# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_jk2_62
_database_code_depnum_ccdc_archive 'CCDC 1565545'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H42 N Ni P3'
_chemical_formula_weight         460.18

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   7.6605(16)
_cell_length_b                   11.777(2)
_cell_length_c                   27.694(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.670(3)
_cell_angle_gamma                90.00
_cell_volume                     2495.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6745
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      24.71

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6501
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44437
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4387
_reflns_number_gt                3351
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0414P)²+2.7127P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4387
_refine_ls_number_parameters     233
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.0940
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.28050(5) 0.27971(3) 0.134537(13) 0.01388(12) Uani 1 1 d . . .
C1 C 0.0660(4) 0.0747(3) 0.17945(12) 0.0253(8) Uani 1 1 d . . .
H1A H -0.0621 0.0716 0.1729 0.030 Uiso 1 1 calc R . .
H1B H 0.1051 0.0008 0.1932 0.030 Uiso 1 1 calc R . .
P1 P 0.17746(10) 0.10391(7) 0.12292(3) 0.01762(19) Uani 1 1 d . . .
P2 P 0.39253(10) 0.43493(7) 0.16538(3) 0.01512(19) Uani 1 1 d . . .
C2 C 0.2728(4) 0.4562(3) 0.22072(11) 0.0194(7) Uani 1 1 d . . .
H2A H 0.3522 0.4843 0.2473 0.023 Uiso 1 1 calc R . .
H2B H 0.1772 0.5118 0.2151 0.023 Uiso 1 1 calc R . .
C5 C 0.1485(4) 0.2934(3) 0.27491(11) 0.0214(7) Uani 1 1 d . . .
H5 H 0.1494 0.3278 0.3059 0.026 Uiso 1 1 calc R . .
C3 C 0.1118(4) 0.1684(3) 0.21408(11) 0.0198(7) Uani 1 1 d . . .
P3 P 0.29373(14) 0.26121(8) 0.01802(3) 0.0331(2) Uani 1 1 d . . .
C6 C 0.2010(4) 0.3422(3) 0.23288(11) 0.0178(7) Uani 1 1 d . . .
C4 C 0.0929(4) 0.1821(3) 0.26291(12) 0.0239(8) Uani 1 1 d . . .
H4 H 0.0505 0.1270 0.2845 0.029 Uiso 1 1 calc R . .
N N 0.1801(3) 0.2659(2) 0.19546(9) 0.0179(6) Uani 1 1 d . . .
C42 C 0.0175(4) 0.0598(3) 0.07457(12) 0.0251(8) Uani 1 1 d . . .
H42 H 0.0786 0.0631 0.0435 0.030 Uiso 1 1 calc R . .
C41 C 0.3448(4) -0.0083(3) 0.12279(12) 0.0240(8) Uani 1 1 d . . .
H41 H 0.2864 -0.0817 0.1304 0.029 Uiso 1 1 calc R . .
C46 C -0.1334(4) 0.1448(3) 0.07046(14) 0.0368(9) Uani 1 1 d . . .
H46A H -0.0870 0.2210 0.0651 0.055 Uiso 1 1 calc R . .
H46B H -0.1966 0.1441 0.1004 0.055 Uiso 1 1 calc R . .
H46C H -0.2132 0.1236 0.0433 0.055 Uiso 1 1 calc R . .
C45 C -0.0496(5) -0.0615(3) 0.07988(14) 0.0351(9) Uani 1 1 d . . .
H45A H -0.1320 -0.0792 0.0528 0.053 Uiso 1 1 calc R . .
H45B H -0.1088 -0.0685 0.1104 0.053 Uiso 1 1 calc R . .
H45C H 0.0490 -0.1145 0.0799 0.053 Uiso 1 1 calc R . .
C43 C 0.4271(5) -0.0220(3) 0.07419(13) 0.0311(9) Uani 1 1 d . . .
H43A H 0.3380 -0.0471 0.0500 0.047 Uiso 1 1 calc R . .
H43B H 0.5207 -0.0787 0.0770 0.047 Uiso 1 1 calc R . .
H43C H 0.4757 0.0509 0.0643 0.047 Uiso 1 1 calc R . .
C51 C 0.6234(4) 0.4261(3) 0.18759(12) 0.0223(7) Uani 1 1 d . . .
H51 H 0.6480 0.4939 0.2085 0.027 Uiso 1 1 calc R . .
C53 C 0.6510(5) 0.3209(3) 0.21911(14) 0.0343(9) Uani 1 1 d . . .
H53A H 0.6289 0.2527 0.1995 0.051 Uiso 1 1 calc R . .
H53B H 0.5702 0.3229 0.2455 0.051 Uiso 1 1 calc R . .
H53C H 0.7716 0.3197 0.2326 0.051 Uiso 1 1 calc R . .
C54 C 0.7516(4) 0.4291(3) 0.14692(14) 0.0342(9) Uani 1 1 d . . .
H54A H 0.7263 0.3661 0.1245 0.051 Uiso 1 1 calc R . .
H54B H 0.8713 0.4217 0.1607 0.051 Uiso 1 1 calc R . .
H54C H 0.7395 0.5013 0.1295 0.051 Uiso 1 1 calc R . .
C52 C 0.3750(4) 0.5698(3) 0.13217(11) 0.0199(7) Uani 1 1 d . . .
H52 H 0.4493 0.5628 0.1036 0.024 Uiso 1 1 calc R . .
C55 C 0.4419(5) 0.6717(3) 0.16131(14) 0.0350(9) Uani 1 1 d . . .
H55A H 0.4374 0.7395 0.1408 0.053 Uiso 1 1 calc R . .
H55B H 0.5628 0.6579 0.1730 0.053 Uiso 1 1 calc R . .
H55C H 0.3686 0.6833 0.1890 0.053 Uiso 1 1 calc R . .
C56 C 0.1876(4) 0.5895(3) 0.11279(12) 0.0286(8) Uani 1 1 d . . .
H56A H 0.1859 0.6508 0.0888 0.043 Uiso 1 1 calc R . .
H56B H 0.1147 0.6107 0.1395 0.043 Uiso 1 1 calc R . .
H56C H 0.1421 0.5198 0.0976 0.043 Uiso 1 1 calc R . .
C44 C 0.4840(5) 0.0147(3) 0.16318(13) 0.0344(9) Uani 1 1 d . . .
H44A H 0.5630 -0.0506 0.1664 0.052 Uiso 1 1 calc R . .
H44B H 0.4270 0.0267 0.1937 0.052 Uiso 1 1 calc R . .
H44C H 0.5508 0.0826 0.1553 0.052 Uiso 1 1 calc R . .
C31 C 0.4049(4) 0.2997(3) 0.07459(11) 0.0201(7) Uani 1 1 d . . .
H31A H 0.4388 0.3806 0.0725 0.024 Uiso 1 1 calc R . .
H31B H 0.5142 0.2550 0.0777 0.024 Uiso 1 1 calc R . .
C33 C 0.1401(5) 0.3786(3) 0.00879(12) 0.0331(2) Uani 1 1 d . . .
H33A H 0.0870 0.3749 -0.0240 0.050 Uiso 1 1 calc R . .
H33B H 0.2024 0.4509 0.0132 0.050 Uiso 1 1 calc R . .
H33C H 0.0486 0.3731 0.0323 0.050 Uiso 1 1 calc R . .
C32 C 0.4552(5) 0.3077(3) -0.02517(12) 0.0331(2) Uani 1 1 d . . .
H32A H 0.4050 0.3004 -0.0582 0.050 Uiso 1 1 calc R . .
H32B H 0.5601 0.2603 -0.0214 0.050 Uiso 1 1 calc R . .
H32C H 0.4864 0.3872 -0.0188 0.050 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N 1.894(3) . ?
Ni C31 1.966(3) . ?
Ni P2 2.1769(9) . ?
Ni P1 2.2337(10) . ?
C1 C3 1.493(4) . ?
C1 P1 1.850(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
P1 C41 1.841(3) . ?
P1 C42 1.847(3) . ?
P2 C52 1.837(3) . ?
P2 C2 1.840(3) . ?
P2 C51 1.848(3) . ?
C2 C6 1.495(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C5 C6 1.375(4) . ?
C5 C4 1.414(5) . ?
C5 H5 0.9500 . ?
C3 N 1.372(4) . ?
C3 C4 1.376(4) . ?
P3 C31 1.806(3) . ?
P3 C33 1.826(4) . ?
P3 C32 1.843(4) . ?
C6 N 1.376(4) . ?
C4 H4 0.9500 . ?
C42 C45 1.527(5) . ?
C42 C46 1.529(5) . ?
C42 H42 1.0000 . ?
C41 C43 1.521(5) . ?
C41 C44 1.533(4) . ?
C41 H41 1.0000 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C51 C53 1.524(5) . ?
C51 C54 1.529(5) . ?
C51 H51 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C52 C55 1.522(4) . ?
C52 C56 1.527(4) . ?
C52 H52 1.0000 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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
N Ni C31 174.53(12) . . ?
N Ni P2 83.78(8) . . ?
C31 Ni P2 91.89(9) . . ?
N Ni P1 83.87(8) . . ?
C31 Ni P1 99.87(9) . . ?
P2 Ni P1 164.80(4) . . ?
C3 C1 P1 107.6(2) . . ?
C3 C1 H1A 110.2 . . ?
P1 C1 H1A 110.2 . . ?
C3 C1 H1B 110.2 . . ?
P1 C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
C41 P1 C42 103.59(15) . . ?
C41 P1 C1 102.53(16) . . ?
C42 P1 C1 104.15(15) . . ?
C41 P1 Ni 115.09(11) . . ?
C42 P1 Ni 125.68(12) . . ?
C1 P1 Ni 102.97(11) . . ?
C52 P2 C2 105.77(15) . . ?
C52 P2 C51 105.18(15) . . ?
C2 P2 C51 103.70(15) . . ?
C52 P2 Ni 120.75(10) . . ?
C2 P2 Ni 103.79(10) . . ?
C51 P2 Ni 115.90(11) . . ?
C6 C2 P2 105.6(2) . . ?
C6 C2 H2A 110.6 . . ?
P2 C2 H2A 110.6 . . ?
C6 C2 H2B 110.6 . . ?
P2 C2 H2B 110.6 . . ?
H2A C2 H2B 108.8 . . ?
C6 C5 C4 106.6(3) . . ?
C6 C5 H5 126.7 . . ?
C4 C5 H5 126.7 . . ?
N C3 C4 109.3(3) . . ?
N C3 C1 117.4(3) . . ?
C4 C3 C1 133.3(3) . . ?
C31 P3 C33 101.88(15) . . ?
C31 P3 C32 100.65(16) . . ?
C33 P3 C32 97.56(17) . . ?
C5 C6 N 109.6(3) . . ?
C5 C6 C2 133.7(3) . . ?
N C6 C2 116.6(3) . . ?
C3 C4 C5 107.2(3) . . ?
C3 C4 H4 126.4 . . ?
C5 C4 H4 126.4 . . ?
C3 N C6 107.3(3) . . ?
C3 N Ni 125.8(2) . . ?
C6 N Ni 125.2(2) . . ?
C45 C42 C46 111.3(3) . . ?
C45 C42 P1 114.1(2) . . ?
C46 C42 P1 110.1(2) . . ?
C45 C42 H42 107.0 . . ?
C46 C42 H42 107.0 . . ?
P1 C42 H42 107.0 . . ?
C43 C41 C44 111.2(3) . . ?
C43 C41 P1 113.3(2) . . ?
C44 C41 P1 109.4(2) . . ?
C43 C41 H41 107.6 . . ?
C44 C41 H41 107.6 . . ?
P1 C41 H41 107.6 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C53 C51 C54 111.4(3) . . ?
C53 C51 P2 110.0(2) . . ?
C54 C51 P2 113.0(2) . . ?
C53 C51 H51 107.4 . . ?
C54 C51 H51 107.4 . . ?
P2 C51 H51 107.4 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C55 C52 C56 110.7(3) . . ?
C55 C52 P2 113.7(2) . . ?
C56 C52 P2 110.7(2) . . ?
C55 C52 H52 107.1 . . ?
C56 C52 H52 107.1 . . ?
P2 C52 H52 107.1 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C52 C56 H56A 109.5 . . ?
C52 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C52 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
P3 C31 Ni 118.36(17) . . ?
P3 C31 H31A 107.7 . . ?
Ni C31 H31A 107.7 . . ?
P3 C31 H31B 107.7 . . ?
Ni C31 H31B 107.7 . . ?
H31A C31 H31B 107.1 . . ?
P3 C33 H33A 109.5 . . ?
P3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
P3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
P3 C32 H32A 109.5 . . ?
P3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
P3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.733
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.077

####################################################################### 
# 
# 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. 
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#######################################################################

data_jk2_68
_database_code_depnum_ccdc_archive 'CCDC 1565541'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H45 F6 N Ni P4'
_chemical_formula_weight         716.26

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   16.313(2)
_cell_length_b                   10.5410(16)
_cell_length_c                   19.493(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.416(2)
_cell_angle_gamma                90.00
_cell_volume                     3341.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9834
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      28.15

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1496
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6715
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57265
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         24.99
_reflns_number_total             5886
_reflns_number_gt                5158
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0287P)²+1.9348P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5886
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0608
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.283628(13) 0.90376(2) 0.455872(11) 0.01208(6) Uani 1 1 d . . .
C1 C 0.40365(11) 1.10768(17) 0.47114(9) 0.0177(4) Uani 1 1 d . . .
P1 P 0.27669(3) 1.04382(4) 0.54027(2) 0.01372(10) Uani 1 1 d . . .
C2 C 0.39850(10) 1.01903(17) 0.36713(9) 0.0156(4) Uani 1 1 d . . .
P2 P 0.30296(3) 0.81143(4) 0.35527(2) 0.01342(10) Uani 1 1 d . . .
C3 C 0.45371(11) 1.11669(18) 0.36717(9) 0.0199(4) Uani 1 1 d . . .
H3 H 0.4841 1.1419 0.3298 0.024 Uiso 1 1 calc R . .
P3 P 0.19122(3) 0.77873(4) 0.49445(2) 0.01208(6) Uani 1 1 d . . .
C4 C 0.45716(11) 1.17329(18) 0.43319(9) 0.0209(4) Uani 1 1 d . . .
H4 H 0.4903 1.2435 0.4484 0.025 Uiso 1 1 calc R . .
C11 C 0.37777(11) 1.11962(18) 0.54280(9) 0.0206(4) Uani 1 1 d . . .
H11A H 0.3741 1.2099 0.5562 0.025 Uiso 1 1 calc R . .
H11B H 0.4173 1.0760 0.5760 0.025 Uiso 1 1 calc R . .
H H 0.1407(11) 0.8360(17) 0.5322(9) 0.019(5) Uiso 1 1 d . . .
P5 P 0.53160(3) 0.66333(4) 0.19326(2) 0.01796(11) Uani 1 1 d . . .
C17 C 0.23803(14) 1.1194(2) 0.67321(10) 0.0300(5) Uani 1 1 d . . .
H17A H 0.2290 1.0917 0.7200 0.045 Uiso 1 1 calc R . .
H17B H 0.1887 1.1625 0.6531 0.045 Uiso 1 1 calc R . .
H17C H 0.2848 1.1778 0.6747 0.045 Uiso 1 1 calc R . .
C16 C 0.32670(13) 0.92680(19) 0.66493(10) 0.0272(5) Uani 1 1 d . . .
H16A H 0.3723 0.9837 0.6794 0.041 Uiso 1 1 calc R . .
H16B H 0.3455 0.8634 0.6329 0.041 Uiso 1 1 calc R . .
H16C H 0.3075 0.8839 0.7053 0.041 Uiso 1 1 calc R . .
C15 C 0.11420(12) 1.11514(19) 0.50617(10) 0.0261(4) Uani 1 1 d . . .
H15A H 0.1027 1.0729 0.5492 0.039 Uiso 1 1 calc R . .
H15B H 0.1085 1.0540 0.4682 0.039 Uiso 1 1 calc R . .
H15C H 0.0752 1.1849 0.4970 0.039 Uiso 1 1 calc R . .
C14 C 0.22148(13) 1.22945(19) 0.44474(10) 0.0258(4) Uani 1 1 d . . .
H14A H 0.1805 1.2952 0.4322 0.039 Uiso 1 1 calc R . .
H14B H 0.2202 1.1650 0.4085 0.039 Uiso 1 1 calc R . .
H14C H 0.2763 1.2679 0.4502 0.039 Uiso 1 1 calc R . .
C13 C 0.25613(11) 1.00382(17) 0.62933(9) 0.0178(4) Uani 1 1 d . . .
H13 H 0.2061 0.9488 0.6269 0.021 Uiso 1 1 calc R . .
C12 C 0.20182(11) 1.16754(17) 0.51256(9) 0.0185(4) Uani 1 1 d . . .
H12 H 0.2045 1.2350 0.5487 0.022 Uiso 1 1 calc R . .
C21 C 0.36397(11) 0.93067(17) 0.31258(9) 0.0174(4) Uani 1 1 d . . .
H21A H 0.4089 0.8891 0.2896 0.021 Uiso 1 1 calc R . .
H21B H 0.3287 0.9775 0.2776 0.021 Uiso 1 1 calc R . .
C23 C 0.36838(11) 0.66889(17) 0.35513(9) 0.0178(4) Uani 1 1 d . . .
H23 H 0.3808 0.6529 0.3064 0.021 Uiso 1 1 calc R . .
C22 C 0.21321(10) 0.78305(16) 0.29427(9) 0.0157(4) Uani 1 1 d . . .
H22 H 0.1809 0.7113 0.3122 0.019 Uiso 1 1 calc R . .
C27 C 0.32639(12) 0.55038(17) 0.38049(10) 0.0224(4) Uani 1 1 d . . .
H27A H 0.3623 0.4768 0.3760 0.034 Uiso 1 1 calc R . .
H27B H 0.2744 0.5368 0.3529 0.034 Uiso 1 1 calc R . .
H27C H 0.3156 0.5614 0.4289 0.034 Uiso 1 1 calc R . .
C26 C 0.44995(11) 0.69505(19) 0.39640(10) 0.0251(4) Uani 1 1 d . . .
H26A H 0.4397 0.7146 0.4441 0.038 Uiso 1 1 calc R . .
H26B H 0.4772 0.7673 0.3762 0.038 Uiso 1 1 calc R . .
H26C H 0.4853 0.6200 0.3953 0.038 Uiso 1 1 calc R . .
C25 C 0.23792(12) 0.74668(17) 0.22263(9) 0.0196(4) Uani 1 1 d . . .
H25A H 0.2712 0.6691 0.2259 0.029 Uiso 1 1 calc R . .
H25B H 0.2701 0.8156 0.2043 0.029 Uiso 1 1 calc R . .
H25C H 0.1884 0.7320 0.1920 0.029 Uiso 1 1 calc R . .
C24 C 0.15830(11) 0.90079(17) 0.29000(9) 0.0205(4) Uani 1 1 d . . .
H24A H 0.1486 0.9292 0.3366 0.031 Uiso 1 1 calc R . .
H24B H 0.1056 0.8801 0.2649 0.031 Uiso 1 1 calc R . .
H24C H 0.1854 0.9685 0.2658 0.031 Uiso 1 1 calc R . .
N N 0.36696(9) 1.01207(14) 0.43097(7) 0.0153(3) Uani 1 1 d . . .
C36 C 0.05250(11) 0.76502(18) 0.40310(9) 0.0190(4) Uani 1 1 d . . .
H36 H 0.0463 0.8523 0.4136 0.023 Uiso 1 1 calc R . .
C35 C -0.00217(11) 0.7074(2) 0.35458(10) 0.0254(4) Uani 1 1 d . . .
H35 H -0.0452 0.7555 0.3315 0.030 Uiso 1 1 calc R . .
C34 C 0.00604(12) 0.57957(19) 0.33987(10) 0.0258(4) Uani 1 1 d . . .
H34 H -0.0308 0.5403 0.3062 0.031 Uiso 1 1 calc R . .
C33 C 0.06801(12) 0.50914(18) 0.37423(10) 0.0234(4) Uani 1 1 d . . .
H33 H 0.0728 0.4211 0.3649 0.028 Uiso 1 1 calc R . .
C32 C 0.12303(11) 0.56663(17) 0.42225(9) 0.0186(4) Uani 1 1 d . . .
H32 H 0.1655 0.5179 0.4456 0.022 Uiso 1 1 calc R . .
C31 C 0.11634(10) 0.69558(17) 0.43646(9) 0.0151(4) Uani 1 1 d . . .
C41 C 0.23641(11) 0.65860(16) 0.55231(9) 0.0158(4) Uani 1 1 d . . .
C42 C 0.18710(12) 0.57615(17) 0.58733(9) 0.0200(4) Uani 1 1 d . . .
H42 H 0.1289 0.5822 0.5810 0.024 Uiso 1 1 calc R . .
C43 C 0.22325(13) 0.48567(18) 0.63132(10) 0.0263(4) Uani 1 1 d . . .
H43 H 0.1897 0.4287 0.6545 0.032 Uiso 1 1 calc R . .
C44 C 0.30814(13) 0.47780(19) 0.64172(10) 0.0286(5) Uani 1 1 d . . .
H44 H 0.3326 0.4159 0.6722 0.034 Uiso 1 1 calc R . .
C45 C 0.35714(12) 0.55969(19) 0.60788(10) 0.0270(5) Uani 1 1 d . . .
H45 H 0.4153 0.5545 0.6153 0.032 Uiso 1 1 calc R . .
C46 C 0.32155(11) 0.64978(18) 0.56297(9) 0.0209(4) Uani 1 1 d . . .
H46 H 0.3555 0.7056 0.5394 0.025 Uiso 1 1 calc R . .
F51 F 0.53493(8) 0.53523(11) 0.14954(6) 0.0380(3) Uani 1 1 d . . .
F52 F 0.43365(7) 0.66657(12) 0.18015(6) 0.0335(3) Uani 1 1 d . . .
F53 F 0.52330(7) 0.58224(12) 0.26150(6) 0.0347(3) Uani 1 1 d . . .
F54 F 0.62949(6) 0.66147(12) 0.20673(6) 0.0310(3) Uani 1 1 d . . .
F55 F 0.53925(7) 0.74309(12) 0.12428(6) 0.0338(3) Uani 1 1 d . . .
F56 F 0.52835(7) 0.79177(11) 0.23643(6) 0.0367(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N 1.8678(14) . ?
Ni P3 2.1793(5) . ?
Ni P1 2.2199(5) . ?
Ni P2 2.2333(5) . ?
C1 C4 1.374(3) . ?
C1 N 1.384(2) . ?
C1 C11 1.495(2) . ?
P1 C11 1.8295(18) . ?
P1 C12 1.8392(18) . ?
P1 C13 1.8422(17) . ?
C2 C3 1.368(2) . ?
C2 N 1.385(2) . ?
C2 C21 1.491(2) . ?
P2 C22 1.8383(17) . ?
P2 C21 1.8412(18) . ?
P2 C23 1.8430(18) . ?
C3 C4 1.416(3) . ?
C3 H3 0.9500 . ?
P3 C41 1.8140(18) . ?
P3 C31 1.8236(18) . ?
P3 H 1.296(18) . ?
C4 H4 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
P5 F53 1.5957(12) . ?
P5 F56 1.5971(12) . ?
P5 F54 1.5983(12) . ?
P5 F55 1.5988(12) . ?
P5 F52 1.5990(12) . ?
P5 F51 1.5999(12) . ?
C17 C13 1.530(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C16 C13 1.531(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C15 C12 1.529(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 C12 1.530(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13 1.0000 . ?
C12 H12 1.0000 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C23 C27 1.525(3) . ?
C23 C26 1.526(2) . ?
C23 H23 1.0000 . ?
C22 C24 1.529(2) . ?
C22 C25 1.532(2) . ?
C22 H22 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C36 C35 1.389(3) . ?
C36 C31 1.392(2) . ?
C36 H36 0.9500 . ?
C35 C34 1.386(3) . ?
C35 H35 0.9500 . ?
C34 C33 1.385(3) . ?
C34 H34 0.9500 . ?
C33 C32 1.385(3) . ?
C33 H33 0.9500 . ?
C32 C31 1.393(2) . ?
C32 H32 0.9500 . ?
C41 C46 1.392(3) . ?
C41 C42 1.397(3) . ?
C42 C43 1.384(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.386(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.379(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.388(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?

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
N Ni P3 174.83(5) . . ?
N Ni P1 82.28(5) . . ?
P3 Ni P1 94.035(19) . . ?
N Ni P2 83.30(5) . . ?
P3 Ni P2 100.82(2) . . ?
P1 Ni P2 163.600(19) . . ?
C4 C1 N 109.09(15) . . ?
C4 C1 C11 134.23(17) . . ?
N C1 C11 116.67(15) . . ?
C11 P1 C12 105.96(9) . . ?
C11 P1 C13 107.68(8) . . ?
C12 P1 C13 105.91(8) . . ?
C11 P1 Ni 102.31(6) . . ?
C12 P1 Ni 108.93(6) . . ?
C13 P1 Ni 124.72(6) . . ?
C3 C2 N 109.23(15) . . ?
C3 C2 C21 133.10(16) . . ?
N C2 C21 117.50(15) . . ?
C22 P2 C21 104.48(8) . . ?
C22 P2 C23 107.39(8) . . ?
C21 P2 C23 102.86(8) . . ?
C22 P2 Ni 118.66(6) . . ?
C21 P2 Ni 102.54(6) . . ?
C23 P2 Ni 118.53(6) . . ?
C2 C3 C4 107.33(16) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
C41 P3 C31 105.70(8) . . ?
C41 P3 Ni 112.21(6) . . ?
C31 P3 Ni 121.66(6) . . ?
C41 P3 H 102.6(8) . . ?
C31 P3 H 98.7(8) . . ?
Ni P3 H 113.6(8) . . ?
C1 C4 C3 107.15(16) . . ?
C1 C4 H4 126.4 . . ?
C3 C4 H4 126.4 . . ?
C1 C11 P1 104.88(12) . . ?
C1 C11 H11A 110.8 . . ?
P1 C11 H11A 110.8 . . ?
C1 C11 H11B 110.8 . . ?
P1 C11 H11B 110.8 . . ?
H11A C11 H11B 108.8 . . ?
F53 P5 F56 90.37(7) . . ?
F53 P5 F54 90.25(7) . . ?
F56 P5 F54 89.83(7) . . ?
F53 P5 F55 179.21(8) . . ?
F56 P5 F55 90.30(7) . . ?
F54 P5 F55 90.17(6) . . ?
F53 P5 F52 89.81(6) . . ?
F56 P5 F52 89.59(7) . . ?
F54 P5 F52 179.42(8) . . ?
F55 P5 F52 89.78(6) . . ?
F53 P5 F51 90.03(7) . . ?
F56 P5 F51 179.60(8) . . ?
F54 P5 F51 90.16(7) . . ?
F55 P5 F51 89.30(7) . . ?
F52 P5 F51 90.42(7) . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C13 C16 109.84(15) . . ?
C17 C13 P1 113.69(13) . . ?
C16 C13 P1 111.32(13) . . ?
C17 C13 H13 107.2 . . ?
C16 C13 H13 107.2 . . ?
P1 C13 H13 107.2 . . ?
C15 C12 C14 109.91(15) . . ?
C15 C12 P1 111.31(13) . . ?
C14 C12 P1 112.18(13) . . ?
C15 C12 H12 107.8 . . ?
C14 C12 H12 107.8 . . ?
P1 C12 H12 107.8 . . ?
C2 C21 P2 106.96(12) . . ?
C2 C21 H21A 110.3 . . ?
P2 C21 H21A 110.3 . . ?
C2 C21 H21B 110.3 . . ?
P2 C21 H21B 110.3 . . ?
H21A C21 H21B 108.6 . . ?
C27 C23 C26 111.85(15) . . ?
C27 C23 P2 113.12(13) . . ?
C26 C23 P2 109.47(12) . . ?
C27 C23 H23 107.4 . . ?
C26 C23 H23 107.4 . . ?
P2 C23 H23 107.4 . . ?
C24 C22 C25 110.35(14) . . ?
C24 C22 P2 109.71(12) . . ?
C25 C22 P2 112.21(12) . . ?
C24 C22 H22 108.2 . . ?
C25 C22 H22 108.2 . . ?
P2 C22 H22 108.2 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C1 N C2 107.19(14) . . ?
C1 N Ni 126.15(12) . . ?
C2 N Ni 126.45(12) . . ?
C35 C36 C31 120.40(17) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C34 C35 C36 119.92(18) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C33 C34 C35 119.98(18) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C33 C32 120.20(18) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C32 C31 120.31(17) . . ?
C33 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C36 C31 C32 119.15(16) . . ?
C36 C31 P3 118.56(14) . . ?
C32 C31 P3 122.23(14) . . ?
C46 C41 C42 119.39(16) . . ?
C46 C41 P3 119.52(14) . . ?
C42 C41 P3 121.08(14) . . ?
C43 C42 C41 119.84(18) . . ?
C43 C42 H42 120.1 . . ?
C41 C42 H42 120.1 . . ?
C42 C43 C44 120.33(18) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C45 C44 C43 120.13(18) . . ?
C45 C44 H44 119.9 . . ?
C43 C44 H44 119.9 . . ?
C44 C45 C46 120.02(18) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C41 120.27(18) . . ?
C45 C46 H46 119.9 . . ?
C41 C46 H46 119.9 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.048
####################################################################### 
# 
# 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_jk2_74
_database_code_depnum_ccdc_archive 'CCDC 1565544'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H44 N Ni P3'
_chemical_formula_weight         570.28

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.2144(8)
_cell_length_b                   9.2591(8)
_cell_length_c                   19.2579(16)
_cell_angle_alpha                86.080(3)
_cell_angle_beta                 84.872(3)
_cell_angle_gamma                63.320(2)
_cell_volume                     1461.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      28.42

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6697
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34813
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5134
_reflns_number_gt                4769
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0278P)²+0.8803P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5134
_refine_ls_number_parameters     318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0598
_refine_ls_wR_factor_gt          0.0588
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.66013(2) 0.10843(2) 0.764530(9) 0.01208(6) Uani 1 1 d . . .
P1 P 0.72515(5) -0.03177(5) 0.66704(2) 0.01500(9) Uani 1 1 d . . .
C1 C 0.8458(2) -0.24361(19) 0.69782(9) 0.0218(4) Uani 1 1 d . . .
H1A H 0.7957 -0.3120 0.6848 0.026 Uiso 1 1 calc R . .
H1B H 0.9580 -0.2869 0.6760 0.026 Uiso 1 1 calc R . .
P3 P 0.56659(5) 0.34801(5) 0.70736(2) 0.01433(9) Uani 1 1 d . . .
C3 C 0.84885(18) -0.24530(18) 0.77487(8) 0.0156(3) Uani 1 1 d . . .
C2 C 0.6925(2) 0.00453(18) 0.92502(8) 0.0185(3) Uani 1 1 d . . .
H2A H 0.7596 -0.0003 0.9633 0.022 Uiso 1 1 calc R . .
H2B H 0.5915 0.0014 0.9456 0.022 Uiso 1 1 calc R . .
P2 P 0.64291(5) 0.19104(4) 0.870986(19) 0.01208(6) Uani 1 1 d . . .
N N 0.76824(15) -0.10009(15) 0.80777(7) 0.0140(3) Uani 1 1 d . . .
C5 C 0.87464(18) -0.29763(18) 0.88993(8) 0.0175(3) Uani 1 1 d . . .
H5 H 0.9038 -0.3522 0.9338 0.021 Uiso 1 1 calc R . .
C4 C 0.91537(18) -0.36868(18) 0.82375(8) 0.0174(3) Uani 1 1 d . . .
H4 H 0.9770 -0.4805 0.8148 0.021 Uiso 1 1 calc R . .
C6 C 0.78430(18) -0.13369(18) 0.87817(8) 0.0156(3) Uani 1 1 d . . .
C11 C 0.8704(2) -0.0032(2) 0.60183(9) 0.0254(4) Uani 1 1 d . . .
H11 H 0.9205 -0.1008 0.5724 0.030 Uiso 1 1 calc R . .
C12 C 0.5723(2) -0.04213(19) 0.61450(8) 0.0189(3) Uani 1 1 d . . .
H12 H 0.5049 0.0692 0.5952 0.023 Uiso 1 1 calc R . .
C13 C 0.7906(3) 0.1441(2) 0.55318(10) 0.0354(5) Uani 1 1 d . . .
H13A H 0.8723 0.1480 0.5178 0.053 Uiso 1 1 calc R . .
H13B H 0.7446 0.2426 0.5802 0.053 Uiso 1 1 calc R . .
H13C H 0.7037 0.1365 0.5302 0.053 Uiso 1 1 calc R . .
C14 C 1.0070(2) 0.0028(3) 0.63902(12) 0.0417(5) Uani 1 1 d . . .
H14A H 1.0875 0.0117 0.6044 0.062 Uiso 1 1 calc R . .
H14B H 1.0595 -0.0961 0.6678 0.062 Uiso 1 1 calc R . .
H14C H 0.9618 0.0969 0.6688 0.062 Uiso 1 1 calc R . .
C15 C 0.6482(2) -0.1545(2) 0.55277(9) 0.0297(4) Uani 1 1 d . . .
H15A H 0.5620 -0.1621 0.5292 0.045 Uiso 1 1 calc R . .
H15B H 0.7238 -0.2623 0.5698 0.045 Uiso 1 1 calc R . .
H15C H 0.7072 -0.1110 0.5199 0.045 Uiso 1 1 calc R . .
C16 C 0.4589(2) -0.0940(2) 0.66034(10) 0.0289(4) Uani 1 1 d . . .
H16A H 0.3652 -0.0764 0.6345 0.043 Uiso 1 1 calc R . .
H16B H 0.4211 -0.0300 0.7025 0.043 Uiso 1 1 calc R . .
H16C H 0.5177 -0.2090 0.6735 0.043 Uiso 1 1 calc R . .
C21 C 0.80085(19) 0.25868(19) 0.88386(8) 0.0170(3) Uani 1 1 d . . .
H21 H 0.7455 0.3796 0.8836 0.020 Uiso 1 1 calc R . .
C22 C 0.45079(19) 0.33762(19) 0.91425(8) 0.0172(3) Uani 1 1 d . . .
H22 H 0.4310 0.4482 0.8960 0.021 Uiso 1 1 calc R . .
C23 C 0.92898(19) 0.20841(19) 0.82236(9) 0.0214(4) Uani 1 1 d . . .
H23A H 0.8766 0.2583 0.7791 0.032 Uiso 1 1 calc R . .
H23B H 0.9808 0.0904 0.8191 0.032 Uiso 1 1 calc R . .
H23C H 1.0116 0.2443 0.8295 0.032 Uiso 1 1 calc R . .
C24 C 0.8863(2) 0.2001(3) 0.95210(10) 0.0335(4) Uani 1 1 d . . .
H24A H 0.9552 0.0831 0.9511 0.050 Uiso 1 1 calc R . .
H24B H 0.8046 0.2247 0.9914 0.050 Uiso 1 1 calc R . .
H24C H 0.9539 0.2551 0.9574 0.050 Uiso 1 1 calc R . .
C25 C 0.3101(2) 0.3070(2) 0.89456(9) 0.0253(4) Uani 1 1 d . . .
H25A H 0.3094 0.3087 0.8437 0.038 Uiso 1 1 calc R . .
H25B H 0.2069 0.3916 0.9136 0.038 Uiso 1 1 calc R . .
H25C H 0.3238 0.2012 0.9138 0.038 Uiso 1 1 calc R . .
C26 C 0.4538(2) 0.3356(2) 0.99359(8) 0.0229(4) Uani 1 1 d . . .
H26A H 0.5444 0.3554 1.0055 0.034 Uiso 1 1 calc R . .
H26B H 0.4680 0.2299 1.0131 0.034 Uiso 1 1 calc R . .
H26C H 0.3511 0.4202 1.0130 0.034 Uiso 1 1 calc R . .
C31 C 0.38992(19) 0.37381(18) 0.66041(8) 0.0174(3) Uani 1 1 d . . .
C32 C 0.3599(2) 0.4625(2) 0.59708(9) 0.0252(4) Uani 1 1 d . . .
H32 H 0.4311 0.5069 0.5790 0.030 Uiso 1 1 calc R . .
C33 C 0.2274(2) 0.4868(2) 0.56026(10) 0.0328(4) Uani 1 1 d . . .
H33 H 0.2091 0.5472 0.5173 0.039 Uiso 1 1 calc R . .
C34 C 0.1226(2) 0.4239(2) 0.58562(10) 0.0314(4) Uani 1 1 d . . .
H34 H 0.0326 0.4401 0.5601 0.038 Uiso 1 1 calc R . .
C35 C 0.1487(2) 0.3373(2) 0.64827(10) 0.0271(4) Uani 1 1 d . . .
H35 H 0.0759 0.2946 0.6663 0.033 Uiso 1 1 calc R . .
C36 C 0.2815(2) 0.31238(19) 0.68503(9) 0.0209(3) Uani 1 1 d . . .
H36 H 0.2987 0.2520 0.7280 0.025 Uiso 1 1 calc R . .
C41 C 0.46415(18) 0.52693(17) 0.76186(8) 0.0137(3) Uani 1 1 d . . .
C42 C 0.56191(18) 0.58732(18) 0.78847(8) 0.0146(3) Uani 1 1 d . . .
H42 H 0.6763 0.5348 0.7780 0.018 Uiso 1 1 calc R . .
C43 C 0.49578(19) 0.72188(18) 0.82972(8) 0.0169(3) Uani 1 1 d . . .
H43 H 0.5647 0.7594 0.8480 0.020 Uiso 1 1 calc R . .
C44 C 0.32834(19) 0.80176(19) 0.84435(8) 0.0189(3) Uani 1 1 d . . .
H44 H 0.2824 0.8937 0.8728 0.023 Uiso 1 1 calc R . .
C45 C 0.22897(19) 0.74647(19) 0.81724(8) 0.0187(3) Uani 1 1 d . . .
H45 H 0.1144 0.8014 0.8267 0.022 Uiso 1 1 calc R . .
C46 C 0.29576(18) 0.61118(18) 0.77627(8) 0.0159(3) Uani 1 1 d . . .
H46 H 0.2260 0.5752 0.7577 0.019 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N 1.9012(12) . ?
Ni P2 2.2047(5) . ?
Ni P3 2.2349(5) . ?
Ni P1 2.2367(4) . ?
P1 C12 1.8456(16) . ?
P1 C11 1.8466(17) . ?
P1 C1 1.8534(16) . ?
C1 C3 1.486(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
P3 C41 1.8422(15) . ?
P3 C31 1.8462(16) . ?
C3 C4 1.376(2) . ?
C3 N 1.3771(19) . ?
C2 C6 1.489(2) . ?
C2 P2 1.8452(15) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
P2 C22 1.8448(15) . ?
P2 C21 1.8644(16) . ?
N C6 1.376(2) . ?
C5 C6 1.379(2) . ?
C5 C4 1.416(2) . ?
C5 H5 0.9500 . ?
C4 H4 0.9500 . ?
C11 C13 1.526(3) . ?
C11 C14 1.527(3) . ?
C11 H11 1.0000 . ?
C12 C16 1.526(2) . ?
C12 C15 1.534(2) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 C24 1.531(2) . ?
C21 C23 1.532(2) . ?
C21 H21 1.0000 . ?
C22 C25 1.529(2) . ?
C22 C26 1.529(2) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C31 C36 1.391(2) . ?
C31 C32 1.399(2) . ?
C32 C33 1.389(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.376(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.380(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(2) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.400(2) . ?
C41 C42 1.400(2) . ?
C42 C43 1.386(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.390(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.388(2) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?

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
N Ni P2 83.21(4) . . ?
N Ni P3 172.18(4) . . ?
P2 Ni P3 98.952(17) . . ?
N Ni P1 83.37(4) . . ?
P2 Ni P1 165.900(17) . . ?
P3 Ni P1 93.796(17) . . ?
C12 P1 C11 104.24(8) . . ?
C12 P1 C1 104.00(7) . . ?
C11 P1 C1 101.75(8) . . ?
C12 P1 Ni 123.19(5) . . ?
C11 P1 Ni 117.28(6) . . ?
C1 P1 Ni 103.50(5) . . ?
C3 C1 P1 108.17(11) . . ?
C3 C1 H1A 110.1 . . ?
P1 C1 H1A 110.1 . . ?
C3 C1 H1B 110.1 . . ?
P1 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
C41 P3 C31 98.29(7) . . ?
C41 P3 Ni 115.89(5) . . ?
C31 P3 Ni 108.21(5) . . ?
C4 C3 N 109.56(14) . . ?
C4 C3 C1 132.45(14) . . ?
N C3 C1 117.96(13) . . ?
C6 C2 P2 106.85(10) . . ?
C6 C2 H2A 110.4 . . ?
P2 C2 H2A 110.4 . . ?
C6 C2 H2B 110.4 . . ?
P2 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
C22 P2 C2 103.01(7) . . ?
C22 P2 C21 106.95(7) . . ?
C2 P2 C21 106.87(7) . . ?
C22 P2 Ni 123.08(5) . . ?
C2 P2 Ni 102.79(5) . . ?
C21 P2 Ni 112.54(5) . . ?
C6 N C3 106.97(12) . . ?
C6 N Ni 126.19(10) . . ?
C3 N Ni 126.82(11) . . ?
C6 C5 C4 106.53(14) . . ?
C6 C5 H5 126.7 . . ?
C4 C5 H5 126.7 . . ?
C3 C4 C5 107.09(13) . . ?
C3 C4 H4 126.5 . . ?
C5 C4 H4 126.5 . . ?
N C6 C5 109.84(14) . . ?
N C6 C2 116.42(13) . . ?
C5 C6 C2 133.45(15) . . ?
C13 C11 C14 111.58(16) . . ?
C13 C11 P1 113.47(12) . . ?
C14 C11 P1 109.39(13) . . ?
C13 C11 H11 107.4 . . ?
C14 C11 H11 107.4 . . ?
P1 C11 H11 107.4 . . ?
C16 C12 C15 110.00(14) . . ?
C16 C12 P1 110.45(11) . . ?
C15 C12 P1 113.12(12) . . ?
C16 C12 H12 107.7 . . ?
C15 C12 H12 107.7 . . ?
P1 C12 H12 107.7 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C24 C21 C23 109.14(14) . . ?
C24 C21 P2 115.63(12) . . ?
C23 C21 P2 109.95(11) . . ?
C24 C21 H21 107.3 . . ?
C23 C21 H21 107.3 . . ?
P2 C21 H21 107.3 . . ?
C25 C22 C26 110.28(13) . . ?
C25 C22 P2 109.52(11) . . ?
C26 C22 P2 113.63(11) . . ?
C25 C22 H22 107.7 . . ?
C26 C22 H22 107.7 . . ?
P2 C22 H22 107.7 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C36 C31 C32 117.38(15) . . ?
C36 C31 P3 123.71(12) . . ?
C32 C31 P3 118.90(13) . . ?
C33 C32 C31 121.01(17) . . ?
C33 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
C34 C33 C32 120.39(17) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 119.74(17) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C34 C35 C36 119.91(18) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C35 C36 C31 121.56(16) . . ?
C35 C36 H36 119.2 . . ?
C31 C36 H36 119.2 . . ?
C46 C41 C42 117.48(14) . . ?
C46 C41 P3 125.08(12) . . ?
C42 C41 P3 117.38(11) . . ?
C43 C42 C41 121.56(14) . . ?
C43 C42 H42 119.2 . . ?
C41 C42 H42 119.2 . . ?
C42 C43 C44 119.85(15) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C45 C44 C43 119.59(15) . . ?
C45 C44 H44 120.2 . . ?
C43 C44 H44 120.2 . . ?
C44 C45 C46 120.37(14) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C45 C46 C41 121.12(14) . . ?
C45 C46 H46 119.4 . . ?
C41 C46 H46 119.4 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.044
####################################################################### 
# 
# 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_JK4_165_0m
_database_code_depnum_ccdc_archive 'CCDC 1565543'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H43 F6 N Ni O3 P4'
_chemical_formula_weight         654.15

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.4915(6)
_cell_length_b                   15.0549(6)
_cell_length_c                   16.2395(6)
_cell_angle_alpha                109.950(2)
_cell_angle_beta                 107.078(2)
_cell_angle_gamma                107.074(2)
_cell_volume                     2861.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7855
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      23.51

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_F_000             1368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.965
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6838
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            71121
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.484
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10079
_reflns_number_gt                7500
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0329P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10079
_refine_ls_number_parameters     671
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0803
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.22439(3) 0.23161(3) 0.00771(2) 0.01244(9) Uani 1 1 d . . . . .
N1 N 0.11929(18) 0.09622(17) -0.07778(16) 0.0156(5) Uani 1 1 d . . . . .
Ni2 Ni 0.75400(3) 0.21304(3) 0.49970(2) 0.01176(9) Uani 1 1 d . . . . .
N2 N 0.74155(18) 0.18089(17) 0.59723(16) 0.0149(5) Uani 1 1 d . . . . .
P3 P 0.72002(6) 0.28963(6) 0.03215(6) 0.01853(19) Uani 1 1 d . . . . .
P4 P 0.24072(6) 0.27519(6) 0.51700(6) 0.01926(19) Uani 1 1 d . . . . .
P11 P 0.29607(6) 0.15531(6) 0.08544(5) 0.01386(17) Uani 1 1 d . . . . .
C11 C 0.1854(2) 0.0244(2) 0.0288(2) 0.0197(7) Uani 1 1 d . . . . .
H11A H 0.2126 -0.0298 0.0178 0.024 Uiso 1 1 calc R U . . .
H11B H 0.1493 0.0199 0.0714 0.024 Uiso 1 1 calc R U . . .
O11 O 0.43800(15) 0.39137(14) 0.18722(13) 0.0198(5) Uani 1 1 d . . . . .
P12 P 0.11847(6) 0.27179(6) -0.08739(5) 0.01502(17) Uani 1 1 d . . . . .
C12 C 0.0332(2) 0.1455(2) -0.1972(2) 0.0211(7) Uani 1 1 d . . . . .
H12A H -0.0416 0.1365 -0.2243 0.025 Uiso 1 1 calc R U . . .
H12B H 0.0598 0.1409 -0.2474 0.025 Uiso 1 1 calc R U . . .
O12 O 0.41840(15) 0.42873(14) 0.04535(14) 0.0189(5) Uani 1 1 d . . . . .
P13 P 0.35177(6) 0.38436(6) 0.09604(5) 0.01327(17) Uani 1 1 d . . . . .
C13 C 0.1092(2) 0.0077(2) -0.0657(2) 0.0168(7) Uani 1 1 d . . . . .
O13 O 0.31907(15) 0.47518(14) 0.13586(13) 0.0162(4) Uani 1 1 d . . . . .
C14 C 0.0242(2) -0.0779(2) -0.1455(2) 0.0187(7) Uani 1 1 d . . . . .
H14 H -0.0003 -0.1485 -0.1559 0.022 Uiso 1 1 calc R U . . .
C15 C -0.0213(2) -0.0422(2) -0.2102(2) 0.0194(7) Uani 1 1 d . . . . .
H15 H -0.0819 -0.0842 -0.2721 0.023 Uiso 1 1 calc R U . . .
C19 C 0.3748(3) 0.5837(2) 0.1574(2) 0.0291(8) Uani 1 1 d . . . . .
H19A H 0.3228 0.6127 0.1454 0.044 Uiso 1 1 calc R U . . .
H19B H 0.4112 0.5865 0.1156 0.044 Uiso 1 1 calc R U . . .
H19C H 0.4279 0.6251 0.2259 0.044 Uiso 1 1 calc R U . . .
C18 C 0.4837(3) 0.3801(2) 0.0147(2) 0.0306(8) Uani 1 1 d . . . . .
H18A H 0.5213 0.4176 -0.0132 0.046 Uiso 1 1 calc R U . . .
H18B H 0.4374 0.3065 -0.0345 0.046 Uiso 1 1 calc R U . . .
H18C H 0.5364 0.3833 0.0711 0.046 Uiso 1 1 calc R U . . .
C17 C 0.5245(3) 0.4894(2) 0.2665(2) 0.0378(9) Uani 1 1 d . . . . .
H17A H 0.5691 0.4756 0.3145 0.057 Uiso 1 1 calc R U . . .
H17B H 0.4949 0.5343 0.2975 0.057 Uiso 1 1 calc R U . . .
H17C H 0.5685 0.5250 0.2414 0.057 Uiso 1 1 calc R U . . .
C16 C 0.0382(2) 0.0635(2) -0.1669(2) 0.0169(7) Uani 1 1 d . . . . .
P21 P 0.75911(6) 0.36221(6) 0.59362(5) 0.01399(17) Uani 1 1 d . . . . .
C21 C 0.8000(2) 0.3634(2) 0.71174(19) 0.0169(7) Uani 1 1 d . . . . .
H21A H 0.8788 0.4036 0.7507 0.020 Uiso 1 1 calc R U . . .
H21B H 0.7650 0.3960 0.7487 0.020 Uiso 1 1 calc R U . . .
O21 O 0.89634(15) 0.35634(14) 0.43892(13) 0.0152(4) Uani 1 1 d . . . . .
P22 P 0.72729(6) 0.04755(6) 0.42599(5) 0.01381(17) Uani 1 1 d . . . . .
C22 C 0.6736(2) -0.0069(2) 0.4956(2) 0.0207(7) Uani 1 1 d . . . . .
H22A H 0.5942 -0.0436 0.4613 0.025 Uiso 1 1 calc R U . . .
H22B H 0.7010 -0.0577 0.5042 0.025 Uiso 1 1 calc R U . . .
O22 O 0.70616(15) 0.30704(15) 0.36005(14) 0.0186(5) Uani 1 1 d . . . . .
P23 P 0.78307(6) 0.26065(6) 0.39785(5) 0.01289(17) Uani 1 1 d . . . . .
C24 C 0.7491(2) 0.1990(2) 0.7419(2) 0.0213(7) Uani 1 1 d . . . . .
H24 H 0.7595 0.2288 0.8076 0.026 Uiso 1 1 calc R U . . .
C25 C 0.7142(2) 0.0914(2) 0.6795(2) 0.0204(7) Uani 1 1 d . . . . .
H25 H 0.6971 0.0355 0.6956 0.024 Uiso 1 1 calc R U . . .
C26 C 0.7096(2) 0.0830(2) 0.5920(2) 0.0182(7) Uani 1 1 d . . . . .
C27 C 0.9938(2) 0.3440(2) 0.4725(2) 0.0258(8) Uani 1 1 d . . . . .
H27A H 1.0559 0.4132 0.5103 0.039 Uiso 1 1 calc R U . . .
H27B H 1.0012 0.3008 0.4163 0.039 Uiso 1 1 calc R U . . .
H27C H 0.9904 0.3095 0.5137 0.039 Uiso 1 1 calc R U . . .
C28 C 0.7185(3) 0.3648(3) 0.3057(2) 0.0290(8) Uani 1 1 d . . . . .
H28A H 0.7178 0.4324 0.3389 0.043 Uiso 1 1 calc R U . . .
H28B H 0.6592 0.3240 0.2399 0.043 Uiso 1 1 calc R U . . .
H28C H 0.7869 0.3772 0.3016 0.043 Uiso 1 1 calc R U . . .
C29 C 0.8103(3) 0.1868(2) 0.2360(2) 0.0238(7) Uani 1 1 d . . . . .
H29A H 0.8387 0.1368 0.2124 0.036 Uiso 1 1 calc R U . . .
H29B H 0.8664 0.2588 0.2661 0.036 Uiso 1 1 calc R U . . .
H29C H 0.7488 0.1757 0.1811 0.036 Uiso 1 1 calc R U . . .
C31 C 0.3408(2) 0.2051(2) 0.2170(2) 0.0163(7) Uani 1 1 d . . . . .
H31 H 0.4183 0.2564 0.2504 0.020 Uiso 1 1 calc R U . . .
F31 F 0.71787(15) 0.18740(14) -0.04240(14) 0.0433(5) Uani 1 1 d . . . . .
C32 C 0.4070(2) 0.1418(2) 0.0588(2) 0.0161(7) Uani 1 1 d . . . . .
H32 H 0.4638 0.2147 0.0865 0.019 Uiso 1 1 calc R U . . .
F32 F 0.79178(14) 0.35897(14) -0.00033(13) 0.0371(5) Uani 1 1 d . . . . .
C33 C 0.3306(2) 0.1193(2) 0.2488(2) 0.0230(7) Uani 1 1 d . . . . .
H33A H 0.3669 0.1519 0.3201 0.035 Uiso 1 1 calc R U . . .
H33B H 0.3639 0.0767 0.2210 0.035 Uiso 1 1 calc R U . . .
H33C H 0.2545 0.0744 0.2257 0.035 Uiso 1 1 calc R U . . .
F33 F 0.82573(14) 0.30801(15) 0.11495(13) 0.0384(5) Uani 1 1 d . . . . .
C34 C 0.2787(3) 0.2635(2) 0.2518(2) 0.0254(8) Uani 1 1 d . . . . .
H34A H 0.3033 0.2891 0.3221 0.038 Uiso 1 1 calc R U . . .
H34B H 0.2019 0.2158 0.2177 0.038 Uiso 1 1 calc R U . . .
H34C H 0.2912 0.3233 0.2378 0.038 Uiso 1 1 calc R U . . .
F34 F 0.72085(15) 0.39145(15) 0.10678(14) 0.0473(6) Uani 1 1 d . . . . .
C35 C 0.4599(2) 0.0856(2) 0.1041(2) 0.0244(7) Uani 1 1 d . . . . .
H35A H 0.5171 0.0813 0.0848 0.037 Uiso 1 1 calc R U . . .
H35B H 0.4061 0.0146 0.0815 0.037 Uiso 1 1 calc R U . . .
H35C H 0.4905 0.1248 0.1753 0.037 Uiso 1 1 calc R U . . .
F35 F 0.64769(14) 0.22040(15) 0.06490(13) 0.0402(5) Uani 1 1 d . . . . .
C36 C 0.3709(3) 0.0905(2) -0.0513(2) 0.0269(8) Uani 1 1 d . . . . .
H36A H 0.4335 0.0956 -0.0644 0.040 Uiso 1 1 calc R U . . .
H36B H 0.3356 0.1267 -0.0791 0.040 Uiso 1 1 calc R U . . .
H36C H 0.3204 0.0164 -0.0808 0.040 Uiso 1 1 calc R U . . .
F36 F 0.61354(14) 0.27140(15) -0.05035(12) 0.0348(5) Uani 1 1 d . . . . .
C41 C 0.0234(2) 0.3025(2) -0.0433(2) 0.0200(7) Uani 1 1 d . . . . .
H41 H -0.0365 0.2943 -0.0998 0.024 Uiso 1 1 calc R U . . .
F41 F 0.22938(16) 0.37069(15) 0.58726(13) 0.0449(6) Uani 1 1 d . . . . .
C42 C 0.1685(2) 0.3658(2) -0.1295(2) 0.0204(7) Uani 1 1 d . . . . .
H42 H 0.2176 0.4355 -0.0705 0.024 Uiso 1 1 calc R U . . .
F42 F 0.32547(15) 0.28114(14) 0.60962(12) 0.0368(5) Uani 1 1 d . . . . .
C43 C -0.0254(3) 0.2234(3) -0.0123(3) 0.0373(9) Uani 1 1 d . . . . .
H43A H -0.0812 0.2363 0.0049 0.056 Uiso 1 1 calc R U . . .
H43B H 0.0307 0.2305 0.0443 0.056 Uiso 1 1 calc R U . . .
H43C H -0.0571 0.1521 -0.0661 0.056 Uiso 1 1 calc R U . . .
F43 F 0.33642(15) 0.35681(15) 0.51352(14) 0.0439(5) Uani 1 1 d . . . . .
C44 C 0.0704(2) 0.4146(2) 0.0373(2) 0.0266(8) Uani 1 1 d . . . . .
H44A H 0.0134 0.4275 0.0525 0.040 Uiso 1 1 calc R U . . .
H44B H 0.1019 0.4641 0.0157 0.040 Uiso 1 1 calc R U . . .
H44C H 0.1261 0.4243 0.0958 0.040 Uiso 1 1 calc R U . . .
F44 F 0.25377(16) 0.18168(15) 0.44691(13) 0.0492(6) Uani 1 1 d . . . . .
C45 C 0.0781(3) 0.3794(3) -0.1932(2) 0.0313(8) Uani 1 1 d . . . . .
H45A H 0.1075 0.4261 -0.2182 0.047 Uiso 1 1 calc R U . . .
H45B H 0.0446 0.4101 -0.1543 0.047 Uiso 1 1 calc R U . . .
H45C H 0.0242 0.3107 -0.2479 0.047 Uiso 1 1 calc R U . . .
F45 F 0.15703(14) 0.26990(14) 0.42467(12) 0.0344(5) Uani 1 1 d . . . . .
C46 C 0.2338(3) 0.3353(3) -0.1826(2) 0.0306(8) Uani 1 1 d . . . . .
H46A H 0.2730 0.3943 -0.1909 0.046 Uiso 1 1 calc R U . . .
H46B H 0.1855 0.2741 -0.2466 0.046 Uiso 1 1 calc R U . . .
H46C H 0.2850 0.3178 -0.1444 0.046 Uiso 1 1 calc R U . . .
F46 F 0.14690(16) 0.19450(17) 0.52115(15) 0.0614(7) Uani 1 1 d . . . . .
C51 C 0.8514(2) 0.4904(2) 0.6168(2) 0.0177(7) Uani 1 1 d . . . . .
H51 H 0.8372 0.4900 0.5526 0.021 Uiso 1 1 calc R U . . .
C52 C 0.6256(2) 0.3599(2) 0.5662(2) 0.0214(7) Uani 1 1 d . . . . .
H52 H 0.6326 0.4176 0.6249 0.026 Uiso 1 1 calc R U . . .
C53 C 0.9671(2) 0.5058(2) 0.6628(2) 0.0247(8) Uani 1 1 d . . . . .
H53A H 1.0125 0.5534 0.6469 0.037 Uiso 1 1 calc R U . . .
H53B H 0.9694 0.4378 0.6372 0.037 Uiso 1 1 calc R U . . .
H53C H 0.9936 0.5362 0.7337 0.037 Uiso 1 1 calc R U . . .
C54 C 0.8370(3) 0.5811(2) 0.6799(2) 0.0316(8) Uani 1 1 d . . . . .
H54A H 0.8916 0.6477 0.6934 0.047 Uiso 1 1 calc R U . . .
H54B H 0.8446 0.5798 0.7414 0.047 Uiso 1 1 calc R U . . .
H54C H 0.7653 0.5746 0.6456 0.047 Uiso 1 1 calc R U . . .
C55 C 0.5832(3) 0.3805(3) 0.4803(2) 0.0306(8) Uani 1 1 d . . . . .
H55A H 0.5162 0.3864 0.4744 0.046 Uiso 1 1 calc R U . . .
H55B H 0.5696 0.3222 0.4203 0.046 Uiso 1 1 calc R U . . .
H55C H 0.6366 0.4462 0.4910 0.046 Uiso 1 1 calc R U . . .
C56 C 0.5456(2) 0.2569(2) 0.5509(2) 0.0287(8) Uani 1 1 d . . . . .
H56A H 0.4775 0.2604 0.5443 0.043 Uiso 1 1 calc R U . . .
H56B H 0.5743 0.2454 0.6070 0.043 Uiso 1 1 calc R U . . .
H56C H 0.5335 0.1988 0.4916 0.043 Uiso 1 1 calc R U . . .
C61 C 0.8466(2) 0.0245(2) 0.4396(2) 0.0172(7) Uani 1 1 d . . . . .
H61 H 0.8257 -0.0502 0.4267 0.021 Uiso 1 1 calc R U . . .
C62 C 0.6287(2) -0.0371(2) 0.2985(2) 0.0167(7) Uani 1 1 d . . . . .
H62 H 0.6608 -0.0161 0.2574 0.020 Uiso 1 1 calc R U . . .
C63 C 0.9319(2) 0.0946(2) 0.5455(2) 0.0240(7) Uani 1 1 d . . . . .
H63A H 0.9955 0.0815 0.5538 0.036 Uiso 1 1 calc R U . . .
H63B H 0.9029 0.0786 0.5889 0.036 Uiso 1 1 calc R U . . .
H63C H 0.9518 0.1686 0.5617 0.036 Uiso 1 1 calc R U . . .
C64 C 0.8914(2) 0.0387(2) 0.3688(2) 0.0224(7) Uani 1 1 d . . . . .
H64A H 0.9534 0.0226 0.3789 0.034 Uiso 1 1 calc R U . . .
H64B H 0.9139 0.1115 0.3801 0.034 Uiso 1 1 calc R U . . .
H64C H 0.8359 -0.0089 0.3017 0.034 Uiso 1 1 calc R U . . .
C65 C 0.6028(3) -0.1529(2) 0.2675(2) 0.0274(8) Uani 1 1 d . . . . .
H65A H 0.5526 -0.1953 0.1982 0.041 Uiso 1 1 calc R U . . .
H65B H 0.5701 -0.1759 0.3060 0.041 Uiso 1 1 calc R U . . .
H65C H 0.6691 -0.1615 0.2786 0.041 Uiso 1 1 calc R U . . .
C66 C 0.5282(2) -0.0196(2) 0.2811(2) 0.0276(8) Uani 1 1 d . . . . .
H66A H 0.4783 -0.0609 0.2116 0.041 Uiso 1 1 calc R U . . .
H66B H 0.5477 0.0552 0.3014 0.041 Uiso 1 1 calc R U . . .
H66C H 0.4937 -0.0416 0.3189 0.041 Uiso 1 1 calc R U . . .
C23 C 0.7652(2) 0.2518(2) 0.6902(2) 0.0161(7) Uani 1 1 d . . . . .
O23 O 0.77642(15) 0.17079(14) 0.30729(13) 0.0169(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.845(2) . ?
Ni1 P13 2.1106(8) . ?
Ni1 P12 2.2131(8) . ?
Ni1 P11 2.2163(8) . ?
N1 C16 1.376(3) . ?
N1 C13 1.384(3) . ?
Ni2 N2 1.848(2) . ?
Ni2 P23 2.1137(8) . ?
Ni2 P21 2.2075(8) . ?
Ni2 P22 2.2174(8) . ?
N2 C26 1.372(3) . ?
N2 C23 1.385(3) . ?
P3 F32 1.5842(18) . ?
P3 F31 1.5854(19) . ?
P3 F33 1.5870(18) . ?
P3 F34 1.591(2) . ?
P3 F35 1.5912(18) . ?
P3 F36 1.5929(18) . ?
P4 F46 1.571(2) . ?
P4 F44 1.5820(19) . ?
P4 F45 1.5872(18) . ?
P4 F41 1.5891(19) . ?
P4 F43 1.5904(19) . ?
P4 F42 1.5929(18) . ?
P11 C11 1.829(3) . ?
P11 C32 1.831(3) . ?
P11 C31 1.832(3) . ?
C11 C13 1.490(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
O11 C17 1.441(3) . ?
O11 P13 1.5794(19) . ?
P12 C12 1.826(3) . ?
P12 C42 1.829(3) . ?
P12 C41 1.831(3) . ?
C12 C16 1.488(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O12 C18 1.454(3) . ?
O12 P13 1.5873(19) . ?
P13 O13 1.5715(19) . ?
C13 C14 1.360(4) . ?
O13 C19 1.453(3) . ?
C14 C15 1.421(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.358(4) . ?
C15 H15 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
P21 C21 1.826(3) . ?
P21 C51 1.829(3) . ?
P21 C52 1.841(3) . ?
C21 C23 1.483(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
O21 C27 1.449(3) . ?
O21 P23 1.5898(19) . ?
P22 C22 1.825(3) . ?
P22 C61 1.828(3) . ?
P22 C62 1.829(3) . ?
C22 C26 1.487(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
O22 C28 1.446(3) . ?
O22 P23 1.5667(19) . ?
P23 O23 1.5763(19) . ?
C24 C23 1.361(4) . ?
C24 C25 1.416(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.364(4) . ?
C25 H25 0.9500 . ?
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 O23 1.448(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 C34 1.525(4) . ?
C31 C33 1.530(4) . ?
C31 H31 1.0000 . ?
C32 C35 1.522(4) . ?
C32 C36 1.529(4) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C41 C43 1.516(4) . ?
C41 C44 1.523(4) . ?
C41 H41 1.0000 . ?
C42 C46 1.521(4) . ?
C42 C45 1.528(4) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C51 C54 1.517(4) . ?
C51 C53 1.530(4) . ?
C51 H51 1.0000 . ?
C52 C56 1.523(4) . ?
C52 C55 1.525(4) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
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 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C61 C64 1.521(4) . ?
C61 C63 1.532(4) . ?
C61 H61 1.0000 . ?
C62 C66 1.518(4) . ?
C62 C65 1.529(4) . ?
C62 H62 1.0000 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 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
N1 Ni1 P13 174.34(8) . . ?
N1 Ni1 P12 83.01(7) . . ?
P13 Ni1 P12 96.75(3) . . ?
N1 Ni1 P11 83.88(7) . . ?
P13 Ni1 P11 96.66(3) . . ?
P12 Ni1 P11 166.38(3) . . ?
C16 N1 C13 107.0(2) . . ?
C16 N1 Ni1 126.57(19) . . ?
C13 N1 Ni1 126.40(19) . . ?
N2 Ni2 P23 174.60(8) . . ?
N2 Ni2 P21 82.54(7) . . ?
P23 Ni2 P21 95.33(3) . . ?
N2 Ni2 P22 83.58(7) . . ?
P23 Ni2 P22 98.99(3) . . ?
P21 Ni2 P22 164.94(3) . . ?
C26 N2 C23 107.3(2) . . ?
C26 N2 Ni2 126.56(19) . . ?
C23 N2 Ni2 126.17(18) . . ?
F32 P3 F31 90.04(11) . . ?
F32 P3 F33 89.63(10) . . ?
F31 P3 F33 90.66(11) . . ?
F32 P3 F34 90.51(11) . . ?
F31 P3 F34 179.35(12) . . ?
F33 P3 F34 89.68(11) . . ?
F32 P3 F35 179.71(12) . . ?
F31 P3 F35 90.21(11) . . ?
F33 P3 F35 90.51(10) . . ?
F34 P3 F35 89.24(11) . . ?
F32 P3 F36 90.68(10) . . ?
F31 P3 F36 89.66(10) . . ?
F33 P3 F36 179.55(12) . . ?
F34 P3 F36 89.99(11) . . ?
F35 P3 F36 89.18(10) . . ?
F46 P4 F44 90.37(13) . . ?
F46 P4 F45 90.32(11) . . ?
F44 P4 F45 89.56(10) . . ?
F46 P4 F41 90.74(13) . . ?
F44 P4 F41 178.89(13) . . ?
F45 P4 F41 90.39(10) . . ?
F46 P4 F43 179.50(13) . . ?
F44 P4 F43 89.57(12) . . ?
F45 P4 F43 90.17(11) . . ?
F41 P4 F43 89.32(11) . . ?
F46 P4 F42 90.14(11) . . ?
F44 P4 F42 90.43(10) . . ?
F45 P4 F42 179.54(13) . . ?
F41 P4 F42 89.61(10) . . ?
F43 P4 F42 89.37(11) . . ?
C11 P11 C32 108.60(14) . . ?
C11 P11 C31 105.56(13) . . ?
C32 P11 C31 107.64(13) . . ?
C11 P11 Ni1 102.30(9) . . ?
C32 P11 Ni1 110.43(9) . . ?
C31 P11 Ni1 121.52(9) . . ?
C13 C11 P11 106.78(19) . . ?
C13 C11 H11A 110.4 . . ?
P11 C11 H11A 110.4 . . ?
C13 C11 H11B 110.4 . . ?
P11 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
C17 O11 P13 122.98(18) . . ?
C12 P12 C42 105.68(14) . . ?
C12 P12 C41 103.29(14) . . ?
C42 P12 C41 107.84(14) . . ?
C12 P12 Ni1 102.35(10) . . ?
C42 P12 Ni1 123.20(10) . . ?
C41 P12 Ni1 112.29(10) . . ?
C16 C12 P12 106.21(19) . . ?
C16 C12 H12A 110.5 . . ?
P12 C12 H12A 110.5 . . ?
C16 C12 H12B 110.5 . . ?
P12 C12 H12B 110.5 . . ?
H12A C12 H12B 108.7 . . ?
C18 O12 P13 119.44(17) . . ?
O13 P13 O11 106.93(10) . . ?
O13 P13 O12 99.99(10) . . ?
O11 P13 O12 104.85(11) . . ?
O13 P13 Ni1 115.90(8) . . ?
O11 P13 Ni1 111.65(8) . . ?
O12 P13 Ni1 116.26(8) . . ?
C14 C13 N1 109.2(2) . . ?
C14 C13 C11 133.8(3) . . ?
N1 C13 C11 116.9(2) . . ?
C19 O13 P13 126.32(18) . . ?
C13 C14 C15 107.1(3) . . ?
C13 C14 H14 126.4 . . ?
C15 C14 H14 126.4 . . ?
C16 C15 C14 107.0(2) . . ?
C16 C15 H15 126.5 . . ?
C14 C15 H15 126.5 . . ?
O13 C19 H19A 109.5 . . ?
O13 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O13 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O12 C18 H18A 109.5 . . ?
O12 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O12 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O11 C17 H17A 109.5 . . ?
O11 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O11 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C16 N1 109.6(2) . . ?
C15 C16 C12 133.3(3) . . ?
N1 C16 C12 117.0(2) . . ?
C21 P21 C51 105.22(13) . . ?
C21 P21 C52 103.59(14) . . ?
C51 P21 C52 107.77(13) . . ?
C21 P21 Ni2 101.95(9) . . ?
C51 P21 Ni2 122.70(10) . . ?
C52 P21 Ni2 113.37(10) . . ?
C23 C21 P21 105.87(19) . . ?
C23 C21 H21A 110.6 . . ?
P21 C21 H21A 110.6 . . ?
C23 C21 H21B 110.6 . . ?
P21 C21 H21B 110.6 . . ?
H21A C21 H21B 108.7 . . ?
C27 O21 P23 119.71(17) . . ?
C22 P22 C61 103.95(13) . . ?
C22 P22 C62 105.75(14) . . ?
C61 P22 C62 107.19(13) . . ?
C22 P22 Ni2 101.52(10) . . ?
C61 P22 Ni2 116.94(10) . . ?
C62 P22 Ni2 119.53(9) . . ?
C26 C22 P22 106.88(19) . . ?
C26 C22 H22A 110.3 . . ?
P22 C22 H22A 110.3 . . ?
C26 C22 H22B 110.3 . . ?
P22 C22 H22B 110.3 . . ?
H22A C22 H22B 108.6 . . ?
C28 O22 P23 126.05(19) . . ?
O22 P23 O23 108.64(11) . . ?
O22 P23 O21 100.20(10) . . ?
O23 P23 O21 104.72(10) . . ?
O22 P23 Ni2 112.61(8) . . ?
O23 P23 Ni2 113.74(7) . . ?
O21 P23 Ni2 115.79(7) . . ?
C23 C24 C25 107.2(3) . . ?
C23 C24 H24 126.4 . . ?
C25 C24 H24 126.4 . . ?
C26 C25 C24 107.1(3) . . ?
C26 C25 H25 126.5 . . ?
C24 C25 H25 126.5 . . ?
C25 C26 N2 109.4(3) . . ?
C25 C26 C22 134.1(3) . . ?
N2 C26 C22 116.4(2) . . ?
O21 C27 H27A 109.5 . . ?
O21 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O21 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O22 C28 H28A 109.5 . . ?
O22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O23 C29 H29A 109.5 . . ?
O23 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O23 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C34 C31 C33 109.0(2) . . ?
C34 C31 P11 110.61(19) . . ?
C33 C31 P11 113.6(2) . . ?
C34 C31 H31 107.8 . . ?
C33 C31 H31 107.8 . . ?
P11 C31 H31 107.8 . . ?
C35 C32 C36 110.8(2) . . ?
C35 C32 P11 115.6(2) . . ?
C36 C32 P11 110.1(2) . . ?
C35 C32 H32 106.6 . . ?
C36 C32 H32 106.6 . . ?
P11 C32 H32 106.6 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C32 C36 H36A 109.5 . . ?
C32 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C32 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C43 C41 C44 111.1(3) . . ?
C43 C41 P12 110.2(2) . . ?
C44 C41 P12 114.1(2) . . ?
C43 C41 H41 107.0 . . ?
C44 C41 H41 107.0 . . ?
P12 C41 H41 107.0 . . ?
C46 C42 C45 110.7(2) . . ?
C46 C42 P12 111.3(2) . . ?
C45 C42 P12 112.1(2) . . ?
C46 C42 H42 107.5 . . ?
C45 C42 H42 107.5 . . ?
P12 C42 H42 107.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C54 C51 C53 110.6(2) . . ?
C54 C51 P21 113.2(2) . . ?
C53 C51 P21 109.45(19) . . ?
C54 C51 H51 107.8 . . ?
C53 C51 H51 107.8 . . ?
P21 C51 H51 107.8 . . ?
C56 C52 C55 110.9(3) . . ?
C56 C52 P21 110.6(2) . . ?
C55 C52 P21 113.6(2) . . ?
C56 C52 H52 107.1 . . ?
C55 C52 H52 107.1 . . ?
P21 C52 H52 107.1 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C52 C56 H56A 109.5 . . ?
C52 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C52 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C64 C61 C63 111.4(2) . . ?
C64 C61 P22 114.26(19) . . ?
C63 C61 P22 108.94(19) . . ?
C64 C61 H61 107.3 . . ?
C63 C61 H61 107.3 . . ?
P22 C61 H61 107.3 . . ?
C66 C62 C65 111.7(2) . . ?
C66 C62 P22 110.1(2) . . ?
C65 C62 P22 111.79(19) . . ?
C66 C62 H62 107.7 . . ?
C65 C62 H62 107.7 . . ?
P22 C62 H62 107.7 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C62 C65 H65A 109.5 . . ?
C62 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C62 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C62 C66 H66A 109.5 . . ?
C62 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C62 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C24 C23 N2 109.0(2) . . ?
C24 C23 C21 134.4(3) . . ?
N2 C23 C21 116.5(2) . . ?
C29 O23 P23 124.64(17) . . ?

_refine_diff_density_max         0.428
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.078

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_jk2_58
_database_code_depnum_ccdc_archive 'CCDC 1565542'
_audit_update_record             
;
2017-07-28 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H43 F6 N Ni P4'
_chemical_formula_weight         606.15

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   8.2850(17)
_cell_length_b                   15.792(3)
_cell_length_c                   21.433(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.379(3)
_cell_angle_gamma                90.00
_cell_volume                     2796.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5197
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      23.47

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6732
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
'Bruker AXS area detector scaling and absorption correction'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40751
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4861
_reflns_number_gt                3825
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0582P)²+1.1155P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4861
_refine_ls_number_parameters     312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1713
_refine_ls_wR_factor_gt          0.1642
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.38187(8) 0.17841(4) 0.24940(3) 0.0158(2) Uani 1 1 d . . .
F1 F 0.1833(4) 0.0045(2) 0.48131(17) 0.0330(9) Uani 1 1 d . . .
C1 C 0.5668(8) 0.2658(4) 0.1403(3) 0.0253(13) Uani 1 1 d . . .
H1A H 0.6609 0.2325 0.1284 0.030 Uiso 1 1 calc R . .
H1B H 0.5425 0.3102 0.1082 0.030 Uiso 1 1 calc R . .
P1 P 0.39082(18) 0.19686(9) 0.14638(7) 0.0189(3) Uani 1 1 d . . .
P2 P 0.41815(18) 0.18760(9) 0.35377(7) 0.0188(3) Uani 1 1 d . . .
C2 C 0.5122(8) 0.2921(4) 0.3657(3) 0.0256(13) Uani 1 1 d . . .
H2A H 0.4306 0.3342 0.3767 0.031 Uiso 1 1 calc R . .
H2B H 0.5991 0.2897 0.4000 0.031 Uiso 1 1 calc R . .
F2 F -0.0335(4) 0.0924(2) 0.47058(16) 0.0322(9) Uani 1 1 d . . .
P3 P 0.21570(19) 0.06889(10) 0.24118(7) 0.0224(4) Uani 1 1 d . . .
F3 F -0.0540(5) -0.0415(2) 0.43384(16) 0.0363(9) Uani 1 1 d . . .
C3 C 0.6021(7) 0.3052(4) 0.2036(3) 0.0223(13) Uani 1 1 d . . .
N N 0.5234(6) 0.2722(3) 0.2524(2) 0.0194(10) Uani 1 1 d . . .
P4 P 0.5000 0.5000 0.5000 0.0241(5) Uani 1 2 d S . .
F4 F 0.6138(5) 0.4743(3) 0.4468(2) 0.0493(11) Uani 1 1 d . . .
C4 C 0.7039(7) 0.3684(4) 0.2256(3) 0.0238(13) Uani 1 1 d . . .
H4 H 0.7712 0.4020 0.2015 0.029 Uiso 1 1 calc R . .
P5 P 0.0000 0.0000 0.5000 0.0215(5) Uani 1 2 d S . .
F5 F 0.4772(5) 0.5925(2) 0.47024(18) 0.0411(10) Uani 1 1 d . . .
C5 C 0.6908(7) 0.3746(4) 0.2903(3) 0.0246(13) Uani 1 1 d . . .
H5 H 0.7483 0.4128 0.3182 0.030 Uiso 1 1 calc R . .
C6 C 0.5802(7) 0.3159(4) 0.3059(3) 0.0219(12) Uani 1 1 d . . .
F6 F 0.6534(5) 0.5328(2) 0.54307(19) 0.0432(10) Uani 1 1 d . . .
C11 C 0.4243(9) 0.1090(4) 0.0933(3) 0.0308(15) Uani 1 1 d . . .
H11 H 0.3304 0.0695 0.0949 0.037 Uiso 1 1 calc R . .
C12 C 0.2074(8) 0.2553(4) 0.1147(3) 0.0290(14) Uani 1 1 d . . .
H12 H 0.1292 0.2130 0.0952 0.035 Uiso 1 1 calc R . .
C13 C 0.5748(9) 0.0606(5) 0.1170(4) 0.0449(19) Uani 1 1 d . . .
H13A H 0.5747 0.0048 0.0971 0.067 Uiso 1 1 calc R . .
H13B H 0.5757 0.0537 0.1625 0.067 Uiso 1 1 calc R . .
H13C H 0.6713 0.0921 0.1068 0.067 Uiso 1 1 calc R . .
C14 C 0.4324(10) 0.1357(5) 0.0249(3) 0.047(2) Uani 1 1 d . . .
H14A H 0.4546 0.0859 -0.0004 0.070 Uiso 1 1 calc R . .
H14B H 0.5190 0.1774 0.0220 0.070 Uiso 1 1 calc R . .
H14C H 0.3288 0.1607 0.0095 0.070 Uiso 1 1 calc R . .
C15 C 0.1258(9) 0.2996(5) 0.1678(3) 0.0406(17) Uani 1 1 d . . .
H15A H 0.1933 0.3470 0.1837 0.061 Uiso 1 1 calc R . .
H15B H 0.1126 0.2591 0.2018 0.061 Uiso 1 1 calc R . .
H15C H 0.0194 0.3208 0.1519 0.061 Uiso 1 1 calc R . .
C16 C 0.2391(10) 0.3216(5) 0.0652(4) 0.049(2) Uani 1 1 d . . .
H16A H 0.2822 0.2938 0.0291 0.073 Uiso 1 1 calc R . .
H16B H 0.3179 0.3631 0.0830 0.073 Uiso 1 1 calc R . .
H16C H 0.1377 0.3505 0.0518 0.073 Uiso 1 1 calc R . .
C23 C 0.1187(8) 0.2479(4) 0.3820(3) 0.0312(15) Uani 1 1 d . . .
H23A H 0.1554 0.3066 0.3876 0.047 Uiso 1 1 calc R . .
H23B H 0.0228 0.2388 0.4052 0.047 Uiso 1 1 calc R . .
H23C H 0.0914 0.2370 0.3375 0.047 Uiso 1 1 calc R . .
C22 C 0.5784(7) 0.1144(4) 0.3853(3) 0.0221(13) Uani 1 1 d . . .
H22 H 0.6225 0.1372 0.4267 0.027 Uiso 1 1 calc R . .
C21 C 0.2543(7) 0.1874(4) 0.4067(3) 0.0211(12) Uani 1 1 d . . .
H21 H 0.2079 0.1290 0.4065 0.025 Uiso 1 1 calc R . .
C31 C 0.1216(7) 0.0302(4) 0.3093(3) 0.0250(13) Uani 1 1 d . . .
H31A H 0.0538 0.0748 0.3253 0.038 Uiso 1 1 calc R . .
H31B H 0.2057 0.0140 0.3417 0.038 Uiso 1 1 calc R . .
H31C H 0.0545 -0.0193 0.2976 0.038 Uiso 1 1 calc R . .
C26 C 0.5201(8) 0.0247(4) 0.3958(3) 0.0284(14) Uani 1 1 d . . .
H26A H 0.4871 -0.0015 0.3554 0.043 Uiso 1 1 calc R . .
H26B H 0.4277 0.0262 0.4217 0.043 Uiso 1 1 calc R . .
H26C H 0.6080 -0.0084 0.4171 0.043 Uiso 1 1 calc R . .
C25 C 0.7167(7) 0.1135(4) 0.3419(3) 0.0312(15) Uani 1 1 d . . .
H25A H 0.6757 0.0941 0.3002 0.047 Uiso 1 1 calc R . .
H25B H 0.8020 0.0751 0.3588 0.047 Uiso 1 1 calc R . .
H25C H 0.7609 0.1708 0.3388 0.047 Uiso 1 1 calc R . .
C24 C 0.3140(9) 0.2085(4) 0.4740(3) 0.0335(16) Uani 1 1 d . . .
H24A H 0.3586 0.2660 0.4757 0.050 Uiso 1 1 calc R . .
H24B H 0.3983 0.1681 0.4886 0.050 Uiso 1 1 calc R . .
H24C H 0.2235 0.2050 0.5007 0.050 Uiso 1 1 calc R . .
C32 C 0.3056(10) -0.0293(4) 0.2129(3) 0.0390(18) Uani 1 1 d . . .
H32A H 0.2267 -0.0755 0.2137 0.058 Uiso 1 1 calc R . .
H32B H 0.4024 -0.0437 0.2399 0.058 Uiso 1 1 calc R . .
H32C H 0.3354 -0.0209 0.1699 0.058 Uiso 1 1 calc R . .
C33 C 0.0364(9) 0.0812(5) 0.1878(3) 0.045(2) Uani 1 1 d . . .
H33A H 0.0687 0.0897 0.1452 0.067 Uiso 1 1 calc R . .
H33B H -0.0258 0.1303 0.2003 0.067 Uiso 1 1 calc R . .
H33C H -0.0306 0.0301 0.1890 0.067 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni N 1.887(5) . ?
Ni P3 2.2093(16) . ?
Ni P1 2.2340(16) . ?
Ni P2 2.2388(16) . ?
F1 P5 1.601(3) . ?
C1 C3 1.502(8) . ?
C1 P1 1.833(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
P1 C11 1.829(6) . ?
P1 C12 1.861(6) . ?
P2 C2 1.834(6) . ?
P2 C21 1.834(6) . ?
P2 C22 1.849(6) . ?
C2 C6 1.486(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
F2 P5 1.605(3) . ?
P3 C31 1.812(6) . ?
P3 C33 1.815(7) . ?
P3 C32 1.843(7) . ?
F3 P5 1.595(3) . ?
C3 C4 1.367(8) . ?
C3 N 1.377(7) . ?
N C6 1.389(7) . ?
P4 F4 1.586(4) 3_666 ?
P4 F4 1.586(4) . ?
P4 F5 1.599(3) 3_666 ?
P4 F5 1.599(3) . ?
P4 F6 1.599(4) 3_666 ?
P4 F6 1.599(4) . ?
C4 C5 1.404(8) . ?
C4 H4 0.9500 . ?
P5 F3 1.595(4) 3_556 ?
P5 F1 1.601(3) 3_556 ?
P5 F2 1.605(3) 3_556 ?
C5 C6 1.363(8) . ?
C5 H5 0.9500 . ?
C11 C13 1.516(10) . ?
C11 C14 1.530(9) . ?
C11 H11 1.0000 . ?
C12 C16 1.528(9) . ?
C12 C15 1.536(9) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C23 C21 1.537(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C22 C26 1.518(8) . ?
C22 C25 1.530(8) . ?
C22 H22 1.0000 . ?
C21 C24 1.525(8) . ?
C21 H21 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 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
N Ni P3 177.41(15) . . ?
N Ni P1 82.20(14) . . ?
P3 Ni P1 95.21(6) . . ?
N Ni P2 83.05(15) . . ?
P3 Ni P2 99.54(6) . . ?
P1 Ni P2 165.24(6) . . ?
C3 C1 P1 106.4(4) . . ?
C3 C1 H1A 110.4 . . ?
P1 C1 H1A 110.4 . . ?
C3 C1 H1B 110.4 . . ?
P1 C1 H1B 110.4 . . ?
H1A C1 H1B 108.6 . . ?
C11 P1 C1 104.3(3) . . ?
C11 P1 C12 107.9(3) . . ?
C1 P1 C12 108.1(3) . . ?
C11 P1 Ni 122.3(2) . . ?
C1 P1 Ni 103.59(19) . . ?
C12 P1 Ni 109.7(2) . . ?
C2 P2 C21 104.0(3) . . ?
C2 P2 C22 103.1(3) . . ?
C21 P2 C22 108.5(3) . . ?
C2 P2 Ni 102.7(2) . . ?
C21 P2 Ni 124.6(2) . . ?
C22 P2 Ni 111.25(19) . . ?
C6 C2 P2 107.0(4) . . ?
C6 C2 H2A 110.3 . . ?
P2 C2 H2A 110.3 . . ?
C6 C2 H2B 110.3 . . ?
P2 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
C31 P3 C33 99.3(3) . . ?
C31 P3 C32 101.0(3) . . ?
C33 P3 C32 102.4(4) . . ?
C31 P3 Ni 120.2(2) . . ?
C33 P3 Ni 116.2(2) . . ?
C32 P3 Ni 114.8(2) . . ?
C4 C3 N 109.3(5) . . ?
C4 C3 C1 133.3(5) . . ?
N C3 C1 117.3(5) . . ?
C3 N C6 106.8(5) . . ?
C3 N Ni 126.9(4) . . ?
C6 N Ni 126.1(4) . . ?
F4 P4 F4 180.000(1) 3_666 . ?
F4 P4 F5 90.3(2) 3_666 3_666 ?
F4 P4 F5 89.7(2) . 3_666 ?
F4 P4 F5 89.7(2) 3_666 . ?
F4 P4 F5 90.3(2) . . ?
F5 P4 F5 180.0(3) 3_666 . ?
F4 P4 F6 90.4(2) 3_666 3_666 ?
F4 P4 F6 89.6(2) . 3_666 ?
F5 P4 F6 90.0(2) 3_666 3_666 ?
F5 P4 F6 90.0(2) . 3_666 ?
F4 P4 F6 89.6(2) 3_666 . ?
F4 P4 F6 90.4(2) . . ?
F5 P4 F6 90.0(2) 3_666 . ?
F5 P4 F6 90.0(2) . . ?
F6 P4 F6 180.000(1) 3_666 . ?
C3 C4 C5 107.4(5) . . ?
C3 C4 H4 126.3 . . ?
C5 C4 H4 126.3 . . ?
F3 P5 F3 180.000(1) 3_556 . ?
F3 P5 F1 89.8(2) 3_556 . ?
F3 P5 F1 90.2(2) . . ?
F3 P5 F1 90.2(2) 3_556 3_556 ?
F3 P5 F1 89.8(2) . 3_556 ?
F1 P5 F1 180.0(2) . 3_556 ?
F3 P5 F2 90.24(19) 3_556 . ?
F3 P5 F2 89.76(19) . . ?
F1 P5 F2 90.04(18) . . ?
F1 P5 F2 89.96(18) 3_556 . ?
F3 P5 F2 89.76(19) 3_556 3_556 ?
F3 P5 F2 90.24(19) . 3_556 ?
F1 P5 F2 89.96(18) . 3_556 ?
F1 P5 F2 90.04(18) 3_556 3_556 ?
F2 P5 F2 180.0(2) . 3_556 ?
C6 C5 C4 107.4(5) . . ?
C6 C5 H5 126.3 . . ?
C4 C5 H5 126.3 . . ?
C5 C6 N 109.1(5) . . ?
C5 C6 C2 133.6(5) . . ?
N C6 C2 117.3(5) . . ?
C13 C11 C14 111.4(6) . . ?
C13 C11 P1 109.5(5) . . ?
C14 C11 P1 114.0(5) . . ?
C13 C11 H11 107.2 . . ?
C14 C11 H11 107.2 . . ?
P1 C11 H11 107.2 . . ?
C16 C12 C15 108.1(6) . . ?
C16 C12 P1 114.5(5) . . ?
C15 C12 P1 110.4(4) . . ?
C16 C12 H12 107.9 . . ?
C15 C12 H12 107.9 . . ?
P1 C12 H12 107.9 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 H16A 109.5 . . ?
C12 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C12 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C22 C25 110.1(5) . . ?
C26 C22 P2 114.2(4) . . ?
C25 C22 P2 109.5(4) . . ?
C26 C22 H22 107.6 . . ?
C25 C22 H22 107.6 . . ?
P2 C22 H22 107.6 . . ?
C24 C21 C23 111.4(5) . . ?
C24 C21 P2 112.5(4) . . ?
C23 C21 P2 110.0(4) . . ?
C24 C21 H21 107.6 . . ?
C23 C21 H21 107.6 . . ?
P2 C21 H21 107.6 . . ?
P3 C31 H31A 109.5 . . ?
P3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
P3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P3 C32 H32A 109.5 . . ?
P3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
P3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
P3 C33 H33A 109.5 . . ?
P3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
P3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.120
