# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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#  except for the purpose of generating routine backup copies 
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data_rc038_0m
_database_code_depnum_ccdc_archive 'CCDC 915323'
#TrackingRef 'CIFs-revised.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H37 F6 N5 Ni P3'
_chemical_formula_weight         913.42
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           orthorhombic
_symmetry_space_group_name_H-M   Ibca
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'-x, -y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x, -y, -z'
'-x, y, z-1/2'
'x-1/2, -y, z'
'x, y-1/2, -z'
'-x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z+1/2'
'x+1/2, y, -z+1/2'
_cell_length_a                   15.7941(10)
_cell_length_b                   18.9012(11)
_cell_length_c                   28.6202(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8543.9(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3752
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6002
_exptl_absorpt_correction_T_max  0.8788
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(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  ?
_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            61503
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         27.59
_reflns_number_total             4929
_reflns_number_gt                3225
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1046P)^2^+23.0499P] where P=(Fo^2^+2Fc^2^)/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         4929
_refine_ls_number_parameters     287
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1979
_refine_ls_wR_factor_gt          0.1655
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Ni1 Ni 0.45687(4) 1.0000 0.2500 0.0237(2) Uani 1 2 d S . .
H100 H 0.564(5) 1.0000 0.2500 0.060 Uiso 1 2 d S . .
P1 P 0.7500 0.85498(12) 0.5000 0.1226(15) Uani 1 2 d S . .
P2 P 0.52046(6) 0.94712(5) 0.34759(3) 0.0266(2) Uani 1 1 d . A .
F1 F 0.7207(4) 0.9096(4) 0.5370(4) 0.350(9) Uani 1 1 d . . .
F2 F 0.7773(4) 0.7940(4) 0.4657(2) 0.182(3) Uani 1 1 d . . .
F3 F 0.8397(4) 0.8545(2) 0.52200(18) 0.139(2) Uani 1 1 d . . .
N1 N 0.4110(6) 0.1855(4) 0.3426(3) 0.144(4) Uani 1 1 d . . .
N2 N 0.3325(3) 1.0000 0.2500 0.0315(10) Uani 1 2 d S . .
N3 N 0.4467(2) 0.97239(18) 0.31340(11) 0.0299(7) Uani 1 1 d . . .
C1 C 0.4287(7) 0.1779(6) 0.3799(4) 0.134(4) Uani 1 1 d . . .
C2 C 0.4583(10) 0.1756(10) 0.4278(4) 0.279(12) Uani 1 1 d . . .
H2A H 0.4384 0.1319 0.4427 0.419 Uiso 1 1 calc R . .
H2B H 0.4360 0.2165 0.4449 0.419 Uiso 1 1 calc R . .
H2C H 0.5203 0.1768 0.4283 0.419 Uiso 1 1 calc R . .
C3 C 0.5835(3) 0.8770(2) 0.32271(15) 0.0364(9) Uani 1 1 d . . .
C4 C 0.6533(3) 0.8520(3) 0.3477(2) 0.0591(14) Uani 1 1 d . A .
H4A H 0.6703 0.8752 0.3756 0.071 Uiso 1 1 calc R . .
C5 C 0.6977(4) 0.7934(3) 0.3320(3) 0.087(2) Uani 1 1 d . . .
H5A H 0.7446 0.7761 0.3494 0.104 Uiso 1 1 calc R A .
C6 C 0.6745(5) 0.7613(3) 0.2925(3) 0.091(3) Uani 1 1 d . A .
H6A H 0.7056 0.7214 0.2818 0.110 Uiso 1 1 calc R . .
C7 C 0.6056(5) 0.7851(3) 0.2665(2) 0.084(2) Uani 1 1 d . . .
H7A H 0.5904 0.7618 0.2383 0.101 Uiso 1 1 calc R A .
C8 C 0.5587(4) 0.8435(2) 0.28211(18) 0.0545(13) Uani 1 1 d . A .
H8A H 0.5108 0.8596 0.2651 0.065 Uiso 1 1 calc R . .
C9 C 0.5918(2) 1.0167(2) 0.36623(14) 0.0301(8) Uani 1 1 d . . .
C10 C 0.6466(3) 1.0083(2) 0.40416(15) 0.0389(10) Uani 1 1 d . A .
H10A H 0.6472 0.9649 0.4209 0.047 Uiso 1 1 calc R . .
C11 C 0.7000(3) 1.0627(3) 0.41736(16) 0.0443(11) Uani 1 1 d . . .
H11A H 0.7371 1.0566 0.4432 0.053 Uiso 1 1 calc R A .
C12 C 0.6995(3) 1.1261(3) 0.39301(17) 0.0460(11) Uani 1 1 d . A .
H12A H 0.7359 1.1637 0.4021 0.055 Uiso 1 1 calc R . .
C13 C 0.6461(3) 1.1343(2) 0.35577(16) 0.0439(11) Uani 1 1 d . . .
H13A H 0.6459 1.1777 0.3390 0.053 Uiso 1 1 calc R A .
C14 C 0.5919(3) 1.0800(2) 0.34191(15) 0.0366(9) Uani 1 1 d . A .
H14A H 0.5553 1.0864 0.3159 0.044 Uiso 1 1 calc R . .
C15 C 0.4754(2) 0.9101(2) 0.40020(13) 0.0307(8) Uani 1 1 d . . .
C16 C 0.4504(3) 0.8388(2) 0.40035(16) 0.0399(10) Uani 1 1 d . A .
H16A H 0.4615 0.8097 0.3740 0.048 Uiso 1 1 calc R . .
C17 C 0.4094(3) 0.8111(3) 0.43918(18) 0.0481(12) Uani 1 1 d . . .
H17A H 0.3937 0.7626 0.4397 0.058 Uiso 1 1 calc R A .
C18 C 0.3915(3) 0.8541(3) 0.47703(16) 0.0468(12) Uani 1 1 d . A .
H18A H 0.3629 0.8351 0.5034 0.056 Uiso 1 1 calc R . .
C19 C 0.4152(3) 0.9250(3) 0.47662(15) 0.0497(12) Uani 1 1 d . . .
H19A H 0.4026 0.9544 0.5026 0.060 Uiso 1 1 calc R A .
C20 C 0.4571(3) 0.9528(3) 0.43846(15) 0.0422(10) Uani 1 1 d . A .
H20A H 0.4735 1.0012 0.4383 0.051 Uiso 1 1 calc R . .
C22 C 0.3608(3) 0.9863(3) 0.33263(16) 0.0465(12) Uani 1 1 d . A .
C23 C 0.3089(5) 1.0272(5) 0.2954(3) 0.041(2) Uani 0.50 1 d P A 2
C24 C 0.3002(5) 0.9658(5) 0.2909(3) 0.0370(19) Uani 0.50 1 d P A 1
C25 C 0.3016(6) 0.9198(4) 0.2487(4) 0.047(2) Uani 0.50 1 d P A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0260(3) 0.0211(3) 0.0239(3) 0.0020(3) 0.000 0.000
P1 0.169(3) 0.0399(12) 0.159(3) 0.000 -0.129(3) 0.000
P2 0.0301(5) 0.0233(5) 0.0264(5) 0.0041(4) 0.0025(4) 0.0012(4)
F1 0.174(8) 0.216(7) 0.66(2) -0.321(10) -0.241(11) 0.104(6)
F2 0.199(7) 0.177(6) 0.169(5) -0.072(5) -0.030(5) -0.060(5)
F3 0.167(5) 0.096(3) 0.154(4) -0.034(3) -0.115(4) 0.047(3)
N1 0.200(9) 0.091(5) 0.139(7) -0.005(5) -0.071(7) 0.039(5)
N2 0.030(2) 0.035(2) 0.029(2) 0.003(2) 0.000 0.000
N3 0.0284(17) 0.0334(16) 0.0279(17) 0.0035(13) 0.0018(13) 0.0010(13)
C1 0.154(9) 0.135(9) 0.114(8) -0.009(6) -0.043(7) 0.071(7)
C2 0.250(19) 0.48(3) 0.107(9) -0.051(13) -0.045(10) 0.206(19)
C3 0.045(2) 0.0229(18) 0.041(2) 0.0062(16) 0.0151(19) 0.0015(17)
C4 0.048(3) 0.040(3) 0.090(4) 0.015(3) 0.011(3) 0.014(2)
C5 0.072(4) 0.044(3) 0.143(7) 0.021(4) 0.047(4) 0.028(3)
C6 0.114(6) 0.030(3) 0.130(7) 0.023(4) 0.081(5) 0.030(3)
C7 0.152(7) 0.029(3) 0.071(4) -0.003(3) 0.059(4) -0.002(3)
C8 0.086(4) 0.027(2) 0.051(3) 0.003(2) 0.020(3) 0.002(2)
C9 0.0302(19) 0.029(2) 0.031(2) 0.0020(15) 0.0051(16) -0.0009(15)
C10 0.032(2) 0.044(2) 0.041(2) 0.0081(19) -0.0021(17) -0.0011(18)
C11 0.032(2) 0.061(3) 0.039(2) -0.007(2) -0.0026(18) -0.006(2)
C12 0.040(2) 0.050(3) 0.048(3) -0.009(2) 0.005(2) -0.015(2)
C13 0.048(3) 0.033(2) 0.051(3) 0.0014(19) 0.005(2) -0.0095(19)
C14 0.043(2) 0.031(2) 0.036(2) 0.0024(17) -0.0011(18) -0.0009(17)
C15 0.030(2) 0.032(2) 0.030(2) 0.0088(16) 0.0003(16) -0.0001(16)
C16 0.045(2) 0.029(2) 0.046(3) 0.0089(18) 0.0096(19) 0.0055(18)
C17 0.043(3) 0.041(2) 0.061(3) 0.025(2) 0.009(2) -0.002(2)
C18 0.039(2) 0.065(3) 0.036(2) 0.022(2) 0.005(2) -0.002(2)
C19 0.048(3) 0.071(3) 0.030(2) -0.004(2) 0.005(2) -0.016(2)
C20 0.046(2) 0.049(3) 0.031(2) 0.0021(19) 0.0025(18) -0.012(2)
C22 0.032(2) 0.072(3) 0.035(2) 0.013(2) 0.0062(18) 0.012(2)
C23 0.031(5) 0.056(6) 0.037(5) -0.001(4) 0.008(3) 0.017(4)
C24 0.037(5) 0.039(5) 0.034(5) 0.013(4) -0.002(3) -0.002(4)
C25 0.048(5) 0.027(4) 0.067(6) 0.006(4) -0.003(5) -0.020(4)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3 1.895(3) . ?
Ni1 N3 1.895(3) 2_575 ?
Ni1 N2 1.965(5) . ?
Ni1 H100 1.70(8) . ?
P1 F1 1.549(7) 3_656 ?
P1 F1 1.549(7) . ?
P1 F3 1.550(4) 3_656 ?
P1 F3 1.550(4) . ?
P1 F2 1.575(7) 3_656 ?
P1 F2 1.575(7) . ?
P2 N3 1.595(3) . ?
P2 C3 1.803(4) . ?
P2 C15 1.807(4) . ?
P2 C9 1.812(4) . ?
N1 C1 1.113(11) . ?
N2 C24 1.430(8) . ?
N2 C24 1.431(8) 2_575 ?
N2 C23 1.447(9) . ?
N2 C23 1.447(9) 2_575 ?
N2 C25 1.592(8) . ?
N2 C25 1.592(8) 2_575 ?
N3 C22 1.487(5) . ?
C1 C2 1.451(15) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C8 1.381(7) . ?
C3 C4 1.397(7) . ?
C4 C5 1.386(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.336(11) . ?
C5 H5A 0.9500 . ?
C6 C7 1.391(11) . ?
C6 H6A 0.9500 . ?
C7 C8 1.402(7) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 C14 1.383(5) . ?
C9 C10 1.398(6) . ?
C10 C11 1.382(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.387(7) . ?
C11 H11A 0.9500 . ?
C12 C13 1.368(7) . ?
C12 H12A 0.9500 . ?
C13 C14 1.394(6) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C20 1.391(6) . ?
C15 C16 1.403(6) . ?
C16 C17 1.389(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.384(7) . ?
C17 H17A 0.9500 . ?
C18 C19 1.392(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.381(6) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
C22 C23 1.550(10) . ?
C22 C24 1.579(10) . ?
C24 C25 1.489(13) . ?
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
N3 Ni1 N3 170.25(19) . 2_575 ?
N3 Ni1 N2 85.12(10) . . ?
N3 Ni1 N2 85.12(10) 2_575 . ?
N3 Ni1 H100 94.88(10) . . ?
N3 Ni1 H100 94.88(10) 2_575 . ?
N2 Ni1 H100 180.000(7) . . ?
F1 P1 F1 96.5(9) 3_656 . ?
F1 P1 F3 90.0(3) 3_656 3_656 ?
F1 P1 F3 90.5(3) . 3_656 ?
F1 P1 F3 90.5(3) 3_656 . ?
F1 P1 F3 90.0(3) . . ?
F3 P1 F3 179.3(4) 3_656 . ?
F1 P1 F2 174.7(5) 3_656 3_656 ?
F1 P1 F2 88.8(5) . 3_656 ?
F3 P1 F2 89.9(3) 3_656 3_656 ?
F3 P1 F2 89.5(3) . 3_656 ?
F1 P1 F2 88.8(5) 3_656 . ?
F1 P1 F2 174.7(5) . . ?
F3 P1 F2 89.5(3) 3_656 . ?
F3 P1 F2 89.9(3) . . ?
F2 P1 F2 86.0(6) 3_656 . ?
N3 P2 C3 112.4(2) . . ?
N3 P2 C15 109.83(17) . . ?
C3 P2 C15 105.20(18) . . ?
N3 P2 C9 114.66(18) . . ?
C3 P2 C9 107.85(19) . . ?
C15 P2 C9 106.32(18) . . ?
C24 N2 C24 138.3(7) . 2_575 ?
C24 N2 C23 48.2(5) . . ?
C24 N2 C23 118.9(5) 2_575 . ?
C24 N2 C23 118.9(5) . 2_575 ?
C24 N2 C23 48.2(5) 2_575 2_575 ?
C23 N2 C23 150.1(8) . 2_575 ?
C24 N2 C25 58.7(5) . . ?
C24 N2 C25 107.5(5) 2_575 . ?
C23 N2 C25 106.3(6) . . ?
C23 N2 C25 64.0(5) 2_575 . ?
C24 N2 C25 107.5(5) . 2_575 ?
C24 N2 C25 58.7(5) 2_575 2_575 ?
C23 N2 C25 64.0(5) . 2_575 ?
C23 N2 C25 106.3(6) 2_575 2_575 ?
C25 N2 C25 144.3(8) . 2_575 ?
C24 N2 Ni1 110.9(4) . . ?
C24 N2 Ni1 110.9(4) 2_575 . ?
C23 N2 Ni1 104.9(4) . . ?
C23 N2 Ni1 104.9(4) 2_575 . ?
C25 N2 Ni1 107.8(4) . . ?
C25 N2 Ni1 107.8(4) 2_575 . ?
C22 N3 P2 119.5(3) . . ?
C22 N3 Ni1 112.5(2) . . ?
P2 N3 Ni1 127.44(19) . . ?
N1 C1 C2 173.0(16) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C8 C3 C4 119.9(4) . . ?
C8 C3 P2 120.9(4) . . ?
C4 C3 P2 118.8(4) . . ?
C5 C4 C3 120.3(6) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C6 C5 C4 119.9(7) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C5 C6 C7 121.4(5) . . ?
C5 C6 H6A 119.3 . . ?
C7 C6 H6A 119.3 . . ?
C6 C7 C8 119.8(6) . . ?
C6 C7 H7A 120.1 . . ?
C8 C7 H7A 120.1 . . ?
C3 C8 C7 118.7(6) . . ?
C3 C8 H8A 120.7 . . ?
C7 C8 H8A 120.7 . . ?
C14 C9 C10 119.3(4) . . ?
C14 C9 P2 118.7(3) . . ?
C10 C9 P2 122.0(3) . . ?
C11 C10 C9 120.4(4) . . ?
C11 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C10 C11 C12 120.1(4) . . ?
C10 C11 H11A 119.9 . . ?
C12 C11 H11A 119.9 . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 H12A 120.3 . . ?
C11 C12 H12A 120.3 . . ?
C12 C13 C14 121.2(4) . . ?
C12 C13 H13A 119.4 . . ?
C14 C13 H13A 119.4 . . ?
C9 C14 C13 119.6(4) . . ?
C9 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C20 C15 C16 119.8(4) . . ?
C20 C15 P2 120.9(3) . . ?
C16 C15 P2 119.0(3) . . ?
C17 C16 C15 119.7(4) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C18 C17 C16 120.0(4) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C19 120.3(4) . . ?
C17 C18 H18A 119.9 . . ?
C19 C18 H18A 119.9 . . ?
C20 C19 C18 120.1(4) . . ?
C20 C19 H19A 119.9 . . ?
C18 C19 H19A 119.9 . . ?
C19 C20 C15 120.1(4) . . ?
C19 C20 H20A 120.0 . . ?
C15 C20 H20A 120.0 . . ?
N3 C22 C23 108.5(4) . . ?
N3 C22 C24 103.2(4) . . ?
C23 C22 C24 44.1(5) . . ?
N2 C23 C22 107.7(6) . . ?
N2 C24 C25 66.1(5) . . ?
N2 C24 C22 107.0(6) . . ?
C25 C24 C22 138.5(7) . . ?
C24 C25 N2 55.2(4) . . ?
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.59
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.102


data_rc039_0m
_database_code_depnum_ccdc_archive 'CCDC 915324'
#TrackingRef 'CIFs-revised.txt'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H43 F6 N4 Ni P3'
_chemical_formula_weight         869.42
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           triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.2878(9)
_cell_length_b                   12.0048(9)
_cell_length_c                   16.3353(11)
_cell_angle_alpha                99.854(2)
_cell_angle_beta                 100.657(2)
_cell_angle_gamma                106.872(2)
_cell_volume                     2021.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3462
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      23.11
_exptl_crystal_description       Block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             900
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9071
_exptl_absorpt_correction_T_max  0.9367
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(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  ?
_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            21734
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0805
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7002
_reflns_number_gt                4853
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0484P)^2^+1.3365P] where P=(Fo^2^+2Fc^2^)/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         7002
_refine_ls_number_parameters     510
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1161
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_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
Ni1 Ni 0.21094(4) 0.03290(4) 0.29953(3) 0.02011(14) Uani 1 1 d . . .
P1 P 0.21939(9) -0.12874(9) 0.13555(6) 0.0186(2) Uani 1 1 d . . .
P2 P 0.02423(9) 0.14723(9) 0.35999(6) 0.0189(2) Uani 1 1 d . . .
N1 N 0.2848(3) -0.0606(3) 0.23370(17) 0.0204(7) Uani 1 1 d . . .
N2 N 0.3797(3) 0.0976(3) 0.3805(2) 0.0369(9) Uani 1 1 d . . .
H2B H 0.4234 0.1679 0.3670 0.044 Uiso 1 1 calc R . .
N3 N 0.1544(3) 0.1194(3) 0.38416(17) 0.0214(7) Uani 1 1 d . . .
C1 C 0.0695(3) -0.2463(3) 0.1226(2) 0.0169(8) Uani 1 1 d . . .
C2 C 0.0104(3) -0.2581(3) 0.1899(2) 0.0219(8) Uani 1 1 d . . .
H2A H 0.0490 -0.2036 0.2444 0.026 Uiso 1 1 calc R . .
C3 C -0.1041(3) -0.3487(3) 0.1776(2) 0.0238(9) Uani 1 1 d . . .
H3A H -0.1426 -0.3573 0.2242 0.029 Uiso 1 1 calc R . .
C4 C -0.1630(4) -0.4268(3) 0.0984(2) 0.0251(9) Uani 1 1 d . . .
H4A H -0.2437 -0.4865 0.0897 0.030 Uiso 1 1 calc R . .
C5 C -0.1034(4) -0.4174(3) 0.0313(2) 0.0254(9) Uani 1 1 d . . .
H5A H -0.1426 -0.4720 -0.0231 0.030 Uiso 1 1 calc R . .
C6 C 0.0127(3) -0.3287(3) 0.0437(2) 0.0220(9) Uani 1 1 d . . .
H6A H 0.0541 -0.3240 -0.0018 0.026 Uiso 1 1 calc R . .
C7 C 0.1934(3) -0.0301(3) 0.0672(2) 0.0192(8) Uani 1 1 d . . .
C8 C 0.2586(3) 0.0919(3) 0.1001(2) 0.0244(9) Uani 1 1 d . . .
H8A H 0.3092 0.1203 0.1575 0.029 Uiso 1 1 calc R . .
C9 C 0.2500(4) 0.1722(4) 0.0497(3) 0.0304(10) Uani 1 1 d . . .
H9A H 0.2946 0.2555 0.0727 0.036 Uiso 1 1 calc R . .
C10 C 0.1768(4) 0.1319(4) -0.0341(2) 0.0303(10) Uani 1 1 d . . .
H10A H 0.1721 0.1871 -0.0689 0.036 Uiso 1 1 calc R . .
C11 C 0.1103(4) 0.0105(4) -0.0672(2) 0.0283(9) Uani 1 1 d . . .
H11A H 0.0585 -0.0171 -0.1243 0.034 Uiso 1 1 calc R . .
C12 C 0.1189(3) -0.0702(4) -0.0177(2) 0.0248(9) Uani 1 1 d . . .
H12A H 0.0743 -0.1533 -0.0411 0.030 Uiso 1 1 calc R . .
C13 C 0.3162(3) -0.2069(3) 0.0899(2) 0.0222(8) Uani 1 1 d . . .
C14 C 0.3685(4) -0.1772(4) 0.0224(2) 0.0303(10) Uani 1 1 d . . .
H14A H 0.3540 -0.1139 -0.0012 0.036 Uiso 1 1 calc R . .
C15 C 0.4419(4) -0.2404(4) -0.0104(3) 0.0395(11) Uani 1 1 d . . .
H15A H 0.4770 -0.2205 -0.0566 0.047 Uiso 1 1 calc R . .
C16 C 0.4634(4) -0.3313(4) 0.0242(3) 0.0386(11) Uani 1 1 d . . .
H16A H 0.5142 -0.3738 0.0020 0.046 Uiso 1 1 calc R . .
C17 C 0.4119(4) -0.3616(4) 0.0910(3) 0.0334(10) Uani 1 1 d . . .
H17A H 0.4269 -0.4250 0.1142 0.040 Uiso 1 1 calc R . .
C18 C 0.3386(3) -0.3000(3) 0.1239(2) 0.0258(9) Uani 1 1 d . . .
H18A H 0.3033 -0.3210 0.1699 0.031 Uiso 1 1 calc R . .
C19 C 0.4242(3) -0.0291(3) 0.2705(2) 0.0252(9) Uani 1 1 d . . .
H19A H 0.4731 0.0333 0.2455 0.030 Uiso 1 1 calc R . .
H19B H 0.4508 -0.1006 0.2580 0.030 Uiso 1 1 calc R . .
C20 C 0.4486(4) 0.0168(4) 0.3655(3) 0.0381(11) Uani 1 1 d . . .
H20A H 0.4200 -0.0508 0.3925 0.046 Uiso 1 1 calc R . .
H20B H 0.5411 0.0586 0.3910 0.046 Uiso 1 1 calc R . .
C21 C 0.3583(4) 0.1333(4) 0.4667(2) 0.0318(10) Uani 1 1 d . . .
H21A H 0.4394 0.1862 0.5078 0.038 Uiso 1 1 calc R . .
H21B H 0.3238 0.0617 0.4886 0.038 Uiso 1 1 calc R . .
C22 C 0.2643(4) 0.1983(4) 0.4551(2) 0.0288(9) Uani 1 1 d . . .
H22A H 0.2362 0.2152 0.5084 0.035 Uiso 1 1 calc R . .
H22B H 0.3033 0.2752 0.4406 0.035 Uiso 1 1 calc R . .
C23 C -0.1065(3) 0.0090(3) 0.3163(2) 0.0180(8) Uani 1 1 d . . .
C24 C -0.1066(4) -0.0868(3) 0.3542(2) 0.0242(9) Uani 1 1 d . . .
H24A H -0.0354 -0.0796 0.3986 0.029 Uiso 1 1 calc R . .
C25 C -0.2092(4) -0.1915(3) 0.3276(2) 0.0270(9) Uani 1 1 d . . .
H25A H -0.2088 -0.2559 0.3542 0.032 Uiso 1 1 calc R . .
C26 C -0.3129(4) -0.2035(4) 0.2627(2) 0.0287(9) Uani 1 1 d . . .
H26A H -0.3839 -0.2757 0.2450 0.034 Uiso 1 1 calc R . .
C27 C -0.3132(4) -0.1104(3) 0.2237(2) 0.0272(9) Uani 1 1 d . . .
H27A H -0.3838 -0.1194 0.1781 0.033 Uiso 1 1 calc R . .
C28 C -0.2110(3) -0.0033(3) 0.2503(2) 0.0225(9) Uani 1 1 d . . .
H28A H -0.2123 0.0610 0.2238 0.027 Uiso 1 1 calc R . .
C29 C -0.0125(3) 0.2227(3) 0.4533(2) 0.0196(8) Uani 1 1 d . . .
C30 C -0.1114(4) 0.1658(4) 0.4867(2) 0.0311(10) Uani 1 1 d . . .
H30A H -0.1633 0.0853 0.4596 0.037 Uiso 1 1 calc R . .
C31 C -0.1353(4) 0.2248(4) 0.5591(3) 0.0395(11) Uani 1 1 d . . .
H31A H -0.2032 0.1846 0.5814 0.047 Uiso 1 1 calc R . .
C32 C -0.0611(4) 0.3414(4) 0.5988(2) 0.0340(10) Uani 1 1 d . . .
H32A H -0.0777 0.3818 0.6485 0.041 Uiso 1 1 calc R . .
C33 C 0.0370(4) 0.3994(4) 0.5663(2) 0.0366(11) Uani 1 1 d . . .
H33A H 0.0889 0.4798 0.5939 0.044 Uiso 1 1 calc R . .
C34 C 0.0603(4) 0.3405(3) 0.4930(2) 0.0305(10) Uani 1 1 d . . .
H34A H 0.1270 0.3817 0.4701 0.037 Uiso 1 1 calc R . .
C35 C 0.0234(3) 0.2471(3) 0.2884(2) 0.0193(8) Uani 1 1 d . . .
C36 C -0.0729(4) 0.2977(3) 0.2750(2) 0.0271(9) Uani 1 1 d . . .
H36A H -0.1427 0.2757 0.3005 0.033 Uiso 1 1 calc R . .
C37 C -0.0674(4) 0.3795(3) 0.2247(2) 0.0284(9) Uani 1 1 d . . .
H37A H -0.1348 0.4118 0.2141 0.034 Uiso 1 1 calc R . .
C38 C 0.0359(4) 0.4146(3) 0.1896(2) 0.0295(10) Uani 1 1 d . . .
H38A H 0.0408 0.4730 0.1566 0.035 Uiso 1 1 calc R . .
C39 C 0.1318(4) 0.3652(3) 0.2025(2) 0.0296(10) Uani 1 1 d . . .
H39A H 0.2022 0.3887 0.1777 0.035 Uiso 1 1 calc R . .
C40 C 0.1254(4) 0.2813(3) 0.2514(2) 0.0258(9) Uani 1 1 d . . .
H40A H 0.1913 0.2468 0.2597 0.031 Uiso 1 1 calc R . .
P3 P 0.57149(11) 0.40764(10) 0.29208(7) 0.0364(3) Uani 1 1 d . . .
F5 F 0.4673(3) 0.3474(3) 0.3395(2) 0.0881(11) Uani 1 1 d . . .
F1 F 0.6766(3) 0.4684(3) 0.2482(2) 0.0934(12) Uani 1 1 d . . .
F2 F 0.5356(3) 0.2843(3) 0.2267(2) 0.1007(13) Uani 1 1 d . . .
F3 F 0.6103(3) 0.5286(3) 0.3616(2) 0.0989(12) Uani 1 1 d . . .
F6 F 0.6724(3) 0.3688(3) 0.3508(2) 0.0975(12) Uani 1 1 d . . .
F4 F 0.4707(4) 0.4474(4) 0.2386(3) 0.1293(17) Uani 1 1 d . . .
C41 C 0.6414(4) 0.3633(4) 0.6254(3) 0.0410(11) Uani 1 1 d . . .
C42 C 0.6451(5) 0.4475(4) 0.5714(3) 0.0618(15) Uani 1 1 d . . .
H42A H 0.6771 0.4221 0.5221 0.093 Uiso 1 1 calc R . .
H42B H 0.7020 0.5274 0.6045 0.093 Uiso 1 1 calc R . .
H42C H 0.5589 0.4501 0.5512 0.093 Uiso 1 1 calc R . .
N4 N 0.6379(5) 0.2961(4) 0.6657(3) 0.0667(13) Uani 1 1 d . . .
H100 H 0.091(4) -0.002(3) 0.236(2) 0.039(11) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0179(3) 0.0250(3) 0.0141(2) -0.0007(2) -0.00114(19) 0.0086(2)
P1 0.0174(5) 0.0212(6) 0.0164(5) 0.0026(4) 0.0037(4) 0.0065(4)
P2 0.0201(5) 0.0204(6) 0.0145(5) 0.0023(4) 0.0032(4) 0.0060(4)
N1 0.0177(17) 0.0217(18) 0.0185(15) 0.0006(13) -0.0010(13) 0.0076(14)
N2 0.032(2) 0.045(2) 0.0255(18) -0.0048(17) -0.0042(16) 0.0166(18)
N3 0.0201(17) 0.0239(18) 0.0142(15) -0.0029(13) 0.0003(13) 0.0054(14)
C1 0.018(2) 0.0131(19) 0.0188(18) 0.0020(15) 0.0015(15) 0.0060(16)
C2 0.030(2) 0.017(2) 0.0200(19) 0.0032(16) 0.0076(17) 0.0082(18)
C3 0.028(2) 0.018(2) 0.028(2) 0.0077(17) 0.0133(18) 0.0061(18)
C4 0.019(2) 0.020(2) 0.034(2) 0.0053(18) 0.0044(17) 0.0039(18)
C5 0.026(2) 0.020(2) 0.023(2) -0.0018(17) 0.0013(17) 0.0037(18)
C6 0.024(2) 0.023(2) 0.0146(18) -0.0006(16) 0.0052(16) 0.0048(18)
C7 0.0136(19) 0.025(2) 0.0215(19) 0.0090(17) 0.0074(16) 0.0063(17)
C8 0.023(2) 0.028(2) 0.025(2) 0.0076(18) 0.0075(17) 0.0103(19)
C9 0.029(2) 0.025(2) 0.042(2) 0.012(2) 0.017(2) 0.0090(19)
C10 0.034(2) 0.039(3) 0.035(2) 0.023(2) 0.018(2) 0.023(2)
C11 0.028(2) 0.045(3) 0.0202(19) 0.0131(19) 0.0091(17) 0.018(2)
C12 0.025(2) 0.029(2) 0.023(2) 0.0053(17) 0.0079(17) 0.0115(19)
C13 0.016(2) 0.026(2) 0.0178(18) -0.0015(16) -0.0004(15) 0.0045(17)
C14 0.026(2) 0.043(3) 0.027(2) 0.0115(19) 0.0087(18) 0.016(2)
C15 0.030(3) 0.057(3) 0.035(2) 0.006(2) 0.014(2) 0.019(2)
C16 0.026(2) 0.041(3) 0.042(3) -0.011(2) 0.006(2) 0.015(2)
C17 0.024(2) 0.024(2) 0.043(3) -0.004(2) -0.002(2) 0.0081(19)
C18 0.021(2) 0.021(2) 0.026(2) -0.0043(17) -0.0004(17) 0.0038(18)
C19 0.016(2) 0.031(2) 0.026(2) 0.0019(18) 0.0010(16) 0.0087(18)
C20 0.022(2) 0.052(3) 0.031(2) -0.004(2) -0.0028(19) 0.013(2)
C21 0.026(2) 0.040(3) 0.0170(19) -0.0045(18) -0.0059(17) 0.006(2)
C22 0.026(2) 0.030(2) 0.023(2) -0.0019(18) -0.0009(17) 0.0071(19)
C23 0.017(2) 0.018(2) 0.0177(18) 0.0002(16) 0.0058(15) 0.0047(16)
C24 0.028(2) 0.024(2) 0.0169(18) 0.0008(16) 0.0008(16) 0.0077(19)
C25 0.036(3) 0.021(2) 0.025(2) 0.0049(17) 0.0142(19) 0.008(2)
C26 0.023(2) 0.026(2) 0.032(2) 0.0009(19) 0.0100(19) 0.0023(19)
C27 0.018(2) 0.030(2) 0.029(2) 0.0009(18) 0.0030(17) 0.0070(19)
C28 0.021(2) 0.027(2) 0.0212(19) 0.0051(17) 0.0046(16) 0.0113(18)
C29 0.020(2) 0.022(2) 0.0159(18) 0.0029(16) 0.0010(15) 0.0076(17)
C30 0.037(3) 0.027(2) 0.028(2) 0.0015(18) 0.0113(19) 0.008(2)
C31 0.046(3) 0.040(3) 0.035(2) 0.005(2) 0.023(2) 0.012(2)
C32 0.047(3) 0.039(3) 0.020(2) 0.0007(19) 0.012(2) 0.021(2)
C33 0.037(3) 0.033(3) 0.029(2) -0.011(2) -0.002(2) 0.013(2)
C34 0.031(2) 0.026(2) 0.029(2) 0.0007(19) 0.0096(18) 0.005(2)
C35 0.023(2) 0.014(2) 0.0170(18) -0.0011(15) 0.0029(16) 0.0033(17)
C36 0.027(2) 0.026(2) 0.028(2) 0.0042(18) 0.0087(18) 0.0078(19)
C37 0.038(3) 0.024(2) 0.027(2) 0.0075(18) 0.0096(19) 0.016(2)
C38 0.045(3) 0.023(2) 0.022(2) 0.0072(17) 0.0099(19) 0.012(2)
C39 0.041(3) 0.030(2) 0.025(2) 0.0106(18) 0.0183(19) 0.013(2)
C40 0.025(2) 0.026(2) 0.027(2) 0.0043(18) 0.0100(17) 0.0082(18)
P3 0.0252(6) 0.0326(7) 0.0463(7) 0.0082(6) 0.0117(5) 0.0010(5)
F5 0.091(3) 0.053(2) 0.142(3) 0.039(2) 0.082(2) 0.0140(18)
F1 0.086(3) 0.085(2) 0.127(3) 0.038(2) 0.079(2) 0.015(2)
F2 0.107(3) 0.069(2) 0.084(2) -0.0321(19) 0.032(2) -0.009(2)
F3 0.099(3) 0.047(2) 0.131(3) -0.017(2) 0.056(2) -0.0002(19)
F6 0.085(3) 0.112(3) 0.100(3) 0.035(2) -0.001(2) 0.050(2)
F4 0.085(3) 0.180(4) 0.158(4) 0.107(3) 0.014(3) 0.067(3)
C41 0.035(3) 0.042(3) 0.036(3) 0.002(2) 0.004(2) 0.004(2)
C42 0.082(4) 0.052(3) 0.063(3) 0.026(3) 0.033(3) 0.025(3)
N4 0.084(4) 0.067(3) 0.052(3) 0.026(3) 0.012(2) 0.024(3)
_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 1.891(3) . ?
Ni1 N3 1.902(3) . ?
Ni1 N2 1.959(3) . ?
Ni1 H100 1.45(4) . ?
P1 N1 1.596(3) . ?
P1 C7 1.809(3) . ?
P1 C1 1.810(3) . ?
P1 C13 1.813(4) . ?
P2 N3 1.594(3) . ?
P2 C23 1.795(4) . ?
P2 C35 1.813(3) . ?
P2 C29 1.815(3) . ?
N1 C19 1.486(4) . ?
N2 C20 1.425(5) . ?
N2 C21 1.485(5) . ?
N2 H2B 0.9300 . ?
N3 C22 1.479(4) . ?
C1 C6 1.392(5) . ?
C1 C2 1.394(5) . ?
C2 C3 1.381(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.377(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.393(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.382(5) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 C8 1.391(5) . ?
C7 C12 1.401(5) . ?
C8 C9 1.383(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.383(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.388(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.376(5) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 C18 1.394(5) . ?
C13 C14 1.394(5) . ?
C14 C15 1.392(5) . ?
C14 H14A 0.9500 . ?
C15 C16 1.373(6) . ?
C15 H15A 0.9500 . ?
C16 C17 1.381(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.381(5) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
C19 C20 1.500(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.493(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C28 1.396(5) . ?
C23 C24 1.397(5) . ?
C24 C25 1.376(5) . ?
C24 H24A 0.9500 . ?
C25 C26 1.380(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.379(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.391(5) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C29 C34 1.382(5) . ?
C29 C30 1.386(5) . ?
C30 C31 1.384(5) . ?
C30 H30A 0.9500 . ?
C31 C32 1.375(6) . ?
C31 H31A 0.9500 . ?
C32 C33 1.374(6) . ?
C32 H32A 0.9500 . ?
C33 C34 1.392(5) . ?
C33 H33A 0.9500 . ?
C34 H34A 0.9500 . ?
C35 C40 1.389(5) . ?
C35 C36 1.393(5) . ?
C36 C37 1.380(5) . ?
C36 H36A 0.9500 . ?
C37 C38 1.382(5) . ?
C37 H37A 0.9500 . ?
C38 C39 1.378(5) . ?
C38 H38A 0.9500 . ?
C39 C40 1.383(5) . ?
C39 H39A 0.9500 . ?
C40 H40A 0.9500 . ?
P3 F4 1.541(3) . ?
P3 F1 1.563(3) . ?
P3 F2 1.564(3) . ?
P3 F3 1.572(3) . ?
P3 F6 1.579(3) . ?
P3 F5 1.594(3) . ?
C41 N4 1.121(5) . ?
C41 C42 1.448(6) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 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 N3 168.85(12) . . ?
N1 Ni1 N2 85.36(13) . . ?
N3 Ni1 N2 86.33(13) . . ?
N1 Ni1 H100 95.8(14) . . ?
N3 Ni1 H100 93.3(14) . . ?
N2 Ni1 H100 173.3(14) . . ?
N1 P1 C7 113.54(16) . . ?
N1 P1 C1 112.20(16) . . ?
C7 P1 C1 108.97(16) . . ?
N1 P1 C13 111.79(16) . . ?
C7 P1 C13 105.91(16) . . ?
C1 P1 C13 103.80(16) . . ?
N3 P2 C23 109.55(16) . . ?
N3 P2 C35 114.91(16) . . ?
C23 P2 C35 110.44(16) . . ?
N3 P2 C29 112.22(15) . . ?
C23 P2 C29 105.81(16) . . ?
C35 P2 C29 103.41(16) . . ?
C19 N1 P1 121.7(2) . . ?
C19 N1 Ni1 112.3(2) . . ?
P1 N1 Ni1 122.59(17) . . ?
C20 N2 C21 120.4(3) . . ?
C20 N2 Ni1 109.1(2) . . ?
C21 N2 Ni1 106.6(2) . . ?
C20 N2 H2B 106.6 . . ?
C21 N2 H2B 106.6 . . ?
Ni1 N2 H2B 106.6 . . ?
C22 N3 P2 122.8(2) . . ?
C22 N3 Ni1 110.5(2) . . ?
P2 N3 Ni1 121.05(16) . . ?
C6 C1 C2 118.9(3) . . ?
C6 C1 P1 119.2(3) . . ?
C2 C1 P1 121.8(3) . . ?
C3 C2 C1 120.2(3) . . ?
C3 C2 H2A 119.9 . . ?
C1 C2 H2A 119.9 . . ?
C4 C3 C2 120.7(3) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C6 C5 C4 120.1(3) . . ?
C6 C5 H5A 120.0 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C1 120.5(3) . . ?
C5 C6 H6A 119.8 . . ?
C1 C6 H6A 119.8 . . ?
C8 C7 C12 119.0(3) . . ?
C8 C7 P1 117.0(3) . . ?
C12 C7 P1 123.9(3) . . ?
C9 C8 C7 120.3(3) . . ?
C9 C8 H8A 119.8 . . ?
C7 C8 H8A 119.8 . . ?
C10 C9 C8 120.3(4) . . ?
C10 C9 H9A 119.9 . . ?
C8 C9 H9A 119.9 . . ?
C9 C10 C11 119.7(3) . . ?
C9 C10 H10A 120.1 . . ?
C11 C10 H10A 120.1 . . ?
C12 C11 C10 120.4(4) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C7 120.2(4) . . ?
C11 C12 H12A 119.9 . . ?
C7 C12 H12A 119.9 . . ?
C18 C13 C14 119.3(3) . . ?
C18 C13 P1 118.4(3) . . ?
C14 C13 P1 122.3(3) . . ?
C15 C14 C13 120.0(4) . . ?
C15 C14 H14A 120.0 . . ?
C13 C14 H14A 120.0 . . ?
C16 C15 C14 119.9(4) . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C15 C16 C17 120.5(4) . . ?
C15 C16 H16A 119.7 . . ?
C17 C16 H16A 119.7 . . ?
C18 C17 C16 120.2(4) . . ?
C18 C17 H17A 119.9 . . ?
C16 C17 H17A 119.9 . . ?
C17 C18 C13 120.1(4) . . ?
C17 C18 H18A 119.9 . . ?
C13 C18 H18A 119.9 . . ?
N1 C19 C20 107.0(3) . . ?
N1 C19 H19A 110.3 . . ?
C20 C19 H19A 110.3 . . ?
N1 C19 H19B 110.3 . . ?
C20 C19 H19B 110.3 . . ?
H19A C19 H19B 108.6 . . ?
N2 C20 C19 108.4(3) . . ?
N2 C20 H20A 110.0 . . ?
C19 C20 H20A 110.0 . . ?
N2 C20 H20B 110.0 . . ?
C19 C20 H20B 110.0 . . ?
H20A C20 H20B 108.4 . . ?
N2 C21 C22 105.8(3) . . ?
N2 C21 H21A 110.6 . . ?
C22 C21 H21A 110.6 . . ?
N2 C21 H21B 110.6 . . ?
C22 C21 H21B 110.6 . . ?
H21A C21 H21B 108.7 . . ?
N3 C22 C21 106.9(3) . . ?
N3 C22 H22A 110.4 . . ?
C21 C22 H22A 110.4 . . ?
N3 C22 H22B 110.4 . . ?
C21 C22 H22B 110.4 . . ?
H22A C22 H22B 108.6 . . ?
C28 C23 C24 119.2(3) . . ?
C28 C23 P2 122.6(3) . . ?
C24 C23 P2 118.0(3) . . ?
C25 C24 C23 120.4(3) . . ?
C25 C24 H24A 119.8 . . ?
C23 C24 H24A 119.8 . . ?
C24 C25 C26 120.5(4) . . ?
C24 C25 H25A 119.8 . . ?
C26 C25 H25A 119.8 . . ?
C27 C26 C25 119.8(4) . . ?
C27 C26 H26A 120.1 . . ?
C25 C26 H26A 120.1 . . ?
C26 C27 C28 120.6(4) . . ?
C26 C27 H27A 119.7 . . ?
C28 C27 H27A 119.7 . . ?
C27 C28 C23 119.6(3) . . ?
C27 C28 H28A 120.2 . . ?
C23 C28 H28A 120.2 . . ?
C34 C29 C30 118.5(3) . . ?
C34 C29 P2 119.4(3) . . ?
C30 C29 P2 122.1(3) . . ?
C31 C30 C29 120.8(4) . . ?
C31 C30 H30A 119.6 . . ?
C29 C30 H30A 119.6 . . ?
C32 C31 C30 120.2(4) . . ?
C32 C31 H31A 119.9 . . ?
C30 C31 H31A 119.9 . . ?
C33 C32 C31 119.8(4) . . ?
C33 C32 H32A 120.1 . . ?
C31 C32 H32A 120.1 . . ?
C32 C33 C34 120.0(4) . . ?
C32 C33 H33A 120.0 . . ?
C34 C33 H33A 120.0 . . ?
C29 C34 C33 120.7(4) . . ?
C29 C34 H34A 119.7 . . ?
C33 C34 H34A 119.7 . . ?
C40 C35 C36 119.1(3) . . ?
C40 C35 P2 119.6(3) . . ?
C36 C35 P2 121.2(3) . . ?
C37 C36 C35 120.3(3) . . ?
C37 C36 H36A 119.9 . . ?
C35 C36 H36A 119.9 . . ?
C36 C37 C38 120.1(4) . . ?
C36 C37 H37A 120.0 . . ?
C38 C37 H37A 120.0 . . ?
C39 C38 C37 120.1(3) . . ?
C39 C38 H38A 119.9 . . ?
C37 C38 H38A 119.9 . . ?
C38 C39 C40 120.0(4) . . ?
C38 C39 H39A 120.0 . . ?
C40 C39 H39A 120.0 . . ?
C39 C40 C35 120.4(4) . . ?
C39 C40 H40A 119.8 . . ?
C35 C40 H40A 119.8 . . ?
F4 P3 F1 92.2(2) . . ?
F4 P3 F2 94.1(3) . . ?
F1 P3 F2 91.61(19) . . ?
F4 P3 F3 88.7(2) . . ?
F1 P3 F3 89.58(19) . . ?
F2 P3 F3 177.0(2) . . ?
F4 P3 F6 177.2(2) . . ?
F1 P3 F6 89.8(2) . . ?
F2 P3 F6 87.8(2) . . ?
F3 P3 F6 89.4(2) . . ?
F4 P3 F5 89.0(2) . . ?
F1 P3 F5 178.3(2) . . ?
F2 P3 F5 89.54(18) . . ?
F3 P3 F5 89.20(18) . . ?
F6 P3 F5 88.9(2) . . ?
N4 C41 C42 178.5(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.071
#===end