# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

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

data_compound_4-OTf
_database_code_depnum_ccdc_archive 'CCDC 1057574'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

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

# 5. CHEMICAL DATA

_chemical_formula_moiety         'C24 H28 N12, 4(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C30 H31 F12 N13 O12 S4'
_chemical_formula_weight         1121.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 ' 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_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_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                   21.1486(12)
_cell_length_b                   12.7425(7)
_cell_length_c                   18.4902(10)
_cell_angle_alpha                90
_cell_angle_beta                 114.813(2)
_cell_angle_gamma                90
_cell_volume                     4522.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123
_cell_measurement_reflns_used    9975
_cell_measurement_theta_min      2.5237
_cell_measurement_theta_max      26.3854

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.214
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             2280
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.5132
_exptl_absorpt_correction_T_max  0.7454

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             A. Poethig
scanspeed                           10 s per frame
dx                                  35 mm
3974 frames measured in 8 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            56097
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             8270
# number of observed reflections (> n sig(I))
_reflns_number_gt                7024
_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, 2014)'

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

# 8. REFINEMENT DATA

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.0563P)²+6.3127P] 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         8270
_refine_ls_number_parameters     787
_refine_ls_number_restraints     266
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1300
_refine_ls_wR_factor_gt          0.1226
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.066

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

# 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
S1 S 0.59283(3) 0.09849(5) 0.44139(4) 0.02444(16) Uani 1 1 d . . . . .
F1 F 0.71444(10) 0.1588(2) 0.45896(17) 0.0885(9) Uani 1 1 d . . . . .
F2 F 0.71445(12) 0.0567(2) 0.55242(15) 0.0933(9) Uani 1 1 d . . . . .
F3 F 0.68336(16) 0.2179(3) 0.54803(17) 0.1161(11) Uani 1 1 d . . . . .
O1 O 0.56507(10) 0.19131(15) 0.39353(12) 0.0375(5) Uani 1 1 d . . . . .
O2 O 0.60045(12) 0.01076(15) 0.39752(13) 0.0419(5) Uani 1 1 d . . . . .
O3 O 0.56334(12) 0.07470(17) 0.49643(15) 0.0506(6) Uani 1 1 d . . . . .
C27 C 0.68116(17) 0.1359(3) 0.5042(2) 0.0564(9) Uani 1 1 d . . . . .
N1 N 0.04576(11) 0.70264(17) -0.09905(13) 0.0289(5) Uani 1 1 d . . . . .
N2 N 0.09909(12) 0.69725(16) 0.02802(13) 0.0308(5) Uani 1 1 d . . . . .
N3 N 0.05238(16) 0.8059(2) 0.15468(16) 0.0542(8) Uani 1 1 d . . . . .
H3 H 0.0117 0.7764 0.1269 0.065 Uiso 1 1 calc R U . . .
N4 N 0.06085(14) 0.8924(3) 0.19897(17) 0.0543(8) Uani 1 1 d . . . . .
N5 N 0.13043(11) 1.10475(17) 0.24532(13) 0.0267(5) Uani 1 1 d . . . . .
N6 N 0.06489(12) 1.23971(17) 0.19979(13) 0.0306(5) Uani 1 1 d . . . . .
C1 C -0.00764(17) 0.6855(3) -0.17957(17) 0.0474(9) Uani 1 1 d . . . . .
H1A H -0.0260 0.6132 -0.1838 0.057 Uiso 1 1 calc R U . . .
H1B H 0.0134 0.6926 -0.2181 0.057 Uiso 1 1 calc R U . . .
C2 C 0.04264(14) 0.66822(19) -0.03339(16) 0.0286(6) Uani 1 1 d . . . . .
H2 H 0.0055 0.6287 -0.0310 0.034 Uiso 1 1 calc R U . . .
C3 C 0.10769(16) 0.7552(2) -0.0785(2) 0.0419(8) Uani 1 1 d . . . . .
H3A H 0.1239 0.7877 -0.1138 0.050 Uiso 1 1 calc R U . . .
C4 C 0.14068(15) 0.7517(2) 0.0013(2) 0.0423(8) Uani 1 1 d . . . . .
H4 H 0.1848 0.7815 0.0333 0.051 Uiso 1 1 calc R U . . .
C5 C 0.1147(2) 0.6731(2) 0.11243(18) 0.0549(10) Uani 1 1 d . . . . .
H5A H 0.1615 0.6407 0.1383 0.066 Uiso 1 1 calc R U . . .
H5B H 0.0803 0.6218 0.1143 0.066 Uiso 1 1 calc R U . . .
C6 C 0.11270(18) 0.7693(2) 0.15739(16) 0.0396(7) Uani 1 1 d . . . . .
C7 C 0.16360(16) 0.8370(2) 0.20530(17) 0.0387(7) Uani 1 1 d . . . . .
H7 H 0.2121 0.8333 0.2189 0.046 Uiso 1 1 calc R U . . .
C8 C 0.12925(14) 0.9115(2) 0.22937(15) 0.0280(6) Uani 1 1 d . . . . .
C9 C 0.15815(14) 1.0027(2) 0.28398(16) 0.0318(6) Uani 1 1 d . . . . .
H9A H 0.1471 0.9942 0.3306 0.038 Uiso 1 1 calc R U . . .
H9B H 0.2095 1.0029 0.3036 0.038 Uiso 1 1 calc R U . . .
C10 C 0.07067(14) 1.1476(2) 0.23663(15) 0.0300(6) Uani 1 1 d . . . . .
H10 H 0.0378 1.1183 0.2535 0.036 Uiso 1 1 calc R U . . .
C11 C 0.16318(14) 1.1702(2) 0.21291(17) 0.0323(6) Uani 1 1 d . . . . .
H11 H 0.2068 1.1581 0.2111 0.039 Uiso 1 1 calc R U . . .
C12 C 0.12216(15) 1.2546(2) 0.18425(18) 0.0353(6) Uani 1 1 d . . . . .
H12 H 0.1311 1.3133 0.1582 0.042 Uiso 1 1 calc R U . . .
S2 S 0.14728(3) 0.53958(5) 0.30116(4) 0.02910(17) Uani 1 1 d . . . . .
F4 F 0.10909(10) 0.36472(13) 0.34680(10) 0.0479(5) Uani 1 1 d . . . . .
F5 F 0.21639(10) 0.40575(16) 0.41455(11) 0.0526(5) Uani 1 1 d . . . . .
F6 F 0.13621(10) 0.48903(14) 0.43271(10) 0.0482(5) Uani 1 1 d . . . . .
O4 O 0.19665(11) 0.61876(16) 0.34583(14) 0.0449(5) Uani 1 1 d . . . . .
O5 O 0.16732(12) 0.47987(17) 0.24825(12) 0.0443(5) Uani 1 1 d . . . . .
O6 O 0.07620(11) 0.57324(18) 0.26865(13) 0.0471(6) Uani 1 1 d . . . . .
C28 C 0.15249(15) 0.4454(2) 0.37782(16) 0.0330(6) Uani 1 1 d . . . . .
S3_a S 0.33849(9) 0.45558(14) 0.72525(9) 0.0243(4) Uani 0.827(6) 1 d D U P A 1
F7_a F 0.29906(16) 0.4779(2) 0.57252(13) 0.0464(7) Uani 0.827(6) 1 d D U P A 1
F8_a F 0.22014(12) 0.5164(2) 0.61233(14) 0.0485(7) Uani 0.827(6) 1 d D U P A 1
F9_a F 0.30480(19) 0.62319(18) 0.63433(17) 0.0538(8) Uani 0.827(6) 1 d D U P A
1
O7_a O 0.3183(2) 0.5098(3) 0.78069(19) 0.0404(9) Uani 0.827(6) 1 d D U P A 1
O8_a O 0.40958(15) 0.4701(4) 0.7374(2) 0.0377(9) Uani 0.827(6) 1 d D U P A 1
O9_a O 0.3134(2) 0.3496(2) 0.7081(2) 0.0330(7) Uani 0.827(6) 1 d D U P A 1
C29_a C 0.2888(2) 0.5216(3) 0.63185(19) 0.0325(7) Uani 0.827(6) 1 d D U P A 1
S3A_b S 0.3453(5) 0.4562(7) 0.7182(5) 0.057(4) Uani 0.173(6) 1 d D U P A 2
F7A_b F 0.3413(8) 0.4918(8) 0.5777(5) 0.067(4) Uani 0.173(6) 1 d D U P A 2
F8A_b F 0.2514(6) 0.5470(9) 0.5919(6) 0.071(5) Uani 0.173(6) 1 d D U P A 2
F9A_b F 0.3478(8) 0.6319(6) 0.6453(6) 0.067(5) Uani 0.173(6) 1 d D U P A 2
O7A_b O 0.3217(10) 0.5175(13) 0.7676(7) 0.064(6) Uani 0.173(6) 1 d D U P A 2
O8A_b O 0.4195(5) 0.4458(15) 0.7470(8) 0.051(5) Uani 0.173(6) 1 d D U P A 2
O9A_b O 0.3066(10) 0.3613(9) 0.6875(9) 0.055(6) Uani 0.173(6) 1 d D U P A 2
C29A_b C 0.3209(6) 0.5355(6) 0.6294(5) 0.060(4) Uani 0.173(6) 1 d D U P A 2
S4_c S 0.09717(11) 0.1011(2) 0.47146(18) 0.0232(7) Uani 0.517(8) 1 d D U P B 3
F10_c F 0.2129(2) 0.1892(6) 0.5685(3) 0.073(2) Uani 0.517(8) 1 d D U P B 3
F11_c F 0.2234(2) 0.0321(5) 0.5368(3) 0.0681(16) Uani 0.517(8) 1 d D U P B 3
F12_c F 0.2076(2) 0.1565(5) 0.4525(3) 0.0509(18) Uani 0.517(8) 1 d D U P B 3
O10_c O 0.0879(3) 0.0561(5) 0.5378(2) 0.0316(19) Uani 0.517(8) 1 d D U P B 3
O11_c O 0.0698(3) 0.2057(4) 0.4514(5) 0.0556(18) Uani 0.517(8) 1 d D U P B 3
O12_c O 0.0816(3) 0.0331(5) 0.4053(3) 0.0434(14) Uani 0.517(8) 1 d D U P B 3
C30_c C 0.1897(2) 0.1220(6) 0.5094(3) 0.0382(12) Uani 0.517(8) 1 d D U P B 3
S4A_d S 0.10374(16) 0.0896(2) 0.4662(2) 0.0325(9) Uani 0.483(8) 1 d D U P B 4
F10A_d F 0.1840(3) 0.2485(5) 0.5344(4) 0.0689(18) Uani 0.483(8) 1 d D U P B 4
F11A_d F 0.23570(19) 0.1013(7) 0.5546(3) 0.082(3) Uani 0.483(8) 1 d D U P B 4
F12A_d F 0.2036(2) 0.1772(5) 0.4409(3) 0.0433(17) Uani 0.483(8) 1 d D U P B 4
O10A_d O 0.0955(3) 0.0668(6) 0.5381(3) 0.039(2) Uani 0.483(8) 1 d D U P B 4
O11A_d O 0.0552(2) 0.1660(6) 0.4157(4) 0.0552(18) Uani 0.483(8) 1 d D U P B 4
O12A_d O 0.1135(4) 0.0006(4) 0.4256(5) 0.067(2) Uani 0.483(8) 1 d D U P B 4
C30A_d C 0.1854(2) 0.1587(5) 0.5006(3) 0.0393(13) Uani 0.483(8) 1 d D U P B 4
N7 N 0.46975(10) 0.20913(15) 0.63572(12) 0.0221(4) Uani 1 1 d . . . . .
N8 N 0.40280(11) 0.19874(16) 0.51065(13) 0.0249(5) Uani 1 1 d . . . . .
N9 N 0.43309(11) 0.27756(17) 0.35814(13) 0.0299(5) Uani 1 1 d . . . . .
H9 H 0.4716 0.2401 0.3786 0.036 Uiso 1 1 calc R U . . .
N10 N 0.42346(11) 0.35725(18) 0.30661(13) 0.0307(5) Uani 1 1 d . . . . .
N11 N 0.35502(11) 0.58357(17) 0.26033(13) 0.0283(5) Uani 1 1 d . . . . .
N12 N 0.41576(11) 0.72537(16) 0.28295(13) 0.0272(5) Uani 1 1 d . . . . .
C13 C 0.53039(13) 0.1991(2) 0.71153(16) 0.0288(6) Uani 1 1 d . . . . .
H13A H 0.5493 0.1270 0.7169 0.035 Uiso 1 1 calc R U . . .
H13B H 0.5164 0.2112 0.7557 0.035 Uiso 1 1 calc R U . . .
C14 C 0.46382(13) 0.17003(18) 0.56630(15) 0.0236(5) Uani 1 1 d . . . . .
H14 H 0.4977 0.1286 0.5582 0.028 Uiso 1 1 calc R U . . .
C15 C 0.41012(13) 0.2638(2) 0.62364(17) 0.0294(6) Uani 1 1 d . . . . .
H15 H 0.4003 0.2992 0.6630 0.035 Uiso 1 1 calc R U . . .
C16 C 0.36844(13) 0.2574(2) 0.54570(17) 0.0301(6) Uani 1 1 d . . . . .
H16 H 0.3235 0.2878 0.5194 0.036 Uiso 1 1 calc R U . . .
C17 C 0.37588(16) 0.1710(2) 0.42564(16) 0.0355(6) Uani 1 1 d . . . . .
H17A H 0.3273 0.1460 0.4071 0.043 Uiso 1 1 calc R U . . .
H17B H 0.4040 0.1127 0.4191 0.043 Uiso 1 1 calc R U . . .
C18 C 0.37768(14) 0.2611(2) 0.37508(15) 0.0280(6) Uani 1 1 d . . . . .
C19 C 0.32871(14) 0.3354(2) 0.33287(16) 0.0285(6) Uani 1 1 d . . . . .
H19 H 0.2839 0.3457 0.3320 0.034 Uiso 1 1 calc R U . . .
C20 C 0.35958(13) 0.3924(2) 0.29153(15) 0.0261(5) Uani 1 1 d . . . . .
C21 C 0.32809(14) 0.4768(2) 0.23112(17) 0.0326(6) Uani 1 1 d . . . . .
H21A H 0.3371 0.4609 0.1839 0.039 Uiso 1 1 calc R U . . .
H21B H 0.2770 0.4764 0.2139 0.039 Uiso 1 1 calc R U . . .
C22 C 0.41047(13) 0.6271(2) 0.25662(15) 0.0275(6) Uani 1 1 d . . . . .
H22 H 0.4412 0.5938 0.2383 0.033 Uiso 1 1 calc R U . . .
C23 C 0.32455(14) 0.6554(2) 0.29124(18) 0.0362(7) Uani 1 1 d . . . . .
H23 H 0.2843 0.6444 0.3009 0.043 Uiso 1 1 calc R U . . .
C24 C 0.36222(14) 0.7439(2) 0.30515(19) 0.0367(7) Uani 1 1 d . . . . .
H24 H 0.3536 0.8074 0.3263 0.044 Uiso 1 1 calc R U . . .
N13 N 0.48176(16) 0.6235(2) 0.45032(18) 0.0548(8) Uani 1 1 d . . . . .
C25 C 0.4457(2) 0.5954(3) 0.4783(2) 0.0538(9) Uani 1 1 d . . . . .
C26 C 0.4006(3) 0.5588(3) 0.5146(3) 0.0780(13) Uani 1 1 d . . . . .
H26A H 0.4085 0.4837 0.5264 0.117 Uiso 1 1 calc R U . . .
H26B H 0.3519 0.5705 0.4778 0.117 Uiso 1 1 calc R U . . .
H26C H 0.4112 0.5976 0.5642 0.117 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
S1 O2 1.429(2) . ?
S1 O3 1.432(2) . ?
S1 O1 1.4459(19) . ?
S1 C27 1.801(3) . ?
F1 C27 1.332(4) . ?
F2 C27 1.335(4) . ?
F3 C27 1.312(5) . ?
N1 C2 1.318(3) . ?
N1 C3 1.375(4) . ?
N1 C1 1.459(4) . ?
N2 C2 1.309(3) . ?
N2 C4 1.365(4) . ?
N2 C5 1.486(4) . ?
N3 N4 1.339(4) . ?
N3 C6 1.340(4) . ?
N3 H3 0.8800 . ?
N4 C8 1.336(4) . ?
N5 C10 1.323(3) . ?
N5 C11 1.373(3) . ?
N5 C9 1.482(3) . ?
N6 C10 1.336(4) . ?
N6 C12 1.370(4) . ?
N6 C1 1.461(3) 3_575 ?
C1 N6 1.461(3) 3_575 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2 0.9500 . ?
C3 C4 1.343(5) . ?
C3 H3A 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.491(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.374(4) . ?
C7 C8 1.378(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.491(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10 0.9500 . ?
C11 C12 1.343(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
S2 O6 1.431(2) . ?
S2 O5 1.437(2) . ?
S2 O4 1.438(2) . ?
S2 C28 1.825(3) . ?
F4 C28 1.337(3) . ?
F5 C28 1.331(3) . ?
F6 C28 1.323(3) . ?
S3_a O8_a 1.435(2) . ?
S3_a O9_a 1.436(2) . ?
S3_a O7_a 1.441(2) . ?
S3_a C29_a 1.808(3) . ?
F7_a C29_a 1.326(4) . ?
F8_a C29_a 1.344(4) . ?
F9_a C29_a 1.334(4) . ?
S3A_b O8A_b 1.435(3) . ?
S3A_b O9A_b 1.437(2) . ?
S3A_b O7A_b 1.441(3) . ?
S3A_b C29A_b 1.808(4) . ?
F7A_b C29A_b 1.326(4) . ?
F8A_b C29A_b 1.344(4) . ?
F9A_b C29A_b 1.334(4) . ?
S4_c O12_c 1.421(3) . ?
S4_c O11_c 1.439(3) . ?
S4_c O10_c 1.441(3) . ?
S4_c C30_c 1.799(4) . ?
F10_c C30_c 1.311(5) . ?
F11_c C30_c 1.331(6) . ?
F12_c C30_c 1.334(4) . ?
S4A_d O12A_d 1.421(3) . ?
S4A_d O11A_d 1.438(3) . ?
S4A_d O10A_d 1.440(3) . ?
S4A_d C30A_d 1.800(4) . ?
F10A_d C30A_d 1.311(5) . ?
F11A_d C30A_d 1.331(6) . ?
F12A_d C30A_d 1.334(4) . ?
N7 C14 1.333(3) . ?
N7 C15 1.374(3) . ?
N7 C13 1.455(3) . ?
N8 C14 1.320(3) . ?
N8 C16 1.379(3) . ?
N8 C17 1.473(3) . ?
N9 N10 1.348(3) . ?
N9 C18 1.350(3) . ?
N9 H9 0.8800 . ?
N10 C20 1.337(3) . ?
N11 C22 1.325(3) . ?
N11 C23 1.374(4) . ?
N11 C21 1.486(3) . ?
N12 C22 1.331(3) . ?
N12 C24 1.377(3) . ?
N12 C13 1.462(3) 3_666 ?
C13 N12 1.462(3) 3_666 ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14 0.9500 . ?
C15 C16 1.339(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.491(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.379(4) . ?
C19 C20 1.399(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.492(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22 0.9500 . ?
C23 C24 1.342(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
N13 C25 1.145(4) . ?
C25 C26 1.453(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 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
O2 S1 O3 115.11(13) . . ?
O2 S1 O1 113.95(12) . . ?
O3 S1 O1 114.97(12) . . ?
O2 S1 C27 103.83(17) . . ?
O3 S1 C27 103.96(17) . . ?
O1 S1 C27 102.89(15) . . ?
F3 C27 F1 108.8(3) . . ?
F3 C27 F2 108.5(3) . . ?
F1 C27 F2 108.4(3) . . ?
F3 C27 S1 111.5(3) . . ?
F1 C27 S1 109.4(3) . . ?
F2 C27 S1 110.2(3) . . ?
C2 N1 C3 108.5(2) . . ?
C2 N1 C1 125.0(3) . . ?
C3 N1 C1 126.5(3) . . ?
C2 N2 C4 108.7(2) . . ?
C2 N2 C5 124.9(3) . . ?
C4 N2 C5 126.3(3) . . ?
N4 N3 C6 112.5(3) . . ?
N4 N3 H3 123.7 . . ?
C6 N3 H3 123.7 . . ?
C8 N4 N3 104.5(3) . . ?
C10 N5 C11 109.1(2) . . ?
C10 N5 C9 125.8(2) . . ?
C11 N5 C9 125.1(2) . . ?
C10 N6 C12 109.2(2) . . ?
C10 N6 C1 126.3(3) . 3_575 ?
C12 N6 C1 124.5(3) . 3_575 ?
N1 C1 N6 111.5(2) . 3_575 ?
N1 C1 H1A 109.3 . . ?
N6 C1 H1A 109.3 3_575 . ?
N1 C1 H1B 109.3 . . ?
N6 C1 H1B 109.3 3_575 . ?
H1A C1 H1B 108.0 . . ?
N2 C2 N1 109.0(2) . . ?
N2 C2 H2 125.5 . . ?
N1 C2 H2 125.5 . . ?
C4 C3 N1 106.4(3) . . ?
C4 C3 H3A 126.8 . . ?
N1 C3 H3A 126.8 . . ?
C3 C4 N2 107.4(3) . . ?
C3 C4 H4 126.3 . . ?
N2 C4 H4 126.3 . . ?
N2 C5 C6 111.7(2) . . ?
N2 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
N2 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
N3 C6 C7 106.3(3) . . ?
N3 C6 C5 121.0(3) . . ?
C7 C6 C5 132.7(3) . . ?
C6 C7 C8 105.4(3) . . ?
C6 C7 H7 127.3 . . ?
C8 C7 H7 127.3 . . ?
N4 C8 C7 111.3(3) . . ?
N4 C8 C9 119.4(2) . . ?
C7 C8 C9 129.3(3) . . ?
N5 C9 C8 113.0(2) . . ?
N5 C9 H9A 109.0 . . ?
C8 C9 H9A 109.0 . . ?
N5 C9 H9B 109.0 . . ?
C8 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
N5 C10 N6 107.6(2) . . ?
N5 C10 H10 126.2 . . ?
N6 C10 H10 126.2 . . ?
C12 C11 N5 107.3(2) . . ?
C12 C11 H11 126.3 . . ?
N5 C11 H11 126.3 . . ?
C11 C12 N6 106.7(2) . . ?
C11 C12 H12 126.6 . . ?
N6 C12 H12 126.6 . . ?
O6 S2 O5 115.53(14) . . ?
O6 S2 O4 114.38(14) . . ?
O5 S2 O4 114.34(13) . . ?
O6 S2 C28 103.53(13) . . ?
O5 S2 C28 103.99(13) . . ?
O4 S2 C28 102.86(13) . . ?
F6 C28 F5 107.7(2) . . ?
F6 C28 F4 107.4(2) . . ?
F5 C28 F4 107.1(2) . . ?
F6 C28 S2 111.67(19) . . ?
F5 C28 S2 111.3(2) . . ?
F4 C28 S2 111.45(18) . . ?
O8_a S3_a O9_a 114.91(16) . . ?
O8_a S3_a O7_a 115.43(16) . . ?
O9_a S3_a O7_a 114.55(17) . . ?
O8_a S3_a C29_a 103.9(2) . . ?
O9_a S3_a C29_a 102.33(19) . . ?
O7_a S3_a C29_a 103.29(16) . . ?
F7_a C29_a F9_a 108.0(3) . . ?
F7_a C29_a F8_a 106.9(3) . . ?
F9_a C29_a F8_a 106.6(3) . . ?
F7_a C29_a S3_a 111.4(2) . . ?
F9_a C29_a S3_a 112.4(2) . . ?
F8_a C29_a S3_a 111.3(2) . . ?
O8A_b S3A_b O9A_b 114.9(2) . . ?
O8A_b S3A_b O7A_b 115.5(2) . . ?
O9A_b S3A_b O7A_b 114.5(2) . . ?
O8A_b S3A_b C29A_b 103.9(2) . . ?
O9A_b S3A_b C29A_b 102.3(2) . . ?
O7A_b S3A_b C29A_b 103.3(2) . . ?
F7A_b C29A_b F9A_b 108.0(3) . . ?
F7A_b C29A_b F8A_b 106.9(3) . . ?
F9A_b C29A_b F8A_b 106.6(3) . . ?
F7A_b C29A_b S3A_b 111.4(3) . . ?
F9A_b C29A_b S3A_b 112.4(3) . . ?
F8A_b C29A_b S3A_b 111.3(3) . . ?
O12_c S4_c O11_c 114.9(3) . . ?
O12_c S4_c O10_c 115.2(2) . . ?
O11_c S4_c O10_c 113.9(2) . . ?
O12_c S4_c C30_c 104.3(2) . . ?
O11_c S4_c C30_c 102.6(3) . . ?
O10_c S4_c C30_c 104.0(2) . . ?
F10_c C30_c F11_c 106.9(4) . . ?
F10_c C30_c F12_c 108.1(4) . . ?
F11_c C30_c F12_c 107.4(3) . . ?
F10_c C30_c S4_c 112.8(3) . . ?
F11_c C30_c S4_c 110.0(4) . . ?
F12_c C30_c S4_c 111.3(3) . . ?
O12A_d S4A_d O11A_d 114.8(3) . . ?
O12A_d S4A_d O10A_d 115.2(2) . . ?
O11A_d S4A_d O10A_d 113.9(2) . . ?
O12A_d S4A_d C30A_d 104.3(2) . . ?
O11A_d S4A_d C30A_d 102.5(3) . . ?
O10A_d S4A_d C30A_d 104.0(2) . . ?
F10A_d C30A_d F11A_d 107.1(4) . . ?
F10A_d C30A_d F12A_d 108.2(4) . . ?
F11A_d C30A_d F12A_d 107.4(3) . . ?
F10A_d C30A_d S4A_d 112.7(3) . . ?
F11A_d C30A_d S4A_d 110.1(4) . . ?
F12A_d C30A_d S4A_d 111.2(3) . . ?
C14 N7 C15 108.9(2) . . ?
C14 N7 C13 125.7(2) . . ?
C15 N7 C13 125.4(2) . . ?
C14 N8 C16 108.6(2) . . ?
C14 N8 C17 125.4(2) . . ?
C16 N8 C17 126.0(2) . . ?
N10 N9 C18 113.1(2) . . ?
N10 N9 H9 123.4 . . ?
C18 N9 H9 123.4 . . ?
C20 N10 N9 103.8(2) . . ?
C22 N11 C23 108.8(2) . . ?
C22 N11 C21 125.2(2) . . ?
C23 N11 C21 125.8(2) . . ?
C22 N12 C24 108.5(2) . . ?
C22 N12 C13 126.0(2) . 3_666 ?
C24 N12 C13 125.5(2) . 3_666 ?
N7 C13 N12 110.8(2) . 3_666 ?
N7 C13 H13A 109.5 . . ?
N12 C13 H13A 109.5 3_666 . ?
N7 C13 H13B 109.5 . . ?
N12 C13 H13B 109.5 3_666 . ?
H13A C13 H13B 108.1 . . ?
N8 C14 N7 108.2(2) . . ?
N8 C14 H14 125.9 . . ?
N7 C14 H14 125.9 . . ?
C16 C15 N7 106.8(2) . . ?
C16 C15 H15 126.6 . . ?
N7 C15 H15 126.6 . . ?
C15 C16 N8 107.4(2) . . ?
C15 C16 H16 126.3 . . ?
N8 C16 H16 126.3 . . ?
N8 C17 C18 112.6(2) . . ?
N8 C17 H17A 109.1 . . ?
C18 C17 H17A 109.1 . . ?
N8 C17 H17B 109.1 . . ?
C18 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
N9 C18 C19 106.3(2) . . ?
N9 C18 C17 121.2(2) . . ?
C19 C18 C17 132.3(3) . . ?
C18 C19 C20 104.7(2) . . ?
C18 C19 H19 127.6 . . ?
C20 C19 H19 127.6 . . ?
N10 C20 C19 112.0(2) . . ?
N10 C20 C21 119.5(2) . . ?
C19 C20 C21 128.3(2) . . ?
N11 C21 C20 113.9(2) . . ?
N11 C21 H21A 108.8 . . ?
C20 C21 H21A 108.8 . . ?
N11 C21 H21B 108.8 . . ?
C20 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
N11 C22 N12 108.4(2) . . ?
N11 C22 H22 125.8 . . ?
N12 C22 H22 125.8 . . ?
C24 C23 N11 107.2(2) . . ?
C24 C23 H23 126.4 . . ?
N11 C23 H23 126.4 . . ?
C23 C24 N12 107.2(3) . . ?
C23 C24 H24 126.4 . . ?
N12 C24 H24 126.4 . . ?
N13 C25 C26 179.2(5) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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
O2 S1 C27 F3 178.9(3) . . . . ?
O3 S1 C27 F3 -60.4(3) . . . . ?
O1 S1 C27 F3 59.9(3) . . . . ?
O2 S1 C27 F1 58.5(3) . . . . ?
O3 S1 C27 F1 179.2(3) . . . . ?
O1 S1 C27 F1 -60.5(3) . . . . ?
O2 S1 C27 F2 -60.6(3) . . . . ?
O3 S1 C27 F2 60.2(3) . . . . ?
O1 S1 C27 F2 -179.6(3) . . . . ?
C6 N3 N4 C8 1.2(4) . . . . ?
C2 N1 C1 N6 81.4(4) . . . 3_575 ?
C3 N1 C1 N6 -99.7(3) . . . 3_575 ?
C4 N2 C2 N1 -0.6(3) . . . . ?
C5 N2 C2 N1 -179.9(2) . . . . ?
C3 N1 C2 N2 0.7(3) . . . . ?
C1 N1 C2 N2 179.8(2) . . . . ?
C2 N1 C3 C4 -0.6(3) . . . . ?
C1 N1 C3 C4 -179.7(2) . . . . ?
N1 C3 C4 N2 0.2(3) . . . . ?
C2 N2 C4 C3 0.2(3) . . . . ?
C5 N2 C4 C3 179.6(3) . . . . ?
C2 N2 C5 C6 -111.2(3) . . . . ?
C4 N2 C5 C6 69.6(4) . . . . ?
N4 N3 C6 C7 -1.1(4) . . . . ?
N4 N3 C6 C5 179.7(3) . . . . ?
N2 C5 C6 N3 83.5(4) . . . . ?
N2 C5 C6 C7 -95.5(4) . . . . ?
N3 C6 C7 C8 0.5(3) . . . . ?
C5 C6 C7 C8 179.6(3) . . . . ?
N3 N4 C8 C7 -0.8(3) . . . . ?
N3 N4 C8 C9 -178.8(2) . . . . ?
C6 C7 C8 N4 0.2(3) . . . . ?
C6 C7 C8 C9 178.0(3) . . . . ?
C10 N5 C9 C8 83.2(3) . . . . ?
C11 N5 C9 C8 -97.0(3) . . . . ?
N4 C8 C9 N5 -62.3(3) . . . . ?
C7 C8 C9 N5 120.1(3) . . . . ?
C11 N5 C10 N6 -0.5(3) . . . . ?
C9 N5 C10 N6 179.3(2) . . . . ?
C12 N6 C10 N5 0.6(3) . . . . ?
C1 N6 C10 N5 -178.7(2) 3_575 . . . ?
C10 N5 C11 C12 0.2(3) . . . . ?
C9 N5 C11 C12 -179.6(2) . . . . ?
N5 C11 C12 N6 0.2(3) . . . . ?
C10 N6 C12 C11 -0.5(3) . . . . ?
C1 N6 C12 C11 178.8(2) 3_575 . . . ?
O6 S2 C28 F6 -59.7(2) . . . . ?
O5 S2 C28 F6 179.2(2) . . . . ?
O4 S2 C28 F6 59.7(2) . . . . ?
O6 S2 C28 F5 179.9(2) . . . . ?
O5 S2 C28 F5 58.8(2) . . . . ?
O4 S2 C28 F5 -60.7(2) . . . . ?
O6 S2 C28 F4 60.4(2) . . . . ?
O5 S2 C28 F4 -60.7(2) . . . . ?
O4 S2 C28 F4 179.81(19) . . . . ?
O8_a S3_a C29_a F7_a 61.8(3) . . . . ?
O9_a S3_a C29_a F7_a -58.1(3) . . . . ?
O7_a S3_a C29_a F7_a -177.3(3) . . . . ?
O8_a S3_a C29_a F9_a -59.5(3) . . . . ?
O9_a S3_a C29_a F9_a -179.4(3) . . . . ?
O7_a S3_a C29_a F9_a 61.3(3) . . . . ?
O8_a S3_a C29_a F8_a -179.1(3) . . . . ?
O9_a S3_a C29_a F8_a 61.1(3) . . . . ?
O7_a S3_a C29_a F8_a -58.2(3) . . . . ?
O8A_b S3A_b C29A_b F7A_b 56.8(9) . . . . ?
O9A_b S3A_b C29A_b F7A_b -63.0(9) . . . . ?
O7A_b S3A_b C29A_b F7A_b 177.7(9) . . . . ?
O8A_b S3A_b C29A_b F9A_b -64.5(9) . . . . ?
O9A_b S3A_b C29A_b F9A_b 175.7(9) . . . . ?
O7A_b S3A_b C29A_b F9A_b 56.4(9) . . . . ?
O8A_b S3A_b C29A_b F8A_b 176.0(9) . . . . ?
O9A_b S3A_b C29A_b F8A_b 56.1(9) . . . . ?
O7A_b S3A_b C29A_b F8A_b -63.1(9) . . . . ?
O12_c S4_c C30_c F10_c 176.0(5) . . . . ?
O11_c S4_c C30_c F10_c 55.9(5) . . . . ?
O10_c S4_c C30_c F10_c -63.0(5) . . . . ?
O12_c S4_c C30_c F11_c -64.8(4) . . . . ?
O11_c S4_c C30_c F11_c 175.1(4) . . . . ?
O10_c S4_c C30_c F11_c 56.3(4) . . . . ?
O12_c S4_c C30_c F12_c 54.2(5) . . . . ?
O11_c S4_c C30_c F12_c -65.9(5) . . . . ?
O10_c S4_c C30_c F12_c 175.2(4) . . . . ?
O12A_d S4A_d C30A_d F10A_d 174.9(5) . . . . ?
O11A_d S4A_d C30A_d F10A_d 54.9(5) . . . . ?
O10A_d S4A_d C30A_d F10A_d -64.0(5) . . . . ?
O12A_d S4A_d C30A_d F11A_d -65.7(5) . . . . ?
O11A_d S4A_d C30A_d F11A_d 174.3(4) . . . . ?
O10A_d S4A_d C30A_d F11A_d 55.4(4) . . . . ?
O12A_d S4A_d C30A_d F12A_d 53.2(5) . . . . ?
O11A_d S4A_d C30A_d F12A_d -66.8(5) . . . . ?
O10A_d S4A_d C30A_d F12A_d 174.4(4) . . . . ?
C18 N9 N10 C20 0.6(3) . . . . ?
C14 N7 C13 N12 79.5(3) . . . 3_666 ?
C15 N7 C13 N12 -98.1(3) . . . 3_666 ?
C16 N8 C14 N7 -0.4(3) . . . . ?
C17 N8 C14 N7 -179.6(2) . . . . ?
C15 N7 C14 N8 0.5(3) . . . . ?
C13 N7 C14 N8 -177.4(2) . . . . ?
C14 N7 C15 C16 -0.4(3) . . . . ?
C13 N7 C15 C16 177.5(2) . . . . ?
N7 C15 C16 N8 0.1(3) . . . . ?
C14 N8 C16 C15 0.2(3) . . . . ?
C17 N8 C16 C15 179.3(2) . . . . ?
C14 N8 C17 C18 -105.9(3) . . . . ?
C16 N8 C17 C18 75.1(3) . . . . ?
N10 N9 C18 C19 -0.8(3) . . . . ?
N10 N9 C18 C17 174.9(2) . . . . ?
N8 C17 C18 N9 91.9(3) . . . . ?
N8 C17 C18 C19 -93.6(3) . . . . ?
N9 C18 C19 C20 0.6(3) . . . . ?
C17 C18 C19 C20 -174.4(3) . . . . ?
N9 N10 C20 C19 -0.2(3) . . . . ?
N9 N10 C20 C21 -175.4(2) . . . . ?
C18 C19 C20 N10 -0.3(3) . . . . ?
C18 C19 C20 C21 174.4(3) . . . . ?
C22 N11 C21 C20 88.5(3) . . . . ?
C23 N11 C21 C20 -95.5(3) . . . . ?
N10 C20 C21 N11 -77.7(3) . . . . ?
C19 C20 C21 N11 107.9(3) . . . . ?
C23 N11 C22 N12 -1.1(3) . . . . ?
C21 N11 C22 N12 175.5(2) . . . . ?
C24 N12 C22 N11 0.9(3) . . . . ?
C13 N12 C22 N11 -179.8(2) 3_666 . . . ?
C22 N11 C23 C24 0.8(3) . . . . ?
C21 N11 C23 C24 -175.7(2) . . . . ?
N11 C23 C24 N12 -0.3(3) . . . . ?
C22 N12 C24 C23 -0.4(3) . . . . ?
C13 N12 C24 C23 -179.7(2) 3_666 . . . ?

_shelxl_version_number           2014-1



####################################################################### 
# 
# 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_compound_4-PF6
_database_code_depnum_ccdc_archive 'CCDC 1057575'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

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

# 5. CHEMICAL DATA

_chemical_formula_moiety         'C24 H28 N12, 4(F6 P), 3(C2 H3 N)'
_chemical_formula_sum            'C30 H37 F24 N15 P4'
_chemical_formula_weight         1187.63

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           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_Int_Tables_number      62

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

_cell_length_a                   17.748(2)
_cell_length_b                   14.432(2)
_cell_length_c                   17.585(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4504.2(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    123
_cell_measurement_reflns_used    9980
_cell_measurement_theta_min      2.3164
_cell_measurement_theta_max      24.7997

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.140
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             2392
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_T_max  0.7452

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             A. Poethig
scanspeed                           20 s per frame
dx                                  35 mm
2557 frames measured in 5 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            105935
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             4306
# number of observed reflections (> n sig(I))
_reflns_number_gt                3733
_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, 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)+(0.0609P)²+8.9144P] 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         4306
_refine_ls_number_parameters     418
_refine_ls_number_restraints     148
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1360
_refine_ls_wR_factor_gt          0.1300
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.115
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.069

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

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P3 P Uani 0.14453(6) 0.25000 0.55467(6) 1.000 0.0299(3) d STU . .
P1 P Uani 0.14631(4) 0.55362(5) 0.33133(4) 1.000 0.0254(2) d . . .
P2_a P Uani 0.41299(15) 0.25000 0.27560(9) 0.746(4) 0.0362(5) . . . .
N1 N Uani 0.09248(11) 0.66650(14) 0.53451(12) 1.000 0.0197(6) d . . .
N2 N Uani 0.15009(12) 0.56308(15) 0.60200(12) 1.000 0.0236(6) d . . .
P2A_b P Uani 0.4542(4) 0.25000 0.2821(2) 0.254(4) 0.0370(7) . . . .
N3 N Uani 0.34819(13) 0.52817(18) 0.61588(13) 1.000 0.0307(7) d . . .
N4 N Uani 0.40198(13) 0.51513(18) 0.56249(13) 1.000 0.0303(7) d . . .
N5 N Uani 0.40258(12) 0.54151(15) 0.37494(12) 1.000 0.0205(6) d . . .
N6 N Uani 0.36733(12) 0.66572(15) 0.31577(12) 1.000 0.0209(6) d . . .
F11 F Uani 0.1363(2) 0.3607(3) 0.5319(3) 0.500 0.0535(11) d UP . .
F12 F Uani 0.1968(2) 0.2883(3) 0.6239(2) 0.500 0.0472(10) d UP . .
F13 F Uani 0.1532(3) 0.3481(3) 0.5818(3) 0.500 0.0758(13) d UP . .
F14 F Uani 0.09056(18) 0.2285(5) 0.48564(19) 0.500 0.055(2) d UP . .
F15 F Uani 0.07313(17) 0.2330(9) 0.60868(19) 0.500 0.055(3) d UP . .
F16 F Uani 0.21612(17) 0.2378(17) 0.50230(19) 0.500 0.050(4) d UP . .
C1 C Uani 0.0823(2) 0.75000 0.4883(2) 1.000 0.0215(10) d STP . .
C2 C Uani 0.15940(15) 0.63788(18) 0.55871(14) 1.000 0.0227(8) d . . .
C3 C Uani 0.03816(15) 0.60776(18) 0.56326(16) 1.000 0.0275(8) d . . .
C4 C Uani 0.07387(16) 0.5429(2) 0.60493(16) 1.000 0.0293(8) d . . .
C5 C Uani 0.21179(16) 0.5150(2) 0.64221(16) 1.000 0.0310(8) d . . .
C6 C Uani 0.27904(15) 0.50613(18) 0.59167(15) 1.000 0.0248(8) d . . .
C7 C Uani 0.28673(15) 0.47789(18) 0.51741(15) 1.000 0.0262(8) d . . .
C8 C Uani 0.36418(15) 0.48488(17) 0.50216(15) 1.000 0.0224(7) d . . .
C9 C Uani 0.40569(15) 0.46323(18) 0.43006(15) 1.000 0.0252(8) d . . .
C10 C Uani 0.35521(14) 0.61258(17) 0.37668(14) 1.000 0.0203(7) d . . .
C11 C Uani 0.44715(15) 0.54935(19) 0.31075(15) 1.000 0.0263(8) d . . .
C12 C Uani 0.42551(15) 0.62716(19) 0.27375(15) 1.000 0.0264(8) d . . .
C13 C Uani 0.3251(2) 0.75000 0.2977(2) 1.000 0.0223(10) d STP . .
F1 F Uani 0.18687(9) 0.63078(11) 0.38401(9) 1.000 0.0312(5) d . . .
F2 F Uani 0.10620(10) 0.47684(13) 0.27832(10) 1.000 0.0421(6) d . . .
F3 F Uani 0.17604(14) 0.60614(14) 0.25782(10) 1.000 0.0554(7) d . . .
F4 F Uani 0.07138(11) 0.61321(16) 0.33206(13) 1.000 0.0590(8) d . . .
F5 F Uani 0.11896(12) 0.49994(15) 0.40519(10) 1.000 0.0500(7) d . . .
F6 F Uani 0.22178(10) 0.49313(13) 0.33163(11) 1.000 0.0454(6) d . . .
F7_a F Uani 0.4150(4) 0.25000 0.1854(2) 0.746(4) 0.0701(19) . . . .
F8_a F Uani 0.4087(3) 0.25000 0.36672(17) 0.746(4) 0.0387(13) . . . .
F7A_b F Uani 0.4810(7) 0.25000 0.1961(3) 0.254(4) 0.062(4) . . . .
F8A_b F Uani 0.4249(6) 0.25000 0.3684(3) 0.254(4) 0.059(5) . . . .
N7 N Uani 0.3098(2) 0.75000 0.5074(2) 1.000 0.0342(11) d STP . .
C14 C Uani 0.3581(4) 0.75000 0.5365(3) 1.000 0.0480(17) d STP . .
C15 C Uani 0.4302(3) 0.75000 0.5829(4) 1.000 0.073(2) d STP . .
N8 N Uani 0.5104(3) 0.25000 0.5752(4) 1.000 0.088(3) d STU . .
C16 C Uani 0.4486(3) 0.25000 0.5911(3) 1.000 0.0507(19) d STU . .
C17 C Uani 0.3708(3) 0.25000 0.6105(4) 1.000 0.0597(19) d STU . .
F9_a F Uani 0.4771(2) 0.32866(16) 0.27954(15) 0.746(4) 0.0457(9) . . . .
N9 N Uani 0.7126(4) 0.25000 0.3166(3) 1.000 0.105(3) d STP . .
C18 C Uani 0.6958(5) 0.25000 0.2542(4) 1.000 0.077(3) d STP . .
C19 C Uani 0.6758(7) 0.25000 0.1747(4) 1.000 0.106(4) d STP . .
F10_a F Uani 0.3499(2) 0.33000(19) 0.27391(18) 0.746(4) 0.0587(11) . . . .
F9A_b F Uani 0.5141(4) 0.3295(4) 0.3037(4) 0.254(4) 0.051(2) . . . .
F10A_b F Uani 0.3935(5) 0.3292(4) 0.2625(4) 0.254(4) 0.054(2) . . . .
H1A H Uiso 0.03110 0.75000 0.46600 1.000 0.0260 c RUP . .
H1B H Uiso 0.11920 0.75000 0.44610 1.000 0.0260 c RUP . .
H2 H Uiso 0.20630 0.66620 0.54700 1.000 0.0270 c RU . .
H3 H Uiso -0.01460 0.61220 0.55520 1.000 0.0330 c RU . .
H3A H Uiso 0.35770 0.54900 0.66190 1.000 0.0370 c RU . .
H4 H Uiso 0.05110 0.49280 0.63140 1.000 0.0350 c RU . .
H5A H Uiso 0.19470 0.45270 0.65810 1.000 0.0370 c RU . .
H5B H Uiso 0.22560 0.55030 0.68840 1.000 0.0370 c RU . .
H7 H Uiso 0.24810 0.45800 0.48380 1.000 0.0310 c RU . .
H9A H Uiso 0.45900 0.44940 0.44220 1.000 0.0300 c RU . .
H9B H Uiso 0.38340 0.40740 0.40640 1.000 0.0300 c RU . .
H10 H Uiso 0.31860 0.62380 0.41500 1.000 0.0240 c RU . .
H11 H Uiso 0.48580 0.50780 0.29550 1.000 0.0320 c RU . .
H12 H Uiso 0.44620 0.65080 0.22790 1.000 0.0320 c RU . .
H13A H Uiso 0.31250 0.75000 0.24280 1.000 0.0270 c RUP . .
H13B H Uiso 0.27720 0.75000 0.32660 1.000 0.0270 c RUP . .
H15A H Uiso 0.41780 0.75000 0.63720 1.000 0.1100 c RUP . .
H15B H Uiso 0.45970 0.80540 0.57070 0.500 0.1100 c RUP . .
H15C H Uiso 0.45970 0.69460 0.57070 0.500 0.1100 c RUP . .
H17A H Uiso 0.36330 0.21400 0.65720 0.500 0.0890 c RUP . .
H17B H Uiso 0.34170 0.22210 0.56900 0.500 0.0890 c RUP . .
H17C H Uiso 0.35390 0.31380 0.61870 0.500 0.0890 c RUP . .
H19A H Uiso 0.71700 0.27720 0.14500 0.500 0.1590 c RUP . .
H19B H Uiso 0.62990 0.28660 0.16720 0.500 0.1590 c RUP . .
H19C H Uiso 0.66700 0.18620 0.15770 0.500 0.1590 c RUP . .


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

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P3 F14 1.577(4) . 8_555 yes
P3 F15 1.603(4) . 8_555 yes
P3 F16 1.579(4) . 8_555 yes
P3 F15 1.603(4) . . yes
P3 F16 1.579(4) . . yes
P3 F11 1.654(4) . 8_555 yes
P3 F11 1.654(4) . . yes
P3 F12 1.627(4) . . yes
P3 F13 1.502(4) . . yes
P3 F14 1.577(4) . . yes
P3 F12 1.627(4) . 8_555 yes
P3 F13 1.502(4) . 8_555 yes
P1 F1 1.6175(18) . . yes
P1 F5 1.588(2) . . yes
P1 F6 1.599(2) . . yes
P1 F3 1.589(2) . . yes
P1 F4 1.584(2) . . yes
P1 F2 1.614(2) . . yes
P2_a F8_a 1.604(3) 8_555 8_555 yes
P2_a F7_a 1.587(4) 8_555 8_555 yes
N1 C3 1.380(3) . . yes
N1 C1 1.465(3) . . yes
N1 C2 1.328(3) . . yes
N2 C4 1.385(4) . . yes
N2 C2 1.331(3) . . yes
N2 C5 1.477(4) . . yes
P2A_b F7A_b 1.585(7) 8_565 8_565 yes
P2A_b F8A_b 1.604(7) 8_565 8_565 yes
N3 C6 1.337(4) . . yes
N3 N4 1.352(3) . . yes
N4 C8 1.329(4) . . yes
N5 C9 1.490(3) . . yes
N5 C11 1.383(3) . . yes
N5 C10 1.327(3) . . yes
N6 C10 1.335(3) . . yes
N6 C12 1.386(3) . . yes
N6 C13 1.464(3) . . yes
F11 F13 0.945(7) . . yes
F12 F13 1.375(6) . . yes
N3 H3A 0.8800 . . no
C3 C4 1.347(4) . . no
C5 C6 1.494(4) . . no
C6 C7 1.375(4) . . no
C7 C8 1.404(4) . . no
C8 C9 1.499(4) . . no
C11 C12 1.354(4) . . no
C1 H1A 0.9900 . . no
C1 H1B 0.9900 . . no
C2 H2 0.9500 . . no
C3 H3 0.9500 . . no
C4 H4 0.9500 . . no
C5 H5A 0.9900 . . no
C5 H5B 0.9900 . . no
C7 H7 0.9500 . . no
C9 H9A 0.9900 . . no
C9 H9B 0.9900 . . no
C10 H10 0.9500 . . no
C11 H11 0.9500 . . no
C12 H12 0.9500 . . no
C13 H13B 0.9900 . . no
C13 H13A 0.9900 . . no
N7 C14 0.998(8) . . yes
C14 C15 1.518(9) . . no
N8 C16 1.132(8) . . yes
C15 H15B 0.9800 . . no
C15 H15C 0.9800 . . no
C15 H15A 0.9800 . . no
C16 C17 1.422(8) . . no
N9 C18 1.137(9) . . yes
C17 H17B 0.9800 . . no
C17 H17C 0.9800 . . no
C17 H17A 0.9800 . . no
C17 H17B 0.9800 . 8_555 no
C17 H17C 0.9800 . 8_555 no
C17 H17A 0.9800 . 8_555 no
C18 C19 1.442(10) . . no
C19 H19A 0.9800 . . no
C19 H19B 0.9800 . . no
C19 H19C 0.9800 . . no
C19 H19A 0.9800 . 8_555 no
C19 H19B 0.9800 . 8_555 no
C19 H19C 0.9800 . 8_555 no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F13 P3 F14 119.5(3) 8_555 . 8_555 yes
F13 P3 F15 92.1(5) 8_555 . 8_555 yes
F13 P3 F16 102.0(9) 8_555 . 8_555 yes
F14 P3 F15 86.9(2) 8_555 . 8_555 yes
F14 P3 F16 91.0(2) 8_555 . 8_555 yes
F15 P3 F16 164.8(10) 8_555 . 8_555 yes
F11 P3 F14 87.1(3) . . . yes
F11 P3 F15 102.8(5) . . . yes
F11 P3 F16 92.2(9) . . . yes
F11 P3 F11 150.1(3) . . 8_555 yes
F11 P3 F12 124.0(2) . . 8_555 yes
F11 P3 F13 175.4(3) . . 8_555 yes
F11 P3 F14 64.5(3) . . 8_555 yes
F11 P3 F15 85.7(5) . . 8_555 yes
F11 P3 F16 79.8(9) . . 8_555 yes
F12 P3 F13 52.0(2) . . . yes
F12 P3 F14 171.4(3) . . . yes
F12 P3 F15 93.4(2) . . . yes
F12 P3 F16 90.9(3) . . . yes
F11 P3 F12 124.0(2) 8_555 . . yes
F12 P3 F12 39.7(2) . . 8_555 yes
F12 P3 F13 91.4(3) . . 8_555 yes
F12 P3 F14 148.8(3) . . 8_555 yes
F12 P3 F15 87.4(2) . . 8_555 yes
F12 P3 F16 86.5(3) . . 8_555 yes
F13 P3 F14 119.5(3) . . . yes
F13 P3 F15 92.1(5) . . . yes
F13 P3 F16 102.0(9) . . . yes
F11 P3 F13 175.4(3) 8_555 . . yes
F12 P3 F13 91.4(3) 8_555 . . yes
F13 P3 F13 141.0(3) . . 8_555 yes
F13 P3 F14 97.0(3) . . 8_555 yes
F13 P3 F15 75.4(5) . . 8_555 yes
F13 P3 F16 89.9(9) . . 8_555 yes
F14 P3 F15 86.9(2) . . . yes
F14 P3 F16 91.0(2) . . . yes
F11 P3 F14 64.5(3) 8_555 . . yes
F12 P3 F14 148.8(3) 8_555 . . yes
F13 P3 F14 97.0(3) 8_555 . . yes
F14 P3 F14 22.7(4) . . 8_555 yes
F14 P3 F15 90.4(2) . . 8_555 yes
F14 P3 F16 93.5(2) . . 8_555 yes
F15 P3 F16 164.8(10) . . . yes
F11 P3 F15 85.7(5) 8_555 . . yes
F12 P3 F15 87.4(2) 8_555 . . yes
F13 P3 F15 75.4(5) 8_555 . . yes
F14 P3 F15 90.4(2) 8_555 . . yes
F15 P3 F15 17.6(6) . . 8_555 yes
F15 P3 F16 177.4(9) . . 8_555 yes
F11 P3 F16 79.8(9) 8_555 . . yes
F12 P3 F16 86.5(3) 8_555 . . yes
F13 P3 F16 89.9(9) 8_555 . . yes
F14 P3 F16 93.5(2) 8_555 . . yes
F15 P3 F16 177.4(10) 8_555 . . yes
F16 P3 F16 12.8(13) . . 8_555 yes
F11 P3 F12 84.5(2) 8_555 . 8_555 yes
F11 P3 F13 34.4(3) 8_555 . 8_555 yes
F11 P3 F14 87.1(3) 8_555 . 8_555 yes
F11 P3 F15 102.8(5) 8_555 . 8_555 yes
F11 P3 F16 92.2(9) 8_555 . 8_555 yes
F12 P3 F13 52.0(2) 8_555 . 8_555 yes
F12 P3 F14 171.4(3) 8_555 . 8_555 yes
F12 P3 F15 93.4(2) 8_555 . 8_555 yes
F12 P3 F16 90.9(3) 8_555 . 8_555 yes
F11 P3 F12 84.5(2) . . . yes
F11 P3 F13 34.4(3) . . . yes
F2 P1 F5 90.15(10) . . . yes
F2 P1 F3 90.24(10) . . . yes
F2 P1 F4 90.41(11) . . . yes
F3 P1 F5 178.35(13) . . . yes
F3 P1 F6 89.14(11) . . . yes
F4 P1 F5 90.09(12) . . . yes
F4 P1 F6 179.32(12) . . . yes
F5 P1 F6 89.26(11) . . . yes
F1 P1 F2 179.63(10) . . . yes
F1 P1 F3 89.41(10) . . . yes
F1 P1 F4 89.73(11) . . . yes
F1 P1 F5 90.20(10) . . . yes
F1 P1 F6 90.07(9) . . . yes
F2 P1 F6 89.80(10) . . . yes
F3 P1 F4 91.51(12) . . . yes
F7_a P2_a F8_a 178.6(4) 8_555 8_555 8_555 yes
C2 N1 C3 108.5(2) . . . yes
C1 N1 C2 123.0(2) . . . yes
C1 N1 C3 128.5(2) . . . yes
C4 N2 C5 127.4(2) . . . yes
C2 N2 C5 124.3(2) . . . yes
C2 N2 C4 108.3(2) . . . yes
F7A_b P2A_b F8A_b 178.5(7) 8_565 8_565 8_565 yes
N4 N3 C6 113.2(2) . . . yes
N3 N4 C8 104.1(2) . . . yes
C10 N5 C11 108.6(2) . . . yes
C9 N5 C10 126.5(2) . . . yes
C9 N5 C11 124.9(2) . . . yes
C10 N6 C13 124.7(2) . . . yes
C12 N6 C13 126.8(2) . . . yes
C10 N6 C12 108.5(2) . . . yes
P3 F11 F13 64.0(4) . . . yes
P3 F12 F13 59.3(2) . . . yes
F11 F13 F12 143.1(6) . . . yes
P3 F13 F11 81.6(4) . . . yes
P3 F13 F12 68.7(3) . . . yes
N1 C1 N1 110.7(3) . . 8_565 yes
N1 C2 N2 108.9(2) . . . yes
N1 C3 C4 107.3(2) . . . yes
N4 N3 H3A 123.00 . . . no
C6 N3 H3A 123.00 . . . no
N2 C4 C3 107.1(2) . . . yes
N2 C5 C6 110.4(2) . . . yes
N3 C6 C5 121.6(2) . . . yes
C5 C6 C7 132.1(2) . . . no
N3 C6 C7 106.4(2) . . . yes
C6 C7 C8 104.9(2) . . . no
C7 C8 C9 128.9(2) . . . no
N4 C8 C7 111.4(2) . . . yes
N4 C8 C9 119.7(2) . . . yes
N5 C9 C8 112.0(2) . . . yes
N5 C10 N6 108.9(2) . . . yes
N5 C11 C12 107.3(2) . . . yes
N6 C12 C11 106.8(2) . . . yes
N6 C13 N6 112.4(3) . . 8_565 yes
N1 C1 H1A 109.00 . . . no
N1 C1 H1B 110.00 . . . no
H1A C1 H1B 108.00 . . . no
N1 C1 H1B 110.00 8_565 . . no
N1 C1 H1A 109.00 8_565 . . no
N1 C2 H2 125.00 . . . no
N2 C2 H2 126.00 . . . no
C4 C3 H3 126.00 . . . no
N1 C3 H3 126.00 . . . no
N2 C4 H4 126.00 . . . no
C3 C4 H4 127.00 . . . no
C6 C5 H5A 110.00 . . . no
C6 C5 H5B 110.00 . . . no
N2 C5 H5B 110.00 . . . no
N2 C5 H5A 110.00 . . . no
H5A C5 H5B 108.00 . . . no
C8 C7 H7 128.00 . . . no
C6 C7 H7 128.00 . . . no
N5 C9 H9B 109.00 . . . no
C8 C9 H9A 109.00 . . . no
C8 C9 H9B 109.00 . . . no
H9A C9 H9B 108.00 . . . no
N5 C9 H9A 109.00 . . . no
N5 C10 H10 126.00 . . . no
N6 C10 H10 126.00 . . . no
C12 C11 H11 126.00 . . . no
N5 C11 H11 126.00 . . . no
N6 C12 H12 127.00 . . . no
C11 C12 H12 127.00 . . . no
N6 C13 H13B 109.00 . . . no
N6 C13 H13B 109.00 8_565 . . no
H13A C13 H13B 108.00 . . . no
N6 C13 H13A 109.00 8_565 . . no
N6 C13 H13A 109.00 . . . no
N7 C14 C15 178.3(6) . . . yes
C14 C15 H15A 110.00 . . . no
C14 C15 H15B 109.00 . . . no
C14 C15 H15C 109.00 . . . no
H15A C15 H15B 109.00 . . . no
H15A C15 H15C 109.00 . . . no
H15B C15 H15C 109.00 . . . no
N8 C16 C17 179.6(7) . . . yes
C16 C17 H17A 109.00 . . . no
C16 C17 H17B 109.00 . . . no
C16 C17 H17C 109.00 . . . no
C16 C17 H17A 109.00 . . 8_555 no
C16 C17 H17B 109.00 . . 8_555 no
C16 C17 H17C 109.00 . . 8_555 no
H17A C17 H17B 110.00 . . . no
H17A C17 H17C 109.00 . . . no
H17A C17 H17A 64.00 . . 8_555 no
H17A C17 H17B 140.00 . . 8_555 no
H17A C17 H17C 48.00 . . 8_555 no
H17B C17 H17C 110.00 . . . no
H17A C17 H17B 140.00 8_555 . . no
H17B C17 H17B 48.00 . . 8_555 no
H17B C17 H17C 64.00 . . 8_555 no
H17A C17 H17C 48.00 8_555 . . no
H17B C17 H17C 64.00 8_555 . . no
H17C C17 H17C 140.00 . . 8_555 no
H17A C17 H17B 110.00 8_555 . 8_555 no
H17A C17 H17C 109.00 8_555 . 8_555 no
H17B C17 H17C 110.00 8_555 . 8_555 no
N9 C18 C19 179.0(10) . . . yes
C18 C19 H19A 109.00 . . . no
C18 C19 H19B 110.00 . . . no
C18 C19 H19C 110.00 . . . no
C18 C19 H19A 109.00 . . 8_555 no
C18 C19 H19B 110.00 . . 8_555 no
C18 C19 H19C 110.00 . . 8_555 no
H19A C19 H19B 109.00 . . . no
H19A C19 H19C 109.00 . . . no
H19A C19 H19A 47.00 . . 8_555 no
H19A C19 H19B 140.00 . . 8_555 no
H19A C19 H19C 65.00 . . 8_555 no
H19B C19 H19C 109.00 . . . no
H19A C19 H19B 140.00 8_555 . . no
H19B C19 H19B 65.00 . . 8_555 no
H19B C19 H19C 47.00 . . 8_555 no
H19A C19 H19C 65.00 8_555 . . no
H19B C19 H19C 47.00 8_555 . . no
H19C C19 H19C 140.00 . . 8_555 no
H19A C19 H19B 109.00 8_555 . 8_555 no
H19A C19 H19C 109.00 8_555 . 8_555 no
H19B C19 H19C 109.00 8_555 . 8_555 no

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
F16 P3 F13 F11 76.0(5) . . . . no
F16 P3 F13 F12 -81.6(4) . . . . no
F12 P3 F13 F11 162.8(4) 8_555 . . . no
F12 P3 F13 F12 5.2(3) 8_555 . . . no
F13 P3 F13 F11 -179.0(4) 8_555 . . . no
F13 P3 F13 F12 23.4(5) 8_555 . . . no
F14 P3 F13 F11 -19.2(4) 8_555 . . . no
F14 P3 F13 F12 -176.7(2) 8_555 . . . no
F15 P3 F13 F11 -104.1(4) 8_555 . . . no
F15 P3 F13 F12 98.3(3) 8_555 . . . no
F16 P3 F13 F11 71.9(5) 8_555 . . . no
F16 P3 F13 F12 -85.7(4) 8_555 . . . no
F11 P3 F11 F13 178.7(5) 8_555 . . . no
F12 P3 F11 F13 -21.0(5) 8_555 . . . no
F14 P3 F11 F13 158.9(5) 8_555 . . . no
F15 P3 F11 F13 70.3(4) 8_555 . . . no
F16 P3 F11 F13 -105.1(5) 8_555 . . . no
F11 P3 F12 F13 12.5(3) . . . . no
F15 P3 F12 F13 -90.0(5) . . . . no
F16 P3 F12 F13 104.6(9) . . . . no
F11 P3 F12 F13 -177.2(3) 8_555 . . . no
F12 P3 F12 F13 -171.9(4) 8_555 . . . no
F13 P3 F12 F13 -165.5(3) 8_555 . . . no
F14 P3 F12 F13 6.3(5) 8_555 . . . no
F15 P3 F12 F13 -73.5(5) 8_555 . . . no
F16 P3 F12 F13 92.5(9) 8_555 . . . no
F11 P3 F13 F12 -157.6(5) . . . . no
F12 P3 F13 F11 157.6(5) . . . . no
F14 P3 F13 F11 -22.1(5) . . . . no
F14 P3 F13 F12 -179.7(2) . . . . no
F15 P3 F13 F11 -109.8(4) . . . . no
F15 P3 F13 F12 92.7(3) . . . . no
F12 P3 F11 F13 -17.6(4) . . . . no
F14 P3 F11 F13 160.8(4) . . . . no
F15 P3 F11 F13 74.7(4) . . . . no
F16 P3 F11 F13 -108.3(5) . . . . no
C1 N1 C3 C4 -177.3(3) . . . . no
C2 N1 C3 C4 -0.3(3) . . . . no
C1 N1 C2 N2 177.1(2) . . . . no
C2 N1 C1 N1 -73.4(3) . . . 8_565 no
C3 N1 C1 N1 103.3(3) . . . 8_565 no
C3 N1 C2 N2 -0.1(3) . . . . no
C4 N2 C2 N1 0.5(3) . . . . no
C4 N2 C5 C6 140.4(3) . . . . no
C2 N2 C5 C6 -43.1(3) . . . . no
C5 N2 C2 N1 -176.6(2) . . . . no
C2 N2 C4 C3 -0.7(3) . . . . no
C5 N2 C4 C3 176.3(2) . . . . no
N4 N3 C6 C7 -0.9(3) . . . . no
C6 N3 N4 C8 0.9(3) . . . . no
N4 N3 C6 C5 179.6(2) . . . . no
N3 N4 C8 C9 179.5(2) . . . . no
N3 N4 C8 C7 -0.6(3) . . . . no
C10 N5 C11 C12 0.1(3) . . . . no
C9 N5 C10 N6 -176.9(2) . . . . no
C10 N5 C9 C8 -16.6(3) . . . . no
C11 N5 C9 C8 166.7(2) . . . . no
C11 N5 C10 N6 0.3(3) . . . . no
C9 N5 C11 C12 177.3(2) . . . . no
C12 N6 C10 N5 -0.6(3) . . . . no
C12 N6 C13 N6 -77.5(3) . . . 8_565 no
C10 N6 C12 C11 0.6(3) . . . . no
C13 N6 C12 C11 -179.1(2) . . . . no
C13 N6 C10 N5 179.2(2) . . . . no
C10 N6 C13 N6 102.8(3) . . . 8_565 no
P3 F11 F13 F12 36.3(8) . . . . no
P3 F12 F13 F11 -38.9(8) . . . . no
N1 C3 C4 N2 0.6(3) . . . . no
N2 C5 C6 C7 -47.0(4) . . . . no
N2 C5 C6 N3 132.4(3) . . . . no
N3 C6 C7 C8 0.5(3) . . . . no
C5 C6 C7 C8 179.9(3) . . . . no
C6 C7 C8 N4 0.1(3) . . . . no
C6 C7 C8 C9 -180.0(2) . . . . no
N4 C8 C9 N5 -97.4(3) . . . . no
C7 C8 C9 N5 82.7(3) . . . . no
N5 C11 C12 N6 -0.4(3) . . . . no


#===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_compound_5
_database_code_depnum_ccdc_archive 'CCDC 1057576'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

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

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H22 N12 Ni2, 2(F6 P), C3 H7 N O'
_chemical_formula_structural     ?
_chemical_formula_sum            'C27 H29 F12 N13 Ni2 O P2'
_chemical_formula_iupac          ?
_chemical_formula_weight         958.95
_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'
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  '-P 2yn'
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,1/2+y,1/2-z
3 -x,-y,-z
4 1/2+x,1/2-y,1/2+z

_cell_length_a                   16.9279(10)
_cell_length_b                   14.4946(8)
_cell_length_c                   28.0590(15)
_cell_angle_alpha                90
_cell_angle_beta                 93.054(4)
_cell_angle_gamma                90
_cell_volume                     6874.9(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    123
_cell_measurement_reflns_used    6373
_cell_measurement_theta_min      2.4116
_cell_measurement_theta_max      23.6473
_cell_special_details            
;
;

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.335
_exptl_crystal_size_min          0.321
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             3872
_exptl_absorpt_coefficient_mu    1.303
_exptl_crystal_density_meas_temp ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_T_max  0.7454

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             C. Jandl
scanspeed                           10 s per frame
dx                                  60 mm
4228 frames measured in 12 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         '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            120413
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.37
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             12603
# number of observed reflections (> n sig(I))
_reflns_number_gt                8369
_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)+(0.0333P)²+9.8331P] 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         12603
_refine_ls_number_parameters     1095
_refine_ls_number_restraints     21
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1179
_refine_ls_wR_factor_gt          0.1007
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.093

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

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni Uani 0.42485(3) 0.25861(3) 0.35643(2) 1.000 0.0168(2) d . . .
Ni2 Ni Uani 0.57087(3) 0.25768(3) 0.45473(2) 1.000 0.0181(2) d . . .
Ni3 Ni Uani -0.07843(3) 0.26741(3) 0.35309(2) 1.000 0.0164(2) d . . .
Ni4 Ni Uani 0.06634(3) 0.23632(3) 0.45025(2) 1.000 0.0157(2) d . . .
P1 P Uani 0.33630(12) 0.2439(2) 0.49811(8) 0.737(6) 0.0197(9) d DP A 1
P2 P Uani 0.16422(6) 0.72288(7) 0.50876(4) 1.000 0.0211(3) d . . .
N1 N Uani 0.2696(2) 0.3418(2) 0.33694(12) 1.000 0.0234(12) d . . .
N2 N Uani 0.3646(2) 0.4306(2) 0.31896(12) 1.000 0.0223(11) d . . .
N3 N Uani 0.49811(19) 0.3546(2) 0.37203(12) 1.000 0.0175(11) d . . .
P3 P Uani 0.57182(7) 0.27403(8) 0.21563(4) 1.000 0.0280(4) d . . .
N4 N Uani 0.55230(19) 0.3549(2) 0.41024(12) 1.000 0.0178(11) d . . .
N5 N Uani 0.6200(2) 0.4312(2) 0.49698(13) 1.000 0.0241(12) d . . .
N6 N Uani 0.5843(2) 0.3367(2) 0.54993(13) 1.000 0.0261(12) d . . .
N7 N Uani 0.5884(2) 0.1743(2) 0.54904(12) 1.000 0.0265(12) d . . .
N8 N Uani 0.6265(2) 0.0849(2) 0.49476(13) 1.000 0.0252(12) d . . .
N9 N Uani 0.55388(19) 0.1612(2) 0.40889(12) 1.000 0.0179(11) d . . .
N10 N Uani 0.49816(19) 0.1619(2) 0.37166(11) 1.000 0.0165(10) d . . .
N11 N Uani 0.3617(2) 0.0877(2) 0.31956(12) 1.000 0.0212(11) d . . .
N12 N Uani 0.2681(2) 0.1790(2) 0.33659(12) 1.000 0.0208(11) d . . .
C1 C Uani 0.2281(2) 0.2605(3) 0.35327(15) 1.000 0.0247(14) d . . .
C2 C Uani 0.3500(2) 0.3467(3) 0.33709(14) 1.000 0.0199(12) d . . .
C3 C Uani 0.2352(3) 0.4227(3) 0.31924(15) 1.000 0.0280(17) d . . .
C4 C Uani 0.2948(3) 0.4780(3) 0.30787(15) 1.000 0.0283(16) d . . .
C5 C Uani 0.4448(3) 0.4622(3) 0.31017(15) 1.000 0.0239(14) d . . .
C6 C Uani 0.5005(2) 0.4386(3) 0.35115(15) 1.000 0.0211(12) d . . .
C7 C Uani 0.5556(2) 0.4936(3) 0.37520(15) 1.000 0.0212(14) d . . .
C8 C Uani 0.5860(2) 0.4394(3) 0.41218(15) 1.000 0.0221(14) d . . .
C9 C Uani 0.6447(3) 0.4653(3) 0.45132(16) 1.000 0.0271(14) d . . .
C10 C Uani 0.5919(2) 0.3451(3) 0.50234(15) 1.000 0.0224(14) d . . .
C11 C Uani 0.6298(3) 0.4754(3) 0.54083(17) 1.000 0.0310(17) d . . .
C12 C Uani 0.6079(3) 0.4163(3) 0.57373(18) 1.000 0.0344(17) d . . .
C13 C Uani 0.5542(3) 0.2533(3) 0.57172(16) 1.000 0.0321(16) d . . .
C14 C Uani 0.5956(2) 0.1685(3) 0.50131(15) 1.000 0.0234(14) d . . .
C15 C Uani 0.6144(3) 0.0941(3) 0.57163(17) 1.000 0.0347(17) d . . .
C16 C Uani 0.6392(3) 0.0379(3) 0.53761(17) 1.000 0.0346(17) d . . .
C17 C Uani 0.6482(3) 0.0509(3) 0.44811(15) 1.000 0.0258(16) d . . .
C18 C Uani 0.5864(2) 0.0761(3) 0.41086(15) 1.000 0.0197(12) d . . .
C19 C Uani 0.5521(3) 0.0215(3) 0.37506(15) 1.000 0.0229(16) d . . .
C20 C Uani 0.4972(2) 0.0774(3) 0.35157(14) 1.000 0.0173(12) d . . .
C21 C Uani 0.4418(2) 0.0548(3) 0.31033(14) 1.000 0.0211(12) d . . .
C22 C Uani 0.3484(2) 0.1717(3) 0.33779(14) 1.000 0.0197(12) d . . .
C23 C Uani 0.2913(3) 0.0433(3) 0.30678(15) 1.000 0.0259(14) d . . .
C24 C Uani 0.2325(3) 0.1007(3) 0.31772(15) 1.000 0.0271(17) d . . .
F1 F Uani 0.3027(3) 0.3080(3) 0.45512(16) 0.737(6) 0.0412(17) d DP A 1
F2 F Uani 0.3707(2) 0.1817(3) 0.54125(16) 0.737(6) 0.0410(16) d DP A 1
F3 F Uani 0.4015(2) 0.3210(2) 0.51108(16) 0.737(6) 0.0396(14) d DP A 1
P4 P Uani 0.41008(8) 0.75647(8) 0.28130(4) 1.000 0.0302(4) d . . .
F4 F Uani 0.2776(3) 0.2942(3) 0.53258(15) 0.737(6) 0.0479(17) d DP A 1
F5 F Uani 0.2714(3) 0.1687(3) 0.4856(2) 0.737(6) 0.062(2) d DP A 1
F6 F Uani 0.3945(2) 0.1963(3) 0.46406(15) 0.737(6) 0.0493(17) d DP A 1
N13 N Uani -0.2270(2) 0.3668(2) 0.33844(12) 1.000 0.0224(12) d . . .
N14 N Uani -0.1270(2) 0.4491(2) 0.32309(12) 1.000 0.0205(11) d . . .
N15 N Uani 0.00171(19) 0.3537(2) 0.37277(12) 1.000 0.0175(11) d . . .
N16 N Uani 0.05224(19) 0.3442(2) 0.41232(12) 1.000 0.0171(11) d . . .
N17 N Uani 0.1193(2) 0.3963(2) 0.50448(13) 1.000 0.0226(11) d . . .
N18 N Uani 0.0796(2) 0.2899(2) 0.54973(12) 1.000 0.0227(11) d . . .
N19 N Uani 0.0768(2) 0.1293(2) 0.53771(12) 1.000 0.0207(11) d . . .
N20 N Uani 0.1165(2) 0.0536(2) 0.47838(12) 1.000 0.0199(11) d . . .
N21 N Uani 0.04590(19) 0.1523(2) 0.39852(12) 1.000 0.0171(10) d . . .
N22 N Uani -0.01254(19) 0.1627(2) 0.36337(11) 1.000 0.0163(10) d . . .
N23 N Uani -0.15365(19) 0.1090(2) 0.31041(12) 1.000 0.0196(11) d . . .
N24 N Uani -0.2398(2) 0.2056(2) 0.33334(12) 1.000 0.0214(11) d . . .
C25 C Uani -0.2740(2) 0.2877(3) 0.35270(15) 1.000 0.0246(14) d . . .
C26 C Uani -0.1475(2) 0.3644(3) 0.33803(14) 1.000 0.0186(12) d . . .
C27 C Uani -0.2564(3) 0.4522(3) 0.32410(14) 1.000 0.0255(14) d . . .
C28 C Uani -0.1932(3) 0.5035(3) 0.31416(15) 1.000 0.0241(14) d . . .
C29 C Uani -0.0443(2) 0.4737(3) 0.31567(15) 1.000 0.0235(14) d . . .
C30 C Uani 0.0068(2) 0.4411(3) 0.35739(14) 1.000 0.0195(12) d . . .
C31 C Uani 0.0600(2) 0.4897(3) 0.38648(15) 1.000 0.0205(14) d . . .
C32 C Uani 0.0869(2) 0.4272(3) 0.42043(15) 1.000 0.0216(14) d . . .
C33 C Uani 0.1446(3) 0.4435(3) 0.46155(16) 1.000 0.0271(16) d . . .
C34 C Uani 0.0892(2) 0.3102(3) 0.50322(15) 1.000 0.0207(12) d . . .
C35 C Uani 0.1281(3) 0.4288(3) 0.55069(16) 1.000 0.0303(16) d . . .
C36 C Uani 0.1030(3) 0.3623(3) 0.57912(16) 1.000 0.0295(17) d . . .
C37 C Uani 0.0443(3) 0.2043(3) 0.56499(15) 1.000 0.0243(12) d . . .
C38 C Uani 0.0867(2) 0.1359(3) 0.49034(15) 1.000 0.0194(12) d . . .
C39 C Uani 0.1005(3) 0.0434(3) 0.55513(16) 1.000 0.0270(16) d . . .
C40 C Uani 0.1256(3) -0.0038(3) 0.51758(15) 1.000 0.0256(16) d . . .
C41 C Uani 0.1387(2) 0.0329(3) 0.42978(15) 1.000 0.0231(14) d . . .
C42 C Uani 0.0756(2) 0.0664(3) 0.39464(15) 1.000 0.0185(12) d . . .
C43 C Uani 0.0376(2) 0.0210(3) 0.35679(14) 1.000 0.0184(12) d . . .
C44 C Uani -0.0177(2) 0.0836(3) 0.33797(14) 1.000 0.0196(12) d . . .
C45 C Uani -0.0774(2) 0.0720(3) 0.29750(15) 1.000 0.0221(14) d . . .
C46 C Uani -0.1607(3) 0.1920(3) 0.33186(14) 1.000 0.0213(12) d . . .
C47 C Uani -0.2279(3) 0.0714(3) 0.29882(16) 1.000 0.0288(16) d . . .
C48 C Uani -0.2817(3) 0.1317(3) 0.31333(15) 1.000 0.0269(16) d . . .
P1A P Uani 0.3350(3) 0.2287(4) 0.49458(19) 0.263(6) 0.046(4) d DP A 2
F7 F Uani 0.09939(15) 0.77669(16) 0.53707(9) 1.000 0.0343(9) d . . .
F8 F Uani 0.22947(15) 0.66880(18) 0.48079(9) 1.000 0.0372(9) d . . .
F9 F Uani 0.23182(15) 0.78245(17) 0.53623(9) 1.000 0.0354(9) d . . .
F10 F Uani 0.17120(16) 0.64667(16) 0.55018(9) 1.000 0.0361(9) d . . .
F11 F Uani 0.09641(15) 0.66393(16) 0.48145(10) 1.000 0.0375(9) d . . .
F12 F Uani 0.15758(16) 0.79975(16) 0.46750(9) 1.000 0.0338(9) d . . .
F13 F Uani 0.64999(17) 0.2224(2) 0.20332(14) 1.000 0.0662(13) d . . .
F14 F Uani 0.49194(18) 0.3278(2) 0.22585(12) 1.000 0.0610(11) d . . .
F15 F Uani 0.52341(17) 0.21578(18) 0.17553(10) 1.000 0.0430(10) d . . .
F16 F Uani 0.59031(18) 0.35113(17) 0.17659(9) 1.000 0.0447(10) d . . .
F17 F Uani 0.61897(19) 0.3345(2) 0.25492(10) 1.000 0.0604(11) d . . .
F18 F Uani 0.55312(19) 0.1985(2) 0.25375(11) 1.000 0.0666(14) d . . .
F19 F Uani 0.3866(2) 0.83459(19) 0.31796(11) 1.000 0.0676(13) d . . .
F20 F Uani 0.4271(2) 0.6755(2) 0.24555(11) 1.000 0.0749(16) d . . .
F21 F Uani 0.4880(2) 0.7389(4) 0.31014(14) 1.000 0.123(2) d . . .
F22 F Uani 0.4446(3) 0.8279(3) 0.24751(14) 1.000 0.132(3) d . . .
F23 F Uani 0.3266(2) 0.7680(3) 0.25404(12) 1.000 0.0826(16) d . . .
F24 F Uani 0.3700(2) 0.6853(2) 0.31610(11) 1.000 0.0633(13) d . . .
F1A F Uani 0.2715(5) 0.3006(7) 0.4722(4) 0.263(6) 0.058(6) d DP A 2
F2A F Uani 0.3982(5) 0.1580(5) 0.5178(4) 0.263(6) 0.042(5) d DP A 2
F3A F Uani 0.3439(7) 0.2920(6) 0.5412(3) 0.263(6) 0.059(6) d DP A 2
F4A F Uani 0.2647(5) 0.1740(7) 0.5180(4) 0.263(6) 0.064(6) d DP A 2
F5A F Uani 0.3252(7) 0.1659(6) 0.4489(3) 0.263(6) 0.055(5) d DP A 2
F6A F Uani 0.4035(5) 0.2838(6) 0.4720(4) 0.263(6) 0.060(6) d DP A 2
O1 O Uani 0.1373(2) 0.5936(2) 0.29137(12) 1.000 0.0410(11) d . . .
N25 N Uani 0.1789(2) 0.7272(3) 0.32521(14) 1.000 0.0316(12) d . . .
O2 O Uani 0.6561(2) 0.6405(2) 0.30471(13) 1.000 0.0430(11) d . . .
C49 C Uani 0.1483(3) 0.6760(3) 0.29014(18) 1.000 0.0353(17) d . . .
C50 C Uani 0.2039(3) 0.6857(4) 0.37027(18) 1.000 0.050(2) d . . .
C51 C Uani 0.1848(3) 0.8265(4) 0.3212(3) 1.000 0.073(3) d . . .
N26 N Uani 0.6869(2) 0.7862(2) 0.32855(13) 1.000 0.0299(12) d . . .
C52 C Uani 0.6811(3) 0.6955(3) 0.33507(19) 1.000 0.0366(17) d . . .
C53 C Uani 0.6664(3) 0.8267(3) 0.28292(17) 1.000 0.0399(17) d . . .
C54 C Uani 0.7288(3) 0.8445(3) 0.36440(17) 1.000 0.0404(17) d . . .
H1A H Uiso 0.22830 0.26020 0.38860 1.000 0.0300 c RU . .
H1B H Uiso 0.17250 0.26120 0.34050 1.000 0.0300 c RU . .
H3 H Uiso 0.18030 0.43620 0.31590 1.000 0.0340 c RU . .
H4 H Uiso 0.29020 0.53830 0.29470 1.000 0.0340 c RU . .
H5A H Uiso 0.44440 0.52980 0.30530 1.000 0.0290 c RU . .
H5B H Uiso 0.46280 0.43280 0.28080 1.000 0.0290 c RU . .
H7 H Uiso 0.56970 0.55530 0.36790 1.000 0.0250 c RU . .
H9A H Uiso 0.69700 0.43900 0.44480 1.000 0.0330 c RU . .
H9B H Uiso 0.65000 0.53330 0.45270 1.000 0.0330 c RU . .
H11 H Uiso 0.64870 0.53640 0.54620 1.000 0.0370 c RU . .
H12 H Uiso 0.60830 0.42670 0.60720 1.000 0.0410 c RU . .
H13A H Uiso 0.56880 0.25280 0.60640 1.000 0.0380 c RU . .
H13B H Uiso 0.49580 0.25120 0.56740 1.000 0.0380 c RU . .
H15 H Uiso 0.61470 0.08130 0.60490 1.000 0.0410 c RU . .
H16 H Uiso 0.66100 -0.02200 0.54190 1.000 0.0410 c RU . .
H17A H Uiso 0.65430 -0.01700 0.44930 1.000 0.0310 c RU . .
H17B H Uiso 0.69950 0.07810 0.44000 1.000 0.0310 c RU . .
H19 H Uiso 0.56400 -0.04100 0.36820 1.000 0.0270 c RU . .
H21A H Uiso 0.46010 0.08450 0.28110 1.000 0.0250 c RU . .
H21B H Uiso 0.44080 -0.01280 0.30520 1.000 0.0250 c RU . .
H23 H Uiso 0.28570 -0.01630 0.29290 1.000 0.0310 c RU . .
H24 H Uiso 0.17740 0.08940 0.31330 1.000 0.0330 c RU . .
H25A H Uiso -0.27340 0.28360 0.38790 1.000 0.0300 c RU . .
H25B H Uiso -0.32950 0.29460 0.34030 1.000 0.0300 c RU . .
H27 H Uiso -0.31030 0.47070 0.32180 1.000 0.0300 c RU . .
H28 H Uiso -0.19380 0.56540 0.30310 1.000 0.0290 c RU . .
H29A H Uiso -0.03940 0.54140 0.31230 1.000 0.0280 c RU . .
H29B H Uiso -0.02720 0.44460 0.28600 1.000 0.0280 c RU . .
H31 H Uiso 0.07490 0.55260 0.38370 1.000 0.0240 c RU . .
H33A H Uiso 0.19740 0.42050 0.45360 1.000 0.0320 c RU . .
H33B H Uiso 0.14900 0.51060 0.46780 1.000 0.0320 c RU . .
H35 H Uiso 0.14810 0.48750 0.56040 1.000 0.0360 c RU . .
H36 H Uiso 0.10160 0.36440 0.61290 1.000 0.0360 c RU . .
H37A H Uiso -0.01380 0.20680 0.55930 1.000 0.0290 c RU . .
H37B H Uiso 0.05650 0.19460 0.59950 1.000 0.0290 c RU . .
H39 H Uiso 0.09920 0.02220 0.58710 1.000 0.0330 c RU . .
H40 H Uiso 0.14580 -0.06490 0.51790 1.000 0.0310 c RU . .
H41A H Uiso 0.14580 -0.03450 0.42610 1.000 0.0280 c RU . .
H41B H Uiso 0.18950 0.06340 0.42370 1.000 0.0280 c RU . .
H43 H Uiso 0.04720 -0.03980 0.34600 1.000 0.0220 c RU . .
H45A H Uiso -0.05950 0.10480 0.26910 1.000 0.0270 c RU . .
H45B H Uiso -0.08300 0.00570 0.28950 1.000 0.0270 c RU . .
H47 H Uiso -0.23850 0.01390 0.28350 1.000 0.0350 c RU . .
H48 H Uiso -0.33760 0.12510 0.31050 1.000 0.0320 c RU . .
H49 H Uiso 0.13360 0.70660 0.26110 1.000 0.0420 c RU . .
H50A H Uiso 0.21060 0.61910 0.36600 1.000 0.0750 c RU . .
H50B H Uiso 0.16370 0.69690 0.39350 1.000 0.0750 c RU . .
H50C H Uiso 0.25420 0.71300 0.38190 1.000 0.0750 c RU . .
H51A H Uiso 0.16960 0.84530 0.28850 1.000 0.1090 c RU . .
H51B H Uiso 0.23930 0.84580 0.32930 1.000 0.1090 c RU . .
H51C H Uiso 0.14930 0.85560 0.34330 1.000 0.1090 c RU . .
H52 H Uiso 0.69770 0.67160 0.36550 1.000 0.0440 c RU . .
H53A H Uiso 0.71460 0.83720 0.26580 1.000 0.0600 c RU . .
H53B H Uiso 0.63940 0.88570 0.28750 1.000 0.0600 c RU . .
H53C H Uiso 0.63120 0.78500 0.26430 1.000 0.0600 c RU . .
H54A H Uiso 0.77900 0.86520 0.35220 1.000 0.0600 c RU . .
H54B H Uiso 0.73930 0.80900 0.39380 1.000 0.0600 c RU . .
H54C H Uiso 0.69610 0.89830 0.37120 1.000 0.0600 c RU . .


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

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3 1.899(3) . . yes
Ni1 N10 1.906(3) . . yes
Ni1 C2 1.859(4) . . yes
Ni1 C22 1.861(4) . . yes
Ni2 N4 1.898(3) . . yes
Ni2 N9 1.911(3) . . yes
Ni2 C10 1.862(4) . . yes
Ni2 C14 1.870(4) . . yes
Ni3 C26 1.863(4) . . yes
Ni3 N15 1.905(3) . . yes
Ni3 N22 1.896(3) . . yes
Ni3 C46 1.844(5) . . yes
Ni4 C34 1.856(4) . . yes
Ni4 N16 1.899(3) . . yes
Ni4 N21 1.912(3) . . yes
Ni4 C38 1.861(4) . . yes
P1 F6 1.568(5) . . yes
P1 F1 1.603(5) . . yes
P1 F2 1.594(5) . . yes
P1 F3 1.599(4) . . yes
P1 F4 1.599(5) . . yes
P1 F5 1.574(5) . . yes
P2 F7 1.593(3) . . yes
P2 F10 1.603(3) . . yes
P2 F8 1.595(3) . . yes
P2 F9 1.599(3) . . yes
P2 F11 1.594(3) . . yes
P2 F12 1.606(3) . . yes
N1 C1 1.458(5) . . yes
N1 C3 1.389(5) . . yes
N1 C2 1.363(5) . . yes
N2 C5 1.466(6) . . yes
N2 C4 1.388(6) . . yes
N2 C2 1.346(5) . . yes
P3 F15 1.598(3) . . yes
P3 F16 1.607(3) . . yes
P3 F17 1.590(3) . . yes
P3 F13 1.575(3) . . yes
P3 F14 1.600(3) . . yes
N3 N4 1.373(5) . . yes
N3 C6 1.353(5) . . yes
P3 F18 1.574(3) . . yes
N4 C8 1.351(5) . . yes
N5 C10 1.347(5) . . yes
N5 C11 1.389(6) . . yes
N5 C9 1.455(6) . . yes
N6 C12 1.381(6) . . yes
N6 C13 1.459(5) . . yes
N6 C10 1.354(6) . . yes
N7 C13 1.446(5) . . yes
N7 C14 1.354(5) . . yes
N7 C15 1.385(5) . . yes
N8 C14 1.336(5) . . yes
N8 C16 1.389(6) . . yes
N8 C17 1.464(6) . . yes
N9 N10 1.370(5) . . yes
N9 C18 1.351(5) . . yes
N10 C20 1.348(5) . . yes
N11 C22 1.344(5) . . yes
N11 C21 1.473(5) . . yes
N11 C23 1.385(6) . . yes
N12 C24 1.378(5) . . yes
N12 C1 1.452(5) . . yes
N12 C22 1.362(5) . . yes
C3 C4 1.340(7) . . no
C5 C6 1.488(6) . . no
C6 C7 1.376(6) . . no
C7 C8 1.379(6) . . no
C8 C9 1.489(6) . . no
C11 C12 1.327(7) . . no
C15 C16 1.339(7) . . no
C17 C18 1.485(6) . . no
C18 C19 1.382(6) . . no
C19 C20 1.375(6) . . no
C20 C21 1.487(5) . . no
C23 C24 1.345(7) . . no
C1 H1B 0.9900 . . no
C1 H1A 0.9900 . . no
C3 H3 0.9500 . . no
P4 F21 1.532(4) . . yes
P4 F19 1.594(3) . . yes
P4 F22 1.540(4) . . yes
P4 F20 1.580(3) . . yes
P4 F24 1.596(3) . . yes
C4 H4 0.9500 . . no
P4 F23 1.580(4) . . yes
C5 H5B 0.9900 . . no
C5 H5A 0.9900 . . no
C7 H7 0.9500 . . no
C9 H9B 0.9900 . . no
C9 H9A 0.9900 . . no
C11 H11 0.9500 . . no
C12 H12 0.9500 . . no
C13 H13A 0.9900 . . no
N13 C25 1.463(5) . . yes
N13 C26 1.347(5) . . yes
C13 H13B 0.9900 . . no
N13 C27 1.386(5) . . yes
N14 C28 1.382(6) . . yes
N14 C29 1.470(5) . . yes
N14 C26 1.349(5) . . yes
C15 H15 0.9500 . . no
N15 C30 1.343(5) . . yes
N15 N16 1.372(5) . . yes
N16 C32 1.353(5) . . yes
C16 H16 0.9500 . . no
C17 H17A 0.9900 . . no
N17 C34 1.348(5) . . yes
N17 C35 1.380(6) . . yes
N17 C33 1.469(6) . . yes
C17 H17B 0.9900 . . no
N18 C36 1.380(5) . . yes
N18 C34 1.356(5) . . yes
N18 C37 1.452(5) . . yes
C19 H19 0.9500 . . no
N19 C39 1.389(5) . . yes
N19 C37 1.454(5) . . yes
N19 C38 1.352(5) . . yes
N20 C41 1.465(5) . . yes
N20 C40 1.381(5) . . yes
N20 C38 1.345(5) . . yes
N21 N22 1.368(5) . . yes
N21 C42 1.349(5) . . yes
C21 H21A 0.9900 . . no
C21 H21B 0.9900 . . no
N22 C44 1.350(5) . . yes
C23 H23 0.9500 . . no
N23 C45 1.461(5) . . yes
N23 C47 1.393(6) . . yes
N23 C46 1.353(5) . . yes
N24 C46 1.356(6) . . yes
N24 C48 1.387(5) . . yes
C24 H24 0.9500 . . no
N24 C25 1.442(5) . . yes
C27 C28 1.344(7) . . no
C29 C30 1.495(6) . . no
C30 C31 1.377(6) . . no
C31 C32 1.375(6) . . no
C32 C33 1.490(6) . . no
C35 C36 1.335(6) . . no
C39 C40 1.344(6) . . no
C41 C42 1.496(5) . . no
C42 C43 1.379(6) . . no
C43 C44 1.388(6) . . no
C44 C45 1.489(5) . . no
C47 C48 1.341(7) . . no
P1A F3A 1.598(10) . . yes
P1A F4A 1.600(11) . . yes
P1A F2A 1.595(10) . . yes
P1A F6A 1.569(10) . . yes
P1A F5A 1.574(10) . . yes
P1A F1A 1.601(11) . . yes
C25 H25A 0.9900 . . no
C25 H25B 0.9900 . . no
C27 H27 0.9500 . . no
C28 H28 0.9500 . . no
C29 H29B 0.9900 . . no
C29 H29A 0.9900 . . no
C31 H31 0.9500 . . no
C33 H33B 0.9900 . . no
C33 H33A 0.9900 . . no
C35 H35 0.9500 . . no
C36 H36 0.9500 . . no
C37 H37B 0.9900 . . no
C37 H37A 0.9900 . . no
C39 H39 0.9500 . . no
C40 H40 0.9500 . . no
C41 H41A 0.9900 . . no
C41 H41B 0.9900 . . no
C43 H43 0.9500 . . no
C45 H45B 0.9900 . . no
C45 H45A 0.9900 . . no
C47 H47 0.9500 . . no
C48 H48 0.9500 . . no
O1 C49 1.210(5) . . yes
N25 C49 1.317(6) . . yes
N25 C50 1.443(7) . . yes
N25 C51 1.448(7) . . yes
O2 C52 1.226(6) . . yes
N26 C52 1.332(5) . . yes
N26 C53 1.434(6) . . yes
N26 C54 1.467(6) . . yes
C49 H49 0.9500 . . no
C50 H50A 0.9800 . . no
C50 H50B 0.9800 . . no
C50 H50C 0.9800 . . no
C51 H51B 0.9800 . . no
C51 H51C 0.9800 . . no
C51 H51A 0.9800 . . no
C52 H52 0.9500 . . no
C53 H53A 0.9800 . . no
C53 H53B 0.9800 . . no
C53 H53C 0.9800 . . no
C54 H54A 0.9800 . . no
C54 H54B 0.9800 . . no
C54 H54C 0.9800 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 N10 94.46(13) . . . yes
N3 Ni1 C2 89.46(15) . . . yes
N3 Ni1 C22 175.13(16) . . . yes
N10 Ni1 C2 174.99(16) . . . yes
N10 Ni1 C22 89.99(15) . . . yes
C2 Ni1 C22 85.98(17) . . . yes
N4 Ni2 N9 94.99(14) . . . yes
N4 Ni2 C10 89.16(16) . . . yes
N4 Ni2 C14 175.05(16) . . . yes
N9 Ni2 C10 175.54(16) . . . yes
N9 Ni2 C14 89.12(16) . . . yes
C10 Ni2 C14 86.67(19) . . . yes
N15 Ni3 C26 89.94(15) . . . yes
N15 Ni3 C46 175.25(17) . . . yes
N22 Ni3 C26 174.59(16) . . . yes
N22 Ni3 C46 90.16(17) . . . yes
C26 Ni3 C46 85.41(19) . . . yes
N15 Ni3 N22 94.44(13) . . . yes
N16 Ni4 N21 94.98(14) . . . yes
N16 Ni4 C34 89.33(17) . . . yes
N21 Ni4 C34 175.57(16) . . . yes
N21 Ni4 C38 88.91(16) . . . yes
N16 Ni4 C38 175.24(16) . . . yes
C34 Ni4 C38 86.74(19) . . . yes
F1 P1 F5 91.0(3) . . . yes
F1 P1 F6 90.3(3) . . . yes
F1 P1 F4 89.1(3) . . . yes
F2 P1 F4 90.7(2) . . . yes
F2 P1 F5 90.0(3) . . . yes
F2 P1 F3 90.2(2) . . . yes
F3 P1 F4 89.3(3) . . . yes
F3 P1 F5 179.4(3) . . . yes
F3 P1 F6 89.9(2) . . . yes
F4 P1 F5 90.1(3) . . . yes
F4 P1 F6 179.0(3) . . . yes
F5 P1 F6 90.8(3) . . . yes
F1 P1 F2 178.9(3) . . . yes
F2 P1 F6 89.9(2) . . . yes
F1 P1 F3 88.8(3) . . . yes
F7 P2 F10 90.11(14) . . . yes
F7 P2 F8 179.57(15) . . . yes
F8 P2 F9 90.34(14) . . . yes
F8 P2 F10 89.53(14) . . . yes
F8 P2 F11 89.99(14) . . . yes
F7 P2 F9 89.40(14) . . . yes
F9 P2 F10 89.97(14) . . . yes
F9 P2 F11 179.65(15) . . . yes
F9 P2 F12 89.64(14) . . . yes
F10 P2 F11 90.15(14) . . . yes
F10 P2 F12 179.59(15) . . . yes
F11 P2 F12 90.25(14) . . . yes
F7 P2 F11 90.26(14) . . . yes
F7 P2 F12 89.78(14) . . . yes
F8 P2 F12 90.57(14) . . . yes
C1 N1 C2 122.6(3) . . . yes
C2 N1 C3 110.9(3) . . . yes
C1 N1 C3 126.5(3) . . . yes
C4 N2 C5 126.3(3) . . . yes
C2 N2 C4 111.1(3) . . . yes
C2 N2 C5 122.4(3) . . . yes
F13 P3 F16 89.11(17) . . . yes
F13 P3 F15 89.99(17) . . . yes
F14 P3 F18 90.83(17) . . . yes
F14 P3 F15 88.68(16) . . . yes
F14 P3 F16 88.89(16) . . . yes
F14 P3 F17 90.29(17) . . . yes
F13 P3 F14 177.6(2) . . . yes
Ni1 N3 N4 125.7(2) . . . yes
Ni1 N3 C6 126.4(3) . . . yes
N4 N3 C6 107.5(3) . . . yes
F13 P3 F17 91.00(18) . . . yes
F13 P3 F18 91.16(18) . . . yes
F16 P3 F18 179.62(18) . . . yes
F17 P3 F18 91.37(16) . . . yes
F15 P3 F18 89.82(16) . . . yes
F15 P3 F16 89.92(15) . . . yes
F15 P3 F17 178.44(16) . . . yes
F16 P3 F17 88.88(15) . . . yes
Ni2 N4 N3 126.3(2) . . . yes
Ni2 N4 C8 126.3(3) . . . yes
N3 N4 C8 107.3(3) . . . yes
C10 N5 C11 110.8(4) . . . yes
C9 N5 C10 122.2(3) . . . yes
C9 N5 C11 126.6(3) . . . yes
C12 N6 C13 126.0(4) . . . yes
C10 N6 C12 111.2(3) . . . yes
C10 N6 C13 122.8(3) . . . yes
C14 N7 C15 111.0(3) . . . yes
C13 N7 C14 122.9(3) . . . yes
C13 N7 C15 126.0(4) . . . yes
C14 N8 C17 123.2(3) . . . yes
C16 N8 C17 125.1(3) . . . yes
C14 N8 C16 111.7(4) . . . yes
Ni2 N9 N10 125.5(2) . . . yes
N10 N9 C18 107.5(3) . . . yes
Ni2 N9 C18 126.5(3) . . . yes
Ni1 N10 N9 126.2(2) . . . yes
Ni1 N10 C20 125.6(3) . . . yes
N9 N10 C20 107.7(3) . . . yes
C21 N11 C23 126.3(3) . . . yes
C21 N11 C22 122.3(3) . . . yes
C22 N11 C23 111.1(3) . . . yes
C22 N12 C24 111.2(3) . . . yes
C1 N12 C22 122.5(3) . . . yes
C1 N12 C24 126.3(4) . . . yes
N1 C1 N12 108.4(3) . . . yes
Ni1 C2 N1 129.1(3) . . . yes
Ni1 C2 N2 126.5(3) . . . yes
N1 C2 N2 104.4(3) . . . yes
N1 C3 C4 106.5(4) . . . yes
N2 C4 C3 107.1(4) . . . yes
N2 C5 C6 110.7(3) . . . yes
C5 C6 C7 129.1(4) . . . no
N3 C6 C5 120.6(4) . . . yes
N3 C6 C7 110.1(4) . . . yes
C6 C7 C8 104.8(4) . . . no
C7 C8 C9 128.2(4) . . . no
N4 C8 C7 110.3(3) . . . yes
N4 C8 C9 121.5(4) . . . yes
N5 C9 C8 110.6(4) . . . yes
Ni2 C10 N6 128.5(3) . . . yes
Ni2 C10 N5 127.3(3) . . . yes
N5 C10 N6 104.3(3) . . . yes
N5 C11 C12 107.1(4) . . . yes
N6 C12 C11 106.7(4) . . . yes
N6 C13 N7 108.4(4) . . . yes
Ni2 C14 N8 127.3(3) . . . yes
N7 C14 N8 104.4(3) . . . yes
Ni2 C14 N7 128.3(3) . . . yes
N7 C15 C16 106.8(4) . . . yes
N8 C16 C15 106.2(4) . . . yes
N8 C17 C18 110.2(4) . . . yes
N9 C18 C17 121.6(4) . . . yes
C17 C18 C19 128.6(4) . . . no
N9 C18 C19 109.8(4) . . . yes
C18 C19 C20 105.0(4) . . . no
N10 C20 C21 121.3(3) . . . yes
C19 C20 C21 128.7(4) . . . no
N10 C20 C19 110.0(3) . . . yes
N11 C21 C20 109.9(3) . . . yes
N11 C22 N12 104.4(3) . . . yes
Ni1 C22 N12 129.2(3) . . . yes
Ni1 C22 N11 126.3(3) . . . yes
N11 C23 C24 106.9(4) . . . yes
N12 C24 C23 106.5(4) . . . yes
N1 C1 H1B 110.00 . . . no
N12 C1 H1A 110.00 . . . no
N12 C1 H1B 110.00 . . . no
H1A C1 H1B 108.00 . . . no
N1 C1 H1A 110.00 . . . no
C4 C3 H3 127.00 . . . no
N1 C3 H3 127.00 . . . no
F20 P4 F21 91.8(2) . . . yes
F19 P4 F20 175.67(19) . . . yes
F19 P4 F21 90.8(2) . . . yes
F19 P4 F22 92.0(2) . . . yes
F19 P4 F23 89.4(2) . . . yes
F19 P4 F24 86.31(16) . . . yes
N2 C4 H4 126.00 . . . no
C3 C4 H4 127.00 . . . no
F22 P4 F23 89.4(2) . . . yes
F22 P4 F24 177.0(2) . . . yes
F23 P4 F24 88.06(19) . . . yes
F20 P4 F23 87.7(2) . . . yes
F20 P4 F24 90.35(17) . . . yes
F21 P4 F22 95.3(3) . . . yes
F21 P4 F23 175.3(2) . . . yes
F20 P4 F22 91.2(2) . . . yes
F21 P4 F24 87.2(2) . . . yes
N2 C5 H5B 110.00 . . . no
C6 C5 H5B 110.00 . . . no
N2 C5 H5A 109.00 . . . no
H5A C5 H5B 108.00 . . . no
C6 C5 H5A 110.00 . . . no
C6 C7 H7 128.00 . . . no
C8 C7 H7 128.00 . . . no
N5 C9 H9B 109.00 . . . no
C8 C9 H9A 110.00 . . . no
C8 C9 H9B 110.00 . . . no
H9A C9 H9B 108.00 . . . no
N5 C9 H9A 109.00 . . . no
N5 C11 H11 126.00 . . . no
C12 C11 H11 127.00 . . . no
C11 C12 H12 127.00 . . . no
N6 C12 H12 127.00 . . . no
N7 C13 H13A 110.00 . . . no
C26 N13 C27 111.4(4) . . . yes
H13A C13 H13B 108.00 . . . no
C25 N13 C27 126.0(4) . . . yes
N7 C13 H13B 110.00 . . . no
C25 N13 C26 122.7(3) . . . yes
N6 C13 H13A 110.00 . . . no
N6 C13 H13B 110.00 . . . no
C26 N14 C29 121.8(3) . . . yes
C26 N14 C28 110.9(3) . . . yes
C28 N14 C29 127.2(3) . . . yes
N7 C15 H15 127.00 . . . no
Ni3 N15 N16 124.9(2) . . . yes
C16 C15 H15 127.00 . . . no
N16 N15 C30 107.9(3) . . . yes
Ni3 N15 C30 125.7(3) . . . yes
C15 C16 H16 127.00 . . . no
N15 N16 C32 107.0(3) . . . yes
N8 C16 H16 127.00 . . . no
Ni4 N16 N15 126.2(2) . . . yes
Ni4 N16 C32 126.7(3) . . . yes
C33 N17 C35 126.2(3) . . . yes
C34 N17 C35 111.3(4) . . . yes
C33 N17 C34 122.4(4) . . . yes
N8 C17 H17A 110.00 . . . no
N8 C17 H17B 110.00 . . . no
C18 C17 H17A 110.00 . . . no
C18 C17 H17B 109.00 . . . no
H17A C17 H17B 108.00 . . . no
C34 N18 C37 122.8(3) . . . yes
C36 N18 C37 125.7(3) . . . yes
C34 N18 C36 111.4(3) . . . yes
C37 N19 C39 126.5(3) . . . yes
C37 N19 C38 122.3(3) . . . yes
C20 C19 H19 128.00 . . . no
C18 C19 H19 127.00 . . . no
C38 N19 C39 111.2(3) . . . yes
C38 N20 C41 122.2(3) . . . yes
C40 N20 C41 126.5(3) . . . yes
C38 N20 C40 111.3(3) . . . yes
C20 C21 H21A 110.00 . . . no
N22 N21 C42 107.6(3) . . . yes
N11 C21 H21B 110.00 . . . no
C20 C21 H21B 110.00 . . . no
H21A C21 H21B 108.00 . . . no
N11 C21 H21A 110.00 . . . no
Ni4 N21 N22 124.9(2) . . . yes
Ni4 N21 C42 126.6(3) . . . yes
Ni3 N22 C44 125.3(3) . . . yes
N21 N22 C44 108.1(3) . . . yes
Ni3 N22 N21 126.5(2) . . . yes
N11 C23 H23 126.00 . . . no
C45 N23 C47 126.6(3) . . . yes
C46 N23 C47 110.6(4) . . . yes
C24 C23 H23 127.00 . . . no
C45 N23 C46 122.5(4) . . . yes
C25 N24 C46 123.3(3) . . . yes
C46 N24 C48 111.1(3) . . . yes
C23 C24 H24 127.00 . . . no
C25 N24 C48 125.7(3) . . . yes
N12 C24 H24 127.00 . . . no
N13 C25 N24 108.0(3) . . . yes
N13 C26 N14 104.7(3) . . . yes
Ni3 C26 N13 129.3(3) . . . yes
Ni3 C26 N14 126.1(3) . . . yes
N13 C27 C28 106.1(4) . . . yes
N14 C28 C27 107.1(4) . . . yes
N14 C29 C30 109.2(3) . . . yes
N15 C30 C29 120.4(3) . . . yes
N15 C30 C31 110.1(4) . . . yes
C29 C30 C31 129.5(4) . . . no
C30 C31 C32 104.8(4) . . . no
N16 C32 C33 122.1(4) . . . yes
N16 C32 C31 110.2(3) . . . yes
C31 C32 C33 127.7(4) . . . no
N17 C33 C32 110.7(4) . . . yes
Ni4 C34 N17 128.2(3) . . . yes
Ni4 C34 N18 128.0(3) . . . yes
N17 C34 N18 103.9(3) . . . yes
N17 C35 C36 107.0(4) . . . yes
N18 C36 C35 106.4(4) . . . yes
N18 C37 N19 108.1(3) . . . yes
Ni4 C38 N19 128.4(3) . . . yes
Ni4 C38 N20 127.1(3) . . . yes
N19 C38 N20 104.5(3) . . . yes
N19 C39 C40 106.1(4) . . . yes
N20 C40 C39 106.9(4) . . . yes
N20 C41 C42 109.7(3) . . . yes
N21 C42 C41 120.2(4) . . . yes
N21 C42 C43 110.0(3) . . . yes
C41 C42 C43 129.8(4) . . . no
C42 C43 C44 105.0(4) . . . no
N22 C44 C45 121.4(4) . . . yes
C43 C44 C45 129.3(4) . . . no
N22 C44 C43 109.3(3) . . . yes
N23 C45 C44 110.0(3) . . . yes
Ni3 C46 N23 126.0(4) . . . yes
Ni3 C46 N24 129.3(3) . . . yes
N23 C46 N24 104.7(4) . . . yes
N23 C47 C48 107.1(4) . . . yes
N24 C48 C47 106.6(4) . . . yes
F1A P1A F4A 89.2(5) . . . yes
F1A P1A F3A 88.8(6) . . . yes
F1A P1A F2A 179.0(7) . . . yes
F5A P1A F6A 90.8(6) . . . yes
F2A P1A F5A 90.0(6) . . . yes
F2A P1A F6A 89.9(5) . . . yes
F3A P1A F4A 89.3(6) . . . yes
F1A P1A F5A 91.0(6) . . . yes
F1A P1A F6A 90.3(6) . . . yes
F2A P1A F3A 90.2(6) . . . yes
F2A P1A F4A 90.6(5) . . . yes
F3A P1A F5A 179.3(6) . . . yes
F3A P1A F6A 89.9(6) . . . yes
F4A P1A F5A 90.0(6) . . . yes
F4A P1A F6A 179.1(7) . . . yes
N24 C25 H25A 110.00 . . . no
N24 C25 H25B 110.00 . . . no
N13 C25 H25B 110.00 . . . no
N13 C25 H25A 110.00 . . . no
H25A C25 H25B 108.00 . . . no
N13 C27 H27 127.00 . . . no
C28 C27 H27 127.00 . . . no
C27 C28 H28 127.00 . . . no
N14 C28 H28 126.00 . . . no
N14 C29 H29A 110.00 . . . no
N14 C29 H29B 110.00 . . . no
C30 C29 H29A 110.00 . . . no
C30 C29 H29B 110.00 . . . no
H29A C29 H29B 108.00 . . . no
C32 C31 H31 128.00 . . . no
C30 C31 H31 128.00 . . . no
N17 C33 H33B 110.00 . . . no
C32 C33 H33A 110.00 . . . no
N17 C33 H33A 110.00 . . . no
C32 C33 H33B 109.00 . . . no
H33A C33 H33B 108.00 . . . no
C36 C35 H35 127.00 . . . no
N17 C35 H35 126.00 . . . no
N18 C36 H36 127.00 . . . no
C35 C36 H36 127.00 . . . no
N18 C37 H37A 110.00 . . . no
H37A C37 H37B 108.00 . . . no
N18 C37 H37B 110.00 . . . no
N19 C37 H37A 110.00 . . . no
N19 C37 H37B 110.00 . . . no
N19 C39 H39 127.00 . . . no
C40 C39 H39 127.00 . . . no
C39 C40 H40 127.00 . . . no
N20 C40 H40 126.00 . . . no
N20 C41 H41A 110.00 . . . no
N20 C41 H41B 110.00 . . . no
C42 C41 H41A 110.00 . . . no
C42 C41 H41B 110.00 . . . no
H41A C41 H41B 108.00 . . . no
C44 C43 H43 128.00 . . . no
C42 C43 H43 127.00 . . . no
N23 C45 H45A 110.00 . . . no
N23 C45 H45B 110.00 . . . no
C44 C45 H45A 110.00 . . . no
C44 C45 H45B 110.00 . . . no
H45A C45 H45B 108.00 . . . no
N23 C47 H47 127.00 . . . no
C48 C47 H47 126.00 . . . no
C47 C48 H48 127.00 . . . no
N24 C48 H48 127.00 . . . no
C49 N25 C50 120.4(4) . . . yes
C49 N25 C51 121.9(5) . . . yes
C50 N25 C51 117.7(5) . . . yes
O1 C49 N25 126.2(5) . . . yes
C52 N26 C54 120.7(4) . . . yes
C53 N26 C54 117.5(3) . . . yes
C52 N26 C53 120.7(4) . . . yes
N25 C49 H49 117.00 . . . no
O1 C49 H49 117.00 . . . no
N25 C50 H50B 109.00 . . . no
H50A C50 H50C 110.00 . . . no
N25 C50 H50C 109.00 . . . no
H50A C50 H50B 109.00 . . . no
N25 C50 H50A 110.00 . . . no
H50B C50 H50C 109.00 . . . no
N25 C51 H51C 109.00 . . . no
H51A C51 H51C 109.00 . . . no
H51B C51 H51C 109.00 . . . no
H51A C51 H51B 110.00 . . . no
N25 C51 H51A 110.00 . . . no
N25 C51 H51B 110.00 . . . no
O2 C52 N26 124.9(5) . . . yes
O2 C52 H52 118.00 . . . no
N26 C52 H52 118.00 . . . no
N26 C53 H53A 109.00 . . . no
N26 C53 H53B 109.00 . . . no
N26 C53 H53C 110.00 . . . no
H53A C53 H53B 110.00 . . . no
H53A C53 H53C 109.00 . . . no
H53B C53 H53C 109.00 . . . no
N26 C54 H54A 109.00 . . . no
N26 C54 H54B 110.00 . . . no
N26 C54 H54C 110.00 . . . no
H54A C54 H54B 109.00 . . . no
H54A C54 H54C 109.00 . . . no
H54B C54 H54C 109.00 . . . no

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
N10 Ni1 N3 N4 -40.3(3) . . . . no
N10 Ni1 N3 C6 147.8(3) . . . . no
C2 Ni1 N3 N4 142.9(3) . . . . no
C2 Ni1 N3 C6 -29.1(3) . . . . no
N3 Ni1 N10 N9 38.4(3) . . . . no
N3 Ni1 N10 C20 -151.1(3) . . . . no
C22 Ni1 N10 N9 -143.6(3) . . . . no
C22 Ni1 N10 C20 27.0(3) . . . . no
N3 Ni1 C2 N1 -151.8(4) . . . . no
N3 Ni1 C2 N2 29.5(4) . . . . no
C22 Ni1 C2 N1 29.9(4) . . . . no
C22 Ni1 C2 N2 -148.8(4) . . . . no
N10 Ni1 C22 N11 -29.5(4) . . . . no
N10 Ni1 C22 N12 154.6(4) . . . . no
C2 Ni1 C22 N11 147.5(4) . . . . no
C2 Ni1 C22 N12 -28.4(4) . . . . no
N9 Ni2 N4 N3 36.1(3) . . . . no
N9 Ni2 N4 C8 -148.8(3) . . . . no
C10 Ni2 N4 N3 -145.6(3) . . . . no
C10 Ni2 N4 C8 29.5(3) . . . . no
N4 Ni2 N9 N10 -37.8(3) . . . . no
N4 Ni2 N9 C18 151.8(3) . . . . no
C14 Ni2 N9 N10 145.0(3) . . . . no
C14 Ni2 N9 C18 -25.4(3) . . . . no
N4 Ni2 C10 N5 -27.5(3) . . . . no
N4 Ni2 C10 N6 154.0(3) . . . . no
C14 Ni2 C10 N5 149.8(3) . . . . no
C14 Ni2 C10 N6 -28.7(3) . . . . no
N9 Ni2 C14 N7 -153.5(3) . . . . no
N9 Ni2 C14 N8 28.3(3) . . . . no
C10 Ni2 C14 N7 27.9(3) . . . . no
C10 Ni2 C14 N8 -150.2(3) . . . . no
N22 Ni3 N15 C30 151.5(3) . . . . no
C26 Ni3 N15 N16 138.8(3) . . . . no
C26 Ni3 N15 C30 -25.3(3) . . . . no
N15 Ni3 N22 N21 34.7(3) . . . . no
N15 Ni3 N22 C44 -148.1(3) . . . . no
C46 Ni3 N22 N21 -146.6(3) . . . . no
C46 Ni3 N22 C44 30.7(3) . . . . no
N15 Ni3 C26 N13 -151.1(4) . . . . no
N15 Ni3 C26 N14 30.3(4) . . . . no
C46 Ni3 C26 N13 29.9(4) . . . . no
C46 Ni3 C26 N14 -148.7(4) . . . . no
N22 Ni3 C46 N23 -28.6(4) . . . . no
N22 Ni3 C46 N24 152.1(4) . . . . no
C26 Ni3 C46 N23 148.3(4) . . . . no
N22 Ni3 N15 N16 -44.4(3) . . . . no
C26 Ni3 C46 N24 -31.0(4) . . . . no
N16 Ni4 N21 N22 -41.8(3) . . . . no
N16 Ni4 N21 C42 150.9(3) . . . . no
C38 Ni4 N21 N22 140.9(3) . . . . no
C38 Ni4 N21 C42 -26.4(3) . . . . no
N16 Ni4 C34 N17 -26.4(3) . . . . no
N16 Ni4 C34 N18 153.8(3) . . . . no
C34 Ni4 N16 C32 27.5(3) . . . . no
C38 Ni4 C34 N18 -29.0(3) . . . . no
N21 Ni4 C38 N19 -151.1(3) . . . . no
N21 Ni4 C38 N20 30.4(3) . . . . no
C34 Ni4 C38 N19 29.7(3) . . . . no
C34 Ni4 C38 N20 -148.8(3) . . . . no
N21 Ni4 N16 C32 -151.5(3) . . . . no
C38 Ni4 C34 N17 150.9(4) . . . . no
N21 Ni4 N16 N15 32.1(3) . . . . no
C34 Ni4 N16 N15 -149.0(3) . . . . no
C1 N1 C2 Ni1 0.1(6) . . . . no
C2 N1 C1 N12 -40.3(5) . . . . no
C3 N1 C1 N12 139.3(4) . . . . no
C3 N1 C2 N2 -0.6(4) . . . . no
C1 N1 C2 N2 179.0(3) . . . . no
C3 N1 C2 Ni1 -179.5(3) . . . . no
C1 N1 C3 C4 -179.0(4) . . . . no
C2 N1 C3 C4 0.6(5) . . . . no
C5 N2 C4 C3 176.5(4) . . . . no
C4 N2 C2 Ni1 179.3(3) . . . . no
C4 N2 C2 N1 0.4(4) . . . . no
C5 N2 C2 Ni1 2.7(6) . . . . no
C5 N2 C2 N1 -176.3(3) . . . . no
C2 N2 C5 C6 -44.1(5) . . . . no
C4 N2 C5 C6 139.8(4) . . . . no
C2 N2 C4 C3 0.0(5) . . . . no
Ni1 N3 N4 C8 -172.5(3) . . . . no
C6 N3 N4 Ni2 176.5(3) . . . . no
C6 N3 N4 C8 0.7(4) . . . . no
Ni1 N3 C6 C5 -3.2(5) . . . . no
Ni1 N3 C6 C7 173.2(3) . . . . no
N4 N3 C6 C5 -176.3(3) . . . . no
Ni1 N3 N4 Ni2 3.4(4) . . . . no
N4 N3 C6 C7 0.1(4) . . . . no
Ni2 N4 C8 C9 0.6(5) . . . . no
N3 N4 C8 C7 -1.2(4) . . . . no
Ni2 N4 C8 C7 -177.0(3) . . . . no
N3 N4 C8 C9 176.5(4) . . . . no
C10 N5 C9 C8 44.6(5) . . . . no
C11 N5 C9 C8 -143.4(4) . . . . no
C9 N5 C10 N6 173.3(4) . . . . no
C11 N5 C10 Ni2 -178.6(3) . . . . no
C11 N5 C10 N6 0.1(4) . . . . no
C9 N5 C11 C12 -172.6(4) . . . . no
C10 N5 C11 C12 0.2(5) . . . . no
C9 N5 C10 Ni2 -5.4(5) . . . . no
C12 N6 C10 Ni2 178.3(3) . . . . no
C12 N6 C10 N5 -0.4(4) . . . . no
C13 N6 C10 N5 179.1(4) . . . . no
C10 N6 C12 C11 0.6(5) . . . . no
C13 N6 C12 C11 -179.0(4) . . . . no
C10 N6 C13 N7 41.8(5) . . . . no
C12 N6 C13 N7 -138.7(4) . . . . no
C13 N6 C10 Ni2 -2.1(6) . . . . no
C14 N7 C13 N6 -42.6(5) . . . . no
C15 N7 C13 N6 140.6(4) . . . . no
C13 N7 C14 Ni2 3.9(6) . . . . no
C13 N7 C14 N8 -177.6(4) . . . . no
C15 N7 C14 Ni2 -178.9(3) . . . . no
C15 N7 C14 N8 -0.4(4) . . . . no
C13 N7 C15 C16 178.0(4) . . . . no
C14 N7 C15 C16 0.8(5) . . . . no
C16 N8 C14 Ni2 178.3(3) . . . . no
C16 N8 C14 N7 -0.2(4) . . . . no
C17 N8 C14 Ni2 1.7(6) . . . . no
C17 N8 C14 N7 -176.8(4) . . . . no
C14 N8 C16 C15 0.7(5) . . . . no
C17 N8 C16 C15 177.2(4) . . . . no
C14 N8 C17 C18 -42.2(5) . . . . no
C16 N8 C17 C18 141.7(4) . . . . no
Ni2 N9 N10 Ni1 0.3(4) . . . . no
Ni2 N9 N10 C20 -171.7(3) . . . . no
C18 N9 N10 Ni1 172.2(3) . . . . no
C18 N9 N10 C20 0.2(4) . . . . no
Ni2 N9 C18 C17 -6.8(5) . . . . no
Ni2 N9 C18 C19 171.8(3) . . . . no
N10 N9 C18 C17 -178.6(4) . . . . no
N10 N9 C18 C19 0.0(4) . . . . no
Ni1 N10 C20 C19 -172.4(3) . . . . no
Ni1 N10 C20 C21 7.1(5) . . . . no
N9 N10 C20 C19 -0.4(4) . . . . no
N9 N10 C20 C21 179.1(3) . . . . no
C22 N11 C21 C20 44.6(5) . . . . no
C23 N11 C21 C20 -142.5(4) . . . . no
C21 N11 C22 Ni1 -2.3(5) . . . . no
C21 N11 C22 N12 174.4(3) . . . . no
C23 N11 C22 N12 0.5(4) . . . . no
C21 N11 C23 C24 -174.2(4) . . . . no
C22 N11 C23 C24 -0.6(5) . . . . no
C23 N11 C22 Ni1 -176.2(3) . . . . no
C24 N12 C1 N1 -137.8(4) . . . . no
C1 N12 C22 Ni1 -3.4(6) . . . . no
C22 N12 C1 N1 41.9(5) . . . . no
C24 N12 C22 Ni1 176.3(3) . . . . no
C24 N12 C22 N11 -0.2(4) . . . . no
C1 N12 C22 N11 -179.9(3) . . . . no
C22 N12 C24 C23 -0.1(5) . . . . no
C1 N12 C24 C23 179.6(4) . . . . no
N1 C3 C4 N2 -0.3(5) . . . . no
N2 C5 C6 N3 43.6(5) . . . . no
N2 C5 C6 C7 -132.0(4) . . . . no
N3 C6 C7 C8 -0.8(4) . . . . no
C5 C6 C7 C8 175.2(4) . . . . no
C6 C7 C8 C9 -176.3(4) . . . . no
C6 C7 C8 N4 1.2(4) . . . . no
C7 C8 C9 N5 135.6(4) . . . . no
N4 C8 C9 N5 -41.7(5) . . . . no
N5 C11 C12 N6 -0.4(5) . . . . no
N7 C15 C16 N8 -0.9(5) . . . . no
N8 C17 C18 N9 44.2(5) . . . . no
N8 C17 C18 C19 -134.2(4) . . . . no
C17 C18 C19 C20 178.3(4) . . . . no
N9 C18 C19 C20 -0.3(5) . . . . no
C18 C19 C20 N10 0.4(5) . . . . no
C18 C19 C20 C21 -179.0(4) . . . . no
C19 C20 C21 N11 132.8(4) . . . . no
N10 C20 C21 N11 -46.5(5) . . . . no
N11 C23 C24 N12 0.4(5) . . . . no
C26 N13 C25 N24 -40.1(5) . . . . no
C27 N13 C25 N24 140.2(4) . . . . no
C25 N13 C26 Ni3 1.2(6) . . . . no
C25 N13 C26 N14 -180.0(3) . . . . no
C27 N13 C26 Ni3 -179.1(3) . . . . no
C27 N13 C26 N14 -0.2(4) . . . . no
C25 N13 C27 C28 -179.7(4) . . . . no
C26 N13 C27 C28 0.6(5) . . . . no
C28 N14 C26 Ni3 178.7(3) . . . . no
C28 N14 C26 N13 -0.2(4) . . . . no
C29 N14 C26 Ni3 1.7(5) . . . . no
C29 N14 C26 N13 -177.2(3) . . . . no
C26 N14 C28 C27 0.6(5) . . . . no
C29 N14 C28 C27 177.4(4) . . . . no
C26 N14 C29 C30 -46.1(5) . . . . no
C28 N14 C29 C30 137.4(4) . . . . no
Ni3 N15 N16 Ni4 11.0(4) . . . . no
Ni3 N15 N16 C32 -166.0(3) . . . . no
C30 N15 N16 Ni4 177.5(3) . . . . no
C30 N15 N16 C32 0.5(4) . . . . no
Ni3 N15 C30 C29 -11.1(5) . . . . no
Ni3 N15 C30 C31 166.1(3) . . . . no
N16 N15 C30 C29 -177.4(3) . . . . no
N16 N15 C30 C31 -0.2(4) . . . . no
Ni4 N16 C32 C31 -177.5(3) . . . . no
Ni4 N16 C32 C33 1.6(5) . . . . no
N15 N16 C32 C31 -0.5(4) . . . . no
N15 N16 C32 C33 178.6(4) . . . . no
C34 N17 C33 C32 41.9(5) . . . . no
C35 N17 C33 C32 -143.4(4) . . . . no
C33 N17 C34 Ni4 -4.6(6) . . . . no
C33 N17 C34 N18 175.3(4) . . . . no
C35 N17 C34 Ni4 -180.0(3) . . . . no
C35 N17 C34 N18 -0.1(4) . . . . no
C33 N17 C35 C36 -175.3(4) . . . . no
C34 N17 C35 C36 -0.1(5) . . . . no
C36 N18 C34 Ni4 -179.8(3) . . . . no
C36 N18 C34 N17 0.3(4) . . . . no
C37 N18 C34 Ni4 -3.4(6) . . . . no
C37 N18 C34 N17 176.7(4) . . . . no
C34 N18 C36 C35 -0.4(5) . . . . no
C37 N18 C36 C35 -176.7(4) . . . . no
C34 N18 C37 N19 43.4(5) . . . . no
C36 N18 C37 N19 -140.7(4) . . . . no
C38 N19 C37 N18 -42.6(5) . . . . no
C39 N19 C37 N18 138.2(4) . . . . no
C37 N19 C38 Ni4 2.1(6) . . . . no
C37 N19 C38 N20 -179.2(4) . . . . no
C39 N19 C38 Ni4 -178.6(3) . . . . no
C39 N19 C38 N20 0.1(4) . . . . no
C37 N19 C39 C40 179.3(4) . . . . no
C38 N19 C39 C40 0.1(5) . . . . no
C40 N20 C38 Ni4 178.5(3) . . . . no
C40 N20 C38 N19 -0.3(4) . . . . no
C41 N20 C38 Ni4 1.0(5) . . . . no
C41 N20 C38 N19 -177.8(3) . . . . no
C38 N20 C40 C39 0.3(5) . . . . no
C41 N20 C40 C39 177.7(4) . . . . no
C38 N20 C41 C42 -44.6(5) . . . . no
C40 N20 C41 C42 138.3(4) . . . . no
Ni4 N21 N22 Ni3 7.7(4) . . . . no
Ni4 N21 N22 C44 -169.9(3) . . . . no
C42 N21 N22 Ni3 177.0(3) . . . . no
C42 N21 N22 C44 -0.6(4) . . . . no
Ni4 N21 C42 C41 -8.3(5) . . . . no
Ni4 N21 C42 C43 169.8(3) . . . . no
N22 N21 C42 C41 -177.4(3) . . . . no
N22 N21 C42 C43 0.8(4) . . . . no
Ni3 N22 C44 C43 -177.5(3) . . . . no
Ni3 N22 C44 C45 1.0(5) . . . . no
N21 N22 C44 C43 0.2(4) . . . . no
N21 N22 C44 C45 178.7(3) . . . . no
C46 N23 C45 C44 46.0(5) . . . . no
C47 N23 C45 C44 -141.0(4) . . . . no
C45 N23 C46 Ni3 -5.6(6) . . . . no
C45 N23 C46 N24 173.9(3) . . . . no
C47 N23 C46 Ni3 -179.6(3) . . . . no
C47 N23 C46 N24 -0.2(4) . . . . no
C45 N23 C47 C48 -173.8(4) . . . . no
C46 N23 C47 C48 -0.1(5) . . . . no
C46 N24 C25 N13 39.3(5) . . . . no
C48 N24 C25 N13 -139.6(4) . . . . no
C25 N24 C46 Ni3 0.8(6) . . . . no
C25 N24 C46 N23 -178.6(3) . . . . no
C48 N24 C46 Ni3 179.8(3) . . . . no
C48 N24 C46 N23 0.4(4) . . . . no
C25 N24 C48 C47 178.5(4) . . . . no
C46 N24 C48 C47 -0.5(5) . . . . no
N13 C27 C28 N14 -0.7(4) . . . . no
N14 C29 C30 N15 50.5(5) . . . . no
N14 C29 C30 C31 -126.1(4) . . . . no
N15 C30 C31 C32 -0.1(4) . . . . no
C29 C30 C31 C32 176.8(4) . . . . no
C30 C31 C32 N16 0.4(4) . . . . no
C30 C31 C32 C33 -178.7(4) . . . . no
N16 C32 C33 N17 -40.0(5) . . . . no
C31 C32 C33 N17 139.0(4) . . . . no
N17 C35 C36 N18 0.3(5) . . . . no
N19 C39 C40 N20 -0.2(5) . . . . no
N20 C41 C42 N21 47.6(5) . . . . no
N20 C41 C42 C43 -130.2(4) . . . . no
N21 C42 C43 C44 -0.6(4) . . . . no
C41 C42 C43 C44 177.3(4) . . . . no
C42 C43 C44 N22 0.2(4) . . . . no
C42 C43 C44 C45 -178.1(4) . . . . no
N22 C44 C45 N23 -42.9(5) . . . . no
C43 C44 C45 N23 135.2(4) . . . . no
N23 C47 C48 N24 0.3(5) . . . . no
C50 N25 C49 O1 0.8(8) . . . . no
C51 N25 C49 O1 -175.8(5) . . . . no
C53 N26 C52 O2 -2.7(7) . . . . no
C54 N26 C52 O2 -170.4(5) . . . . no


# Loop Mechanism for Extra Tables(s)

#loop_
#_publ_manuscript_incl_extra_item
#'_geom_extra_tableA_col_1'
#'_geom_extra_tableA_col_2'
#'_geom_extra_tableA_col_3'
#'_geom_extra_table_head_A'
#'_geom_table_footnote_A'
#'_geom_extra_tableB_col_1'
#'_geom_extra_tableB_col_2'
#'_geom_extra_tableB_col_3'
#'_geom_extra_table_head_B'
#'_geom_table_footnote_B'


#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
# ? ? ?


#
#loop_
#_geom_extra_tableB_col_1
#_geom_extra_tableB_col_2
#_geom_extra_tableB_col_3
# ? ? ?


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;


#===END
