#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/98/4119847.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4119847
loop_
_publ_author_name
'Cheng-Pan Zhang'
'Huan Wang'
'Axel Klein'
'Christian Biewer'
'Kathrin Stirnat'
'Yoshitaka Yamaguchi'
'Long Xu'
'Valente Gomez-Benitez'
'David A. Vicic'
_publ_section_title
;
 A Five-Coordinate Nickel(II) Fluoroalkyl Complex as a Precursor to a
 Spectroscopically Detectable Ni(III) Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8141
_journal_page_last               8144
_journal_paper_doi               10.1021/ja4030462
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C30 H35 F9 N3 Ni O0.5 P'
_chemical_formula_weight         706.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.893(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6900(12)
_cell_length_b                   15.1528(12)
_cell_length_c                   33.412(2)
_cell_measurement_temperature    100(2)
_cell_volume                     6409.9(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.830
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16149
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.8978
_exptl_absorpt_correction_T_min  0.7883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.493
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         11666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1796
_refine_ls_R_factor_gt           0.1136
_refine_ls_shift/su_max          1.495
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1771P)²+16.7963P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3057
_refine_ls_wR_factor_ref         0.3392
_reflns_number_gt                6901
_reflns_number_total             11666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4030462_si_002_5.cif
_cod_data_source_block           Complex_14
_cod_original_cell_volume        6410.0(9)
_cod_original_formula_sum        'C30 H35 F9 N3 Ni O0.50 P'
_cod_database_code               4119847
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni2 Ni 0.56047(7) 0.07274(5) 1.06849(3) 0.0450(3) Uani 1 1 d .
Ni1 Ni 0.70023(10) 0.27107(6) 0.67664(4) 0.0608(4) Uani 1 1 d .
P1 P 0.2599(2) 0.30185(15) 0.24917(8) 0.0653(7) Uani 1 1 d .
P2 P 1.0000 0.0000 0.0000 0.0868(14) Uani 1 2 d S
P3 P 0.5000 0.5000 1.0000 0.0779(12) Uani 1 2 d S
N1 N 0.5723(8) 0.2459(4) 0.6430(2) 0.070(3) Uani 1 1 d .
N2 N 0.6102(5) 0.3475(4) 0.7015(2) 0.0499(17) Uani 1 1 d .
N3 N 0.7980(5) 0.3097(4) 0.7208(2) 0.0586(19) Uani 1 1 d .
N4 N 0.4643(5) 0.1164(4) 1.0250(2) 0.0476(16) Uani 1 1 d .
N5 N 0.6534(5) 0.1498(4) 1.0454(2) 0.0438(15) Uani 1 1 d .
N6 N 0.6873(5) 0.0469(4) 1.10330(19) 0.0448(15) Uani 1 1 d .
F1 F 0.8233(7) 0.1242(4) 0.6754(3) 0.157(4) Uani 1 1 d .
F2 F 0.7718(8) 0.1597(8) 0.6167(4) 0.199(6) Uani 1 1 d .
F3 F 0.8907(6) 0.2342(4) 0.6459(2) 0.110(3) Uani 1 1 d .
F4 F 0.4829(5) -0.0363(5) 1.1301(2) 0.104(2) Uani 1 1 d .
F5 F 0.4270(5) -0.0694(3) 1.0684(2) 0.0853(19) Uani 1 1 d .
F6 F 0.3664(4) 0.0434(3) 1.09901(18) 0.0743(16) Uani 1 1 d .
F7 F 0.3730(6) 0.2582(5) 0.2481(3) 0.120(3) Uani 1 1 d .
F8 F 0.2813(4) 0.3625(3) 0.21172(17) 0.0710(14) Uani 1 1 d .
F9 F 0.1439(7) 0.3422(6) 0.2497(3) 0.147(4) Uani 1 1 d .
F10 F 0.2152(5) 0.2243(3) 0.22134(18) 0.0801(17) Uani 1 1 d .
F11 F 0.3132(6) 0.3751(5) 0.2788(2) 0.110(2) Uani 1 1 d .
F12 F 0.2252(10) 0.2551(7) 0.2863(2) 0.172(5) Uani 1 1 d .
F13 F 1.0297(6) 0.0821(4) 0.0291(2) 0.099(2) Uani 1 1 d .
F14 F 0.9833(9) -0.0612(5) 0.0367(2) 0.149(4) Uani 1 1 d .
F15 F 0.8798(7) 0.0268(5) 0.0007(3) 0.134(3) Uani 1 1 d .
F16 F 0.5836(6) 0.4542(5) 1.0311(2) 0.109(2) Uani 1 1 d .
F17 F 0.4172(8) 0.4403(5) 1.0100(2) 0.140(4) Uani 1 1 d .
F18 F 0.5317(6) 0.4428(5) 0.9634(2) 0.103(2) Uani 1 1 d .
C1 C 0.7993(10) 0.1981(6) 0.6516(4) 0.090(4) Uani 1 1 d .
C2 C 0.4585(7) 0.0010(5) 1.0927(3) 0.060(2) Uani 1 1 d .
C3 C 0.5568(11) 0.1876(6) 0.6144(3) 0.074(3) Uani 1 1 d .
H3A H 0.6160 0.1574 0.6051 0.089 Uiso 1 1 calc R
C4 C 0.4596(13) 0.1687(5) 0.5974(3) 0.086(4) Uani 1 1 d .
H4A H 0.4545 0.1281 0.5757 0.103 Uiso 1 1 calc R
C5 C 0.3627(9) 0.2064(5) 0.6104(3) 0.066(3) Uani 1 1 d .
C6 C 0.3845(8) 0.2702(4) 0.6411(2) 0.055(2) Uani 1 1 d .
H6A H 0.3274 0.3009 0.6517 0.066 Uiso 1 1 calc R
C7 C 0.4838(8) 0.2882(4) 0.6556(3) 0.053(2) Uani 1 1 d .
C8 C 0.2529(11) 0.1812(6) 0.5943(3) 0.081(4) Uani 1 1 d .
C9 C 0.2489(14) 0.1941(14) 0.5503(4) 0.158(8) Uani 1 1 d .
H9A H 0.2252 0.2542 0.5438 0.238 Uiso 1 1 calc R
H9B H 0.1994 0.1516 0.5373 0.238 Uiso 1 1 calc R
H9C H 0.3194 0.1848 0.5408 0.238 Uiso 1 1 calc R
C10 C 0.2533(14) 0.0787(8) 0.6030(6) 0.153(8) Uani 1 1 d .
H10A H 0.2882 0.0674 0.6296 0.230 Uiso 1 1 calc R
H10B H 0.2916 0.0481 0.5826 0.230 Uiso 1 1 calc R
H10C H 0.1805 0.0570 0.6022 0.230 Uiso 1 1 calc R
C11 C 0.1729(10) 0.2227(9) 0.6160(4) 0.099(4) Uani 1 1 d .
H11A H 0.1873 0.2861 0.6182 0.149 Uiso 1 1 calc R
H11B H 0.1729 0.1969 0.6429 0.149 Uiso 1 1 calc R
H11C H 0.1038 0.2134 0.6017 0.149 Uiso 1 1 calc R
C12 C 0.5086(7) 0.3510(4) 0.6884(3) 0.051(2) Uani 1 1 d .
C13 C 0.4388(6) 0.4059(5) 0.7065(3) 0.056(2) Uani 1 1 d .
H13A H 0.3666 0.4076 0.6969 0.068 Uiso 1 1 calc R
C14 C 0.4753(6) 0.4596(5) 0.7393(3) 0.059(2) Uani 1 1 d .
C15 C 0.5834(6) 0.4553(5) 0.7512(3) 0.054(2) Uani 1 1 d .
H15A H 0.6121 0.4919 0.7723 0.065 Uiso 1 1 calc R
C16 C 0.6476(6) 0.3978(4) 0.7323(3) 0.050(2) Uani 1 1 d .
C17 C 0.4007(7) 0.5176(6) 0.7615(4) 0.076(3) Uani 1 1 d .
C18 C 0.2895(8) 0.5120(8) 0.7453(4) 0.096(4) Uani 1 1 d .
H18A H 0.2823 0.5400 0.7188 0.144 Uiso 1 1 calc R
H18B H 0.2440 0.5424 0.7635 0.144 Uiso 1 1 calc R
H18C H 0.2685 0.4499 0.7429 0.144 Uiso 1 1 calc R
C19 C 0.4440(8) 0.6044(8) 0.7693(5) 0.131(7) Uani 1 1 d .
H19A H 0.4775 0.6257 0.7456 0.197 Uiso 1 1 calc R
H19B H 0.4968 0.6016 0.7921 0.197 Uiso 1 1 calc R
H19C H 0.3873 0.6449 0.7757 0.197 Uiso 1 1 calc R
C20 C 0.3993(12) 0.4792(12) 0.8077(4) 0.134(6) Uani 1 1 d .
H20A H 0.3438 0.5091 0.8216 0.201 Uiso 1 1 calc R
H20B H 0.4680 0.4900 0.8221 0.201 Uiso 1 1 calc R
H20C H 0.3852 0.4156 0.8068 0.201 Uiso 1 1 calc R
C21 C 0.7606(7) 0.3752(5) 0.7440(3) 0.060(3) Uani 1 1 d .
C22 C 0.8174(7) 0.4132(5) 0.7764(3) 0.060(2) Uani 1 1 d .
H22A H 0.7872 0.4602 0.7905 0.072 Uiso 1 1 calc R
C23 C 0.9207(7) 0.3825(6) 0.7888(4) 0.077(3) Uani 1 1 d .
C24 C 0.9557(9) 0.3130(8) 0.7652(4) 0.089(4) Uani 1 1 d .
H24A H 1.0233 0.2882 0.7720 0.107 Uiso 1 1 calc R
C25 C 0.8974(9) 0.2799(6) 0.7332(4) 0.083(4) Uani 1 1 d .
H25A H 0.9268 0.2333 0.7185 0.100 Uiso 1 1 calc R
C26 C 0.9840(7) 0.4229(7) 0.8247(4) 0.081(3) Uani 1 1 d .
C27 C 0.9665(10) 0.5220(8) 0.8271(5) 0.110(5) Uani 1 1 d .
H27A H 1.0006 0.5512 0.8053 0.165 Uiso 1 1 calc R
H27B H 0.9971 0.5440 0.8529 0.165 Uiso 1 1 calc R
H27C H 0.8906 0.5345 0.8248 0.165 Uiso 1 1 calc R
C28 C 0.9410(11) 0.3871(10) 0.8636(4) 0.113(5) Uani 1 1 d .
H28A H 0.9445 0.3225 0.8636 0.170 Uiso 1 1 calc R
H28B H 0.8675 0.4058 0.8651 0.170 Uiso 1 1 calc R
H28C H 0.9837 0.4101 0.8868 0.170 Uiso 1 1 calc R
C29 C 1.1011(9) 0.4049(10) 0.8264(5) 0.115(5) Uani 1 1 d .
H29A H 1.1295 0.4240 0.8012 0.173 Uiso 1 1 calc R
H29B H 1.1137 0.3415 0.8302 0.173 Uiso 1 1 calc R
H29C H 1.1363 0.4375 0.8488 0.173 Uiso 1 1 calc R
C30 C 0.3657(8) 0.0884(5) 1.0130(3) 0.062(2) Uani 1 1 d .
H30A H 0.3366 0.0401 1.0266 0.075 Uiso 1 1 calc R
C31 C 0.3066(7) 0.1271(6) 0.9821(3) 0.060(2) Uani 1 1 d .
H31A H 0.2391 0.1032 0.9743 0.073 Uiso 1 1 calc R
C32 C 0.3414(7) 0.1999(5) 0.9616(3) 0.055(2) Uani 1 1 d .
C33 C 0.4469(6) 0.2287(5) 0.9742(3) 0.0500(19) Uani 1 1 d .
H33A H 0.4767 0.2781 0.9616 0.060 Uiso 1 1 calc R
C34 C 0.5036(6) 0.1853(5) 1.0041(3) 0.0466(19) Uani 1 1 d .
C35 C 0.2778(7) 0.2498(6) 0.9286(3) 0.063(2) Uani 1 1 d .
C36 C 0.1689(8) 0.2065(7) 0.9201(3) 0.076(3) Uani 1 1 d .
H36A H 0.1299 0.2081 0.9445 0.114 Uiso 1 1 calc R
H36B H 0.1781 0.1451 0.9119 0.114 Uiso 1 1 calc R
H36C H 0.1292 0.2388 0.8986 0.114 Uiso 1 1 calc R
C37 C 0.2628(9) 0.3465(6) 0.9410(4) 0.082(3) Uani 1 1 d .
H37A H 0.2190 0.3489 0.9640 0.124 Uiso 1 1 calc R
H37B H 0.2280 0.3791 0.9185 0.124 Uiso 1 1 calc R
H37C H 0.3318 0.3730 0.9483 0.124 Uiso 1 1 calc R
C38 C 0.3400(9) 0.2447(8) 0.8896(3) 0.083(3) Uani 1 1 d .
H38A H 0.3702 0.1855 0.8872 0.124 Uiso 1 1 calc R
H38B H 0.3969 0.2885 0.8911 0.124 Uiso 1 1 calc R
H38C H 0.2916 0.2568 0.8661 0.124 Uiso 1 1 calc R
C39 C 0.6166(6) 0.2052(5) 1.0158(3) 0.0455(18) Uani 1 1 d .
C40 C 0.6806(6) 0.2687(5) 1.0008(3) 0.052(2) Uani 1 1 d .
H40A H 0.6524 0.3089 0.9810 0.063 Uiso 1 1 calc R
C41 C 0.7867(7) 0.2741(6) 1.0145(3) 0.063(3) Uani 1 1 d .
C42 C 0.8244(6) 0.2132(6) 1.0440(3) 0.058(2) Uani 1 1 d .
H42A H 0.8965 0.2142 1.0537 0.070 Uiso 1 1 calc R
C43 C 0.7552(6) 0.1517(5) 1.0588(3) 0.0461(18) Uani 1 1 d .
C44 C 0.8622(7) 0.3465(7) 1.0006(3) 0.073(3) Uani 1 1 d .
C45 C 0.8093(8) 0.4118(8) 0.9722(4) 0.098(4) Uani 1 1 d .
H45A H 0.7810 0.3812 0.9480 0.147 Uiso 1 1 calc R
H45B H 0.8607 0.4563 0.9650 0.147 Uiso 1 1 calc R
H45C H 0.7515 0.4407 0.9852 0.147 Uiso 1 1 calc R
C46 C 0.9062(10) 0.4025(9) 1.0375(4) 0.109(5) Uani 1 1 d .
H46A H 0.9551 0.4473 1.0285 0.163 Uiso 1 1 calc R
H46B H 0.9434 0.3638 1.0572 0.163 Uiso 1 1 calc R
H46C H 0.8474 0.4316 1.0498 0.163 Uiso 1 1 calc R
C47 C 0.9591(9) 0.3034(9) 0.9840(5) 0.118(5) Uani 1 1 d .
H47A H 0.9366 0.2655 0.9612 0.177 Uiso 1 1 calc R
H47B H 0.9961 0.2678 1.0050 0.177 Uiso 1 1 calc R
H47C H 1.0066 0.3493 0.9751 0.177 Uiso 1 1 calc R
C48 C 0.7764(6) 0.0870(4) 1.0904(3) 0.0463(19) Uani 1 1 d .
C49 C 0.8780(6) 0.0702(4) 1.1076(2) 0.0446(18) Uani 1 1 d .
H49A H 0.9372 0.0988 1.0975 0.054 Uiso 1 1 calc R
C50 C 0.8926(7) 0.0114(4) 1.1398(3) 0.0483(19) Uani 1 1 d .
C51 C 0.8013(8) -0.0247(5) 1.1536(3) 0.057(2) Uani 1 1 d .
H51A H 0.8067 -0.0630 1.1761 0.068 Uiso 1 1 calc R
C52 C 0.7026(7) -0.0064(5) 1.1354(2) 0.0482(19) Uani 1 1 d .
H52A H 0.6427 -0.0328 1.1460 0.058 Uiso 1 1 calc R
C53 C 1.0030(7) -0.0122(5) 1.1579(2) 0.051(2) Uani 1 1 d .
C54 C 1.0802(11) 0.0488(13) 1.1499(7) 0.205(13) Uani 1 1 d .
H54A H 1.0502 0.0932 1.1310 0.307 Uiso 1 1 calc R
H54B H 1.1389 0.0187 1.1380 0.307 Uiso 1 1 calc R
H54C H 1.1060 0.0778 1.1749 0.307 Uiso 1 1 calc R
C55 C 1.0000(15) -0.0145(19) 1.2020(5) 0.229(14) Uani 1 1 d .
H55A H 1.0638 0.0136 1.2143 0.343 Uiso 1 1 calc R
H55B H 0.9968 -0.0759 1.2110 0.343 Uiso 1 1 calc R
H55C H 0.9375 0.0174 1.2099 0.343 Uiso 1 1 calc R
C56 C 1.0324(17) -0.0937(18) 1.1416(9) 0.34(3) Uani 1 1 d .
H56A H 1.0494 -0.0852 1.1137 0.511 Uiso 1 1 calc R
H56B H 0.9738 -0.1356 1.1426 0.511 Uiso 1 1 calc R
H56C H 1.0945 -0.1169 1.1572 0.511 Uiso 1 1 calc R
O1 O 0.625(2) 0.3543(16) 0.8585(8) 0.290(10) Uiso 1 1 d .
C73 C 0.6307(18) 0.3067(15) 0.9004(7) 0.169(8) Uiso 1 1 d .
C70 C 0.597(2) 0.2694(16) 0.8289(8) 0.184(9) Uiso 1 1 d .
C72 C 0.706(2) 0.2317(16) 0.8897(8) 0.188(9) Uiso 1 1 d .
C71 C 0.6829(18) 0.2099(13) 0.8443(7) 0.158(7) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N5 Ni2 C2 175.8(3) . .
N5 Ni2 N4 82.0(3) . .
C2 Ni2 N4 95.8(3) . .
N5 Ni2 N6 81.6(3) . .
C2 Ni2 N6 100.8(3) . .
N4 Ni2 N6 163.3(3) . .
N2 Ni1 C1 176.5(4) . .
N2 Ni1 N1 82.3(3) . .
C1 Ni1 N1 100.4(5) . .
N2 Ni1 N3 81.6(3) . .
C1 Ni1 N3 95.8(5) . .
N1 Ni1 N3 163.1(3) . .
F12 P1 F10 91.3(4) . .
F12 P1 F7 97.9(7) . .
F10 P1 F7 88.0(4) . .
F12 P1 F8 170.4(6) . .
F10 P1 F8 92.3(3) . .
F7 P1 F8 91.1(4) . .
F12 P1 F9 81.4(7) . .
F10 P1 F9 89.8(4) . .
F7 P1 F9 177.7(5) . .
F8 P1 F9 89.7(4) . .
F12 P1 F11 87.2(4) . .
F10 P1 F11 175.1(5) . .
F7 P1 F11 87.6(4) . .
F8 P1 F11 89.9(3) . .
F9 P1 F11 94.6(5) . .
F14 P2 F14 180.0(4) 3_755 .
F14 P2 F15 92.4(5) 3_755 .
F14 P2 F15 87.6(5) . .
F14 P2 F15 87.6(5) 3_755 3_755
F14 P2 F15 92.4(5) . 3_755
F15 P2 F15 180.0 . 3_755
F14 P2 F13 91.3(4) 3_755 3_755
F14 P2 F13 88.7(4) . 3_755
F15 P2 F13 91.2(4) . 3_755
F15 P2 F13 88.8(4) 3_755 3_755
F14 P2 F13 88.7(4) 3_755 .
F14 P2 F13 91.3(4) . .
F15 P2 F13 88.8(4) . .
F15 P2 F13 91.2(4) 3_755 .
F13 P2 F13 179.998(1) 3_755 .
F17 P3 F17 179.996(2) . 3_667
F17 P3 F18 86.3(5) . 3_667
F17 P3 F18 93.7(5) 3_667 3_667
F17 P3 F18 93.7(5) . .
F17 P3 F18 86.3(5) 3_667 .
F18 P3 F18 179.999(4) 3_667 .
F17 P3 F16 92.2(5) . .
F17 P3 F16 87.8(5) 3_667 .
F18 P3 F16 85.8(4) 3_667 .
F18 P3 F16 94.2(4) . .
F17 P3 F16 87.8(5) . 3_667
F17 P3 F16 92.2(5) 3_667 3_667
F18 P3 F16 94.2(4) 3_667 3_667
F18 P3 F16 85.8(4) . 3_667
F16 P3 F16 180.0(4) . 3_667
C3 N1 C7 116.7(10) . .
C3 N1 Ni1 129.3(8) . .
C7 N1 Ni1 113.4(6) . .
C12 N2 C16 121.0(6) . .
C12 N2 Ni1 119.1(6) . .
C16 N2 Ni1 119.9(5) . .
C21 N3 C25 114.5(9) . .
C21 N3 Ni1 114.8(6) . .
C25 N3 Ni1 130.7(7) . .
C30 N4 C34 116.6(7) . .
C30 N4 Ni2 129.2(6) . .
C34 N4 Ni2 114.1(5) . .
C43 N5 C39 120.5(6) . .
C43 N5 Ni2 119.9(5) . .
C39 N5 Ni2 119.6(5) . .
C52 N6 C48 115.8(7) . .
C52 N6 Ni2 131.4(5) . .
C48 N6 Ni2 112.6(5) . .
F3 C1 F2 103.8(9) . .
F3 C1 F1 104.8(10) . .
F2 C1 F1 100.7(10) . .
F3 C1 Ni1 115.9(7) . .
F2 C1 Ni1 119.8(10) . .
F1 C1 Ni1 109.8(7) . .
F6 C2 F5 103.8(7) . .
F6 C2 F4 101.1(7) . .
F5 C2 F4 104.6(7) . .
F6 C2 Ni2 114.2(5) . .
F5 C2 Ni2 111.6(6) . .
F4 C2 Ni2 119.8(6) . .
N1 C3 C4 122.5(10) . .
N1 C3 H3A 118.8 . .
C4 C3 H3A 118.8 . .
C3 C4 C5 124.1(9) . .
C3 C4 H4A 117.9 . .
C5 C4 H4A 117.9 . .
C6 C5 C4 110.8(10) . .
C6 C5 C8 123.9(9) . .
C4 C5 C8 125.2(9) . .
C7 C6 C5 121.9(9) . .
C7 C6 H6A 119.1 . .
C5 C6 H6A 119.1 . .
C6 C7 N1 123.9(8) . .
C6 C7 C12 123.2(8) . .
N1 C7 C12 112.8(9) . .
C11 C8 C9 117.8(14) . .
C11 C8 C5 112.3(8) . .
C9 C8 C5 106.8(10) . .
C11 C8 C10 109.4(10) . .
C9 C8 C10 108.1(12) . .
C5 C8 C10 101.1(11) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C8 C11 H11A 109.5 . .
C8 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C8 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N2 C12 C13 120.8(8) . .
N2 C12 C7 112.0(7) . .
C13 C12 C7 127.2(9) . .
C12 C13 C14 119.9(8) . .
C12 C13 H13A 120.1 . .
C14 C13 H13A 120.1 . .
C15 C14 C13 117.0(7) . .
C15 C14 C17 121.2(8) . .
C13 C14 C17 121.8(8) . .
C16 C15 C14 119.9(8) . .
C16 C15 H15A 120.1 . .
C14 C15 H15A 120.1 . .
N2 C16 C15 121.5(8) . .
N2 C16 C21 110.7(7) . .
C15 C16 C21 127.6(8) . .
C19 C17 C18 117.5(10) . .
C19 C17 C14 111.9(8) . .
C18 C17 C14 113.5(8) . .
C19 C17 C20 100.4(11) . .
C18 C17 C20 104.6(10) . .
C14 C17 C20 107.3(9) . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C17 C19 H19A 109.5 . .
C17 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C17 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C17 C20 H20A 109.5 . .
C17 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C17 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
N3 C21 C22 124.3(8) . .
N3 C21 C16 112.5(9) . .
C22 C21 C16 123.1(7) . .
C21 C22 C23 120.7(9) . .
C21 C22 H22A 119.6 . .
C23 C22 H22A 119.6 . .
C24 C23 C22 113.7(11) . .
C24 C23 C26 124.9(9) . .
C22 C23 C26 121.4(9) . .
C25 C24 C23 122.9(10) . .
C25 C24 H24A 118.5 . .
C23 C24 H24A 118.5 . .
C24 C25 N3 123.8(9) . .
C24 C25 H25A 118.1 . .
N3 C25 H25A 118.1 . .
C29 C26 C27 108.9(10) . .
C29 C26 C23 114.9(11) . .
C27 C26 C23 111.5(8) . .
C29 C26 C28 108.0(10) . .
C27 C26 C28 104.0(11) . .
C23 C26 C28 108.9(9) . .
C26 C27 H27A 109.5 . .
C26 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C26 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
C26 C28 H28A 109.5 . .
C26 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C26 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C26 C29 H29A 109.5 . .
C26 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C26 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
N4 C30 C31 122.5(8) . .
N4 C30 H30A 118.8 . .
C31 C30 H30A 118.8 . .
C30 C31 C32 122.5(8) . .
C30 C31 H31A 118.8 . .
C32 C31 H31A 118.8 . .
C31 C32 C33 114.7(8) . .
C31 C32 C35 125.5(8) . .
C33 C32 C35 119.7(8) . .
C34 C33 C32 120.1(8) . .
C34 C33 H33A 120.0 . .
C32 C33 H33A 120.0 . .
C33 C34 N4 123.4(7) . .
C33 C34 C39 123.2(7) . .
N4 C34 C39 113.3(7) . .
C32 C35 C37 110.4(7) . .
C32 C35 C36 110.4(9) . .
C37 C35 C36 109.3(8) . .
C32 C35 C38 107.8(8) . .
C37 C35 C38 110.3(9) . .
C36 C35 C38 108.7(8) . .
C35 C36 H36A 109.5 . .
C35 C36 H36B 109.5 . .
H36A C36 H36B 109.5 . .
C35 C36 H36C 109.5 . .
H36A C36 H36C 109.5 . .
H36B C36 H36C 109.5 . .
C35 C37 H37A 109.5 . .
C35 C37 H37B 109.5 . .
H37A C37 H37B 109.5 . .
C35 C37 H37C 109.5 . .
H37A C37 H37C 109.5 . .
H37B C37 H37C 109.5 . .
C35 C38 H38A 109.5 . .
C35 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
C35 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
N5 C39 C40 121.1(7) . .
N5 C39 C34 110.2(6) . .
C40 C39 C34 128.7(7) . .
C39 C40 C41 120.1(7) . .
C39 C40 H40A 120.0 . .
C41 C40 H40A 120.0 . .
C40 C41 C42 117.8(7) . .
C40 C41 C44 123.1(7) . .
C42 C41 C44 119.0(7) . .
C43 C42 C41 119.5(8) . .
C43 C42 H42A 120.2 . .
C41 C42 H42A 120.3 . .
N5 C43 C42 120.9(7) . .
N5 C43 C48 110.8(6) . .
C42 C43 C48 128.2(7) . .
C45 C44 C47 113.0(9) . .
C45 C44 C41 113.4(7) . .
C47 C44 C41 109.6(9) . .
C45 C44 C46 105.0(10) . .
C47 C44 C46 105.4(10) . .
C41 C44 C46 110.0(8) . .
C44 C45 H45A 109.5 . .
C44 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C44 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C44 C46 H46A 109.5 . .
C44 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
C44 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C44 C47 H47A 109.5 . .
C44 C47 H47B 109.5 . .
H47A C47 H47B 109.5 . .
C44 C47 H47C 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
N6 C48 C49 123.0(7) . .
N6 C48 C43 114.1(7) . .
C49 C48 C43 122.8(7) . .
C50 C49 C48 120.1(7) . .
C50 C49 H49A 119.9 . .
C48 C49 H49A 119.9 . .
C51 C50 C49 115.9(8) . .
C51 C50 C53 122.6(7) . .
C49 C50 C53 121.5(7) . .
C52 C51 C50 121.7(7) . .
C52 C51 H51A 119.1 . .
C50 C51 H51A 119.1 . .
N6 C52 C51 123.3(7) . .
N6 C52 H52A 118.4 . .
C51 C52 H52A 118.4 . .
C54 C53 C56 108(2) . .
C54 C53 C55 106.0(15) . .
C56 C53 C55 113.0(19) . .
C54 C53 C50 114.0(8) . .
C56 C53 C50 108.1(8) . .
C55 C53 C50 108.3(11) . .
C53 C54 H54A 109.5 . .
C53 C54 H54B 109.5 . .
H54A C54 H54B 109.5 . .
C53 C54 H54C 109.4 . .
H54A C54 H54C 109.5 . .
H54B C54 H54C 109.5 . .
C53 C55 H55A 109.4 . .
C53 C55 H55B 109.5 . .
H55A C55 H55B 109.5 . .
C53 C55 H55C 109.4 . .
H55A C55 H55C 109.5 . .
H55B C55 H55C 109.5 . .
C53 C56 H56A 112.0 . .
C53 C56 H56B 111.8 . .
H56A C56 H56B 106.9 . .
C53 C56 H56C 111.7 . .
H56A C56 H56C 107.0 . .
H56B C56 H56C 107.0 . .
C73 O1 C70 100.0(18) . .
C72 C73 O1 97(2) . .
C71 C70 O1 98.5(19) . .
C73 C72 C71 107.7(19) . .
C70 C71 C72 107(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni2 N5 1.864(6) .
Ni2 C2 1.911(8) .
Ni2 N4 1.949(7) .
Ni2 N6 1.960(7) .
Ni1 N2 1.862(6) .
Ni1 C1 1.910(10) .
Ni1 N1 1.947(10) .
Ni1 N3 1.952(8) .
P1 F12 1.520(8) .
P1 F10 1.579(6) .
P1 F7 1.583(8) .
P1 F8 1.591(6) .
P1 F9 1.595(9) .
P1 F11 1.606(7) .
P2 F14 1.564(7) 3_755
P2 F14 1.564(7) .
P2 F15 1.580(9) .
P2 F15 1.580(9) 3_755
P2 F13 1.609(6) 3_755
P2 F13 1.609(6) .
P3 F17 1.443(8) .
P3 F17 1.443(8) 3_667
P3 F18 1.574(7) 3_667
P3 F18 1.574(7) .
P3 F16 1.594(7) .
P3 F16 1.594(7) 3_667
N1 C3 1.309(13) .
N1 C7 1.383(11) .
N2 C12 1.334(11) .
N2 C16 1.340(11) .
N3 C21 1.364(11) .
N3 C25 1.376(13) .
N4 C30 1.356(11) .
N4 C34 1.369(10) .
N5 C43 1.338(10) .
N5 C39 1.355(10) .
N6 C52 1.346(10) .
N6 C48 1.378(9) .
F1 C1 1.396(12) .
F2 C1 1.328(16) .
F3 C1 1.308(13) .
F4 C2 1.389(11) .
F5 C2 1.382(10) .
F6 C2 1.364(9) .
C3 C4 1.352(17) .
C3 H3A 0.9500 .
C4 C5 1.448(16) .
C4 H4A 0.9500 .
C5 C6 1.424(11) .
C5 C8 1.507(16) .
C6 C7 1.346(13) .
C6 H6A 0.9500 .
C7 C12 1.469(11) .
C8 C11 1.432(16) .
C8 C9 1.478(16) .
C8 C10 1.581(16) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C13 1.385(10) .
C13 C14 1.419(12) .
C13 H13A 0.9500 .
C14 C15 1.403(11) .
C14 C17 1.521(11) .
C15 C16 1.376(10) .
C15 H15A 0.9500 .
C16 C21 1.500(12) .
C17 C19 1.443(14) .
C17 C18 1.479(13) .
C17 C20 1.651(18) .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 C22 1.385(13) .
C22 C23 1.425(12) .
C22 H22A 0.9500 .
C23 C24 1.404(16) .
C23 C26 1.527(17) .
C24 C25 1.355(17) .
C24 H24A 0.9500 .
C25 H25A 0.9500 .
C26 C29 1.509(14) .
C26 C27 1.520(15) .
C26 C28 1.541(17) .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 H28A 0.9800 .
C28 H28B 0.9800 .
C28 H28C 0.9800 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
C30 C31 1.367(13) .
C30 H30A 0.9500 .
C31 C32 1.385(13) .
C31 H31A 0.9500 .
C32 C33 1.443(11) .
C32 C35 1.523(13) .
C33 C34 1.359(11) .
C33 H33A 0.9500 .
C34 C39 1.492(11) .
C35 C37 1.537(13) .
C35 C36 1.538(13) .
C35 C38 1.573(15) .
C36 H36A 0.9800 .
C36 H36B 0.9800 .
C36 H36C 0.9800 .
C37 H37A 0.9800 .
C37 H37B 0.9800 .
C37 H37C 0.9800 .
C38 H38A 0.9800 .
C38 H38B 0.9800 .
C38 H38C 0.9800 .
C39 C40 1.376(11) .
C40 C41 1.395(12) .
C40 H40A 0.9500 .
C41 C42 1.410(11) .
C41 C44 1.549(12) .
C42 C43 1.395(10) .
C42 H42A 0.9500 .
C43 C48 1.454(10) .
C44 C45 1.497(13) .
C44 C47 1.528(15) .
C44 C46 1.568(17) .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C48 C49 1.400(11) .
C49 C50 1.399(10) .
C49 H49A 0.9500 .
C50 C51 1.388(12) .
C50 C53 1.531(12) .
C51 C52 1.382(12) .
C51 H51A 0.9500 .
C52 H52A 0.9500 .
C53 C54 1.387(15) .
C53 C56 1.409(16) .
C53 C55 1.477(18) .
C54 H54A 0.9800 .
C54 H54B 0.9800 .
C54 H54C 0.9800 .
C55 H55A 0.9800 .
C55 H55B 0.9800 .
C55 H55C 0.9800 .
C56 H56A 1.0022 .
C56 H56B 1.0018 .
C56 H56C 1.0016 .
O1 C73 1.57(3) .
O1 C70 1.65(3) .
C73 C72 1.54(3) .
C70 C71 1.48(3) .
C72 C71 1.56(3) .
