# Electronic Supplementary Material (ESI) for ChemComm.
# 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_altph27_0m
_database_code_depnum_ccdc_archive 'CCDC 1448008'
_audit_update_record             
;
2016-01-17 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H32 N12, 4(F6 P), C2 H3 N'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C28 H35 F24 N13 P4'
_chemical_formula_iupac          ?
_chemical_formula_weight         1133.57
_chemical_compound_source        'see text'

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'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_Int_Tables_number      15

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z

_cell_length_a                   23.2328(16)
_cell_length_b                   9.5152(6)
_cell_length_c                   20.7638(14)
_cell_angle_alpha                90
_cell_angle_beta                 112.516(3)
_cell_angle_gamma                90
_cell_volume                     4240.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    123
_cell_measurement_reflns_used    9473
_cell_measurement_theta_min      2.3414
_cell_measurement_theta_max      29.6318
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'clear colorless'

_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.081
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             2280
_exptl_absorpt_coefficient_mu    0.328
_exptl_crystal_density_meas_temp ?

# Permitted for _exptl_absorpt_correction_type :
# analytical     'analytical from crystal shape'
#                Example: de Meulenaer&Tompa: ABST
# cylinder       'cylindrical'
# gaussian       'Gaussian from crystal shape'
#                Example: PLATON/ABSG
# integration    'integration from crystal shape'
# multi-scan     'symmetry-related measurements'
#                Example: SADABS, MULABS
# none           'no absorption corr. applied'
# numerical      'numerical from crystal shape'
# psi-scan       'psi-scan corrections'
#                Example: PLATON/ABSP
# refdelf        'refined from delta-F'
#                Example: SHELXA,
# sphere         'spherical'
#                Example: PLATON/ABSS
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.6790
_exptl_absorpt_correction_T_max  0.7459

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           10 s per frame
dx                                  46 mm
XYZ frames measured in XYZ data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      123
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_monochromator  'MONTEL optic'

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            68857
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             5704
# number of observed reflections (> n sig(I))
_reflns_number_gt                4899
_reflns_threshold_expression     i>2σ(i)

_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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     
'W=1/[Σ²(FO²)+(0.0658P)²+4.6537P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom


# Permitted for _refine_ls_hydrogen_treatment :
# refall            - refined all H-atom parameters
# refxyz            - refined H-atom coordinates only
# refU              - refined H-atom U only
# noref             - no refinement of H-atom parameters
# constr            - H-atom parameters constrained
# hetero            - H-atom parameters constrained for H on C,
#                     all H-atom parameters refined for H on
#                     heteroatoms
# heteroxyz         - H-atom parameters constrained for H on C,
#                     refined H-atom coordinates only for H
#                     on heteroatoms
# heteroU           - H-atom parameters constrained for H on C,
#                     refined H-atom U's only for H on
#                     heteroatoms
# heteronoref       - H-atom parameters constrained for H on C,
#                     no refinement of H-atom parameters for
#                     H on heteroatoms
# hetero-mixed      - H-atom parameters constrained for H on C
#                     and some heteroatoms, all H-atom
#                     parameters refined for H on remaining
#                     heteroatoms.
# heteroxyz-mixed   - H-atom parameters constrained for H on C
#                     and some heteroatoms, refined H-atom
#                     coordinates only for H on remaining
#                     heteroatoms.
# heteroU-mixed     - H-atom parameters constrained for H on C
#                     and some heteroatoms, refined H-atom
#                     U's only for H on remaining heteroatoms
# heteronoref-mixed - H-atom parameters constrained for H on C
#                     and some heteroatoms, no refinement of
#                     H-atom parameters for H on remaining
#                     heteroatoms
# mixed   - some constrained, some independent
# undef   - H-atom parameters not defined
_refine_ls_hydrogen_treatment    constr

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         5704
_refine_ls_number_parameters     314
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1154
_refine_ls_wR_factor_gt          0.1081
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.080

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
P1 P 0.20868(2) 0.49993(4) 0.40378(2) 0.02526(11) Uani 1 1 d . . . . .
F1 F 0.21902(5) 0.59553(11) 0.47032(5) 0.0333(2) Uani 1 1 d . . . . .
F2 F 0.20007(6) 0.40222(15) 0.33844(6) 0.0498(3) Uani 1 1 d . . . . .
F3 F 0.14956(5) 0.42909(13) 0.41168(7) 0.0452(3) Uani 1 1 d . . . . .
F4 F 0.25335(5) 0.38215(11) 0.45347(6) 0.0387(3) Uani 1 1 d . . . . .
F5 F 0.26877(5) 0.57060(12) 0.39644(7) 0.0450(3) Uani 1 1 d . . . . .
F6 F 0.16517(6) 0.61804(14) 0.35392(6) 0.0469(3) Uani 1 1 d . . . . .
P2 P 0.42158(2) 0.74386(4) 0.34934(2) 0.02244(10) Uani 1 1 d . . . . .
F7 F 0.39239(6) 0.85965(11) 0.38381(7) 0.0431(3) Uani 1 1 d . . . . .
F8 F 0.45226(5) 0.62706(11) 0.31626(5) 0.0306(2) Uani 1 1 d . . . . .
F9 F 0.44200(6) 0.65198(10) 0.41906(5) 0.0356(2) Uani 1 1 d . . . . .
F10 F 0.48748(5) 0.82482(11) 0.38069(6) 0.0355(2) Uani 1 1 d . . . . .
F11 F 0.40269(6) 0.83532(12) 0.28042(6) 0.0423(3) Uani 1 1 d . . . . .
F12 F 0.35665(5) 0.66271(12) 0.31808(7) 0.0415(3) Uani 1 1 d . . . . .
N1 N 0.39725(6) 0.32316(14) 0.42000(7) 0.0259(3) Uani 1 1 d . . . . .
N2 N 0.34400(6) 0.35645(14) 0.36686(7) 0.0246(3) Uani 1 1 d . . . . .
H2 H 0.3187 0.4235 0.3691 0.029 Uiso 1 1 calc R U . . .
N3 N 0.29402(6) 0.40707(13) 0.20030(6) 0.0198(2) Uani 1 1 d . . . . .
N4 N 0.34506(6) 0.54144(13) 0.15692(6) 0.0188(2) Uani 1 1 d . . . . .
N5 N 0.41316(6) 0.43948(13) 0.06518(6) 0.0204(2) Uani 1 1 d . . . . .
N6 N 0.46596(6) 0.25438(13) 0.06241(6) 0.0215(2) Uani 1 1 d . . . . .
C1 C 0.48345(7) 0.16196(15) 0.43939(8) 0.0244(3) Uani 1 1 d . . . . .
H1A H 0.4863 0.1532 0.4880 0.029 Uiso 1 1 calc R U . . .
H1B H 0.4885 0.0670 0.4228 0.029 Uiso 1 1 calc R U . . .
C2 C 0.42117(7) 0.21847(15) 0.39504(8) 0.0211(3) Uani 1 1 d . . . . .
C3 C 0.38264(7) 0.18477(15) 0.32609(8) 0.0224(3) Uani 1 1 d . . . . .
H3 H 0.3893 0.1143 0.2972 0.027 Uiso 1 1 calc R U . . .
C4 C 0.33323(7) 0.27626(15) 0.30953(8) 0.0208(3) Uani 1 1 d . . . . .
C5 C 0.27903(7) 0.29978(16) 0.24315(8) 0.0239(3) Uani 1 1 d . . . . .
H5A H 0.2677 0.2104 0.2168 0.029 Uiso 1 1 calc R U . . .
H5B H 0.2428 0.3313 0.2534 0.029 Uiso 1 1 calc R U . . .
C6 C 0.35072(7) 0.44296(15) 0.20446(7) 0.0193(3) Uani 1 1 d . . . . .
H6 H 0.3888 0.4047 0.2361 0.023 Uiso 1 1 calc R U . . .
C7 C 0.25067(7) 0.48506(18) 0.14810(8) 0.0273(3) Uani 1 1 d . . . . .
H7 H 0.2067 0.4803 0.1338 0.033 Uiso 1 1 calc R U . . .
C8 C 0.28257(7) 0.56944(18) 0.12116(9) 0.0275(3) Uani 1 1 d . . . . .
H8 H 0.2653 0.6356 0.0845 0.033 Uiso 1 1 calc R U . . .
C9 C 0.39768(7) 0.61120(15) 0.14726(7) 0.0205(3) Uani 1 1 d . . . . .
H9A H 0.4372 0.5762 0.1828 0.025 Uiso 1 1 calc R U . . .
H9B H 0.3954 0.7136 0.1545 0.025 Uiso 1 1 calc R U . . .
C10 C 0.39804(7) 0.58553(15) 0.07516(7) 0.0212(3) Uani 1 1 d . . . . .
H10A H 0.3565 0.6091 0.0396 0.025 Uiso 1 1 calc R U . . .
H10B H 0.4290 0.6487 0.0681 0.025 Uiso 1 1 calc R U . . .
C11 C 0.46936(7) 0.39272(15) 0.07292(7) 0.0206(3) Uani 1 1 d . . . . .
H11 H 0.5058 0.4486 0.0841 0.025 Uiso 1 1 calc R U . . .
C12 C 0.37249(8) 0.32747(17) 0.04839(9) 0.0281(3) Uani 1 1 d . . . . .
H12 H 0.3293 0.3308 0.0396 0.034 Uiso 1 1 calc R U . . .
C13 C 0.40564(8) 0.21214(18) 0.04670(9) 0.0288(3) Uani 1 1 d . . . . .
H13 H 0.3901 0.1190 0.0365 0.035 Uiso 1 1 calc R U . . .
N7 N 0.5000 0.3200(2) 0.2500 0.0391(5) Uani 1 2 d S T P . .
C14 C 0.5000 0.2012(3) 0.2500 0.0316(5) Uani 1 2 d S T P . .
C15 C 0.5000 0.0486(3) 0.2500 0.0518(8) Uani 1 2 d S T P . .
H15A H 0.5429 0.0143 0.2722 0.078 Uiso 0.5 1 calc R U P . .
H15B H 0.4817 0.0143 0.2019 0.078 Uiso 0.5 1 calc R U P . .
H15C H 0.4754 0.0143 0.2759 0.078 Uiso 0.5 1 calc R U P . .


_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
P1 F2 1.5929(11) . ?
P1 F1 1.5938(10) . ?
P1 F3 1.5938(12) . ?
P1 F6 1.5985(12) . ?
P1 F4 1.6054(11) . ?
P1 F5 1.6084(12) . ?
P2 F11 1.5865(11) . ?
P2 F12 1.5948(11) . ?
P2 F7 1.5995(11) . ?
P2 F9 1.5997(10) . ?
P2 F8 1.6091(10) . ?
P2 F10 1.6118(11) . ?
N1 C2 1.3379(19) . ?
N1 N2 1.3428(19) . ?
N2 C4 1.3541(19) . ?
N2 H2 0.8800 . ?
N3 C6 1.3312(18) . ?
N3 C7 1.3797(19) . ?
N3 C5 1.4806(19) . ?
N4 C6 1.3306(18) . ?
N4 C8 1.3801(19) . ?
N4 C9 1.4707(18) . ?
N5 C11 1.330(2) . ?
N5 C12 1.3777(19) . ?
N5 C10 1.4674(19) . ?
N6 C11 1.3316(18) . ?
N6 C13 1.372(2) . ?
N6 C1 1.480(2) 2_655 ?
C1 N6 1.480(2) 2_655 ?
C1 C2 1.487(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.404(2) . ?
C3 C4 1.375(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.485(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6 0.9500 . ?
C7 C8 1.351(2) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.520(2) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11 0.9500 . ?
C12 C13 1.349(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
N7 C14 1.130(4) . ?
C14 C15 1.452(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F2 P1 F1 178.45(6) . . ?
F2 P1 F3 90.49(7) . . ?
F1 P1 F3 90.11(6) . . ?
F2 P1 F6 90.96(7) . . ?
F1 P1 F6 90.47(6) . . ?
F3 P1 F6 90.44(7) . . ?
F2 P1 F4 88.82(6) . . ?
F1 P1 F4 89.75(6) . . ?
F3 P1 F4 90.52(7) . . ?
F6 P1 F4 179.01(7) . . ?
F2 P1 F5 89.65(7) . . ?
F1 P1 F5 89.74(6) . . ?
F3 P1 F5 179.46(8) . . ?
F6 P1 F5 90.07(7) . . ?
F4 P1 F5 88.96(7) . . ?
F11 P2 F12 90.37(7) . . ?
F11 P2 F7 90.43(7) . . ?
F12 P2 F7 91.06(7) . . ?
F11 P2 F9 178.91(7) . . ?
F12 P2 F9 90.59(7) . . ?
F7 P2 F9 90.06(6) . . ?
F11 P2 F8 90.50(6) . . ?
F12 P2 F8 89.79(6) . . ?
F7 P2 F8 178.73(7) . . ?
F9 P2 F8 89.00(5) . . ?
F11 P2 F10 89.66(6) . . ?
F12 P2 F10 179.51(7) . . ?
F7 P2 F10 89.43(6) . . ?
F9 P2 F10 89.38(6) . . ?
F8 P2 F10 89.71(6) . . ?
C2 N1 N2 104.24(13) . . ?
N1 N2 C4 113.03(12) . . ?
N1 N2 H2 123.5 . . ?
C4 N2 H2 123.5 . . ?
C6 N3 C7 108.63(12) . . ?
C6 N3 C5 126.33(12) . . ?
C7 N3 C5 125.03(12) . . ?
C6 N4 C8 108.65(12) . . ?
C6 N4 C9 124.60(12) . . ?
C8 N4 C9 126.70(12) . . ?
C11 N5 C12 108.56(13) . . ?
C11 N5 C10 125.23(12) . . ?
C12 N5 C10 126.18(13) . . ?
C11 N6 C13 108.65(13) . . ?
C11 N6 C1 126.42(13) . 2_655 ?
C13 N6 C1 124.67(13) . 2_655 ?
N6 C1 C2 111.31(12) 2_655 . ?
N6 C1 H1A 109.4 2_655 . ?
C2 C1 H1A 109.4 . . ?
N6 C1 H1B 109.4 2_655 . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C3 111.58(13) . . ?
N1 C2 C1 118.65(14) . . ?
C3 C2 C1 129.64(14) . . ?
C4 C3 C2 104.80(13) . . ?
C4 C3 H3 127.6 . . ?
C2 C3 H3 127.6 . . ?
N2 C4 C3 106.35(13) . . ?
N2 C4 C5 122.44(13) . . ?
C3 C4 C5 131.08(14) . . ?
N3 C5 C4 110.53(12) . . ?
N3 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
N3 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N4 C6 N3 108.56(12) . . ?
N4 C6 H6 125.7 . . ?
N3 C6 H6 125.7 . . ?
C8 C7 N3 107.09(13) . . ?
C8 C7 H7 126.5 . . ?
N3 C7 H7 126.5 . . ?
C7 C8 N4 107.06(14) . . ?
C7 C8 H8 126.5 . . ?
N4 C8 H8 126.5 . . ?
N4 C9 C10 112.34(11) . . ?
N4 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
N4 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
N5 C10 C9 112.53(11) . . ?
N5 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
N5 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N5 C11 N6 108.49(13) . . ?
N5 C11 H11 125.8 . . ?
N6 C11 H11 125.8 . . ?
C13 C12 N5 107.03(14) . . ?
C13 C12 H12 126.5 . . ?
N5 C12 H12 126.5 . . ?
C12 C13 N6 107.27(14) . . ?
C12 C13 H13 126.4 . . ?
N6 C13 H13 126.4 . . ?
N7 C14 C15 180.0 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 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
C2 N1 N2 C4 0.38(17) . . . . ?
N2 N1 C2 C3 -0.48(17) . . . . ?
N2 N1 C2 C1 175.79(13) . . . . ?
N6 C1 C2 N1 -79.06(17) 2_655 . . . ?
N6 C1 C2 C3 96.43(18) 2_655 . . . ?
N1 C2 C3 C4 0.41(17) . . . . ?
C1 C2 C3 C4 -175.33(14) . . . . ?
N1 N2 C4 C3 -0.13(17) . . . . ?
N1 N2 C4 C5 -176.38(13) . . . . ?
C2 C3 C4 N2 -0.16(16) . . . . ?
C2 C3 C4 C5 175.64(14) . . . . ?
C6 N3 C5 C4 22.8(2) . . . . ?
C7 N3 C5 C4 -158.42(14) . . . . ?
N2 C4 C5 N3 85.99(17) . . . . ?
C3 C4 C5 N3 -89.23(19) . . . . ?
C8 N4 C6 N3 0.01(16) . . . . ?
C9 N4 C6 N3 177.71(12) . . . . ?
C7 N3 C6 N4 0.22(16) . . . . ?
C5 N3 C6 N4 179.14(13) . . . . ?
C6 N3 C7 C8 -0.37(18) . . . . ?
C5 N3 C7 C8 -179.31(14) . . . . ?
N3 C7 C8 N4 0.37(18) . . . . ?
C6 N4 C8 C7 -0.24(18) . . . . ?
C9 N4 C8 C7 -177.87(14) . . . . ?
C6 N4 C9 C10 118.68(15) . . . . ?
C8 N4 C9 C10 -64.05(18) . . . . ?
C11 N5 C10 C9 -96.79(16) . . . . ?
C12 N5 C10 C9 81.16(18) . . . . ?
N4 C9 C10 N5 -69.62(15) . . . . ?
C12 N5 C11 N6 -0.72(16) . . . . ?
C10 N5 C11 N6 177.54(12) . . . . ?
C13 N6 C11 N5 0.73(17) . . . . ?
C1 N6 C11 N5 174.99(13) 2_655 . . . ?
C11 N5 C12 C13 0.43(18) . . . . ?
C10 N5 C12 C13 -177.80(14) . . . . ?
N5 C12 C13 N6 0.02(19) . . . . ?
C11 N6 C13 C12 -0.46(18) . . . . ?
C1 N6 C13 C12 -174.84(14) 2_655 . . . ?

_shelxl_version_number           2014/6



#===END
####################################################################### 
# 
# 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_altph43_0m
_database_code_depnum_ccdc_archive 'CCDC 1448009'
_audit_update_record             
;
2016-01-17 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_DIFMX01_altph43_0m          
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: A small fraction of whole molecule disorder could not be refinded. Therefore positiv peaks of residual electron density for the heavy atoms are present in the crystal structure.
;
_vrf_PLAT097_altph43_0m          
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.97 eA-3
RESPONSE: A small fraction of whole molecule disorder could not be refinded. Therefore positiv peaks of residual electron density for the heavy atoms are present in the crystal structure.
;
_vrf_PLAT971_altph43_0m          
;
PROBLEM: Check Calcd Residual Density  0.64A From     Ni1       2.83 eA-3
RESPONSE: A small fraction of whole molecule disorder could not be refinded. Therefore positiv peaks of residual electron density for the heavy atoms are present in the crystal structure.
;

# Added during the CSD deposition process: Sunday 17th of January 2016 03:58:00 PM
# end Validation Reply Form


#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H26 N12 Ni2, 2(F6 P), C2 H3 N'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C28 H29 F12 N13 Ni2 P2'
_chemical_formula_iupac          ?
_chemical_formula_weight         954.96
_chemical_compound_source        'see text'

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'
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'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,1/2+y,1/2-z
3 -x,-y,-z
4 x,1/2-y,1/2+z

_cell_length_a                   15.613(3)
_cell_length_b                   13.757(2)
_cell_length_c                   16.854(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.309(9)
_cell_angle_gamma                90
_cell_volume                     3598.1(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9744
_cell_measurement_theta_min      2.2453
_cell_measurement_theta_max      30.5211
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'pale yellow'

_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.190
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    1.242
_exptl_crystal_density_meas_temp ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.6648
_exptl_absorpt_correction_T_max  0.7461

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann	
scanspeed                           3 s per frame
dx                                  35 mm
4069 frames measured in 12 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
shutterless mode
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph monochromator'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Apex II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            164045
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             10093
# number of observed reflections (> n sig(I))
_reflns_number_gt                8365
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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     
'W=1/[Σ²(FO²)+(0.0524P)²+7.9515P] 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_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         10093
_refine_ls_number_parameters     624
_refine_ls_number_restraints     202
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1176
_refine_ls_wR_factor_gt          0.1108
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.968
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.109

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.29042(2) 0.48226(2) 0.75680(2) 0.01134(8) Uani 1 1 d . . . . .
Ni2 Ni 0.07960(2) 0.49120(2) 0.83044(2) 0.00871(7) Uani 1 1 d . . . . .
N1 N 0.24084(12) 0.38606(14) 0.81912(11) 0.0123(4) Uani 1 1 d . . . . .
N2 N 0.16247(12) 0.38987(14) 0.84722(11) 0.0120(3) Uani 1 1 d . . . . .
N3 N -0.00086(12) 0.31482(14) 0.87081(11) 0.0119(3) Uani 1 1 d . . . . .
N4 N -0.07623(12) 0.38327(14) 0.77289(11) 0.0131(4) Uani 1 1 d . . . . .
N5 N -0.08172(12) 0.60797(14) 0.78123(12) 0.0143(4) Uani 1 1 d . . . . .
N6 N 0.00933(12) 0.67389(13) 0.86858(11) 0.0121(3) Uani 1 1 d . . . . .
N7 N 0.16788(12) 0.58607(14) 0.84643(11) 0.0112(3) Uani 1 1 d . . . . .
N8 N 0.24679(12) 0.58282(14) 0.81841(11) 0.0125(4) Uani 1 1 d . . . . .
N9 N 0.37605(12) 0.66152(15) 0.73463(12) 0.0154(4) Uani 1 1 d . . . . .
N10 N 0.33880(14) 0.59364(16) 0.62134(12) 0.0189(4) Uani 1 1 d . . . . .
N11 N 0.36520(14) 0.36883(16) 0.62624(12) 0.0182(4) Uani 1 1 d . . . . .
N12 N 0.37258(12) 0.29980(15) 0.74064(12) 0.0154(4) Uani 1 1 d . . . . .
C1 C 0.36902(15) 0.28250(18) 0.82601(14) 0.0168(4) Uani 1 1 d . . . . .
H1A H 0.4119 0.3241 0.8575 0.020 Uiso 1 1 calc R U . . .
H1B H 0.3835 0.2138 0.8388 0.020 Uiso 1 1 calc R U . . .
C2 C 0.28102(14) 0.30471(17) 0.84790(13) 0.0141(4) Uani 1 1 d . . . . .
C3 C 0.22848(15) 0.25442(17) 0.89580(14) 0.0144(4) Uani 1 1 d . . . . .
H3 H 0.2406 0.1953 0.9239 0.017 Uiso 1 1 calc R U . . .
C4 C 0.15433(14) 0.31091(16) 0.89287(13) 0.0127(4) Uani 1 1 d . . . . .
C5 C 0.07278(14) 0.29517(17) 0.93024(13) 0.0141(4) Uani 1 1 d . . . . .
H5A H 0.0702 0.2273 0.9494 0.017 Uiso 1 1 calc R U . . .
H5B H 0.0711 0.3391 0.9766 0.017 Uiso 1 1 calc R U . . .
C6 C -0.00435(13) 0.39398(15) 0.82373(13) 0.0103(4) Uani 1 1 d . . . . .
C7 C -0.07062(15) 0.25421(17) 0.85034(14) 0.0166(4) Uani 1 1 d . . . . .
H7 H -0.0825 0.1943 0.8749 0.020 Uiso 1 1 calc R U . . .
C8 C -0.11838(16) 0.29748(18) 0.78837(15) 0.0179(5) Uani 1 1 d . . . . .
H8 H -0.1706 0.2738 0.7608 0.021 Uiso 1 1 calc R U . . .
C9 C -0.09724(16) 0.44990(19) 0.70563(14) 0.0192(5) Uani 1 1 d . . . . .
H9A H -0.1371 0.4170 0.6643 0.023 Uiso 1 1 calc R U . . .
H9B H -0.0439 0.4659 0.6817 0.023 Uiso 1 1 calc R U . . .
C10 C -0.13818(16) 0.54229(19) 0.73023(15) 0.0200(5) Uani 1 1 d . . . . .
H10A H -0.1606 0.5781 0.6814 0.024 Uiso 1 1 calc R U . . .
H10B H -0.1881 0.5251 0.7589 0.024 Uiso 1 1 calc R U . . .
C11 C -0.00410(14) 0.59203(16) 0.82389(13) 0.0112(4) Uani 1 1 d . . . . .
C12 C -0.11461(16) 0.69850(18) 0.79916(15) 0.0180(5) Uani 1 1 d . . . . .
H12 H -0.1677 0.7258 0.7767 0.022 Uiso 1 1 calc R U . . .
C13 C -0.05750(15) 0.73976(17) 0.85393(14) 0.0163(4) Uani 1 1 d . . . . .
H13 H -0.0619 0.8018 0.8779 0.020 Uiso 1 1 calc R U . . .
C14 C 0.08432(14) 0.68806(17) 0.92765(13) 0.0141(4) Uani 1 1 d . . . . .
H14A H 0.0800 0.6447 0.9739 0.017 Uiso 1 1 calc R U . . .
H14B H 0.0857 0.7561 0.9469 0.017 Uiso 1 1 calc R U . . .
C15 C 0.16491(14) 0.66625(16) 0.89135(13) 0.0120(4) Uani 1 1 d . . . . .
C16 C 0.24231(14) 0.71698(17) 0.89366(13) 0.0144(4) Uani 1 1 d . . . . .
H16 H 0.2581 0.7757 0.9212 0.017 Uiso 1 1 calc R U . . .
C17 C 0.29130(14) 0.66130(17) 0.84605(13) 0.0134(4) Uani 1 1 d . . . . .
C18 C 0.37953(14) 0.67783(17) 0.82105(14) 0.0156(4) Uani 1 1 d . . . . .
H18A H 0.3986 0.7451 0.8341 0.019 Uiso 1 1 calc R U . . .
H18B H 0.4213 0.6325 0.8499 0.019 Uiso 1 1 calc R U . . .
C19 C 0.33948(14) 0.58035(17) 0.70105(14) 0.0146(4) Uani 1 1 d . . . . .
C20 C 0.39860(16) 0.72585(19) 0.67688(16) 0.0203(5) Uani 1 1 d . . . . .
H20 H 0.4250 0.7877 0.6856 0.024 Uiso 1 1 calc R U . . .
C21 C 0.37528(17) 0.6826(2) 0.60555(16) 0.0227(5) Uani 1 1 d . . . . .
H21 H 0.3825 0.7084 0.5544 0.027 Uiso 1 1 calc R U . . .
C22 C 0.30164(17) 0.5211(2) 0.56346(15) 0.0212(5) Uani 1 1 d . . . . .
H22A H 0.2903 0.5518 0.5102 0.025 Uiso 1 1 calc R U . . .
H22B H 0.2459 0.4982 0.5794 0.025 Uiso 1 1 calc R U . . .
C23 C 0.36062(17) 0.4357(2) 0.55824(15) 0.0213(5) Uani 1 1 d . . . . .
H23A H 0.3413 0.3989 0.5091 0.026 Uiso 1 1 calc R U . . .
H23B H 0.4193 0.4603 0.5531 0.026 Uiso 1 1 calc R U . . .
C24 C 0.34547(14) 0.38300(17) 0.70209(14) 0.0135(4) Uani 1 1 d . . . . .
C25 C 0.40301(17) 0.27822(19) 0.61870(16) 0.0230(5) Uani 1 1 d . . . . .
H25 H 0.4220 0.2520 0.5715 0.028 Uiso 1 1 calc R U . . .
C26 C 0.40765(16) 0.23491(19) 0.69006(16) 0.0203(5) Uani 1 1 d . . . . .
H26 H 0.4304 0.1723 0.7035 0.024 Uiso 1 1 calc R U . . .
P1 P 0.37936(5) 0.52788(6) 0.33320(5) 0.01435(16) Uani 0.917(2) 1 d D U P A 1
F1 F 0.45265(11) 0.57666(15) 0.28771(12) 0.0314(4) Uani 0.917(2) 1 d D U P A 1
F2 F 0.30486(14) 0.47934(15) 0.37937(12) 0.0290(5) Uani 0.917(2) 1 d D U P A 1
F3 F 0.31118(11) 0.60577(12) 0.29409(10) 0.0217(4) Uani 0.917(2) 1 d D U P A 1
F4 F 0.40347(12) 0.59956(14) 0.40801(11) 0.0253(4) Uani 0.917(2) 1 d D U P A 1
F5 F 0.44569(13) 0.44949(14) 0.37334(14) 0.0399(6) Uani 0.917(2) 1 d D U P A 1
F6 F 0.35351(12) 0.45639(13) 0.25980(11) 0.0271(4) Uani 0.917(2) 1 d D U P A 1
P1A P 0.3795(6) 0.4816(10) 0.3384(6) 0.033(2) Uani 0.083(2) 1 d D U P A 2
F1A F 0.3505(12) 0.5606(16) 0.2705(12) 0.042(4) Uani 0.083(2) 1 d D U P A 2
F2A F 0.4043(13) 0.4029(14) 0.4074(11) 0.038(4) Uani 0.083(2) 1 d D U P A 2
F3A F 0.2985(12) 0.5139(14) 0.3824(14) 0.0217(4) Uani 0.083(2) 1 d D U P A 2
F4A F 0.4370(13) 0.5610(16) 0.3927(13) 0.041(4) Uani 0.083(2) 1 d D U P A 2
F5A F 0.4578(11) 0.4438(19) 0.2968(13) 0.048(5) Uani 0.083(2) 1 d D U P A 2
F6A F 0.3156(11) 0.4045(13) 0.2931(11) 0.033(4) Uani 0.083(2) 1 d D U P A 2
P2 P 0.5000 0.0000 0.5000 0.0277(2) Uani 1 2 d S . P . .
F7 F 0.58679(14) -0.01638(16) 0.55756(14) 0.0468(5) Uani 1 1 d . . . . .
F8 F 0.53808(16) 0.10038(17) 0.47144(17) 0.0611(7) Uani 1 1 d . . . . .
F9 F 0.54040(14) -0.0563(2) 0.43044(15) 0.0632(8) Uani 1 1 d . . . . .
P3 P 0.0000 0.5000 0.5000 0.0281(2) Uani 1 2 d S U P . .
F12 F -0.05890(17) 0.52106(18) 0.41813(13) 0.0528(6) Uani 1 1 d . U . . .
F10 F 0.0722(5) 0.4464(4) 0.4525(3) 0.0359(14) Uani 0.76(3) 1 d D U P B 3
F11 F 0.0464(5) 0.6006(3) 0.4895(3) 0.0369(14) Uani 0.76(3) 1 d D U P B 3
F10A F 0.0431(19) 0.4304(14) 0.4495(12) 0.066(4) Uani 0.24(3) 1 d D U P B 4
F11A F 0.0738(19) 0.5833(18) 0.4855(16) 0.072(5) Uani 0.24(3) 1 d D U P B 4
N13 N 0.1256(9) 0.4863(14) 0.0540(13) 0.049(4) Uani 0.538(18) 1 d D U P C 5
C27 C 0.1919(7) 0.5129(12) 0.0641(9) 0.024(2) Uani 0.538(18) 1 d D U P C 5
C28 C 0.2762(4) 0.5557(9) 0.0806(6) 0.049(3) Uani 0.538(18) 1 d D U P C 5
H28A H 0.2934 0.5849 0.0316 0.074 Uiso 0.538(18) 1 calc R U P C 5
H28B H 0.3179 0.5053 0.0996 0.074 Uiso 0.538(18) 1 calc R U P C 5
H28C H 0.2748 0.6060 0.1216 0.074 Uiso 0.538(18) 1 calc R U P C 5
N13A N 0.1107(8) 0.4908(12) 0.0507(13) 0.026(2) Uani 0.462(18) 1 d D U P C 6
C27A C 0.1817(9) 0.4937(16) 0.0531(14) 0.034(4) Uani 0.462(18) 1 d D U P C 6
C28A C 0.2749(7) 0.4906(15) 0.0505(10) 0.074(5) Uani 0.462(18) 1 d D U P C 6
H28D H 0.2883 0.4460 0.0083 0.111 Uiso 0.462(18) 1 calc R U P C 6
H28E H 0.3030 0.4680 0.1020 0.111 Uiso 0.462(18) 1 calc R U P C 6
H28F H 0.2958 0.5559 0.0395 0.111 Uiso 0.462(18) 1 calc R U P C 6


_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 C19 1.857(2) . ?
Ni1 N8 1.900(2) . ?
Ni1 C24 1.905(2) . ?
Ni1 N1 1.9060(19) . ?
Ni2 C6 1.867(2) . ?
Ni2 N7 1.8959(19) . ?
Ni2 C11 1.901(2) . ?
Ni2 N2 1.9019(19) . ?
N1 C2 1.347(3) . ?
N1 N2 1.361(3) . ?
N2 C4 1.345(3) . ?
N3 C6 1.345(3) . ?
N3 C7 1.385(3) . ?
N3 C5 1.465(3) . ?
N4 C6 1.343(3) . ?
N4 C8 1.390(3) . ?
N4 C9 1.467(3) . ?
N5 C11 1.357(3) . ?
N5 C12 1.393(3) . ?
N5 C10 1.472(3) . ?
N6 C11 1.358(3) . ?
N6 C13 1.384(3) . ?
N6 C14 1.464(3) . ?
N7 C15 1.342(3) . ?
N7 N8 1.368(2) . ?
N8 C17 1.340(3) . ?
N9 C19 1.350(3) . ?
N9 C20 1.389(3) . ?
N9 C18 1.469(3) . ?
N10 C19 1.355(3) . ?
N10 C21 1.388(3) . ?
N10 C22 1.469(3) . ?
N11 C24 1.361(3) . ?
N11 C25 1.391(3) . ?
N11 C23 1.465(3) . ?
N12 C24 1.361(3) . ?
N12 C26 1.388(3) . ?
N12 C1 1.465(3) . ?
C1 C2 1.493(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.396(3) . ?
C3 C4 1.391(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.497(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C7 C8 1.353(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.501(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 C13 1.337(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.489(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.392(3) . ?
C16 C17 1.397(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.501(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C20 C21 1.355(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.501(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C25 C26 1.337(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
P1 F5 1.593(2) . ?
P1 F1 1.5939(19) . ?
P1 F6 1.5970(18) . ?
P1 F3 1.6006(18) . ?
P1 F4 1.6124(18) . ?
P1 F2 1.614(2) . ?
P1A F5A 1.564(15) . ?
P1A F6A 1.593(15) . ?
P1A F3A 1.597(15) . ?
P1A F2A 1.605(15) . ?
P1A F1A 1.607(15) . ?
P1A F4A 1.630(15) . ?
P2 F9 1.592(2) 3_656 ?
P2 F9 1.592(2) . ?
P2 F7 1.5934(19) . ?
P2 F7 1.5935(19) 3_656 ?
P2 F8 1.598(2) . ?
P2 F8 1.599(2) 3_656 ?
P3 F10A 1.490(17) 3_566 ?
P3 F10A 1.490(17) . ?
P3 F11 1.581(4) . ?
P3 F11 1.581(4) 3_566 ?
P3 F12 1.598(2) . ?
P3 F12 1.598(2) 3_566 ?
P3 F10 1.629(5) . ?
P3 F10 1.629(5) 3_566 ?
P3 F11A 1.662(19) 3_566 ?
P3 F11A 1.662(19) . ?
N13 C27 1.094(11) . ?
C27 C28 1.441(10) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N13A C27A 1.107(12) . ?
C27A C28A 1.460(14) . ?
C28A H28D 0.9800 . ?
C28A H28E 0.9800 . ?
C28A H28F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 Ni1 N8 86.56(9) . . ?
C19 Ni1 C24 92.46(10) . . ?
N8 Ni1 C24 173.89(9) . . ?
C19 Ni1 N1 176.83(9) . . ?
N8 Ni1 N1 90.73(8) . . ?
C24 Ni1 N1 90.07(9) . . ?
C6 Ni2 N7 175.00(9) . . ?
C6 Ni2 C11 92.62(10) . . ?
N7 Ni2 C11 89.44(9) . . ?
C6 Ni2 N2 86.88(9) . . ?
N7 Ni2 N2 90.65(8) . . ?
C11 Ni2 N2 174.74(9) . . ?
C2 N1 N2 107.92(18) . . ?
C2 N1 Ni1 125.04(16) . . ?
N2 N1 Ni1 126.89(15) . . ?
C4 N2 N1 108.25(18) . . ?
C4 N2 Ni2 124.85(15) . . ?
N1 N2 Ni2 126.83(15) . . ?
C6 N3 C7 111.14(19) . . ?
C6 N3 C5 122.06(19) . . ?
C7 N3 C5 126.58(19) . . ?
C6 N4 C8 110.68(19) . . ?
C6 N4 C9 121.65(19) . . ?
C8 N4 C9 127.3(2) . . ?
C11 N5 C12 111.01(19) . . ?
C11 N5 C10 130.8(2) . . ?
C12 N5 C10 117.7(2) . . ?
C11 N6 C13 112.13(19) . . ?
C11 N6 C14 123.41(19) . . ?
C13 N6 C14 124.41(19) . . ?
C15 N7 N8 108.07(18) . . ?
C15 N7 Ni2 125.21(15) . . ?
N8 N7 Ni2 126.64(15) . . ?
C17 N8 N7 107.83(19) . . ?
C17 N8 Ni1 124.98(16) . . ?
N7 N8 Ni1 127.09(15) . . ?
C19 N9 C20 111.2(2) . . ?
C19 N9 C18 120.67(19) . . ?
C20 N9 C18 127.8(2) . . ?
C19 N10 C21 110.5(2) . . ?
C19 N10 C22 121.8(2) . . ?
C21 N10 C22 127.7(2) . . ?
C24 N11 C25 110.9(2) . . ?
C24 N11 C23 130.4(2) . . ?
C25 N11 C23 118.4(2) . . ?
C24 N12 C26 111.8(2) . . ?
C24 N12 C1 124.2(2) . . ?
C26 N12 C1 124.0(2) . . ?
N12 C1 C2 110.16(18) . . ?
N12 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N12 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C3 109.9(2) . . ?
N1 C2 C1 119.1(2) . . ?
C3 C2 C1 131.0(2) . . ?
C4 C3 C2 104.0(2) . . ?
C4 C3 H3 128.0 . . ?
C2 C3 H3 128.0 . . ?
N2 C4 C3 109.9(2) . . ?
N2 C4 C5 119.71(19) . . ?
C3 C4 C5 130.4(2) . . ?
N3 C5 C4 109.00(18) . . ?
N3 C5 H5A 109.9 . . ?
C4 C5 H5A 109.9 . . ?
N3 C5 H5B 109.9 . . ?
C4 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N4 C6 N3 105.33(18) . . ?
N4 C6 Ni2 130.46(17) . . ?
N3 C6 Ni2 124.16(16) . . ?
C8 C7 N3 106.2(2) . . ?
C8 C7 H7 126.9 . . ?
N3 C7 H7 126.9 . . ?
C7 C8 N4 106.6(2) . . ?
C7 C8 H8 126.7 . . ?
N4 C8 H8 126.7 . . ?
N4 C9 C10 112.4(2) . . ?
N4 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
N4 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
N5 C10 C9 115.8(2) . . ?
N5 C10 H10A 108.3 . . ?
C9 C10 H10A 108.3 . . ?
N5 C10 H10B 108.3 . . ?
C9 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
N5 C11 N6 103.54(18) . . ?
N5 C11 Ni2 135.80(17) . . ?
N6 C11 Ni2 120.65(16) . . ?
C13 C12 N5 107.2(2) . . ?
C13 C12 H12 126.4 . . ?
N5 C12 H12 126.4 . . ?
C12 C13 N6 106.1(2) . . ?
C12 C13 H13 126.9 . . ?
N6 C13 H13 126.9 . . ?
N6 C14 C15 110.02(18) . . ?
N6 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
N6 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N7 C15 C16 110.1(2) . . ?
N7 C15 C14 118.75(19) . . ?
C16 C15 C14 131.1(2) . . ?
C15 C16 C17 103.7(2) . . ?
C15 C16 H16 128.1 . . ?
C17 C16 H16 128.1 . . ?
N8 C17 C16 110.2(2) . . ?
N8 C17 C18 118.8(2) . . ?
C16 C17 C18 130.9(2) . . ?
N9 C18 C17 108.66(18) . . ?
N9 C18 H18A 110.0 . . ?
C17 C18 H18A 110.0 . . ?
N9 C18 H18B 110.0 . . ?
C17 C18 H18B 110.0 . . ?
H18A C18 H18B 108.3 . . ?
N9 C19 N10 105.1(2) . . ?
N9 C19 Ni1 124.60(17) . . ?
N10 C19 Ni1 129.87(18) . . ?
C21 C20 N9 106.1(2) . . ?
C21 C20 H20 126.9 . . ?
N9 C20 H20 126.9 . . ?
C20 C21 N10 107.0(2) . . ?
C20 C21 H21 126.5 . . ?
N10 C21 H21 126.5 . . ?
N10 C22 C23 111.7(2) . . ?
N10 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
N10 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
N11 C23 C22 115.0(2) . . ?
N11 C23 H23A 108.5 . . ?
C22 C23 H23A 108.5 . . ?
N11 C23 H23B 108.5 . . ?
C22 C23 H23B 108.5 . . ?
H23A C23 H23B 107.5 . . ?
N12 C24 N11 103.7(2) . . ?
N12 C24 Ni1 120.35(17) . . ?
N11 C24 Ni1 135.88(18) . . ?
C26 C25 N11 107.4(2) . . ?
C26 C25 H25 126.3 . . ?
N11 C25 H25 126.3 . . ?
C25 C26 N12 106.3(2) . . ?
C25 C26 H26 126.9 . . ?
N12 C26 H26 126.9 . . ?
F5 P1 F1 91.25(12) . . ?
F5 P1 F6 90.53(11) . . ?
F1 P1 F6 91.17(11) . . ?
F5 P1 F3 178.73(13) . . ?
F1 P1 F3 90.01(11) . . ?
F6 P1 F3 89.62(10) . . ?
F5 P1 F4 89.82(11) . . ?
F1 P1 F4 90.02(11) . . ?
F6 P1 F4 178.75(11) . . ?
F3 P1 F4 90.00(10) . . ?
F5 P1 F2 89.11(13) . . ?
F1 P1 F2 179.54(14) . . ?
F6 P1 F2 89.11(11) . . ?
F3 P1 F2 89.64(11) . . ?
F4 P1 F2 89.69(11) . . ?
F5A P1A F6A 92.5(12) . . ?
F5A P1A F3A 176.7(15) . . ?
F6A P1A F3A 85.5(11) . . ?
F5A P1A F2A 87.9(12) . . ?
F6A P1A F2A 89.2(11) . . ?
F3A P1A F2A 89.5(11) . . ?
F5A P1A F1A 94.5(12) . . ?
F6A P1A F1A 89.8(11) . . ?
F3A P1A F1A 88.1(11) . . ?
F2A P1A F1A 177.5(12) . . ?
F5A P1A F4A 93.7(12) . . ?
F6A P1A F4A 173.3(13) . . ?
F3A P1A F4A 88.2(12) . . ?
F2A P1A F4A 88.3(11) . . ?
F1A P1A F4A 92.4(12) . . ?
F9 P2 F9 180.00(18) 3_656 . ?
F9 P2 F7 89.98(12) 3_656 . ?
F9 P2 F7 90.02(12) . . ?
F9 P2 F7 90.02(12) 3_656 3_656 ?
F9 P2 F7 89.98(12) . 3_656 ?
F7 P2 F7 180.0 . 3_656 ?
F9 P2 F8 89.53(15) 3_656 . ?
F9 P2 F8 90.47(15) . . ?
F7 P2 F8 89.20(12) . . ?
F7 P2 F8 90.81(12) 3_656 . ?
F9 P2 F8 90.47(15) 3_656 3_656 ?
F9 P2 F8 89.53(15) . 3_656 ?
F7 P2 F8 90.81(12) . 3_656 ?
F7 P2 F8 89.19(12) 3_656 3_656 ?
F8 P2 F8 180.0 . 3_656 ?
F10A P3 F10A 180.0 3_566 . ?
F11 P3 F11 180.0 . 3_566 ?
F10A P3 F12 97.1(9) 3_566 . ?
F10A P3 F12 82.9(9) . . ?
F11 P3 F12 88.4(3) . . ?
F11 P3 F12 91.6(3) 3_566 . ?
F10A P3 F12 82.9(9) 3_566 3_566 ?
F10A P3 F12 97.1(9) . 3_566 ?
F11 P3 F12 91.6(3) . 3_566 ?
F11 P3 F12 88.4(3) 3_566 3_566 ?
F12 P3 F12 180.0 . 3_566 ?
F11 P3 F10 89.50(19) . . ?
F11 P3 F10 90.50(19) 3_566 . ?
F12 P3 F10 91.2(2) . . ?
F12 P3 F10 88.8(2) 3_566 . ?
F11 P3 F10 90.50(19) . 3_566 ?
F11 P3 F10 89.50(19) 3_566 3_566 ?
F12 P3 F10 88.8(2) . 3_566 ?
F12 P3 F10 91.2(2) 3_566 3_566 ?
F10 P3 F10 180.0 . 3_566 ?
F10A P3 F11A 89.8(8) 3_566 3_566 ?
F10A P3 F11A 90.2(8) . 3_566 ?
F12 P3 F11A 84.8(8) . 3_566 ?
F12 P3 F11A 95.2(8) 3_566 3_566 ?
F10A P3 F11A 90.2(8) 3_566 . ?
F10A P3 F11A 89.8(8) . . ?
F12 P3 F11A 95.2(8) . . ?
F12 P3 F11A 84.8(8) 3_566 . ?
F11A P3 F11A 180.0(12) 3_566 . ?
N13 C27 C28 174.8(18) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N13A C27A C28A 174.7(19) . . ?
C27A C28A H28D 109.5 . . ?
C27A C28A H28E 109.5 . . ?
H28D C28A H28E 109.5 . . ?
C27A C28A H28F 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 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
C2 N1 N2 C4 -0.2(2) . . . . ?
Ni1 N1 N2 C4 -175.86(15) . . . . ?
C2 N1 N2 Ni2 176.90(15) . . . . ?
Ni1 N1 N2 Ni2 1.3(3) . . . . ?
C11 Ni2 N7 C15 39.77(19) . . . . ?
N2 Ni2 N7 C15 -134.97(19) . . . . ?
C11 Ni2 N7 N8 -144.02(18) . . . . ?
N2 Ni2 N7 N8 41.24(18) . . . . ?
C15 N7 N8 C17 -0.3(2) . . . . ?
Ni2 N7 N8 C17 -177.07(15) . . . . ?
C15 N7 N8 Ni1 176.06(15) . . . . ?
Ni2 N7 N8 Ni1 -0.7(3) . . . . ?
C24 N12 C1 C2 50.5(3) . . . . ?
C26 N12 C1 C2 -132.6(2) . . . . ?
N2 N1 C2 C3 -0.2(3) . . . . ?
Ni1 N1 C2 C3 175.54(15) . . . . ?
N2 N1 C2 C1 179.95(19) . . . . ?
Ni1 N1 C2 C1 -4.3(3) . . . . ?
N12 C1 C2 N1 -44.1(3) . . . . ?
N12 C1 C2 C3 136.1(3) . . . . ?
N1 C2 C3 C4 0.5(3) . . . . ?
C1 C2 C3 C4 -179.6(2) . . . . ?
N1 N2 C4 C3 0.6(3) . . . . ?
Ni2 N2 C4 C3 -176.63(15) . . . . ?
N1 N2 C4 C5 -178.59(19) . . . . ?
Ni2 N2 C4 C5 4.2(3) . . . . ?
C2 C3 C4 N2 -0.7(3) . . . . ?
C2 C3 C4 C5 178.4(2) . . . . ?
C6 N3 C5 C4 -46.0(3) . . . . ?
C7 N3 C5 C4 128.3(2) . . . . ?
N2 C4 C5 N3 44.6(3) . . . . ?
C3 C4 C5 N3 -134.4(2) . . . . ?
C8 N4 C6 N3 0.4(2) . . . . ?
C9 N4 C6 N3 -172.7(2) . . . . ?
C8 N4 C6 Ni2 177.90(17) . . . . ?
C9 N4 C6 Ni2 4.8(3) . . . . ?
C7 N3 C6 N4 -0.4(2) . . . . ?
C5 N3 C6 N4 174.65(19) . . . . ?
C7 N3 C6 Ni2 -178.10(16) . . . . ?
C5 N3 C6 Ni2 -3.0(3) . . . . ?
C11 Ni2 C6 N4 48.1(2) . . . . ?
N2 Ni2 C6 N4 -137.1(2) . . . . ?
C11 Ni2 C6 N3 -134.82(19) . . . . ?
N2 Ni2 C6 N3 39.94(19) . . . . ?
C6 N3 C7 C8 0.2(3) . . . . ?
C5 N3 C7 C8 -174.5(2) . . . . ?
N3 C7 C8 N4 0.0(3) . . . . ?
C6 N4 C8 C7 -0.3(3) . . . . ?
C9 N4 C8 C7 172.4(2) . . . . ?
C6 N4 C9 C10 -81.4(3) . . . . ?
C8 N4 C9 C10 106.7(3) . . . . ?
C11 N5 C10 C9 -15.5(4) . . . . ?
C12 N5 C10 C9 174.0(2) . . . . ?
N4 C9 C10 N5 68.7(3) . . . . ?
C12 N5 C11 N6 0.5(2) . . . . ?
C10 N5 C11 N6 -170.4(2) . . . . ?
C12 N5 C11 Ni2 -177.99(19) . . . . ?
C10 N5 C11 Ni2 11.1(4) . . . . ?
C13 N6 C11 N5 -0.5(2) . . . . ?
C14 N6 C11 N5 177.02(19) . . . . ?
C13 N6 C11 Ni2 178.28(16) . . . . ?
C14 N6 C11 Ni2 -4.2(3) . . . . ?
C11 N5 C12 C13 -0.4(3) . . . . ?
C10 N5 C12 C13 171.9(2) . . . . ?
N5 C12 C13 N6 0.0(3) . . . . ?
C11 N6 C13 C12 0.3(3) . . . . ?
C14 N6 C13 C12 -177.2(2) . . . . ?
C11 N6 C14 C15 50.6(3) . . . . ?
C13 N6 C14 C15 -132.1(2) . . . . ?
N8 N7 C15 C16 -0.1(2) . . . . ?
Ni2 N7 C15 C16 176.66(15) . . . . ?
N8 N7 C15 C14 178.60(19) . . . . ?
Ni2 N7 C15 C14 -4.6(3) . . . . ?
N6 C14 C15 N7 -44.9(3) . . . . ?
N6 C14 C15 C16 133.5(2) . . . . ?
N7 C15 C16 C17 0.5(2) . . . . ?
C14 C15 C16 C17 -178.0(2) . . . . ?
N7 N8 C17 C16 0.7(3) . . . . ?
Ni1 N8 C17 C16 -175.81(15) . . . . ?
N7 N8 C17 C18 -177.39(19) . . . . ?
Ni1 N8 C17 C18 6.1(3) . . . . ?
C15 C16 C17 N8 -0.7(3) . . . . ?
C15 C16 C17 C18 177.0(2) . . . . ?
C19 N9 C18 C17 -49.5(3) . . . . ?
C20 N9 C18 C17 123.0(2) . . . . ?
N8 C17 C18 N9 45.4(3) . . . . ?
C16 C17 C18 N9 -132.2(2) . . . . ?
C20 N9 C19 N10 -0.1(3) . . . . ?
C18 N9 C19 N10 173.5(2) . . . . ?
C20 N9 C19 Ni1 -173.53(17) . . . . ?
C18 N9 C19 Ni1 0.1(3) . . . . ?
C21 N10 C19 N9 0.3(3) . . . . ?
C22 N10 C19 N9 -178.5(2) . . . . ?
C21 N10 C19 Ni1 173.26(19) . . . . ?
C22 N10 C19 Ni1 -5.6(3) . . . . ?
N8 Ni1 C19 N9 39.2(2) . . . . ?
C24 Ni1 C19 N9 -134.8(2) . . . . ?
N8 Ni1 C19 N10 -132.5(2) . . . . ?
C24 Ni1 C19 N10 53.5(2) . . . . ?
C19 N9 C20 C21 -0.1(3) . . . . ?
C18 N9 C20 C21 -173.2(2) . . . . ?
N9 C20 C21 N10 0.3(3) . . . . ?
C19 N10 C21 C20 -0.4(3) . . . . ?
C22 N10 C21 C20 178.3(2) . . . . ?
C19 N10 C22 C23 -76.8(3) . . . . ?
C21 N10 C22 C23 104.6(3) . . . . ?
C24 N11 C23 C22 -20.9(4) . . . . ?
C25 N11 C23 C22 166.4(2) . . . . ?
N10 C22 C23 N11 74.1(3) . . . . ?
C26 N12 C24 N11 -0.5(3) . . . . ?
C1 N12 C24 N11 176.8(2) . . . . ?
C26 N12 C24 Ni1 177.45(16) . . . . ?
C1 N12 C24 Ni1 -5.3(3) . . . . ?
C25 N11 C24 N12 0.5(3) . . . . ?
C23 N11 C24 N12 -172.6(2) . . . . ?
C25 N11 C24 Ni1 -177.0(2) . . . . ?
C23 N11 C24 Ni1 9.9(4) . . . . ?
C24 N11 C25 C26 -0.3(3) . . . . ?
C23 N11 C25 C26 173.8(2) . . . . ?
N11 C25 C26 N12 -0.1(3) . . . . ?
C24 N12 C26 C25 0.4(3) . . . . ?
C1 N12 C26 C25 -176.9(2) . . . . ?




#===END
####################################################################### 
# 
# 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_altph50_0m
_database_code_depnum_ccdc_archive 'CCDC 1448010'
_audit_update_record             
;
2016-01-17 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H52 Br N24 Ni4, 3(F6 P), 4(C2 H3 N)'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C60 H64 Br F18 N28 Ni4 P3'
_chemical_formula_iupac          ?
_chemical_formula_weight         1926.96
_chemical_compound_source        'see text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_Int_Tables_number      15

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z

_cell_length_a                   15.985(2)
_cell_length_b                   30.833(4)
_cell_length_c                   15.2616(18)
_cell_angle_alpha                90
_cell_angle_beta                 93.494(8)
_cell_angle_gamma                90
_cell_volume                     7507.9(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9860
_cell_measurement_theta_min      2.3546
_cell_measurement_theta_max      25.2007
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.140
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             3896
_exptl_absorpt_coefficient_mu    1.690
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_absorpt_correction_T_min  0.6574
_exptl_absorpt_correction_T_max  0.7452

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           5 s per frame
dx                                  61 mm
3528 frames measured in 9 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph monochromator'


_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Apex II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            60480
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             6637
# number of observed reflections (> n sig(I))
_reflns_number_gt                5344
_reflns_threshold_expression     I>2σ(I)


_computing_data_collection       'APEX III Control Software (Bruker, 2015)'
_computing_cell_refinement       'SAINT (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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     
'W=1/[Σ²(FO²)+(0.0429P)²+52.9857P] 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_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         6637
_refine_ls_number_parameters     570
_refine_ls_number_restraints     147
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.1191
_refine_ls_wR_factor_gt          0.1099
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.121
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.844
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.094

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
Br1 Br 0.5000 0.34750(2) 0.7500 0.02025(15) Uani 1 2 d S T P . .
Ni1 Ni 0.66667(3) 0.30778(2) 0.77446(3) 0.01867(15) Uani 1 1 d . . . . .
Ni2 Ni 0.59846(3) 0.39129(2) 0.62163(3) 0.01818(14) Uani 1 1 d . . . . .
N1 N 0.7153(2) 0.36407(12) 0.7660(2) 0.0214(8) Uani 1 1 d . . . . .
N2 N 0.6899(2) 0.39560(12) 0.7084(2) 0.0213(8) Uani 1 1 d . . . . .
N3 N 0.6411(2) 0.47992(12) 0.6536(2) 0.0238(8) Uani 1 1 d . . . . .
N4 N 0.5087(2) 0.47854(12) 0.6258(2) 0.0232(8) Uani 1 1 d . . . . .
N5 N 0.4355(2) 0.39899(11) 0.5272(2) 0.0205(8) Uani 1 1 d . . . . .
N6 N 0.5253(2) 0.36585(11) 0.4528(2) 0.0186(8) Uani 1 1 d . . . . .
N7 N 0.6340(2) 0.33369(11) 0.5917(2) 0.0175(7) Uani 1 1 d . . . . .
N8 N 0.6633(2) 0.30277(11) 0.6496(2) 0.0180(7) Uani 1 1 d . . . . .
N9 N 0.6622(2) 0.21799(11) 0.7267(2) 0.0197(8) Uani 1 1 d . . . . .
N10 N 0.5823(2) 0.22966(12) 0.8316(2) 0.0212(8) Uani 1 1 d . . . . .
N11 N 0.6593(2) 0.28820(12) 0.9702(2) 0.0249(9) Uani 1 1 d . . . . .
N12 N 0.7633(2) 0.32700(13) 0.9322(2) 0.0274(9) Uani 1 1 d . . . . .
C1 C 0.8244(3) 0.34885(16) 0.8811(3) 0.0317(11) Uani 1 1 d . . . . .
H1A H 0.8584 0.3269 0.8519 0.038 Uiso 1 1 calc R U . . .
H1B H 0.8626 0.3661 0.9209 0.038 Uiso 1 1 calc R U . . .
C2 C 0.7835(3) 0.37797(15) 0.8134(3) 0.0249(10) Uani 1 1 d . . . . .
C3 C 0.8030(3) 0.41996(16) 0.7866(3) 0.0278(11) Uani 1 1 d . . . . .
H3 H 0.8476 0.4380 0.8087 0.033 Uiso 1 1 calc R U . . .
C4 C 0.7425(3) 0.42915(14) 0.7207(3) 0.0234(10) Uani 1 1 d . . . . .
C5 C 0.7298(3) 0.46831(16) 0.6645(3) 0.0282(11) Uani 1 1 d . . . . .
H5A H 0.7618 0.4929 0.6916 0.034 Uiso 1 1 calc R U . . .
H5B H 0.7516 0.4627 0.6062 0.034 Uiso 1 1 calc R U . . .
C6 C 0.5771(3) 0.45195(15) 0.6336(3) 0.0232(10) Uani 1 1 d . . . . .
C7 C 0.6137(3) 0.52254(15) 0.6584(3) 0.0294(11) Uani 1 1 d . . . . .
H7 H 0.6472 0.5474 0.6718 0.035 Uiso 1 1 calc R U . . .
C8 C 0.5310(3) 0.52162(15) 0.6406(3) 0.0282(11) Uani 1 1 d . . . . .
H8 H 0.4942 0.5459 0.6384 0.034 Uiso 1 1 calc R U . . .
C9 C 0.4199(3) 0.46889(14) 0.6031(3) 0.0263(10) Uani 1 1 d . . . . .
H9A H 0.4042 0.4820 0.5452 0.032 Uiso 1 1 calc R U . . .
H9B H 0.3857 0.4831 0.6468 0.032 Uiso 1 1 calc R U . . .
C10 C 0.3977(3) 0.42158(15) 0.5995(3) 0.0252(10) Uani 1 1 d . . . . .
H10A H 0.4169 0.4077 0.6557 0.030 Uiso 1 1 calc R U . . .
H10B H 0.3360 0.4186 0.5925 0.030 Uiso 1 1 calc R U . . .
C11 C 0.5168(3) 0.38673(13) 0.5302(3) 0.0193(9) Uani 1 1 d . . . . .
C12 C 0.3945(3) 0.38607(14) 0.4500(3) 0.0241(10) Uani 1 1 d . . . . .
H12 H 0.3371 0.3910 0.4329 0.029 Uiso 1 1 calc R U . . .
C13 C 0.4507(3) 0.36515(14) 0.4027(3) 0.0233(10) Uani 1 1 d . . . . .
H13 H 0.4407 0.3525 0.3463 0.028 Uiso 1 1 calc R U . . .
C14 C 0.6027(3) 0.34313(14) 0.4328(3) 0.0211(9) Uani 1 1 d . . . . .
H14A H 0.6464 0.3645 0.4192 0.025 Uiso 1 1 calc R U . . .
H14B H 0.5920 0.3242 0.3810 0.025 Uiso 1 1 calc R U . . .
C15 C 0.6323(3) 0.31632(13) 0.5109(3) 0.0178(9) Uani 1 1 d . . . . .
C16 C 0.6606(3) 0.27356(14) 0.5156(3) 0.0194(9) Uani 1 1 d . . . . .
H16 H 0.6654 0.2537 0.4686 0.023 Uiso 1 1 calc R U . . .
C17 C 0.6800(3) 0.26663(13) 0.6037(3) 0.0179(9) Uani 1 1 d . . . . .
C18 C 0.7137(3) 0.22706(14) 0.6520(3) 0.0202(9) Uani 1 1 d . . . . .
H18A H 0.7124 0.2018 0.6118 0.024 Uiso 1 1 calc R U . . .
H18B H 0.7726 0.2321 0.6736 0.024 Uiso 1 1 calc R U . . .
C19 C 0.6339(3) 0.25000(15) 0.7783(3) 0.0207(9) Uani 1 1 d . . . . .
C20 C 0.6289(3) 0.17800(14) 0.7485(3) 0.0217(9) Uani 1 1 d . . . . .
H20 H 0.6391 0.1508 0.7219 0.026 Uiso 1 1 calc R U . . .
C21 C 0.5793(3) 0.18568(14) 0.8149(3) 0.0233(10) Uani 1 1 d . . . . .
H21 H 0.5479 0.1647 0.8448 0.028 Uiso 1 1 calc R U . . .
C22 C 0.5331(3) 0.25388(16) 0.8934(3) 0.0277(11) Uani 1 1 d . . . . .
H22A H 0.4828 0.2368 0.9059 0.033 Uiso 1 1 calc R U . . .
H22B H 0.5138 0.2814 0.8656 0.033 Uiso 1 1 calc R U . . .
C23 C 0.5819(3) 0.26376(15) 0.9781(3) 0.0262(10) Uani 1 1 d . . . . .
H23A H 0.5453 0.2804 1.0161 0.031 Uiso 1 1 calc R U . . .
H23B H 0.5959 0.2360 1.0082 0.031 Uiso 1 1 calc R U . . .
C24 C 0.6921(3) 0.30718(15) 0.8986(3) 0.0253(10) Uani 1 1 d . . . . .
C25 C 0.7102(3) 0.29589(16) 1.0453(3) 0.0325(12) Uani 1 1 d . . . . .
H25 H 0.7011 0.2859 1.1028 0.039 Uiso 1 1 calc R U . . .
C26 C 0.7746(3) 0.32004(17) 1.0212(3) 0.0357(13) Uani 1 1 d . . . . .
H26 H 0.8198 0.3305 1.0587 0.043 Uiso 1 1 calc R U . . .
P1 P 0.7868(3) 0.43640(15) 0.3829(3) 0.0390(10) Uani 0.758(14) 1 d D U P A 1
F1 F 0.8510(5) 0.4476(4) 0.4640(5) 0.065(2) Uani 0.758(14) 1 d D U P A 1
F2 F 0.7247(6) 0.4224(2) 0.3027(5) 0.088(2) Uani 0.758(14) 1 d D U P A 1
F3 F 0.7928(5) 0.3858(2) 0.4068(5) 0.0409(16) Uani 0.758(14) 1 d D U P A 1
F4 F 0.7104(4) 0.43911(19) 0.4453(5) 0.065(2) Uani 0.758(14) 1 d D U P A 1
F5 F 0.7734(6) 0.48473(19) 0.3546(5) 0.095(3) Uani 0.758(14) 1 d D U P A 1
F6 F 0.8638(5) 0.4314(3) 0.3222(5) 0.083(2) Uani 0.758(14) 1 d D U P A 1
P1A P 0.8020(11) 0.4345(5) 0.3728(12) 0.065(5) Uani 0.242(14) 1 d D U P A 2
F1A F 0.8305(19) 0.4823(5) 0.3475(13) 0.086(6) Uani 0.242(14) 1 d D U P A 2
F2A F 0.786(2) 0.3849(7) 0.387(2) 0.066(7) Uani 0.242(14) 1 d D U P A 2
F3A F 0.8943(12) 0.4192(6) 0.3495(14) 0.064(5) Uani 0.242(14) 1 d D U P A 2
F4A F 0.834(2) 0.4430(11) 0.4723(14) 0.077(7) Uani 0.242(14) 1 d D U P A 2
F5A F 0.7085(12) 0.4447(7) 0.395(2) 0.097(6) Uani 0.242(14) 1 d D U P A 2
F6A F 0.7694(16) 0.4275(6) 0.2732(12) 0.075(5) Uani 0.242(14) 1 d D U P A 2
P2 P 0.5000 0.24517(5) 0.2500 0.0228(4) Uani 1 2 d S T P . .
F7 F 0.5000 0.29749(12) 0.2500 0.0373(10) Uani 1 2 d S T P . .
F8 F 0.5000 0.19354(12) 0.2500 0.0397(10) Uani 1 2 d S T P . .
F9 F 0.5884(2) 0.24587(11) 0.2076(2) 0.0528(9) Uani 1 1 d . . . . .
F10 F 0.5456(2) 0.24577(10) 0.34539(18) 0.0452(8) Uani 1 1 d . . . . .
N13 N 0.9837(3) 0.34176(16) 0.4978(3) 0.0415(11) Uani 1 1 d . . . . .
C27 C 0.9281(3) 0.34508(15) 0.5409(3) 0.0275(10) Uani 1 1 d . . . . .
C28 C 0.8573(3) 0.34952(18) 0.5952(3) 0.0369(12) Uani 1 1 d . . . . .
H28A H 0.8339 0.3788 0.5884 0.055 Uiso 1 1 calc R U . . .
H28B H 0.8758 0.3447 0.6568 0.055 Uiso 1 1 calc R U . . .
H28C H 0.8143 0.3281 0.5771 0.055 Uiso 1 1 calc R U . . .
N14 N 0.1986(4) 0.4269(2) 0.4481(5) 0.0890(14) Uani 1 1 d . . . . .
C29 C 0.1376(5) 0.4413(3) 0.4270(7) 0.0890(14) Uani 1 1 d . . . . .
C30 C 0.0626(5) 0.4643(3) 0.3952(6) 0.0890(14) Uani 1 1 d . . . . .
H30A H 0.0785 0.4916 0.3679 0.134 Uiso 1 1 calc R U . . .
H30B H 0.0279 0.4705 0.4445 0.134 Uiso 1 1 calc R U . . .
H30C H 0.0309 0.4464 0.3518 0.134 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
Ni1 C19 1.859(5) . ?
Ni1 N8 1.909(3) . ?
Ni1 N1 1.909(4) . ?
Ni1 C24 1.913(5) . ?
Ni2 C11 1.857(4) . ?
Ni2 C6 1.912(5) . ?
Ni2 N2 1.917(4) . ?
Ni2 N7 1.928(3) . ?
N1 C2 1.342(6) . ?
N1 N2 1.356(5) . ?
N2 C4 1.339(6) . ?
N3 C6 1.358(6) . ?
N3 C7 1.389(6) . ?
N3 C5 1.462(6) . ?
N4 C6 1.367(6) . ?
N4 C8 1.390(6) . ?
N4 C9 1.470(6) . ?
N5 C11 1.351(6) . ?
N5 C12 1.373(6) . ?
N5 C10 1.465(6) . ?
N6 C11 1.360(5) . ?
N6 C13 1.377(6) . ?
N6 C14 1.470(5) . ?
N7 C15 1.343(5) . ?
N7 N8 1.364(5) . ?
N8 C17 1.352(5) . ?
N9 C19 1.357(5) . ?
N9 C20 1.391(6) . ?
N9 C18 1.473(5) . ?
N10 C19 1.348(6) . ?
N10 C21 1.380(6) . ?
N10 C22 1.468(5) . ?
N11 C24 1.371(6) . ?
N11 C25 1.385(6) . ?
N11 C23 1.461(6) . ?
N12 C24 1.363(6) . ?
N12 C26 1.376(6) . ?
N12 C1 1.453(7) . ?
C1 C2 1.489(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.399(7) . ?
C3 C4 1.381(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.488(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C7 C8 1.334(7) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.501(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 C13 1.350(7) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.503(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.394(6) . ?
C16 C17 1.377(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.509(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C20 C21 1.347(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.500(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C25 C26 1.341(8) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
P1 F5 1.563(6) . ?
P1 F2 1.588(7) . ?
P1 F6 1.593(6) . ?
P1 F1 1.596(7) . ?
P1 F4 1.596(6) . ?
P1 F3 1.604(6) . ?
P1A F2A 1.568(17) . ?
P1A F5A 1.582(16) . ?
P1A F6A 1.592(16) . ?
P1A F4A 1.595(17) . ?
P1A F1A 1.597(16) . ?
P1A F3A 1.609(16) . ?
P2 F10 1.588(3) . ?
P2 F10 1.588(3) 2_655 ?
P2 F9 1.590(3) 2_655 ?
P2 F9 1.590(3) . ?
P2 F8 1.592(4) . ?
P2 F7 1.613(4) . ?
N13 C27 1.142(6) . ?
C27 C28 1.449(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
N14 C29 1.102(9) . ?
C29 C30 1.450(11) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 Ni1 N8 87.87(16) . . ?
C19 Ni1 N1 171.91(17) . . ?
N8 Ni1 N1 89.60(15) . . ?
C19 Ni1 C24 90.18(19) . . ?
N8 Ni1 C24 168.19(17) . . ?
N1 Ni1 C24 90.74(18) . . ?
C11 Ni2 C6 91.41(19) . . ?
C11 Ni2 N2 174.97(17) . . ?
C6 Ni2 N2 89.95(17) . . ?
C11 Ni2 N7 87.48(17) . . ?
C6 Ni2 N7 168.69(16) . . ?
N2 Ni2 N7 90.24(15) . . ?
C2 N1 N2 108.7(4) . . ?
C2 N1 Ni1 125.1(3) . . ?
N2 N1 Ni1 126.1(3) . . ?
C4 N2 N1 107.6(4) . . ?
C4 N2 Ni2 126.6(3) . . ?
N1 N2 Ni2 125.7(3) . . ?
C6 N3 C7 112.2(4) . . ?
C6 N3 C5 125.6(4) . . ?
C7 N3 C5 122.2(4) . . ?
C6 N4 C8 111.3(4) . . ?
C6 N4 C9 130.9(4) . . ?
C8 N4 C9 117.7(4) . . ?
C11 N5 C12 110.9(4) . . ?
C11 N5 C10 123.1(4) . . ?
C12 N5 C10 126.0(4) . . ?
C11 N6 C13 111.1(4) . . ?
C11 N6 C14 122.4(3) . . ?
C13 N6 C14 126.1(4) . . ?
C15 N7 N8 107.7(3) . . ?
C15 N7 Ni2 126.5(3) . . ?
N8 N7 Ni2 125.8(3) . . ?
C17 N8 N7 108.1(3) . . ?
C17 N8 Ni1 126.2(3) . . ?
N7 N8 Ni1 125.3(3) . . ?
C19 N9 C20 111.1(4) . . ?
C19 N9 C18 122.2(4) . . ?
C20 N9 C18 126.4(3) . . ?
C19 N10 C21 111.2(4) . . ?
C19 N10 C22 121.5(4) . . ?
C21 N10 C22 127.1(4) . . ?
C24 N11 C25 110.6(4) . . ?
C24 N11 C23 130.8(4) . . ?
C25 N11 C23 118.5(4) . . ?
C24 N12 C26 111.0(4) . . ?
C24 N12 C1 125.3(4) . . ?
C26 N12 C1 123.4(4) . . ?
N12 C1 C2 111.8(4) . . ?
N12 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N12 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C3 109.0(4) . . ?
N1 C2 C1 119.3(4) . . ?
C3 C2 C1 131.7(4) . . ?
C4 C3 C2 104.2(4) . . ?
C4 C3 H3 127.9 . . ?
C2 C3 H3 127.9 . . ?
N2 C4 C3 110.4(4) . . ?
N2 C4 C5 118.9(4) . . ?
C3 C4 C5 130.6(4) . . ?
N3 C5 C4 111.2(4) . . ?
N3 C5 H5A 109.4 . . ?
C4 C5 H5A 109.4 . . ?
N3 C5 H5B 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
N3 C6 N4 103.1(4) . . ?
N3 C6 Ni2 120.4(3) . . ?
N4 C6 Ni2 136.5(3) . . ?
C8 C7 N3 106.3(4) . . ?
C8 C7 H7 126.8 . . ?
N3 C7 H7 126.8 . . ?
C7 C8 N4 107.1(4) . . ?
C7 C8 H8 126.4 . . ?
N4 C8 H8 126.4 . . ?
N4 C9 C10 115.3(4) . . ?
N4 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N4 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
N5 C10 C9 112.5(4) . . ?
N5 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
N5 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N5 C11 N6 104.5(4) . . ?
N5 C11 Ni2 129.4(3) . . ?
N6 C11 Ni2 125.9(3) . . ?
C13 C12 N5 107.4(4) . . ?
C13 C12 H12 126.3 . . ?
N5 C12 H12 126.3 . . ?
C12 C13 N6 106.2(4) . . ?
C12 C13 H13 126.9 . . ?
N6 C13 H13 126.9 . . ?
N6 C14 C15 109.0(3) . . ?
N6 C14 H14A 109.9 . . ?
C15 C14 H14A 109.9 . . ?
N6 C14 H14B 109.9 . . ?
C15 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
N7 C15 C16 109.9(4) . . ?
N7 C15 C14 119.8(4) . . ?
C16 C15 C14 130.3(4) . . ?
C17 C16 C15 104.5(4) . . ?
C17 C16 H16 127.7 . . ?
C15 C16 H16 127.7 . . ?
N8 C17 C16 109.8(4) . . ?
N8 C17 C18 119.2(4) . . ?
C16 C17 C18 131.0(4) . . ?
N9 C18 C17 109.4(3) . . ?
N9 C18 H18A 109.8 . . ?
C17 C18 H18A 109.8 . . ?
N9 C18 H18B 109.8 . . ?
C17 C18 H18B 109.8 . . ?
H18A C18 H18B 108.2 . . ?
N10 C19 N9 104.5(4) . . ?
N10 C19 Ni1 130.5(3) . . ?
N9 C19 Ni1 125.0(3) . . ?
C21 C20 N9 106.0(4) . . ?
C21 C20 H20 127.0 . . ?
N9 C20 H20 127.0 . . ?
C20 C21 N10 107.2(4) . . ?
C20 C21 H21 126.4 . . ?
N10 C21 H21 126.4 . . ?
N10 C22 C23 112.7(4) . . ?
N10 C22 H22A 109.1 . . ?
C23 C22 H22A 109.1 . . ?
N10 C22 H22B 109.1 . . ?
C23 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
N11 C23 C22 115.6(4) . . ?
N11 C23 H23A 108.4 . . ?
C22 C23 H23A 108.4 . . ?
N11 C23 H23B 108.4 . . ?
C22 C23 H23B 108.4 . . ?
H23A C23 H23B 107.4 . . ?
N12 C24 N11 104.0(4) . . ?
N12 C24 Ni1 119.4(3) . . ?
N11 C24 Ni1 136.4(4) . . ?
C26 C25 N11 106.9(4) . . ?
C26 C25 H25 126.6 . . ?
N11 C25 H25 126.6 . . ?
C25 C26 N12 107.5(4) . . ?
C25 C26 H26 126.3 . . ?
N12 C26 H26 126.3 . . ?
F5 P1 F2 88.7(4) . . ?
F5 P1 F6 91.7(4) . . ?
F2 P1 F6 89.7(4) . . ?
F5 P1 F1 94.5(5) . . ?
F2 P1 F1 176.7(6) . . ?
F6 P1 F1 89.4(5) . . ?
F5 P1 F4 91.0(4) . . ?
F2 P1 F4 90.4(4) . . ?
F6 P1 F4 177.3(5) . . ?
F1 P1 F4 90.3(4) . . ?
F5 P1 F3 174.8(5) . . ?
F2 P1 F3 86.4(4) . . ?
F6 P1 F3 90.0(5) . . ?
F1 P1 F3 90.4(5) . . ?
F4 P1 F3 87.3(4) . . ?
F2A P1A F5A 89.8(15) . . ?
F2A P1A F6A 87.4(13) . . ?
F5A P1A F6A 88.2(13) . . ?
F2A P1A F4A 94.2(16) . . ?
F5A P1A F4A 91.2(14) . . ?
F6A P1A F4A 178.3(17) . . ?
F2A P1A F1A 170.3(16) . . ?
F5A P1A F1A 98.9(13) . . ?
F6A P1A F1A 88.6(12) . . ?
F4A P1A F1A 89.9(15) . . ?
F2A P1A F3A 84.8(15) . . ?
F5A P1A F3A 174.4(15) . . ?
F6A P1A F3A 90.0(12) . . ?
F4A P1A F3A 90.7(15) . . ?
F1A P1A F3A 86.4(12) . . ?
F10 P2 F10 178.7(2) . 2_655 ?
F10 P2 F9 89.82(19) . 2_655 ?
F10 P2 F9 90.16(19) 2_655 2_655 ?
F10 P2 F9 90.16(19) . . ?
F10 P2 F9 89.82(19) 2_655 . ?
F9 P2 F9 178.4(3) 2_655 . ?
F10 P2 F8 90.66(12) . . ?
F10 P2 F8 90.66(12) 2_655 . ?
F9 P2 F8 90.78(14) 2_655 . ?
F9 P2 F8 90.77(14) . . ?
F10 P2 F7 89.34(12) . . ?
F10 P2 F7 89.34(12) 2_655 . ?
F9 P2 F7 89.22(14) 2_655 . ?
F9 P2 F7 89.23(14) . . ?
F8 P2 F7 180.0 . . ?
N13 C27 C28 179.6(6) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N14 C29 C30 173.4(10) . . ?
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 . . ?

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
C2 N1 N2 C4 -0.3(4) . . . . ?
Ni1 N1 N2 C4 -176.9(3) . . . . ?
C2 N1 N2 Ni2 176.9(3) . . . . ?
Ni1 N1 N2 Ni2 0.3(5) . . . . ?
C15 N7 N8 C17 0.5(4) . . . . ?
Ni2 N7 N8 C17 178.8(3) . . . . ?
C15 N7 N8 Ni1 -172.6(3) . . . . ?
Ni2 N7 N8 Ni1 5.7(5) . . . . ?
C24 N12 C1 C2 46.0(6) . . . . ?
C26 N12 C1 C2 -140.7(4) . . . . ?
N2 N1 C2 C3 0.5(5) . . . . ?
Ni1 N1 C2 C3 177.2(3) . . . . ?
N2 N1 C2 C1 -179.3(4) . . . . ?
Ni1 N1 C2 C1 -2.6(6) . . . . ?
N12 C1 C2 N1 -43.1(6) . . . . ?
N12 C1 C2 C3 137.2(5) . . . . ?
N1 C2 C3 C4 -0.5(5) . . . . ?
C1 C2 C3 C4 179.2(5) . . . . ?
N1 N2 C4 C3 0.0(5) . . . . ?
Ni2 N2 C4 C3 -177.2(3) . . . . ?
N1 N2 C4 C5 179.0(4) . . . . ?
Ni2 N2 C4 C5 1.8(6) . . . . ?
C2 C3 C4 N2 0.3(5) . . . . ?
C2 C3 C4 C5 -178.6(4) . . . . ?
C6 N3 C5 C4 -46.5(6) . . . . ?
C7 N3 C5 C4 137.0(4) . . . . ?
N2 C4 C5 N3 42.8(5) . . . . ?
C3 C4 C5 N3 -138.3(5) . . . . ?
C7 N3 C6 N4 0.2(5) . . . . ?
C5 N3 C6 N4 -176.6(4) . . . . ?
C7 N3 C6 Ni2 179.3(3) . . . . ?
C5 N3 C6 Ni2 2.4(6) . . . . ?
C8 N4 C6 N3 0.1(5) . . . . ?
C9 N4 C6 N3 178.4(4) . . . . ?
C8 N4 C6 Ni2 -178.7(4) . . . . ?
C9 N4 C6 Ni2 -0.4(7) . . . . ?
C6 N3 C7 C8 -0.5(5) . . . . ?
C5 N3 C7 C8 176.5(4) . . . . ?
N3 C7 C8 N4 0.5(5) . . . . ?
C6 N4 C8 C7 -0.4(5) . . . . ?
C9 N4 C8 C7 -179.0(4) . . . . ?
C6 N4 C9 C10 9.4(7) . . . . ?
C8 N4 C9 C10 -172.3(4) . . . . ?
C11 N5 C10 C9 77.8(5) . . . . ?
C12 N5 C10 C9 -104.6(5) . . . . ?
N4 C9 C10 N5 -67.0(5) . . . . ?
C12 N5 C11 N6 0.0(4) . . . . ?
C10 N5 C11 N6 177.9(4) . . . . ?
C12 N5 C11 Ni2 -174.2(3) . . . . ?
C10 N5 C11 Ni2 3.7(6) . . . . ?
C13 N6 C11 N5 -0.1(4) . . . . ?
C14 N6 C11 N5 -173.5(3) . . . . ?
C13 N6 C11 Ni2 174.5(3) . . . . ?
C14 N6 C11 Ni2 1.0(6) . . . . ?
C6 Ni2 C11 N5 -53.2(4) . . . . ?
N7 Ni2 C11 N5 138.1(4) . . . . ?
C6 Ni2 C11 N6 133.7(4) . . . . ?
N7 Ni2 C11 N6 -35.1(4) . . . . ?
C11 N5 C12 C13 0.0(5) . . . . ?
C10 N5 C12 C13 -177.8(4) . . . . ?
N5 C12 C13 N6 0.0(5) . . . . ?
C11 N6 C13 C12 0.1(5) . . . . ?
C14 N6 C13 C12 173.2(4) . . . . ?
C11 N6 C14 C15 45.4(5) . . . . ?
C13 N6 C14 C15 -127.0(4) . . . . ?
N8 N7 C15 C16 0.1(5) . . . . ?
Ni2 N7 C15 C16 -178.2(3) . . . . ?
N8 N7 C15 C14 -179.8(4) . . . . ?
Ni2 N7 C15 C14 1.9(6) . . . . ?
N6 C14 C15 N7 -45.8(5) . . . . ?
N6 C14 C15 C16 134.3(5) . . . . ?
N7 C15 C16 C17 -0.6(5) . . . . ?
C14 C15 C16 C17 179.3(4) . . . . ?
N7 N8 C17 C16 -0.9(5) . . . . ?
Ni1 N8 C17 C16 172.1(3) . . . . ?
N7 N8 C17 C18 179.9(4) . . . . ?
Ni1 N8 C17 C18 -7.1(6) . . . . ?
C15 C16 C17 N8 0.9(5) . . . . ?
C15 C16 C17 C18 -180.0(4) . . . . ?
C19 N9 C18 C17 -41.0(5) . . . . ?
C20 N9 C18 C17 131.8(4) . . . . ?
N8 C17 C18 N9 48.5(5) . . . . ?
C16 C17 C18 N9 -130.5(5) . . . . ?
C21 N10 C19 N9 0.9(5) . . . . ?
C22 N10 C19 N9 -174.9(4) . . . . ?
C21 N10 C19 Ni1 -176.4(3) . . . . ?
C22 N10 C19 Ni1 7.7(6) . . . . ?
C20 N9 C19 N10 -0.5(5) . . . . ?
C18 N9 C19 N10 173.3(4) . . . . ?
C20 N9 C19 Ni1 177.0(3) . . . . ?
C18 N9 C19 Ni1 -9.2(6) . . . . ?
N8 Ni1 C19 N10 -143.1(4) . . . . ?
C24 Ni1 C19 N10 48.6(4) . . . . ?
N8 Ni1 C19 N9 40.1(4) . . . . ?
C24 Ni1 C19 N9 -128.3(4) . . . . ?
C19 N9 C20 C21 -0.1(5) . . . . ?
C18 N9 C20 C21 -173.5(4) . . . . ?
N9 C20 C21 N10 0.7(5) . . . . ?
C19 N10 C21 C20 -1.0(5) . . . . ?
C22 N10 C21 C20 174.5(4) . . . . ?
C19 N10 C22 C23 -84.2(5) . . . . ?
C21 N10 C22 C23 100.7(5) . . . . ?
C24 N11 C23 C22 6.5(6) . . . . ?
C25 N11 C23 C22 -175.7(4) . . . . ?
N10 C22 C23 N11 57.4(5) . . . . ?
C26 N12 C24 N11 0.8(5) . . . . ?
C1 N12 C24 N11 174.8(4) . . . . ?
C26 N12 C24 Ni1 -174.8(3) . . . . ?
C1 N12 C24 Ni1 -0.8(6) . . . . ?
C25 N11 C24 N12 -0.8(5) . . . . ?
C23 N11 C24 N12 177.1(4) . . . . ?
C25 N11 C24 Ni1 173.6(4) . . . . ?
C23 N11 C24 Ni1 -8.4(7) . . . . ?
C24 N11 C25 C26 0.6(5) . . . . ?
C23 N11 C25 C26 -177.7(4) . . . . ?
N11 C25 C26 N12 -0.1(5) . . . . ?
C24 N12 C26 C25 -0.5(5) . . . . ?
C1 N12 C26 C25 -174.6(4) . . . . ?




#===END
####################################################################### 
# 
# 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_altph28_0m
_database_code_depnum_ccdc_archive 'CCDC 1448011'
_audit_update_record             
;
2016-01-17 deposited with the CCDC.
2016-02-18 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C26 H26 N12 Ni2), 3(F6 P), 4(C3 H7 N O), Cl'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C64 H80 Cl F18 N28 Ni4 O4 P3'
_chemical_formula_iupac          ?
_chemical_formula_weight         2010.68
_chemical_compound_source        'see text'

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

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_Int_Tables_number      15

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z

_cell_length_a                   16.233(3)
_cell_length_b                   31.342(5)
_cell_length_c                   15.432(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.632(10)
_cell_angle_gamma                90
_cell_volume                     7814(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    4698
_cell_measurement_theta_min      2.5994
_cell_measurement_theta_max      23.8042
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            'pale yellow'

_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.085
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             4112
_exptl_absorpt_coefficient_mu    1.156
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_T_max  0.7452

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             Philipp J. Altmann
scanspeed                           60 s per frame
dx                                  62 mm
2039 frames measured in 7 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            36056
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             6903
# number of observed reflections (> n sig(I))
_reflns_number_gt                4585
_reflns_threshold_expression     i>2σ(i)

_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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     
'W=1/[Σ²(FO²)+(0.0383P)²+2.6705P] 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_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         6903
_refine_ls_number_parameters     668
_refine_ls_number_restraints     203
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0849
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.084

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.33586(3) 0.31013(2) 0.22657(3) 0.01837(14) Uani 1 1 d . . . . .
N1 N 0.2902(2) 0.36526(10) 0.23314(18) 0.0201(8) Uani 1 1 d . . . . .
N2 N 0.3177(2) 0.39637(10) 0.29058(18) 0.0204(8) Uani 1 1 d . . . . .
Ni2 Ni 0.40838(3) 0.39121(2) 0.37863(3) 0.01982(14) Uani 1 1 d . . . . .
N3 N 0.3677(2) 0.47890(10) 0.34708(19) 0.0244(8) Uani 1 1 d . . . . .
N4 N 0.4987(2) 0.47618(10) 0.37602(19) 0.0239(8) Uani 1 1 d . . . . .
N5 N 0.5697(2) 0.39809(10) 0.4758(2) 0.0238(8) Uani 1 1 d . . . . .
N6 N 0.4818(2) 0.36610(10) 0.54779(19) 0.0214(8) Uani 1 1 d . . . . .
N7 N 0.37287(19) 0.33524(9) 0.40798(18) 0.0182(8) Uani 1 1 d . . . . .
N8 N 0.34109(19) 0.30526(10) 0.35026(18) 0.0180(7) Uani 1 1 d . . . . .
N9 N 0.33570(19) 0.22234(10) 0.27440(18) 0.0188(8) Uani 1 1 d . . . . .
N10 N 0.4150(2) 0.23299(10) 0.17405(18) 0.0189(8) Uani 1 1 d . . . . .
N11 N 0.3385(2) 0.29006(10) 0.03370(19) 0.0224(8) Uani 1 1 d . . . . .
N12 N 0.2382(2) 0.32841(10) 0.06895(19) 0.0231(8) Uani 1 1 d . . . . .
C1 C 0.1795(2) 0.35131(13) 0.1189(2) 0.0253(10) Uani 1 1 d . . . . .
H1A H 0.1457 0.3304 0.1480 0.030 Uiso 1 1 calc R U . . .
H1B H 0.1416 0.3685 0.0786 0.030 Uiso 1 1 calc R U . . .
C2 C 0.2231(2) 0.37992(13) 0.1857(2) 0.0215(9) Uani 1 1 d . . . . .
C3 C 0.2045(3) 0.42080(13) 0.2123(2) 0.0236(10) Uani 1 1 d . . . . .
H3 H 0.1597 0.4385 0.1905 0.028 Uiso 1 1 calc R U . . .
C4 C 0.2662(3) 0.42980(13) 0.2781(2) 0.0249(10) Uani 1 1 d . . . . .
C5 C 0.2808(3) 0.46757(13) 0.3360(2) 0.0258(10) Uani 1 1 d . . . . .
H5A H 0.2482 0.4921 0.3107 0.031 Uiso 1 1 calc R U . . .
H5B H 0.2616 0.4611 0.3936 0.031 Uiso 1 1 calc R U . . .
C6 C 0.4303(3) 0.45059(13) 0.3676(2) 0.0219(10) Uani 1 1 d . . . . .
C7 C 0.3962(3) 0.52018(13) 0.3440(3) 0.0314(11) Uani 1 1 d . . . . .
H7 H 0.3637 0.5450 0.3311 0.038 Uiso 1 1 calc R U . . .
C8 C 0.4777(3) 0.51861(13) 0.3624(2) 0.0318(11) Uani 1 1 d . . . . .
H8 H 0.5146 0.5422 0.3657 0.038 Uiso 1 1 calc R U . . .
C9 C 0.5863(3) 0.46557(13) 0.3988(3) 0.0288(11) Uani 1 1 d . . . . .
H9A H 0.6044 0.4783 0.4563 0.035 Uiso 1 1 calc R U . . .
H9B H 0.6194 0.4789 0.3555 0.035 Uiso 1 1 calc R U . . .
C10 C 0.6050(3) 0.41895(13) 0.4026(2) 0.0269(10) Uani 1 1 d . . . . .
H10A H 0.5822 0.4054 0.3474 0.032 Uiso 1 1 calc R U . . .
H10B H 0.6657 0.4148 0.4086 0.032 Uiso 1 1 calc R U . . .
C11 C 0.4902(3) 0.38593(12) 0.4712(2) 0.0221(10) Uani 1 1 d . . . . .
C12 C 0.6114(3) 0.38570(12) 0.5546(2) 0.0274(10) Uani 1 1 d . . . . .
H12 H 0.6681 0.3906 0.5731 0.033 Uiso 1 1 calc R U . . .
C13 C 0.5569(3) 0.36553(13) 0.5998(2) 0.0270(10) Uani 1 1 d . . . . .
H13 H 0.5674 0.3533 0.6561 0.032 Uiso 1 1 calc R U . . .
C14 C 0.4065(3) 0.34412(12) 0.5666(2) 0.0234(10) Uani 1 1 d . . . . .
H14A H 0.3647 0.3652 0.5813 0.028 Uiso 1 1 calc R U . . .
H14B H 0.4187 0.3250 0.6173 0.028 Uiso 1 1 calc R U . . .
C15 C 0.3728(2) 0.31839(13) 0.4886(2) 0.0203(9) Uani 1 1 d . . . . .
C16 C 0.3413(2) 0.27761(12) 0.4839(2) 0.0191(9) Uani 1 1 d . . . . .
H16 H 0.3347 0.2587 0.5308 0.023 Uiso 1 1 calc R U . . .
C17 C 0.3214(2) 0.27020(12) 0.3950(2) 0.0190(9) Uani 1 1 d . . . . .
C18 C 0.2850(2) 0.23262(12) 0.3458(2) 0.0219(9) Uani 1 1 d . . . . .
H18A H 0.2834 0.2078 0.3853 0.026 Uiso 1 1 calc R U . . .
H18B H 0.2276 0.2391 0.3217 0.026 Uiso 1 1 calc R U . . .
C19 C 0.3642(2) 0.25331(12) 0.2239(2) 0.0174(9) Uani 1 1 d . . . . .
C20 C 0.3674(3) 0.18291(12) 0.2551(2) 0.0226(10) Uani 1 1 d . . . . .
H20 H 0.3564 0.1564 0.2815 0.027 Uiso 1 1 calc R U . . .
C21 C 0.4172(2) 0.18963(13) 0.1914(2) 0.0223(9) Uani 1 1 d . . . . .
H21 H 0.4479 0.1687 0.1638 0.027 Uiso 1 1 calc R U . . .
C22 C 0.4629(2) 0.25636(13) 0.1138(2) 0.0235(10) Uani 1 1 d . . . . .
H22A H 0.5125 0.2395 0.1035 0.028 Uiso 1 1 calc R U . . .
H22B H 0.4819 0.2837 0.1410 0.028 Uiso 1 1 calc R U . . .
C23 C 0.4139(3) 0.26543(13) 0.0278(2) 0.0251(10) Uani 1 1 d . . . . .
H23A H 0.4497 0.2811 -0.0097 0.030 Uiso 1 1 calc R U . . .
H23B H 0.3989 0.2379 -0.0012 0.030 Uiso 1 1 calc R U . . .
C24 C 0.3088(2) 0.30936(12) 0.1039(2) 0.0198(9) Uani 1 1 d . . . . .
C25 C 0.2857(3) 0.29715(13) -0.0415(2) 0.0275(11) Uani 1 1 d . . . . .
H25 H 0.2931 0.2868 -0.0981 0.033 Uiso 1 1 calc R U . . .
C26 C 0.2233(3) 0.32101(13) -0.0199(2) 0.0272(11) Uani 1 1 d . . . . .
H26 H 0.1776 0.3310 -0.0577 0.033 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5000 0.34836(4) 0.2500 0.0208(3) Uani 1 2 d S T P . .
O1 O -0.0162(2) 0.34192(11) 0.51912(18) 0.0472(9) Uani 1 1 d . . . . .
N13 N 0.0821(2) 0.35779(10) 0.4292(2) 0.0242(8) Uani 1 1 d . . . . .
C27 C 0.1602(3) 0.34678(15) 0.3971(3) 0.0387(12) Uani 1 1 d . . . . .
H27A H 0.1503 0.3370 0.3366 0.058 Uiso 1 1 calc R U . . .
H27B H 0.1869 0.3240 0.4331 0.058 Uiso 1 1 calc R U . . .
H27C H 0.1963 0.3719 0.3998 0.058 Uiso 1 1 calc R U . . .
C28 C 0.0373(4) 0.39301(17) 0.3877(4) 0.090(2) Uani 1 1 d . . . . .
H28A H 0.0766 0.4135 0.3671 0.134 Uiso 1 1 calc R U . . .
H28B H 0.0045 0.4070 0.4296 0.134 Uiso 1 1 calc R U . . .
H28C H 0.0005 0.3825 0.3382 0.134 Uiso 1 1 calc R U . . .
C29 C 0.0495(3) 0.33560(16) 0.4892(3) 0.0413(13) Uani 1 1 d . . . . .
H29 H 0.0808 0.3118 0.5121 0.050 Uiso 1 1 calc R U . . .
O2 O 0.2076(13) 0.5753(6) 0.4835(15) 0.045(4) Uani 0.443(14) 1 d D U P A 1
N14 N 0.0981(12) 0.5419(6) 0.4238(11) 0.036(4) Uani 0.443(14) 1 d D U P A 1
C30 C 0.1717(14) 0.5423(8) 0.4713(18) 0.056(7) Uani 0.443(14) 1 d D U P A 1
H30 H 0.1951 0.5166 0.4951 0.067 Uiso 0.443(14) 1 calc R U P A 1
C31 C 0.0335(8) 0.5128(4) 0.4389(11) 0.062(5) Uani 0.443(14) 1 d D U P A 1
H31A H 0.0123 0.4994 0.3839 0.093 Uiso 0.443(14) 1 calc R U P A 1
H31B H -0.0114 0.5283 0.4632 0.093 Uiso 0.443(14) 1 calc R U P A 1
H31C H 0.0551 0.4908 0.4802 0.093 Uiso 0.443(14) 1 calc R U P A 1
C32 C 0.0853(15) 0.5676(6) 0.3466(15) 0.054(7) Uani 0.443(14) 1 d D U P A 1
H32A H 0.0764 0.5490 0.2954 0.082 Uiso 0.443(14) 1 calc R U P A 1
H32B H 0.1340 0.5855 0.3417 0.082 Uiso 0.443(14) 1 calc R U P A 1
H32C H 0.0366 0.5857 0.3500 0.082 Uiso 0.443(14) 1 calc R U P A 1
O2A O 0.2230(12) 0.5690(7) 0.4673(15) 0.099(9) Uani 0.557(14) 1 d D U P A 2
N14A N 0.1055(10) 0.5431(5) 0.3972(9) 0.038(3) Uani 0.557(14) 1 d D U P A 2
C30A C 0.1658(8) 0.5450(5) 0.4625(11) 0.031(4) Uani 0.557(14) 1 d D U P A 2
H30A H 0.1629 0.5255 0.5092 0.037 Uiso 0.557(14) 1 calc R U P A 2
C31A C 0.0709(8) 0.5039(3) 0.3645(10) 0.085(6) Uani 0.557(14) 1 d D U P A 2
H31D H 0.0742 0.5024 0.3015 0.128 Uiso 0.557(14) 1 calc R U P A 2
H31E H 0.0129 0.5021 0.3766 0.128 Uiso 0.557(14) 1 calc R U P A 2
H31F H 0.1020 0.4800 0.3929 0.128 Uiso 0.557(14) 1 calc R U P A 2
C32A C 0.0772(14) 0.5820(5) 0.3548(13) 0.054(5) Uani 0.557(14) 1 d D U P A 2
H32D H 0.0861 0.5806 0.2930 0.081 Uiso 0.557(14) 1 calc R U P A 2
H32E H 0.1081 0.6062 0.3820 0.081 Uiso 0.557(14) 1 calc R U P A 2
H32F H 0.0180 0.5858 0.3606 0.081 Uiso 0.557(14) 1 calc R U P A 2
P1 P 0.5000 0.24578(5) 0.7500 0.0319(4) Uani 1 2 d S T P . .
F1 F 0.5838(2) 0.24621(13) 0.7077(3) 0.1115(14) Uani 1 1 d . . . . .
F2 F 0.5000 0.19587(12) 0.7500 0.0944(19) Uani 1 2 d S T P . .
F3 F 0.5000 0.29643(11) 0.7500 0.0662(14) Uani 1 2 d S T P . .
F4 F 0.4525(2) 0.24606(9) 0.65569(17) 0.0745(11) Uani 1 1 d . . . . .
P2 P 0.2327(6) 0.4332(3) 0.6400(6) 0.044(2) Uani 0.425(15) 1 d D U P B 3
F5 F 0.3305(5) 0.4305(3) 0.6500(8) 0.056(3) Uani 0.425(15) 1 d D U P B 3
F6 F 0.1346(6) 0.4369(5) 0.6321(9) 0.068(3) Uani 0.425(15) 1 d D U P B 3
F7 F 0.2324(11) 0.4389(3) 0.5370(6) 0.062(3) Uani 0.425(15) 1 d D U P B 3
F8 F 0.2273(10) 0.3823(3) 0.6282(9) 0.053(3) Uani 0.425(15) 1 d D U P B 3
F9 F 0.2315(7) 0.4277(4) 0.7432(6) 0.050(3) Uani 0.425(15) 1 d D U P B 3
F10 F 0.2426(9) 0.4830(3) 0.6546(9) 0.054(3) Uani 0.425(15) 1 d D U P B 3
P2A P 0.2194(4) 0.4290(2) 0.6236(5) 0.0322(14) Uani 0.575(15) 1 d D U P B 4
F5A F 0.3097(5) 0.4384(2) 0.5974(9) 0.075(3) Uani 0.575(15) 1 d D U P B 4
F6A F 0.1277(4) 0.4179(3) 0.6462(5) 0.045(2) Uani 0.575(15) 1 d D U P B 4
F7A F 0.1829(7) 0.4393(2) 0.5254(4) 0.054(2) Uani 0.575(15) 1 d D U P B 4
F8A F 0.2284(6) 0.3800(2) 0.5960(7) 0.041(2) Uani 0.575(15) 1 d D U P B 4
F9A F 0.2547(7) 0.4176(3) 0.7209(6) 0.068(3) Uani 0.575(15) 1 d D U P B 4
F10A F 0.2062(7) 0.4775(2) 0.6483(7) 0.054(2) Uani 0.575(15) 1 d D U P B 4


_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 C19 1.841(4) . ?
Ni1 N1 1.887(3) . ?
Ni1 C24 1.901(4) . ?
Ni1 N8 1.909(3) . ?
N1 C2 1.333(5) . ?
N1 N2 1.363(4) . ?
N2 C4 1.342(5) . ?
N2 Ni2 1.910(3) . ?
Ni2 C11 1.860(4) . ?
Ni2 C6 1.905(4) . ?
Ni2 N7 1.915(3) . ?
N3 C6 1.363(5) . ?
N3 C7 1.376(5) . ?
N3 C5 1.449(5) . ?
N4 C6 1.366(5) . ?
N4 C8 1.384(5) . ?
N4 C9 1.469(5) . ?
N5 C11 1.341(5) . ?
N5 C12 1.388(5) . ?
N5 C10 1.470(5) . ?
N6 C11 1.354(4) . ?
N6 C13 1.392(5) . ?
N6 C14 1.458(5) . ?
N7 C15 1.351(4) . ?
N7 N8 1.361(4) . ?
N8 C17 1.353(4) . ?
N9 C19 1.355(4) . ?
N9 C20 1.382(5) . ?
N9 C18 1.475(4) . ?
N10 C19 1.342(5) . ?
N10 C21 1.385(5) . ?
N10 C22 1.465(5) . ?
N11 C24 1.369(5) . ?
N11 C25 1.391(5) . ?
N11 C23 1.458(5) . ?
N12 C24 1.356(5) . ?
N12 C26 1.389(4) . ?
N12 C1 1.471(5) . ?
C1 C2 1.491(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.388(5) . ?
C3 C4 1.383(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.488(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C7 C8 1.327(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.492(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 C13 1.337(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.507(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.376(5) . ?
C16 C17 1.398(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.492(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C20 C21 1.350(5) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.506(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C25 C26 1.328(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
O1 C29 1.220(5) . ?
N13 C29 1.310(5) . ?
N13 C28 1.437(5) . ?
N13 C27 1.448(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29 0.9500 . ?
O2 C30 1.192(15) . ?
N14 C30 1.339(13) . ?
N14 C31 1.426(14) . ?
N14 C32 1.436(14) . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O2A C30A 1.193(12) . ?
N14A C30A 1.336(11) . ?
N14A C31A 1.423(13) . ?
N14A C32A 1.438(13) . ?
C30A H30A 0.9500 . ?
C31A H31D 0.9800 . ?
C31A H31E 0.9800 . ?
C31A H31F 0.9800 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?
P1 F2 1.565(4) . ?
P1 F1 1.565(4) 2_656 ?
P1 F1 1.565(4) . ?
P1 F4 1.579(2) 2_656 ?
P1 F4 1.579(2) . ?
P1 F3 1.587(4) . ?
P2 F10 1.581(10) . ?
P2 F5 1.584(10) . ?
P2 F6 1.589(10) . ?
P2 F7 1.598(10) . ?
P2 F9 1.604(10) . ?
P2 F8 1.609(10) . ?
P2A F5A 1.586(7) . ?
P2A F10A 1.588(7) . ?
P2A F9A 1.594(7) . ?
P2A F6A 1.599(7) . ?
P2A F8A 1.604(7) . ?
P2A F7A 1.606(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
C19 Ni1 N1 170.96(15) . . ?
C19 Ni1 C24 89.97(16) . . ?
N1 Ni1 C24 90.66(15) . . ?
C19 Ni1 N8 87.62(14) . . ?
N1 Ni1 N8 89.91(13) . . ?
C24 Ni1 N8 168.01(15) . . ?
C2 N1 N2 107.9(3) . . ?
C2 N1 Ni1 126.2(3) . . ?
N2 N1 Ni1 125.8(2) . . ?
C4 N2 N1 107.8(3) . . ?
C4 N2 Ni2 126.5(3) . . ?
N1 N2 Ni2 125.6(2) . . ?
C11 Ni2 C6 91.73(17) . . ?
C11 Ni2 N2 175.15(15) . . ?
C6 Ni2 N2 89.51(15) . . ?
C11 Ni2 N7 86.88(15) . . ?
C6 Ni2 N7 168.29(14) . . ?
N2 Ni2 N7 90.97(13) . . ?
C6 N3 C7 112.0(4) . . ?
C6 N3 C5 124.3(3) . . ?
C7 N3 C5 123.5(4) . . ?
C6 N4 C8 111.3(4) . . ?
C6 N4 C9 130.4(3) . . ?
C8 N4 C9 118.2(4) . . ?
C11 N5 C12 110.5(3) . . ?
C11 N5 C10 122.1(3) . . ?
C12 N5 C10 127.2(4) . . ?
C11 N6 C13 110.6(3) . . ?
C11 N6 C14 123.3(3) . . ?
C13 N6 C14 125.7(3) . . ?
C15 N7 N8 107.3(3) . . ?
C15 N7 Ni2 127.1(3) . . ?
N8 N7 Ni2 125.5(2) . . ?
C17 N8 N7 108.7(3) . . ?
C17 N8 Ni1 125.9(2) . . ?
N7 N8 Ni1 125.2(2) . . ?
C19 N9 C20 111.2(3) . . ?
C19 N9 C18 121.4(3) . . ?
C20 N9 C18 127.1(3) . . ?
C19 N10 C21 111.1(3) . . ?
C19 N10 C22 121.4(3) . . ?
C21 N10 C22 127.4(3) . . ?
C24 N11 C25 110.7(3) . . ?
C24 N11 C23 130.3(3) . . ?
C25 N11 C23 119.0(3) . . ?
C24 N12 C26 112.2(3) . . ?
C24 N12 C1 124.9(3) . . ?
C26 N12 C1 122.7(3) . . ?
N12 C1 C2 111.6(3) . . ?
N12 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N12 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C3 110.2(3) . . ?
N1 C2 C1 118.6(3) . . ?
C3 C2 C1 131.1(4) . . ?
C4 C3 C2 104.0(4) . . ?
C4 C3 H3 128.0 . . ?
C2 C3 H3 128.0 . . ?
N2 C4 C3 110.0(4) . . ?
N2 C4 C5 118.3(4) . . ?
C3 C4 C5 131.6(4) . . ?
N3 C5 C4 111.2(3) . . ?
N3 C5 H5A 109.4 . . ?
C4 C5 H5A 109.4 . . ?
N3 C5 H5B 109.4 . . ?
C4 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
N3 C6 N4 102.7(3) . . ?
N3 C6 Ni2 121.0(3) . . ?
N4 C6 Ni2 136.2(3) . . ?
C8 C7 N3 106.8(4) . . ?
C8 C7 H7 126.6 . . ?
N3 C7 H7 126.6 . . ?
C7 C8 N4 107.1(4) . . ?
C7 C8 H8 126.4 . . ?
N4 C8 H8 126.4 . . ?
N4 C9 C10 114.8(3) . . ?
N4 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
N4 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.5 . . ?
N5 C10 C9 111.9(3) . . ?
N5 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
N5 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
N5 C11 N6 105.2(3) . . ?
N5 C11 Ni2 128.8(3) . . ?
N6 C11 Ni2 125.9(3) . . ?
C13 C12 N5 107.4(4) . . ?
C13 C12 H12 126.3 . . ?
N5 C12 H12 126.3 . . ?
C12 C13 N6 106.2(3) . . ?
C12 C13 H13 126.9 . . ?
N6 C13 H13 126.9 . . ?
N6 C14 C15 109.9(3) . . ?
N6 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
N6 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N7 C15 C16 110.5(3) . . ?
N7 C15 C14 119.6(3) . . ?
C16 C15 C14 130.0(3) . . ?
C15 C16 C17 104.7(3) . . ?
C15 C16 H16 127.6 . . ?
C17 C16 H16 127.6 . . ?
N8 C17 C16 108.8(3) . . ?
N8 C17 C18 118.9(3) . . ?
C16 C17 C18 132.3(3) . . ?
N9 C18 C17 109.3(3) . . ?
N9 C18 H18A 109.8 . . ?
C17 C18 H18A 109.8 . . ?
N9 C18 H18B 109.8 . . ?
C17 C18 H18B 109.8 . . ?
H18A C18 H18B 108.3 . . ?
N10 C19 N9 104.7(3) . . ?
N10 C19 Ni1 129.9(3) . . ?
N9 C19 Ni1 125.4(3) . . ?
C21 C20 N9 106.2(3) . . ?
C21 C20 H20 126.9 . . ?
N9 C20 H20 126.9 . . ?
C20 C21 N10 106.7(3) . . ?
C20 C21 H21 126.6 . . ?
N10 C21 H21 126.6 . . ?
N10 C22 C23 112.7(3) . . ?
N10 C22 H22A 109.0 . . ?
C23 C22 H22A 109.0 . . ?
N10 C22 H22B 109.0 . . ?
C23 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
N11 C23 C22 114.8(3) . . ?
N11 C23 H23A 108.6 . . ?
C22 C23 H23A 108.6 . . ?
N11 C23 H23B 108.6 . . ?
C22 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
N12 C24 N11 103.3(3) . . ?
N12 C24 Ni1 119.6(3) . . ?
N11 C24 Ni1 136.8(3) . . ?
C26 C25 N11 107.6(4) . . ?
C26 C25 H25 126.2 . . ?
N11 C25 H25 126.2 . . ?
C25 C26 N12 106.2(4) . . ?
C25 C26 H26 126.9 . . ?
N12 C26 H26 126.9 . . ?
C29 N13 C28 120.1(4) . . ?
C29 N13 C27 122.9(4) . . ?
C28 N13 C27 116.9(3) . . ?
N13 C27 H27A 109.5 . . ?
N13 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N13 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N13 C28 H28A 109.5 . . ?
N13 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N13 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O1 C29 N13 127.6(5) . . ?
O1 C29 H29 116.2 . . ?
N13 C29 H29 116.2 . . ?
C30 N14 C31 123.3(13) . . ?
C30 N14 C32 119.8(16) . . ?
C31 N14 C32 116.4(12) . . ?
O2 C30 N14 119(2) . . ?
O2 C30 H30 120.3 . . ?
N14 C30 H30 120.3 . . ?
N14 C31 H31A 109.5 . . ?
N14 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N14 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N14 C32 H32A 109.5 . . ?
N14 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N14 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30A N14A C31A 122.7(13) . . ?
C30A N14A C32A 118.9(12) . . ?
C31A N14A C32A 118.3(10) . . ?
O2A C30A N14A 125.7(16) . . ?
O2A C30A H30A 117.2 . . ?
N14A C30A H30A 117.2 . . ?
N14A C31A H31D 109.5 . . ?
N14A C31A H31E 109.5 . . ?
H31D C31A H31E 109.5 . . ?
N14A C31A H31F 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
N14A C32A H32D 109.5 . . ?
N14A C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
N14A C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
F2 P1 F1 90.49(17) . 2_656 ?
F2 P1 F1 90.49(17) . . ?
F1 P1 F1 179.0(3) 2_656 . ?
F2 P1 F4 90.32(12) . 2_656 ?
F1 P1 F4 88.9(2) 2_656 2_656 ?
F1 P1 F4 91.1(2) . 2_656 ?
F2 P1 F4 90.32(12) . . ?
F1 P1 F4 91.1(2) 2_656 . ?
F1 P1 F4 88.9(2) . . ?
F4 P1 F4 179.4(2) 2_656 . ?
F2 P1 F3 180.0 . . ?
F1 P1 F3 89.51(17) 2_656 . ?
F1 P1 F3 89.51(17) . . ?
F4 P1 F3 89.68(12) 2_656 . ?
F4 P1 F3 89.68(12) . . ?
F10 P2 F5 87.2(7) . . ?
F10 P2 F6 91.5(7) . . ?
F5 P2 F6 178.3(9) . . ?
F10 P2 F7 91.3(7) . . ?
F5 P2 F7 90.4(6) . . ?
F6 P2 F7 90.7(7) . . ?
F10 P2 F9 88.6(7) . . ?
F5 P2 F9 90.4(6) . . ?
F6 P2 F9 88.5(7) . . ?
F7 P2 F9 179.1(9) . . ?
F10 P2 F8 176.9(9) . . ?
F5 P2 F8 90.0(8) . . ?
F6 P2 F8 91.2(8) . . ?
F7 P2 F8 90.2(7) . . ?
F9 P2 F8 89.9(7) . . ?
F5A P2A F10A 91.9(5) . . ?
F5A P2A F9A 91.5(5) . . ?
F10A P2A F9A 91.9(5) . . ?
F5A P2A F6A 177.2(6) . . ?
F10A P2A F6A 90.3(5) . . ?
F9A P2A F6A 90.2(5) . . ?
F5A P2A F8A 90.0(5) . . ?
F10A P2A F8A 177.2(6) . . ?
F9A P2A F8A 90.1(5) . . ?
F6A P2A F8A 87.8(5) . . ?
F5A P2A F7A 89.2(5) . . ?
F10A P2A F7A 89.3(5) . . ?
F9A P2A F7A 178.6(6) . . ?
F6A P2A F7A 89.0(5) . . ?
F8A P2A F7A 88.7(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
C24 Ni1 N1 C2 36.9(3) . . . . ?
N8 Ni1 N1 C2 -131.2(3) . . . . ?
C24 Ni1 N1 N2 -146.9(3) . . . . ?
N8 Ni1 N1 N2 45.1(3) . . . . ?
C2 N1 N2 C4 0.6(4) . . . . ?
Ni1 N1 N2 C4 -176.3(3) . . . . ?
C2 N1 N2 Ni2 176.3(2) . . . . ?
Ni1 N1 N2 Ni2 -0.5(4) . . . . ?
C15 N7 N8 C17 0.1(4) . . . . ?
Ni2 N7 N8 C17 -178.6(3) . . . . ?
C15 N7 N8 Ni1 -174.2(3) . . . . ?
Ni2 N7 N8 Ni1 7.1(4) . . . . ?
C24 N12 C1 C2 44.3(5) . . . . ?
C26 N12 C1 C2 -141.1(4) . . . . ?
N2 N1 C2 C3 -1.0(4) . . . . ?
Ni1 N1 C2 C3 175.8(2) . . . . ?
N2 N1 C2 C1 -178.5(3) . . . . ?
Ni1 N1 C2 C1 -1.6(5) . . . . ?
N12 C1 C2 N1 -43.4(5) . . . . ?
N12 C1 C2 C3 139.8(4) . . . . ?
N1 C2 C3 C4 1.1(4) . . . . ?
C1 C2 C3 C4 178.1(4) . . . . ?
N1 N2 C4 C3 0.1(4) . . . . ?
Ni2 N2 C4 C3 -175.6(3) . . . . ?
N1 N2 C4 C5 177.3(3) . . . . ?
Ni2 N2 C4 C5 1.6(5) . . . . ?
C2 C3 C4 N2 -0.7(4) . . . . ?
C2 C3 C4 C5 -177.4(4) . . . . ?
C6 N3 C5 C4 -48.5(5) . . . . ?
C7 N3 C5 C4 136.2(4) . . . . ?
N2 C4 C5 N3 44.8(5) . . . . ?
C3 C4 C5 N3 -138.7(4) . . . . ?
C7 N3 C6 N4 -0.7(4) . . . . ?
C5 N3 C6 N4 -176.4(3) . . . . ?
C7 N3 C6 Ni2 178.8(3) . . . . ?
C5 N3 C6 Ni2 3.0(5) . . . . ?
C8 N4 C6 N3 1.0(4) . . . . ?
C9 N4 C6 N3 179.0(3) . . . . ?
C8 N4 C6 Ni2 -178.3(3) . . . . ?
C9 N4 C6 Ni2 -0.3(6) . . . . ?
C6 N3 C7 C8 0.1(4) . . . . ?
C5 N3 C7 C8 175.9(3) . . . . ?
N3 C7 C8 N4 0.5(4) . . . . ?
C6 N4 C8 C7 -1.0(4) . . . . ?
C9 N4 C8 C7 -179.2(3) . . . . ?
C6 N4 C9 C10 8.7(6) . . . . ?
C8 N4 C9 C10 -173.5(3) . . . . ?
C11 N5 C10 C9 81.7(5) . . . . ?
C12 N5 C10 C9 -102.7(4) . . . . ?
N4 C9 C10 N5 -68.2(4) . . . . ?
C12 N5 C11 N6 0.4(4) . . . . ?
C10 N5 C11 N6 176.7(3) . . . . ?
C12 N5 C11 Ni2 -175.9(3) . . . . ?
C10 N5 C11 Ni2 0.3(5) . . . . ?
C13 N6 C11 N5 -0.7(4) . . . . ?
C14 N6 C11 N5 -173.7(3) . . . . ?
C13 N6 C11 Ni2 175.8(3) . . . . ?
C14 N6 C11 Ni2 2.8(5) . . . . ?
C6 Ni2 C11 N5 -52.1(4) . . . . ?
N7 Ni2 C11 N5 139.5(4) . . . . ?
C6 Ni2 C11 N6 132.3(3) . . . . ?
N7 Ni2 C11 N6 -36.1(3) . . . . ?
C11 N5 C12 C13 0.0(4) . . . . ?
C10 N5 C12 C13 -176.0(3) . . . . ?
N5 C12 C13 N6 -0.4(4) . . . . ?
C11 N6 C13 C12 0.7(4) . . . . ?
C14 N6 C13 C12 173.5(3) . . . . ?
C11 N6 C14 C15 42.6(5) . . . . ?
C13 N6 C14 C15 -129.4(4) . . . . ?
N8 N7 C15 C16 0.1(4) . . . . ?
Ni2 N7 C15 C16 178.8(3) . . . . ?
N8 N7 C15 C14 178.7(3) . . . . ?
Ni2 N7 C15 C14 -2.6(5) . . . . ?
N6 C14 C15 N7 -41.5(5) . . . . ?
N6 C14 C15 C16 136.7(4) . . . . ?
N7 C15 C16 C17 -0.3(4) . . . . ?
C14 C15 C16 C17 -178.7(4) . . . . ?
N7 N8 C17 C16 -0.3(4) . . . . ?
Ni1 N8 C17 C16 173.9(3) . . . . ?
N7 N8 C17 C18 179.9(3) . . . . ?
Ni1 N8 C17 C18 -5.9(5) . . . . ?
C15 C16 C17 N8 0.4(4) . . . . ?
C15 C16 C17 C18 -179.9(4) . . . . ?
C19 N9 C18 C17 -43.4(5) . . . . ?
C20 N9 C18 C17 129.5(4) . . . . ?
N8 C17 C18 N9 49.1(5) . . . . ?
C16 C17 C18 N9 -130.6(4) . . . . ?
C21 N10 C19 N9 1.3(4) . . . . ?
C22 N10 C19 N9 -175.9(3) . . . . ?
C21 N10 C19 Ni1 -178.3(3) . . . . ?
C22 N10 C19 Ni1 4.5(5) . . . . ?
C20 N9 C19 N10 -1.0(4) . . . . ?
C18 N9 C19 N10 172.9(3) . . . . ?
C20 N9 C19 Ni1 178.6(3) . . . . ?
C18 N9 C19 Ni1 -7.5(5) . . . . ?
C24 Ni1 C19 N10 51.2(4) . . . . ?
N8 Ni1 C19 N10 -140.6(4) . . . . ?
C24 Ni1 C19 N9 -128.4(3) . . . . ?
N8 Ni1 C19 N9 39.9(3) . . . . ?
C19 N9 C20 C21 0.4(4) . . . . ?
C18 N9 C20 C21 -173.1(3) . . . . ?
N9 C20 C21 N10 0.4(4) . . . . ?
C19 N10 C21 C20 -1.1(4) . . . . ?
C22 N10 C21 C20 175.9(3) . . . . ?
C19 N10 C22 C23 -83.7(4) . . . . ?
C21 N10 C22 C23 99.6(4) . . . . ?
C24 N11 C23 C22 6.4(6) . . . . ?
C25 N11 C23 C22 -175.0(3) . . . . ?
N10 C22 C23 N11 58.5(4) . . . . ?
C26 N12 C24 N11 0.7(4) . . . . ?
C1 N12 C24 N11 175.8(3) . . . . ?
C26 N12 C24 Ni1 -173.5(3) . . . . ?
C1 N12 C24 Ni1 1.5(5) . . . . ?
C25 N11 C24 N12 -0.7(4) . . . . ?
C23 N11 C24 N12 178.0(4) . . . . ?
C25 N11 C24 Ni1 171.9(3) . . . . ?
C23 N11 C24 Ni1 -9.3(7) . . . . ?
C24 N11 C25 C26 0.5(5) . . . . ?
C23 N11 C25 C26 -178.4(3) . . . . ?
N11 C25 C26 N12 -0.1(4) . . . . ?
C24 N12 C26 C25 -0.4(5) . . . . ?
C1 N12 C26 C25 -175.6(4) . . . . ?
C28 N13 C29 O1 -3.2(8) . . . . ?
C27 N13 C29 O1 -178.6(4) . . . . ?
C31 N14 C30 O2 -148(3) . . . . ?
C32 N14 C30 O2 41(5) . . . . ?
C31A N14A C30A O2A 141(2) . . . . ?
C32A N14A C30A O2A -36(3) . . . . ?


_shelxl_version_number           2014/6



#===END
