?
C18 N5 C16 120.7(3) . . ?
C28 N6 C19 123.2(3) . . ?
C28 N6 Ni1 113.6(3) . . ?
C19 N6 Ni1 121.3(2) . . ?
C24 N7 C28 117.6(3) . . ?
F5 P1 F4 91.26(17) . . ?
F5 P1 F3 178.26(16) . . ?
F4 P1 F3 90.39(14) . . ?
F5 P1 F2 91.11(13) . . ?
F4 P1 F2 90.58(13) . . ?
F3 P1 F2 88.34(12) . . ?
F5 P1 F6 89.78(17) . . ?
F4 P1 F6 178.68(17) . . ?
F3 P1 F6 88.57(15) . . ?
F2 P1 F6 90.22(13) . . ?
F5 P1 F1 90.14(13) . . ?
F4 P1 F1 89.60(12) . . ?
F3 P1 F1 90.40(12) . . ?
F2 P1 F1 178.73(14) . . ?
F6 P1 F1 89.58(12) . . ?
N1 C1 C2 121.7(4) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 119.1(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 118.0(4) . . ?
C5 C4 H4 121.0 . . ?
C3 C4 H4 121.0 . . ?
N1 C5 C4 123.1(4) . . ?
N1 C5 N2 111.6(3) . . ?
C4 C5 N2 125.3(4) . . ?
N3 C6 N2 105.8(3) . . ?
N3 C6 Ni1 139.9(3) . . ?
N2 C6 Ni1 114.1(3) . . ?
C8 C7 C12 116.9(4) . . ?
C8 C7 H7 121.6 . . ?
C12 C7 H7 121.6 . . ?
C7 C8 C9 122.3(4) . . ?
C7 C8 H8 118.8 . . ?
C9 C8 H8 118.8 . . ?
C10 C9 C8 121.2(4) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 116.5(4) . . ?
C9 C10 H10 121.7 . . ?
C11 C10 H10 121.7 . . ?
C12 C11 C10 122.6(3) . . ?
C12 C11 N3 107.5(3) . . ?
C10 C11 N3 129.9(4) . . ?
C11 C12 C7 120.5(4) . . ?
C11 C12 N2 104.9(3) . . ?
C7 C12 N2 134.6(4) . . ?
N3 C13 C14 113.0(3) . . ?
N3 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
N3 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
N4 C14 C13 114.2(3) . . ?
N4 C14 H14A 108.7 . . ?
C13 C14 H14A 108.7 . . ?
N4 C14 H14B 108.7 . . ?
C13 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
N4 C15 C16 102.4(3) . . ?
N4 C15 H15A 111.3 . . ?
C16 C15 H15A 111.3 . . ?
N4 C15 H15B 111.3 . . ?
C16 C15 H15B 111.3 . . ?
H15A C15 H15B 109.2 . . ?
N5 C16 C15 102.5(3) . . ?
N5 C16 H16A 111.3 . . ?
C15 C16 H16A 111.3 . . ?
N5 C16 H16B 111.3 . . ?
C15 C16 H16B 111.3 . . ?
H16A C16 H16B 109.2 . . ?
N4 C17 N5 109.2(3) . . ?
N4 C17 Ni1 128.9(3) . . ?
N5 C17 Ni1 121.8(3) . . ?
C20 C18 N5 120.2(3) . . ?
C20 C18 C19 121.1(4) . . ?
N5 C18 C19 118.6(3) . . ?
C23 C19 N6 123.7(4) . . ?
C23 C19 C18 117.4(4) . . ?
N6 C19 C18 118.7(3) . . ?
C21 C20 C18 119.7(4) . . ?
C21 C20 H20 120.1 . . ?
C18 C20 H20 120.1 . . ?
C22 C21 C20 120.0(4) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C21 C22 C23 120.3(4) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 H22 119.9 . . ?
C22 C23 C19 121.4(4) . . ?
C22 C23 H23 119.3 . . ?
C19 C23 H23 119.3 . . ?
N7 C24 C25 124.6(4) . . ?
N7 C24 H24 117.7 . . ?
C25 C24 H24 117.7 . . ?
C24 C25 C26 117.6(4) . . ?
C24 C25 H25 121.2 . . ?
C26 C25 H25 121.2 . . ?
C25 C26 C27 120.0(4) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C28 118.8(4) . . ?
C26 C27 H27 120.6 . . ?
C28 C27 H27 120.6 . . ?
N7 C28 N6 113.5(3) . . ?
N7 C28 C27 121.3(3) . . ?
N6 C28 C27 125.2(4) . . ?

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
C17 Ni1 N6 C28 -110.1(3) . . . . ?
N1 Ni1 N6 C28 81.8(3) . . . . ?
C17 Ni1 N6 C19 55.1(3) . . . . ?
N1 Ni1 N6 C19 -113.0(3) . . . . ?
C5 N1 C1 C2 2.5(5) . . . . ?
Ni1 N1 C1 C2 179.8(2) . . . . ?
N1 C1 C2 C3 -0.8(5) . . . . ?
C1 C2 C3 C4 -1.2(5) . . . . ?
C2 C3 C4 C5 1.5(5) . . . . ?
C1 N1 C5 C4 -2.1(4) . . . . ?
Ni1 N1 C5 C4 -179.8(2) . . . . ?
C1 N1 C5 N2 178.6(3) . . . . ?
Ni1 N1 C5 N2 0.9(3) . . . . ?
C3 C4 C5 N1 0.1(5) . . . . ?
C3 C4 C5 N2 179.3(3) . . . . ?
C6 N2 C5 N1 0.7(4) . . . . ?
C12 N2 C5 N1 173.4(3) . . . . ?
C6 N2 C5 C4 -178.6(3) . . . . ?
C12 N2 C5 C4 -5.9(5) . . . . ?
C11 N3 C6 N2 0.2(3) . . . . ?
C13 N3 C6 N2 -177.6(3) . . . . ?
C11 N3 C6 Ni1 174.0(3) . . . . ?
C13 N3 C6 Ni1 -3.8(5) . . . . ?
C12 N2 C6 N3 -0.6(3) . . . . ?
C5 N2 C6 N3 173.6(2) . . . . ?
C12 N2 C6 Ni1 -176.20(19) . . . . ?
C5 N2 C6 Ni1 -2.0(3) . . . . ?
C17 Ni1 C6 N3 20.4(4) . . . . ?
N1 Ni1 C6 N3 -171.6(4) . . . . ?
C17 Ni1 C6 N2 -166.1(2) . . . . ?
N1 Ni1 C6 N2 1.9(2) . . . . ?
C12 C7 C8 C9 1.3(5) . . . . ?
C7 C8 C9 C10 -2.8(5) . . . . ?
C8 C9 C10 C11 1.9(5) . . . . ?
C9 C10 C11 C12 0.3(5) . . . . ?
C9 C10 C11 N3 179.0(3) . . . . ?
C6 N3 C11 C12 0.3(3) . . . . ?
C13 N3 C11 C12 178.2(3) . . . . ?
C6 N3 C11 C10 -178.5(3) . . . . ?
C13 N3 C11 C10 -0.6(5) . . . . ?
C10 C11 C12 C7 -1.7(5) . . . . ?
N3 C11 C12 C7 179.3(3) . . . . ?
C10 C11 C12 N2 178.3(3) . . . . ?
N3 C11 C12 N2 -0.6(3) . . . . ?
C8 C7 C12 C11 0.9(4) . . . . ?
C8 C7 C12 N2 -179.2(3) . . . . ?
C6 N2 C12 C11 0.7(3) . . . . ?
C5 N2 C12 C11 -172.3(3) . . . . ?
C6 N2 C12 C7 -179.2(3) . . . . ?
C5 N2 C12 C7 7.8(6) . . . . ?
C6 N3 C13 C14 28.2(5) . . . . ?
C11 N3 C13 C14 -149.3(3) . . . . ?
C17 N4 C14 C13 76.9(4) . . . . ?
C15 N4 C14 C13 -95.7(4) . . . . ?
N3 C13 C14 N4 -80.3(4) . . . . ?
C17 N4 C15 C16 6.7(4) . . . . ?
C14 N4 C15 C16 -179.9(3) . . . . ?
C17 N5 C16 C15 3.9(3) . . . . ?
C18 N5 C16 C15 171.5(3) . . . . ?
N4 C15 C16 N5 -5.8(3) . . . . ?
C14 N4 C17 N5 -177.6(3) . . . . ?
C15 N4 C17 N5 -4.4(4) . . . . ?
C14 N4 C17 Ni1 -1.8(5) . . . . ?
C15 N4 C17 Ni1 171.3(2) . . . . ?
C18 N5 C17 N4 -166.8(3) . . . . ?
C16 N5 C17 N4 0.1(4) . . . . ?
C18 N5 C17 Ni1 17.2(4) . . . . ?
C16 N5 C17 Ni1 -176.0(2) . . . . ?
C6 Ni1 C17 N4 -36.9(3) . . . . ?
N6 Ni1 C17 N4 140.5(3) . . . . ?
N1 Ni1 C17 N4 -126.3(6) . . . . ?
C6 Ni1 C17 N5 138.4(3) . . . . ?
N6 Ni1 C17 N5 -44.3(3) . . . . ?
N1 Ni1 C17 N5 48.9(8) . . . . ?
C17 N5 C18 C20 -164.0(3) . . . . ?
C16 N5 C18 C20 30.3(5) . . . . ?
C17 N5 C18 C19 18.7(5) . . . . ?
C16 N5 C18 C19 -147.1(3) . . . . ?
C28 N6 C19 C23 -58.0(5) . . . . ?
Ni1 N6 C19 C23 138.2(3) . . . . ?
C28 N6 C19 C18 126.6(4) . . . . ?
Ni1 N6 C19 C18 -37.1(4) . . . . ?
C20 C18 C19 C23 -0.7(5) . . . . ?
N5 C18 C19 C23 176.6(3) . . . . ?
C20 C18 C19 N6 174.9(3) . . . . ?
N5 C18 C19 N6 -7.8(5) . . . . ?
N5 C18 C20 C21 -177.0(3) . . . . ?
C19 C18 C20 C21 0.3(5) . . . . ?
C18 C20 C21 C22 0.7(6) . . . . ?
C20 C21 C22 C23 -1.3(6) . . . . ?
C21 C22 C23 C19 0.9(6) . . . . ?
N6 C19 C23 C22 -175.2(3) . . . . ?
C18 C19 C23 C22 0.1(5) . . . . ?
C28 N7 C24 C25 -1.2(6) . . . . ?
N7 C24 C25 C26 -0.3(7) . . . . ?
C24 C25 C26 C27 0.8(6) . . . . ?
C25 C26 C27 C28 0.2(6) . . . . ?
C24 N7 C28 N6 179.9(3) . . . . ?
C24 N7 C28 C27 2.2(6) . . . . ?
C19 N6 C28 N7 -179.1(3) . . . . ?
Ni1 N6 C28 N7 -14.3(4) . . . . ?
C19 N6 C28 C27 -1.5(6) . . . . ?
Ni1 N6 C28 C27 163.3(3) . . . . ?
C26 C27 C28 N7 -1.7(6) . . . . ?
C26 C27 C28 N6 -179.2(4) . . . . ?

_refine_diff_density_max         1.012
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.093



####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 1839752'
_audit_update_record             
;
2018-05-04 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H31 F12 N9 P2 Pd'
_chemical_formula_weight         938.00


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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.6723(12)
_cell_length_b                   13.3927(12)
_cell_length_c                   19.2473(15)
_cell_angle_alpha                90
_cell_angle_beta                 108.953(2)
_cell_angle_gamma                90
_cell_volume                     3577.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9621
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      32.97

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_F_000             1880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.370
_exptl_absorpt_coefficient_mu    0.711
_shelx_estimated_absorpt_T_min   0.764
_shelx_estimated_absorpt_T_max   0.779
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23460
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.113
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_full        25.020
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6298
_reflns_number_gt                5527
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+10.8419P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6298
_refine_ls_number_parameters     520
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1177
_refine_ls_wR_factor_gt          0.1135
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.127
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.10921(2) 0.24825(2) 0.01604(2) 0.02032(11) Uani 1 1 d . . . . .
P1 P 0.01765(9) 0.72962(8) 0.23428(6) 0.0315(3) Uani 1 1 d . . . . .
P2 P 0.46158(9) 0.70669(11) 0.48719(7) 0.0421(3) Uani 1 1 d . . . . .
F1 F 0.1222(2) 0.6858(2) 0.27369(16) 0.0550(8) Uani 1 1 d . . . . .
F2 F -0.0879(2) 0.7728(2) 0.19468(15) 0.0512(7) Uani 1 1 d . . . . .
F3 F 0.0032(2) 0.74442(19) 0.31265(13) 0.0460(7) Uani 1 1 d . . . . .
F4 F -0.0267(2) 0.61893(19) 0.23067(13) 0.0432(7) Uani 1 1 d . . . . .
F5 F 0.0313(2) 0.7126(2) 0.15611(14) 0.0516(8) Uani 1 1 d . . . . .
F6 F 0.0600(2) 0.8397(2) 0.23785(15) 0.0517(7) Uani 1 1 d . . . . .
F7 F 0.4599(2) 0.7957(3) 0.43173(19) 0.0606(9) Uani 1 1 d . . . . .
F8 F 0.4643(3) 0.6161(3) 0.5409(2) 0.0857(12) Uani 1 1 d . . . . .
F9 F 0.3872(5) 0.7642(4) 0.5150(4) 0.097(2) Uani 0.813(4) 1 d . U P A 1
F10 F 0.3774(3) 0.6533(4) 0.4269(3) 0.0845(16) Uani 0.813(4) 1 d . . P A 1
F11 F 0.5371(3) 0.6498(3) 0.4560(3) 0.0660(12) Uani 0.813(4) 1 d . . P A 1
F12 F 0.5495(4) 0.7624(5) 0.5441(3) 0.099(2) Uani 0.813(4) 1 d . U P A 1
F9' F 0.345(2) 0.716(2) 0.4626(18) 0.097(2) Uani 0.187(4) 1 d . . P A 2
F10' F 0.4526(14) 0.6348(17) 0.4217(12) 0.0845(16) Uani 0.187(4) 1 d . . P A 2
F11' F 0.5654(14) 0.6881(16) 0.5158(13) 0.0660(12) Uani 0.187(4) 1 d . . P A 2
F12' F 0.464(2) 0.773(2) 0.5573(11) 0.099(2) Uani 0.187(4) 1 d . . P A 2
N1 N 0.1526(2) 0.1345(2) -0.03876(16) 0.0236(7) Uani 1 1 d . . . . .
N2 N -0.0064(2) 0.0914(2) -0.06542(15) 0.0217(7) Uani 1 1 d . . . . .
N3 N -0.1041(2) 0.1824(2) -0.02681(16) 0.0239(7) Uani 1 1 d . . . . .
N4 N -0.0174(2) 0.3930(3) 0.05789(17) 0.0252(7) Uani 1 1 d . . . . .
N5 N 0.1275(2) 0.3849(2) 0.13709(17) 0.0258(7) Uani 1 1 d . . . . .
N6 N 0.2392(2) 0.3204(3) 0.05230(17) 0.0253(7) Uani 1 1 d . . . . .
N7 N 0.3453(3) 0.4457(3) 0.0388(2) 0.0404(9) Uani 1 1 d . . . . .
H7N H 0.3704 0.4492 0.0857 0.048 Uiso 1 1 calc R U . . .
N8 N 0.2724(5) 0.6581(6) 0.1619(4) 0.092(2) Uani 1 1 d . . . . .
N9 N 0.4852(6) 0.5064(6) 0.1843(4) 0.115(3) Uani 1 1 d . . . . .
C1 C 0.2429(3) 0.1208(3) -0.0390(2) 0.0292(9) Uani 1 1 d . . . . .
H1 H 0.2902 0.1664 -0.0145 0.035 Uiso 1 1 calc R U . . .
C2 C 0.2679(3) 0.0415(3) -0.0744(2) 0.0335(10) Uani 1 1 d . . . . .
H2 H 0.3311 0.0328 -0.0735 0.040 Uiso 1 1 calc R U . . .
C3 C 0.1966(3) -0.0248(3) -0.1112(2) 0.0346(10) Uani 1 1 d . . . . .
H3 H 0.2116 -0.0784 -0.1362 0.042 Uiso 1 1 calc R U . . .
C4 C 0.1035(3) -0.0123(3) -0.1112(2) 0.0311(9) Uani 1 1 d . . . . .
H4 H 0.0551 -0.0567 -0.1359 0.037 Uiso 1 1 calc R U . . .
C5 C 0.0838(3) 0.0688(3) -0.07312(19) 0.0231(8) Uani 1 1 d . . . . .
C6 C -0.0125(3) 0.1741(3) -0.02400(18) 0.0204(7) Uani 1 1 d . . . . .
C7 C -0.1586(3) 0.1034(3) -0.0687(2) 0.0270(9) Uani 1 1 d . . . . .
C8 C -0.0971(3) 0.0468(3) -0.09462(19) 0.0245(8) Uani 1 1 d . . . . .
C9 C -0.1311(3) -0.0357(3) -0.1397(2) 0.0297(9) Uani 1 1 d . . . . .
H9 H -0.0910 -0.0731 -0.1584 0.036 Uiso 1 1 calc R U . . .
C10 C -0.2270(3) -0.0592(4) -0.1552(2) 0.0391(11) Uani 1 1 d . . . . .
H10 H -0.2521 -0.1141 -0.1847 0.047 Uiso 1 1 calc R U . . .
C11 C -0.2877(3) -0.0028(4) -0.1277(3) 0.0443(12) Uani 1 1 d . . . . .
H11 H -0.3519 -0.0216 -0.1394 0.053 Uiso 1 1 calc R U . . .
C12 C -0.2556(3) 0.0801(4) -0.0838(2) 0.0355(10) Uani 1 1 d . . . . .
H12 H -0.2960 0.1178 -0.0656 0.043 Uiso 1 1 calc R U . . .
C13 C -0.1444(3) 0.2624(3) 0.0058(2) 0.0298(9) Uani 1 1 d . . . . .
H13A H -0.1311 0.2485 0.0576 0.036 Uiso 1 1 calc R U . . .
H13B H -0.2138 0.2636 -0.0174 0.036 Uiso 1 1 calc R U . . .
C14 C -0.1035(3) 0.3654(3) -0.0026(2) 0.0285(9) Uani 1 1 d . . . . .
H14A H -0.0881 0.3663 -0.0480 0.034 Uiso 1 1 calc R U . . .
H14B H -0.1529 0.4153 -0.0068 0.034 Uiso 1 1 calc R U . . .
C17 C 0.0674(3) 0.3495(3) 0.0732(2) 0.0230(8) Uani 1 1 d . . . . .
C16 C 0.0792(3) 0.4579(3) 0.1717(2) 0.0298(9) Uani 1 1 d . . . . .
H16A H 0.1112 0.5222 0.1784 0.036 Uiso 1 1 calc R U . . .
H16B H 0.0773 0.4339 0.2188 0.036 Uiso 1 1 calc R U . . .
C15 C -0.0219(3) 0.4638(3) 0.1153(2) 0.0304(9) Uani 1 1 d . . . . .
H15A H -0.0704 0.4438 0.1368 0.037 Uiso 1 1 calc R U . . .
H15B H -0.0361 0.5309 0.0957 0.037 Uiso 1 1 calc R U . . .
C18 C 0.2233(3) 0.3514(3) 0.1722(2) 0.0287(9) Uani 1 1 d . . . . .
C19 C 0.2808(3) 0.3215(3) 0.1300(2) 0.0280(9) Uani 1 1 d . . . . .
C20 C 0.3733(3) 0.2860(4) 0.1653(3) 0.0393(11) Uani 1 1 d . . . . .
H20 H 0.4121 0.2672 0.1377 0.047 Uiso 1 1 calc R U . . .
C21 C 0.4085(4) 0.2784(5) 0.2413(3) 0.0508(13) Uani 1 1 d . . . . .
H21 H 0.4701 0.2536 0.2645 0.061 Uiso 1 1 calc R U . . .
C22 C 0.3513(4) 0.3081(5) 0.2825(3) 0.0528(14) Uani 1 1 d . . . . .
H22 H 0.3749 0.3034 0.3335 0.063 Uiso 1 1 calc R U . . .
C23 C 0.2600(3) 0.3444(4) 0.2487(2) 0.0415(11) Uani 1 1 d . . . . .
H23 H 0.2224 0.3645 0.2769 0.050 Uiso 1 1 calc R U . . .
C28 C 0.2725(3) 0.3787(3) 0.0099(2) 0.0276(9) Uani 1 1 d . . . . .
C27 C 0.2329(3) 0.3755(3) -0.0676(2) 0.0326(9) Uani 1 1 d . . . . .
H27 H 0.1824 0.3321 -0.0898 0.039 Uiso 1 1 calc R U . . .
C26 C 0.2681(4) 0.4356(5) -0.1099(3) 0.0576(15) Uani 1 1 d . . . . .
H26 H 0.2428 0.4322 -0.1609 0.069 Uiso 1 1 calc R U . . .
C25 C 0.3436(4) 0.5035(5) -0.0759(4) 0.0698(19) Uani 1 1 d . . . . .
H25 H 0.3678 0.5454 -0.1042 0.084 Uiso 1 1 calc R U . . .
C24 C 0.3798(4) 0.5065(5) -0.0025(3) 0.0589(15) Uani 1 1 d . . . . .
H24 H 0.4291 0.5510 0.0202 0.071 Uiso 1 1 calc R U . . .
C29 C 0.2861(5) 0.7214(7) 0.2050(4) 0.076(2) Uani 1 1 d . . . . .
C30 C 0.3015(5) 0.8001(6) 0.2592(4) 0.083(2) Uani 1 1 d . . . . .
H30A H 0.2450 0.8413 0.2478 0.125 Uiso 1 1 calc R U . . .
H30B H 0.3556 0.8399 0.2587 0.125 Uiso 1 1 calc R U . . .
H30C H 0.3140 0.7711 0.3070 0.125 Uiso 1 1 calc R U . . .
C31 C 0.4676(5) 0.5215(5) 0.2379(4) 0.0751(19) Uani 1 1 d . . . . .
C32 C 0.4413(6) 0.5431(6) 0.3047(4) 0.087(2) Uani 1 1 d . . . . .
H32A H 0.4714 0.6042 0.3265 0.130 Uiso 1 1 calc R U . . .
H32B H 0.4630 0.4894 0.3392 0.130 Uiso 1 1 calc R U . . .
H32C H 0.3726 0.5495 0.2914 0.130 Uiso 1 1 calc R U . . .


_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
Pd1 C17 1.965(4) . ?
Pd1 C6 1.968(4) . ?
Pd1 N6 2.048(3) . ?
Pd1 N1 2.067(3) . ?
P1 F1 1.587(3) . ?
P1 F6 1.593(3) . ?
P1 F2 1.596(3) . ?
P1 F5 1.597(3) . ?
P1 F3 1.602(3) . ?
P1 F4 1.611(3) . ?
P2 F11' 1.463(19) . ?
P2 F10' 1.56(2) . ?
P2 F10 1.566(4) . ?
P2 F9 1.566(5) . ?
P2 F12 1.582(5) . ?
P2 F8 1.587(4) . ?
P2 F7 1.594(3) . ?
P2 F12' 1.61(3) . ?
P2 F11 1.612(4) . ?
P2 F9' 1.62(3) . ?
N1 C1 1.339(5) . ?
N1 C5 1.341(5) . ?
N2 C6 1.384(5) . ?
N2 C8 1.399(5) . ?
N2 C5 1.413(5) . ?
N3 C6 1.332(5) . ?
N3 C7 1.410(5) . ?
N3 C13 1.461(5) . ?
N4 C17 1.318(5) . ?
N4 C14 1.460(5) . ?
N4 C15 1.474(5) . ?
N5 C17 1.346(5) . ?
N5 C18 1.421(5) . ?
N5 C16 1.486(5) . ?
N6 C28 1.332(5) . ?
N6 C19 1.421(5) . ?
N7 C24 1.345(6) . ?
N7 C28 1.367(5) . ?
N7 H7N 0.8600 . ?
N8 C29 1.156(10) . ?
N9 C31 1.160(9) . ?
C1 C2 1.373(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.380(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.391(6) . ?
C4 H4 0.9300 . ?
C7 C8 1.389(6) . ?
C7 C12 1.392(6) . ?
C8 C9 1.393(6) . ?
C9 C10 1.377(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.396(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.382(7) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.533(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 C15 1.530(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C18 C23 1.397(6) . ?
C18 C19 1.405(6) . ?
C19 C20 1.390(6) . ?
C20 C21 1.388(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.386(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.374(7) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C28 C27 1.416(6) . ?
C27 C26 1.360(7) . ?
C27 H27 0.9300 . ?
C26 C25 1.418(9) . ?
C26 H26 0.9300 . ?
C25 C24 1.339(8) . ?
C25 H25 0.9300 . ?
C24 H24 0.9300 . ?
C29 C30 1.448(11) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.485(10) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 Pd1 C6 99.15(16) . . ?
C17 Pd1 N6 84.79(14) . . ?
C6 Pd1 N6 175.92(13) . . ?
C17 Pd1 N1 176.05(14) . . ?
C6 Pd1 N1 79.56(14) . . ?
N6 Pd1 N1 96.57(12) . . ?
F1 P1 F6 91.04(17) . . ?
F1 P1 F2 179.54(19) . . ?
F6 P1 F2 89.42(17) . . ?
F1 P1 F5 89.99(17) . . ?
F6 P1 F5 90.35(16) . . ?
F2 P1 F5 90.05(17) . . ?
F1 P1 F3 89.91(17) . . ?
F6 P1 F3 90.79(15) . . ?
F2 P1 F3 90.03(17) . . ?
F5 P1 F3 178.85(17) . . ?
F1 P1 F4 89.71(17) . . ?
F6 P1 F4 179.16(17) . . ?
F2 P1 F4 89.83(17) . . ?
F5 P1 F4 90.03(15) . . ?
F3 P1 F4 88.83(14) . . ?
F11' P2 F10' 90.2(13) . . ?
F10 P2 F9 90.5(4) . . ?
F10 P2 F12 176.3(3) . . ?
F9 P2 F12 91.9(4) . . ?
F11' P2 F8 79.7(8) . . ?
F10' P2 F8 91.9(8) . . ?
F10 P2 F8 88.9(3) . . ?
F9 P2 F8 91.5(3) . . ?
F12 P2 F8 93.8(3) . . ?
F11' P2 F7 99.6(8) . . ?
F10' P2 F7 86.6(8) . . ?
F10 P2 F7 90.5(2) . . ?
F9 P2 F7 90.0(2) . . ?
F12 P2 F7 86.7(2) . . ?
F8 P2 F7 178.4(2) . . ?
F11' P2 F12' 92.3(14) . . ?
F10' P2 F12' 174.3(12) . . ?
F8 P2 F12' 83.6(9) . . ?
F7 P2 F12' 98.0(9) . . ?
F10 P2 F11 88.9(3) . . ?
F9 P2 F11 178.0(3) . . ?
F12 P2 F11 88.7(3) . . ?
F8 P2 F11 90.4(2) . . ?
F7 P2 F11 88.1(2) . . ?
F11' P2 F9' 172.7(12) . . ?
F10' P2 F9' 90.5(13) . . ?
F8 P2 F9' 93.0(9) . . ?
F7 P2 F9' 87.7(9) . . ?
F12' P2 F9' 86.3(15) . . ?
C1 N1 C5 119.6(3) . . ?
C1 N1 Pd1 124.9(3) . . ?
C5 N1 Pd1 115.4(2) . . ?
C6 N2 C8 110.1(3) . . ?
C6 N2 C5 118.0(3) . . ?
C8 N2 C5 131.9(3) . . ?
C6 N3 C7 109.8(3) . . ?
C6 N3 C13 126.0(3) . . ?
C7 N3 C13 124.2(3) . . ?
C17 N4 C14 125.1(3) . . ?
C17 N4 C15 112.7(3) . . ?
C14 N4 C15 121.6(3) . . ?
C17 N5 C18 125.3(3) . . ?
C17 N5 C16 112.0(3) . . ?
C18 N5 C16 122.5(3) . . ?
C28 N6 C19 121.5(3) . . ?
C28 N6 Pd1 123.7(3) . . ?
C19 N6 Pd1 113.4(2) . . ?
C24 N7 C28 123.5(4) . . ?
C24 N7 H7N 118.3 . . ?
C28 N7 H7N 118.3 . . ?
N1 C1 C2 122.1(4) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C1 C2 C3 118.2(4) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 120.6(4) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 118.1(4) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 121.4(4) . . ?
N1 C5 N2 112.8(3) . . ?
C4 C5 N2 125.8(4) . . ?
N3 C6 N2 107.2(3) . . ?
N3 C6 Pd1 138.5(3) . . ?
N2 C6 Pd1 114.2(3) . . ?
C8 C7 C12 122.8(4) . . ?
C8 C7 N3 107.5(3) . . ?
C12 C7 N3 129.7(4) . . ?
C7 C8 C9 120.9(4) . . ?
C7 C8 N2 105.4(3) . . ?
C9 C8 N2 133.7(4) . . ?
C10 C9 C8 116.7(4) . . ?
C10 C9 H9 121.6 . . ?
C8 C9 H9 121.6 . . ?
C9 C10 C11 121.8(4) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 H10 119.1 . . ?
C12 C11 C10 122.2(4) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 C12 C7 115.5(4) . . ?
C11 C12 H12 122.3 . . ?
C7 C12 H12 122.3 . . ?
N3 C13 C14 112.8(3) . . ?
N3 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
N3 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
N4 C14 C13 114.3(3) . . ?
N4 C14 H14A 108.7 . . ?
C13 C14 H14A 108.7 . . ?
N4 C14 H14B 108.7 . . ?
C13 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
N4 C17 N5 109.8(3) . . ?
N4 C17 Pd1 128.6(3) . . ?
N5 C17 Pd1 121.6(3) . . ?
N5 C16 C15 102.2(3) . . ?
N5 C16 H16A 111.3 . . ?
C15 C16 H16A 111.3 . . ?
N5 C16 H16B 111.3 . . ?
C15 C16 H16B 111.3 . . ?
H16A C16 H16B 109.2 . . ?
N4 C15 C16 103.2(3) . . ?
N4 C15 H15A 111.1 . . ?
C16 C15 H15A 111.1 . . ?
N4 C15 H15B 111.1 . . ?
C16 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C23 C18 C19 119.5(4) . . ?
C23 C18 N5 120.4(4) . . ?
C19 C18 N5 120.1(3) . . ?
C20 C19 C18 119.3(4) . . ?
C20 C19 N6 121.8(4) . . ?
C18 C19 N6 118.6(4) . . ?
C21 C20 C19 120.6(4) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C20 119.7(5) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C23 C22 C21 120.6(4) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 C18 120.4(4) . . ?
C22 C23 H23 119.8 . . ?
C18 C23 H23 119.8 . . ?
N6 C28 N7 122.0(4) . . ?
N6 C28 C27 121.4(4) . . ?
N7 C28 C27 116.6(4) . . ?
C26 C27 C28 120.5(5) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C26 C25 119.6(5) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C24 C25 C26 119.3(5) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C25 C24 N7 120.6(5) . . ?
C25 C24 H24 119.7 . . ?
N7 C24 H24 119.7 . . ?
N8 C29 C30 178.9(9) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N9 C31 C32 177.6(9) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

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
C5 N1 C1 C2 0.8(6) . . . . ?
Pd1 N1 C1 C2 177.5(3) . . . . ?
N1 C1 C2 C3 0.7(7) . . . . ?
C1 C2 C3 C4 -1.1(7) . . . . ?
C2 C3 C4 C5 0.0(6) . . . . ?
C1 N1 C5 C4 -2.0(6) . . . . ?
Pd1 N1 C5 C4 -179.0(3) . . . . ?
C1 N1 C5 N2 177.7(3) . . . . ?
Pd1 N1 C5 N2 0.6(4) . . . . ?
C3 C4 C5 N1 1.6(6) . . . . ?
C3 C4 C5 N2 -178.0(4) . . . . ?
C6 N2 C5 N1 -1.1(5) . . . . ?
C8 N2 C5 N1 176.4(3) . . . . ?
C6 N2 C5 C4 178.5(4) . . . . ?
C8 N2 C5 C4 -4.0(6) . . . . ?
C7 N3 C6 N2 1.5(4) . . . . ?
C13 N3 C6 N2 -176.4(3) . . . . ?
C7 N3 C6 Pd1 176.9(3) . . . . ?
C13 N3 C6 Pd1 -1.0(6) . . . . ?
C8 N2 C6 N3 -0.2(4) . . . . ?
C5 N2 C6 N3 177.8(3) . . . . ?
C8 N2 C6 Pd1 -176.9(2) . . . . ?
C5 N2 C6 Pd1 1.1(4) . . . . ?
C6 N3 C7 C8 -2.2(4) . . . . ?
C13 N3 C7 C8 175.7(3) . . . . ?
C6 N3 C7 C12 177.3(4) . . . . ?
C13 N3 C7 C12 -4.8(6) . . . . ?
C12 C7 C8 C9 2.0(6) . . . . ?
N3 C7 C8 C9 -178.4(3) . . . . ?
C12 C7 C8 N2 -177.6(4) . . . . ?
N3 C7 C8 N2 2.0(4) . . . . ?
C6 N2 C8 C7 -1.1(4) . . . . ?
C5 N2 C8 C7 -178.8(3) . . . . ?
C6 N2 C8 C9 179.3(4) . . . . ?
C5 N2 C8 C9 1.6(7) . . . . ?
C7 C8 C9 C10 -1.7(6) . . . . ?
N2 C8 C9 C10 177.8(4) . . . . ?
C8 C9 C10 C11 0.5(6) . . . . ?
C9 C10 C11 C12 0.4(7) . . . . ?
C10 C11 C12 C7 -0.1(7) . . . . ?
C8 C7 C12 C11 -1.1(6) . . . . ?
N3 C7 C12 C11 179.5(4) . . . . ?
C6 N3 C13 C14 39.8(5) . . . . ?
C7 N3 C13 C14 -137.8(4) . . . . ?
C17 N4 C14 C13 67.7(5) . . . . ?
C15 N4 C14 C13 -102.6(4) . . . . ?
N3 C13 C14 N4 -90.2(4) . . . . ?
C14 N4 C17 N5 -172.7(3) . . . . ?
C15 N4 C17 N5 -1.6(5) . . . . ?
C14 N4 C17 Pd1 7.5(6) . . . . ?
C15 N4 C17 Pd1 178.6(3) . . . . ?
C18 N5 C17 N4 176.8(4) . . . . ?
C16 N5 C17 N4 2.3(5) . . . . ?
C18 N5 C17 Pd1 -3.4(5) . . . . ?
C16 N5 C17 Pd1 -177.9(3) . . . . ?
C17 N5 C16 C15 -1.9(4) . . . . ?
C18 N5 C16 C15 -176.6(4) . . . . ?
C17 N4 C15 C16 0.4(4) . . . . ?
C14 N4 C15 C16 171.8(3) . . . . ?
N5 C16 C15 N4 0.9(4) . . . . ?
C17 N5 C18 C23 -142.9(4) . . . . ?
C16 N5 C18 C23 31.1(6) . . . . ?
C17 N5 C18 C19 34.8(6) . . . . ?
C16 N5 C18 C19 -151.3(4) . . . . ?
C23 C18 C19 C20 -0.3(7) . . . . ?
N5 C18 C19 C20 -178.1(4) . . . . ?
C23 C18 C19 N6 174.3(4) . . . . ?
N5 C18 C19 N6 -3.4(6) . . . . ?
C28 N6 C19 C20 -68.1(6) . . . . ?
Pd1 N6 C19 C20 125.3(4) . . . . ?
C28 N6 C19 C18 117.5(4) . . . . ?
Pd1 N6 C19 C18 -49.2(5) . . . . ?
C18 C19 C20 C21 1.1(7) . . . . ?
N6 C19 C20 C21 -173.3(5) . . . . ?
C19 C20 C21 C22 -1.1(9) . . . . ?
C20 C21 C22 C23 0.4(9) . . . . ?
C21 C22 C23 C18 0.4(9) . . . . ?
C19 C18 C23 C22 -0.4(7) . . . . ?
N5 C18 C23 C22 177.3(5) . . . . ?
C19 N6 C28 N7 -2.9(6) . . . . ?
Pd1 N6 C28 N7 162.3(3) . . . . ?
C19 N6 C28 C27 178.2(4) . . . . ?
Pd1 N6 C28 C27 -16.5(5) . . . . ?
C24 N7 C28 N6 -179.2(5) . . . . ?
C24 N7 C28 C27 -0.3(7) . . . . ?
N6 C28 C27 C26 -179.9(5) . . . . ?
N7 C28 C27 C26 1.2(6) . . . . ?
C28 C27 C26 C25 -1.5(8) . . . . ?
C27 C26 C25 C24 0.7(10) . . . . ?
C26 C25 C24 N7 0.2(10) . . . . ?
C28 N7 C24 C25 -0.5(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C32 H32B F8 0.96 2.62 3.552(9) 164.2 3_666
C32 H32A F10' 0.96 1.98 2.52(3) 113.5 .
C32 H32A F11 0.96 2.44 3.137(9) 129.3 .
C23 H23 F2 0.93 2.53 3.205(6) 129.6 2_545
C13 H13B F9' 0.97 2.56 3.25(2) 128.7 2_545
C13 H13B F9 0.97 2.56 3.452(7) 153.3 2_545
C13 H13A F3 0.97 2.59 3.444(5) 146.7 2_545
C4 H4 F4 0.93 2.59 3.344(5) 138.0 4_565
C2 H2 F11' 0.93 2.60 3.052(19) 110.4 2_645
C2 H2 F10 0.93 2.58 3.061(6) 112.4 4_565
C1 H1 N6 0.93 2.66 3.209(5) 118.3 .
C1 H1 F11' 0.93 2.15 2.848(18) 131.3 2_645
C1 H1 F11 0.93 2.43 3.127(6) 132.1 2_645
N7 H7N N9 0.86 2.22 2.998(8) 149.6 .
N7 H7N N9 0.86 2.22 2.998(8) 149.6 .
C1 H1 F11 0.93 2.43 3.127(6) 132.1 2_645
C1 H1 F11' 0.93 2.15 2.848(18) 131.3 2_645
C1 H1 N6 0.93 2.66 3.209(5) 118.3 .
C2 H2 F10 0.93 2.58 3.061(6) 112.4 4_565
C2 H2 F11' 0.93 2.60 3.052(19) 110.4 2_645
C4 H4 F4 0.93 2.59 3.344(5) 138.0 4_565
C13 H13A F3 0.97 2.59 3.444(5) 146.7 2_545
C13 H13B F9 0.97 2.56 3.452(7) 153.3 2_545
C13 H13B F9' 0.97 2.56 3.25(2) 128.7 2_545
C23 H23 F2 0.93 2.53 3.205(6) 129.6 2_545
C27 H27 F2 0.93 2.48 3.328(5) 151.6 3_565
C25 H25 F7 0.93 2.50 3.164(7) 128.9 4_575
C24 H24 F9 0.93 2.54 3.088(8) 117.6 4_575
C24 H24 F12' 0.93 2.47 3.26(3) 143.6 4_575
C32 H32A F11 0.96 2.44 3.137(9) 129.3 .
C32 H32A F10' 0.96 1.98 2.52(3) 113.5 .
C32 H32B F8 0.96 2.62 3.552(9) 164.2 3_666
N7 H7N N9 0.86 2.22 2.998(8) 149.6 .
C1 H1 F11 0.93 2.43 3.127(6) 132.1 2_645
C1 H1 F11' 0.93 2.15 2.848(18) 131.3 2_645
C1 H1 N6 0.93 2.66 3.209(5) 118.3 .
C2 H2 F10 0.93 2.58 3.061(6) 112.4 4_565
C2 H2 F11' 0.93 2.60 3.052(19) 110.4 2_645
C4 H4 F4 0.93 2.59 3.344(5) 138.0 4_565
C13 H13A F3 0.97 2.59 3.444(5) 146.7 2_545
C13 H13B F9 0.97 2.56 3.452(7) 153.3 2_545
C13 H13B F9' 0.97 2.56 3.25(2) 128.7 2_545
C23 H23 F2 0.93 2.53 3.205(6) 129.6 2_545
C27 H27 F2 0.93 2.48 3.328(5) 151.6 3_565
C25 H25 F7 0.93 2.50 3.164(7) 128.9 4_575
C24 H24 F9 0.93 2.54 3.088(8) 117.6 4_575
C24 H24 F12' 0.93 2.47 3.26(3) 143.6 4_575
C32 H32A F11 0.96 2.44 3.137(9) 129.3 .
C32 H32A F10' 0.96 1.98 2.52(3) 113.5 .
C32 H32B F8 0.96 2.62 3.552(9) 164.2 3_666

_refine_diff_density_max         0.668
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.094

