# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wb16dec13_0ma_a

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        PNNiAcrylonitirle
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H27 N2 Ni P'
_chemical_formula_weight         349.08

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'

_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                   7.6066(10)
_cell_length_b                   8.8452(12)
_cell_length_c                   13.6965(18)
_cell_angle_alpha                89.149(4)
_cell_angle_beta                 73.88
_cell_angle_gamma                86.935(5)
_cell_volume                     884.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_F_000             372
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    1.184
_shelx_estimated_absorpt_T_min   0.842
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2506
_diffrn_reflns_av_unetI/netI     0.1106
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.306
_diffrn_reflns_theta_max         24.214
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.564
_diffrn_measured_fraction_theta_full 0.497
_diffrn_reflns_Laue_measured_fraction_max 0.564
_diffrn_reflns_Laue_measured_fraction_full 0.497
_diffrn_reflns_point_group_measured_fraction_max 0.564
_diffrn_reflns_point_group_measured_fraction_full 0.497
_reflns_number_total             1600
_reflns_number_gt                1060
_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)+(0.0770P)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         1600
_refine_ls_number_parameters     202
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1604
_refine_ls_wR_factor_gt          0.1450
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          5.582
_refine_ls_shift/su_mean         0.055

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
C1 C -0.1450(14) -0.2387(11) 0.2775(9) 0.059(3) Uani 1 1 d . U . . .
C2 C 0.0126(14) -0.1997(11) 0.2948(9) 0.057(3) Uani 1 1 d . U . . .
H2 H 0.0212 -0.1925 0.3625 0.068 Uiso 1 1 calc R U . . .
C3 C 0.1700(13) -0.1684(12) 0.2093(9) 0.051(3) Uani 1 1 d . U . . .
H3A H 0.161(13) -0.176(13) 0.142(9) 0.061 Uiso 1 1 calc . U . . .
H3B H 0.281(13) -0.141(12) 0.221(8) 0.061 Uiso 1 1 calc . U . . .
C4 C -0.2387(11) 0.0845(11) 0.4589(7) 0.041(2) Uani 1 1 d . U . . .
H4 H -0.2413 -0.0227 0.4622 0.049 Uiso 1 1 calc R U . . .
C5 C -0.3477(12) 0.1686(12) 0.5380(7) 0.048(2) Uani 1 1 d . U . . .
H5 H -0.4268 0.1207 0.5946 0.057 Uiso 1 1 calc R U . . .
C6 C -0.3408(12) 0.3237(13) 0.5339(7) 0.048(2) Uani 1 1 d . U . . .
H6 H -0.4124 0.3842 0.5888 0.058 Uiso 1 1 calc R U . . .
C7 C -0.2303(11) 0.3894(11) 0.4505(7) 0.041(2) Uani 1 1 d . U . . .
H7 H -0.2262 0.4965 0.4465 0.049 Uiso 1 1 calc R U . . .
C8 C -0.1251(9) 0.3016(9) 0.3724(6) 0.0285(18) Uani 1 1 d . U . . .
C9 C -0.0024(11) 0.3683(9) 0.2770(7) 0.034(2) Uani 1 1 d . U . . .
H9A H 0.0585 0.4556 0.2950 0.041 Uiso 1 1 calc R U . . .
H9B H -0.0772 0.4050 0.2319 0.041 Uiso 1 1 calc R U . . .
C10 C 0.1986(11) 0.2715(10) 0.0733(7) 0.0350(19) Uani 1 1 d . U . . .
C11 C 0.0227(13) 0.2153(13) 0.0526(9) 0.052(3) Uani 1 1 d . U . . .
H11A H 0.0264 0.2346 -0.0185 0.078 Uiso 1 1 calc R U . . .
H11B H -0.0851 0.2693 0.0971 0.078 Uiso 1 1 calc R U . . .
H11C H 0.0155 0.1064 0.0663 0.078 Uiso 1 1 calc R U . . .
C12 C 0.2050(12) 0.4420(11) 0.0474(8) 0.050(2) Uani 1 1 d . U . . .
H12A H 0.3223 0.4789 0.0508 0.075 Uiso 1 1 calc R U . . .
H12B H 0.1045 0.4976 0.0963 0.075 Uiso 1 1 calc R U . . .
H12C H 0.1921 0.4575 -0.0213 0.075 Uiso 1 1 calc R U . . .
C13 C 0.3637(14) 0.1859(14) 0.0059(8) 0.065(3) Uani 1 1 d . U . . .
H13A H 0.3596 0.0784 0.0241 0.097 Uiso 1 1 calc R U . . .
H13B H 0.4756 0.2261 0.0151 0.097 Uiso 1 1 calc R U . . .
H13C H 0.3631 0.1977 -0.0652 0.097 Uiso 1 1 calc R U . . .
C14 C 0.3839(11) 0.2638(10) 0.2486(7) 0.0362(19) Uani 1 1 d . U . . .
C15 C 0.3207(13) 0.2623(11) 0.3635(8) 0.048(2) Uani 1 1 d . U . . .
H15A H 0.4255 0.2755 0.3905 0.073 Uiso 1 1 calc R U . . .
H15B H 0.2671 0.1655 0.3870 0.073 Uiso 1 1 calc R U . . .
H15C H 0.2284 0.3451 0.3876 0.073 Uiso 1 1 calc R U . . .
C16 C 0.4661(12) 0.4130(11) 0.2143(8) 0.050(2) Uani 1 1 d . U . . .
H16A H 0.5625 0.4299 0.2472 0.074 Uiso 1 1 calc R U . . .
H16B H 0.3707 0.4946 0.2330 0.074 Uiso 1 1 calc R U . . .
H16C H 0.5187 0.4117 0.1403 0.074 Uiso 1 1 calc R U . . .
C17 C 0.5250(11) 0.1311(11) 0.2131(8) 0.050(3) Uani 1 1 d . U . . .
H17A H 0.5608 0.1257 0.1387 0.075 Uiso 1 1 calc R U . . .
H17B H 0.4708 0.0364 0.2414 0.075 Uiso 1 1 calc R U . . .
H17C H 0.6332 0.1465 0.2365 0.075 Uiso 1 1 calc R U . . .
N1 N -0.2860(12) -0.2744(12) 0.2655(8) 0.077(3) Uani 1 1 d . U . . .
N2 N -0.1280(9) 0.1487(7) 0.3765(5) 0.0307(15) Uani 1 1 d . U . . .
Ni1 Ni 0.04707(15) 0.02161(12) 0.27350(9) 0.0361(4) Uani 1 1 d . U . . .
P1 P 0.1735(2) 0.2238(2) 0.20914(15) 0.0253(5) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.189(14) . ?
C1 C2 1.348(15) . ?
C2 C3 1.459(14) . ?
C2 Ni1 1.995(10) . ?
C2 H2 0.9500 . ?
C3 H3A 0.89(10) . ?
C3 H3B 0.98(10) . ?
C4 N2 1.345(11) . ?
C4 C5 1.369(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.375(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.359(15) . ?
C6 H6 0.9500 . ?
C7 C8 1.368(10) . ?
C7 H7 0.9500 . ?
C8 N2 1.353(11) . ?
C8 C9 1.512(12) . ?
C9 P1 1.857(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C13 1.509(10) . ?
C10 C12 1.544(13) . ?
C10 C11 1.550(11) . ?
C10 P1 1.861(9) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C16 1.503(13) . ?
C14 C15 1.513(13) . ?
C14 C17 1.536(11) . ?
C14 P1 1.877(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N2 Ni1 1.968(6) . ?
Ni1 P1 2.137(2) . ?

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 C1 C2 177.8(14) . . ?
C1 C2 C3 119.8(11) . . ?
C1 C2 Ni1 111.3(8) . . ?
C3 C2 Ni1 67.6(6) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
Ni1 C2 H2 91.0 . . ?
C2 C3 H3A 129(7) . . ?
C2 C3 H3B 120(7) . . ?
H3A C3 H3B 95(9) . . ?
N2 C4 C5 122.2(9) . . ?
N2 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C4 C5 C6 118.8(9) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C7 C6 C5 119.3(8) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 120.1(9) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
N2 C8 C7 121.1(8) . . ?
N2 C8 C9 116.4(6) . . ?
C7 C8 C9 122.5(7) . . ?
C8 C9 P1 110.4(6) . . ?
C8 C9 H9A 109.6 . . ?
P1 C9 H9A 109.6 . . ?
C8 C9 H9B 109.6 . . ?
P1 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C13 C10 C12 110.2(8) . . ?
C13 C10 C11 109.2(7) . . ?
C12 C10 C11 106.9(8) . . ?
C13 C10 P1 110.3(7) . . ?
C12 C10 P1 115.4(6) . . ?
C11 C10 P1 104.4(7) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C16 C14 C15 108.6(7) . . ?
C16 C14 C17 111.3(7) . . ?
C15 C14 C17 108.3(9) . . ?
C16 C14 P1 115.9(7) . . ?
C15 C14 P1 104.3(6) . . ?
C17 C14 P1 108.0(5) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C4 N2 C8 118.5(7) . . ?
C4 N2 Ni1 120.0(6) . . ?
C8 N2 Ni1 121.0(6) . . ?
N2 Ni1 C2 113.5(4) . . ?
N2 Ni1 P1 88.1(2) . . ?
C2 Ni1 P1 158.3(3) . . ?
C9 P1 C10 102.6(4) . . ?
C9 P1 C14 104.6(3) . . ?
C10 P1 C14 112.1(4) . . ?
C9 P1 Ni1 100.2(3) . . ?
C10 P1 Ni1 120.5(3) . . ?
C14 P1 Ni1 114.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C4 C5 C6 -1.4(14) . . . . ?
C4 C5 C6 C7 1.9(15) . . . . ?
C5 C6 C7 C8 -1.1(15) . . . . ?
C6 C7 C8 N2 -0.3(14) . . . . ?
C6 C7 C8 C9 178.8(8) . . . . ?
N2 C8 C9 P1 -19.9(9) . . . . ?
C7 C8 C9 P1 161.0(7) . . . . ?
C5 C4 N2 C8 0.0(13) . . . . ?
C5 C4 N2 Ni1 172.5(7) . . . . ?
C7 C8 N2 C4 0.8(12) . . . . ?
C9 C8 N2 C4 -178.3(8) . . . . ?
C7 C8 N2 Ni1 -171.6(7) . . . . ?
C9 C8 N2 Ni1 9.3(10) . . . . ?
C8 C9 P1 C10 144.5(6) . . . . ?
C8 C9 P1 C14 -98.3(6) . . . . ?
C8 C9 P1 Ni1 19.9(6) . . . . ?
C13 C10 P1 C9 168.6(7) . . . . ?
C12 C10 P1 C9 42.8(7) . . . . ?
C11 C10 P1 C9 -74.2(6) . . . . ?
C13 C10 P1 C14 57.0(8) . . . . ?
C12 C10 P1 C14 -68.8(7) . . . . ?
C11 C10 P1 C14 174.1(5) . . . . ?
C13 C10 P1 Ni1 -81.4(7) . . . . ?
C12 C10 P1 Ni1 152.8(5) . . . . ?
C11 C10 P1 Ni1 35.7(6) . . . . ?
C16 C14 P1 C9 -65.4(7) . . . . ?
C15 C14 P1 C9 53.9(7) . . . . ?
C17 C14 P1 C9 169.0(7) . . . . ?
C16 C14 P1 C10 45.0(7) . . . . ?
C15 C14 P1 C10 164.3(6) . . . . ?
C17 C14 P1 C10 -80.6(8) . . . . ?
C16 C14 P1 Ni1 -173.7(5) . . . . ?
C15 C14 P1 Ni1 -54.5(6) . . . . ?
C17 C14 P1 Ni1 60.6(7) . . . . ?

_refine_diff_density_max         0.793
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.064

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 997717'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_wb18apr13_0m

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        PNNiCOD
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H36 N Ni P'
_chemical_formula_weight         404.20

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'

_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                   7.6680(4)
_cell_length_b                   9.5525(6)
_cell_length_c                   15.1227(9)
_cell_angle_alpha                77.602(2)
_cell_angle_beta                 87.452(2)
_cell_angle_gamma                72.077(2)
_cell_volume                     1029.10(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    198(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_F_000             436
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.025
_shelx_estimated_absorpt_T_min   0.784
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      198(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28348
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.413
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4205
_reflns_number_gt                3933
_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)+(0.0369P)²+0.5094P]
 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         4205
_refine_ls_number_parameters     232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0253
_refine_ls_wR_factor_ref         0.0681
_refine_ls_wR_factor_gt          0.0666
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_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_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
C1 C 0.3261(2) 0.91096(18) 0.64475(11) 0.0283(3) Uani 1 1 d . . . . .
H1 H 0.2817 0.9650 0.6912 0.034 Uiso 1 1 calc R U . . .
C2 C 0.2481(2) 0.97197(19) 0.55938(12) 0.0327(4) Uani 1 1 d . . . . .
H2 H 0.1531 1.0654 0.5479 0.039 Uiso 1 1 calc R U . . .
C3 C 0.3097(2) 0.8957(2) 0.49073(12) 0.0337(4) Uani 1 1 d . . . . .
H3 H 0.2619 0.9370 0.4306 0.040 Uiso 1 1 calc R U . . .
C4 C 0.4432(2) 0.7571(2) 0.51209(11) 0.0290(4) Uani 1 1 d . . . . .
H4 H 0.4859 0.7005 0.4666 0.035 Uiso 1 1 calc R U . . .
C5 C 0.5149(2) 0.70053(17) 0.59977(10) 0.0209(3) Uani 1 1 d . . . . .
C6 C 0.6505(2) 0.54593(18) 0.62646(10) 0.0238(3) Uani 1 1 d . . . . .
H6A H 0.7349 0.5262 0.5760 0.029 Uiso 1 1 calc R U . . .
H6B H 0.5841 0.4700 0.6375 0.029 Uiso 1 1 calc R U . . .
C7 C 1.0123(2) 0.54352(18) 0.68111(10) 0.0228(3) Uani 1 1 d . . . . .
C8 C 1.1330(2) 0.5511(2) 0.75695(12) 0.0313(4) Uani 1 1 d . . . . .
H8A H 1.1812 0.4509 0.7959 0.047 Uiso 1 1 calc R U . . .
H8B H 1.0599 0.6214 0.7930 0.047 Uiso 1 1 calc R U . . .
H8C H 1.2352 0.5860 0.7304 0.047 Uiso 1 1 calc R U . . .
C9 C 0.9603(3) 0.6962(2) 0.61366(12) 0.0327(4) Uani 1 1 d . . . . .
H9A H 1.0717 0.7227 0.5939 0.049 Uiso 1 1 calc R U . . .
H9B H 0.8804 0.7738 0.6431 0.049 Uiso 1 1 calc R U . . .
H9C H 0.8956 0.6895 0.5610 0.049 Uiso 1 1 calc R U . . .
C10 C 1.1250(2) 0.4237(2) 0.63064(13) 0.0360(4) Uani 1 1 d . . . . .
H10A H 1.0449 0.4070 0.5879 0.054 Uiso 1 1 calc R U . . .
H10B H 1.1800 0.3294 0.6743 0.054 Uiso 1 1 calc R U . . .
H10C H 1.2221 0.4580 0.5975 0.054 Uiso 1 1 calc R U . . .
C11 C 0.8138(2) 0.32247(17) 0.78547(11) 0.0233(3) Uani 1 1 d . . . . .
C12 C 0.6227(2) 0.31435(19) 0.81663(13) 0.0328(4) Uani 1 1 d . . . . .
H12A H 0.6343 0.2156 0.8557 0.049 Uiso 1 1 calc R U . . .
H12B H 0.5450 0.3289 0.7636 0.049 Uiso 1 1 calc R U . . .
H12C H 0.5670 0.3933 0.8504 0.049 Uiso 1 1 calc R U . . .
C13 C 0.9383(2) 0.2784(2) 0.86935(12) 0.0337(4) Uani 1 1 d . . . . .
H13A H 0.9386 0.1790 0.9038 0.050 Uiso 1 1 calc R U . . .
H13B H 0.8931 0.3528 0.9074 0.050 Uiso 1 1 calc R U . . .
H13C H 1.0633 0.2754 0.8508 0.050 Uiso 1 1 calc R U . . .
C14 C 0.8862(3) 0.20757(19) 0.72514(14) 0.0373(4) Uani 1 1 d . . . . .
H14A H 1.0168 0.1941 0.7146 0.056 Uiso 1 1 calc R U . . .
H14B H 0.8184 0.2442 0.6671 0.056 Uiso 1 1 calc R U . . .
H14C H 0.8696 0.1110 0.7552 0.056 Uiso 1 1 calc R U . . .
C15 C 0.7591(2) 0.83979(18) 0.82342(11) 0.0263(3) Uani 1 1 d . . . . .
H15 H 0.8450 0.8168 0.7774 0.032 Uiso 1 1 calc R U . . .
C16 C 0.5835(2) 0.93097(17) 0.79717(11) 0.0261(3) Uani 1 1 d . . . . .
H16 H 0.5544 0.9627 0.7342 0.031 Uiso 1 1 calc R U . . .
C17 C 0.4338(3) 0.98379(19) 0.86250(13) 0.0342(4) Uani 1 1 d . . . . .
H17A H 0.3558 1.0864 0.8347 0.041 Uiso 1 1 calc R U . . .
H17B H 0.4913 0.9898 0.9183 0.041 Uiso 1 1 calc R U . . .
C18 C 0.3115(2) 0.8805(2) 0.88833(12) 0.0330(4) Uani 1 1 d . . . . .
H18A H 0.2664 0.8855 0.9503 0.040 Uiso 1 1 calc R U . . .
H18B H 0.2036 0.9183 0.8465 0.040 Uiso 1 1 calc R U . . .
C19 C 0.4102(2) 0.71820(18) 0.88495(11) 0.0259(3) Uani 1 1 d . . . . .
H19 H 0.3500 0.6679 0.8548 0.031 Uiso 1 1 calc R U . . .
C20 C 0.5823(2) 0.63819(19) 0.92283(10) 0.0260(3) Uani 1 1 d . . . . .
H20 H 0.6355 0.5384 0.9141 0.031 Uiso 1 1 calc R U . . .
C21 C 0.6915(3) 0.7000(2) 0.97756(11) 0.0352(4) Uani 1 1 d . . . . .
H21A H 0.7636 0.6167 1.0254 0.042 Uiso 1 1 calc R U . . .
H21B H 0.6051 0.7748 1.0077 0.042 Uiso 1 1 calc R U . . .
C22 C 0.8228(3) 0.7746(2) 0.92054(12) 0.0344(4) Uani 1 1 d . . . . .
H22A H 0.8362 0.8558 0.9482 0.041 Uiso 1 1 calc R U . . .
H22B H 0.9451 0.6989 0.9220 0.041 Uiso 1 1 calc R U . . .
N1 N 0.46252(17) 0.77852(14) 0.66670(8) 0.0206(3) Uani 1 1 d . . . . .
Ni1 Ni 0.60483(2) 0.71443(2) 0.78333(2) 0.01779(7) Uani 1 1 d . . . . .
P1 P 0.78586(5) 0.52570(4) 0.72985(2) 0.01651(9) 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
C1 N1 1.357(2) . ?
C1 C2 1.377(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(2) . ?
C4 H4 0.9500 . ?
C5 N1 1.358(2) . ?
C5 C6 1.504(2) . ?
C6 P1 1.8575(15) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C10 1.532(2) . ?
C7 C8 1.533(2) . ?
C7 C9 1.538(2) . ?
C7 P1 1.8978(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.526(2) . ?
C11 C14 1.535(2) . ?
C11 C12 1.539(2) . ?
C11 P1 1.8925(15) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
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 C16 1.381(2) . ?
C15 C22 1.506(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.518(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.542(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.513(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.382(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.520(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.538(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
N1 Ni1 1.9933(12) . ?
Ni1 P1 2.1949(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 124.12(16) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C1 C2 C3 119.16(16) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C4 117.95(15) . . ?
C2 C3 H3 121.0 . . ?
C4 C3 H3 121.0 . . ?
C3 C4 C5 120.17(16) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 C4 122.31(14) . . ?
N1 C5 C6 116.31(13) . . ?
C4 C5 C6 121.34(14) . . ?
C5 C6 P1 111.87(10) . . ?
C5 C6 H6A 109.2 . . ?
P1 C6 H6A 109.2 . . ?
C5 C6 H6B 109.2 . . ?
P1 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C10 C7 C8 108.54(14) . . ?
C10 C7 C9 107.82(13) . . ?
C8 C7 C9 108.43(14) . . ?
C10 C7 P1 118.06(12) . . ?
C8 C7 P1 109.07(10) . . ?
C9 C7 P1 104.52(11) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C14 109.55(14) . . ?
C13 C11 C12 108.08(14) . . ?
C14 C11 C12 107.28(14) . . ?
C13 C11 P1 108.83(11) . . ?
C14 C11 P1 115.98(12) . . ?
C12 C11 P1 106.83(11) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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 . . ?
C16 C15 C22 124.01(15) . . ?
C16 C15 H15 118.0 . . ?
C22 C15 H15 118.0 . . ?
C15 C16 C17 124.22(15) . . ?
C15 C16 H16 117.9 . . ?
C17 C16 H16 117.9 . . ?
C16 C17 C18 113.67(14) . . ?
C16 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
C16 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C19 C18 C17 113.05(14) . . ?
C19 C18 H18A 109.0 . . ?
C17 C18 H18A 109.0 . . ?
C19 C18 H18B 109.0 . . ?
C17 C18 H18B 109.0 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C18 124.38(15) . . ?
C20 C19 H19 117.8 . . ?
C18 C19 H19 117.8 . . ?
C19 C20 C21 124.08(16) . . ?
C19 C20 H20 118.0 . . ?
C21 C20 H20 118.0 . . ?
C20 C21 C22 113.69(14) . . ?
C20 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C15 C22 C21 113.33(14) . . ?
C15 C22 H22A 108.9 . . ?
C21 C22 H22A 108.9 . . ?
C15 C22 H22B 108.9 . . ?
C21 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C1 N1 C5 116.12(13) . . ?
C1 N1 Ni1 122.55(11) . . ?
C5 N1 Ni1 120.74(10) . . ?
N1 Ni1 P1 87.62(4) . . ?
C6 P1 C11 100.60(7) . . ?
C6 P1 C7 102.16(7) . . ?
C11 P1 C7 109.68(7) . . ?
C6 P1 Ni1 99.13(5) . . ?
C11 P1 Ni1 122.38(5) . . ?
C7 P1 Ni1 118.02(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.2(3) . . . . ?
C1 C2 C3 C4 2.6(3) . . . . ?
C2 C3 C4 C5 -1.8(3) . . . . ?
C3 C4 C5 N1 -1.9(3) . . . . ?
C3 C4 C5 C6 175.80(16) . . . . ?
N1 C5 C6 P1 -23.30(18) . . . . ?
C4 C5 C6 P1 158.88(13) . . . . ?
C22 C15 C16 C17 3.0(3) . . . . ?
C15 C16 C17 C18 -92.7(2) . . . . ?
C16 C17 C18 C19 28.8(2) . . . . ?
C17 C18 C19 C20 47.3(2) . . . . ?
C18 C19 C20 C21 3.5(2) . . . . ?
C19 C20 C21 C22 -92.4(2) . . . . ?
C16 C15 C22 C21 48.2(2) . . . . ?
C20 C21 C22 C15 28.1(2) . . . . ?
C2 C1 N1 C5 -3.7(2) . . . . ?
C2 C1 N1 Ni1 167.48(14) . . . . ?
C4 C5 N1 C1 4.5(2) . . . . ?
C6 C5 N1 C1 -173.29(14) . . . . ?
C4 C5 N1 Ni1 -166.85(12) . . . . ?
C6 C5 N1 Ni1 15.36(18) . . . . ?
C5 C6 P1 C11 144.87(11) . . . . ?
C5 C6 P1 C7 -102.13(12) . . . . ?
C5 C6 P1 Ni1 19.29(12) . . . . ?
C13 C11 P1 C6 175.01(12) . . . . ?
C14 C11 P1 C6 50.99(14) . . . . ?
C12 C11 P1 C6 -68.52(12) . . . . ?
C13 C11 P1 C7 67.88(13) . . . . ?
C14 C11 P1 C7 -56.14(14) . . . . ?
C12 C11 P1 C7 -175.65(11) . . . . ?
C13 C11 P1 Ni1 -76.95(12) . . . . ?
C14 C11 P1 Ni1 159.03(11) . . . . ?
C12 C11 P1 Ni1 39.52(13) . . . . ?
C10 C7 P1 C6 -63.32(14) . . . . ?
C8 C7 P1 C6 172.24(11) . . . . ?
C9 C7 P1 C6 56.44(12) . . . . ?
C10 C7 P1 C11 42.76(14) . . . . ?
C8 C7 P1 C11 -81.69(13) . . . . ?
C9 C7 P1 C11 162.52(11) . . . . ?
C10 C7 P1 Ni1 -170.68(11) . . . . ?
C8 C7 P1 Ni1 64.88(12) . . . . ?
C9 C7 P1 Ni1 -50.92(12) . . . . ?

_refine_diff_density_max         0.460
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.053

_shelxl_version_number           2013-2

_database_code_depnum_ccdc_archive 'CCDC 997718'
#######################################################################
#
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#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_twin4_a

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        PNNimethyllactone
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H38 N Ni O3 P'
_chemical_formula_weight         454.21

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'
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                   8.594(6)
_cell_length_b                   10.390(9)
_cell_length_c                   13.017(9)
_cell_angle_alpha                91.72(2)
_cell_angle_beta                 91.051(17)
_cell_angle_gamma                90.39(2)
_cell_volume                     1161.6(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_F_000             488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.925
_shelx_estimated_absorpt_T_min   0.851
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            ?
_diffrn_reflns_av_unetI/netI     0.2048
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.961
_diffrn_reflns_theta_max         24.209
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.726
_diffrn_measured_fraction_theta_full 0.643
_diffrn_reflns_Laue_measured_fraction_max 0.726
_diffrn_reflns_Laue_measured_fraction_full 0.643
_diffrn_reflns_point_group_measured_fraction_max 0.726
_diffrn_reflns_point_group_measured_fraction_full 0.643
_reflns_number_total             2704
_reflns_number_gt                1335
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1498P)²+14.5390P] 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         2704
_refine_ls_number_parameters     260
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.2492
_refine_ls_R_factor_gt           0.1344
_refine_ls_wR_factor_ref         0.3633
_refine_ls_wR_factor_gt          0.3141
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.003
_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
C1 C 0.374(2) 1.2146(18) 0.1166(14) 0.036(4) Uani 1 1 d . U . . .
C2 C 0.519(3) 1.198(2) 0.1894(19) 0.072(7) Uani 1 1 d . U . . .
H2 H 0.6077 1.1761 0.1436 0.087 Uiso 1 1 calc R U . . .
C3 C 0.499(3) 1.094(2) 0.2506(16) 0.064(6) Uani 1 1 d . U . . .
H3A H 0.4311 1.1171 0.3089 0.076 Uiso 1 1 calc R U . . .
H3B H 0.6007 1.0655 0.2784 0.076 Uiso 1 1 calc R U . . .
C4 C 0.561(4) 1.324(2) 0.241(2) 0.103(10) Uani 1 1 d . U . . .
H4A H 0.4889 1.3424 0.2969 0.154 Uiso 1 1 calc R U . . .
H4B H 0.5550 1.3926 0.1910 0.154 Uiso 1 1 calc R U . . .
H4C H 0.6675 1.3201 0.2693 0.154 Uiso 1 1 calc R U . . .
C5 C 0.157(2) 0.8700(18) 0.0232(12) 0.033(4) Uani 1 1 d . U . . .
H5 H 0.1328 0.9591 0.0234 0.040 Uiso 1 1 calc R U . . .
C6 C 0.063(2) 0.7835(18) -0.0300(12) 0.031(4) Uani 1 1 d . U . . .
H6 H -0.0244 0.8123 -0.0685 0.038 Uiso 1 1 calc R U . . .
C7 C 0.097(2) 0.651(2) -0.0273(14) 0.048(5) Uani 1 1 d . U . . .
H7 H 0.0315 0.5893 -0.0614 0.057 Uiso 1 1 calc R U . . .
C8 C 0.228(2) 0.6147(19) 0.0261(14) 0.041(4) Uani 1 1 d . U . . .
H8 H 0.2549 0.5262 0.0273 0.049 Uiso 1 1 calc R U . . .
C9 C 0.321(2) 0.7033(18) 0.0771(13) 0.032(4) Uani 1 1 d . U . . .
C10 C 0.462(2) 0.6696(18) 0.1358(12) 0.040(4) Uani 1 1 d . U . . .
H10A H 0.5512 0.6611 0.0888 0.048 Uiso 1 1 calc R U . . .
H10B H 0.4467 0.5861 0.1689 0.048 Uiso 1 1 calc R U . . .
C11 C 0.400(2) 0.7472(19) 0.3524(12) 0.037(4) Uani 1 1 d . U . . .
C12 C 0.228(2) 0.717(2) 0.3185(15) 0.052(5) Uani 1 1 d . U . . .
H12A H 0.2244 0.6399 0.2736 0.077 Uiso 1 1 calc R U . . .
H12B H 0.1857 0.7902 0.2811 0.077 Uiso 1 1 calc R U . . .
H12C H 0.1652 0.7031 0.3794 0.077 Uiso 1 1 calc R U . . .
C13 C 0.458(3) 0.625(2) 0.4016(15) 0.060(6) Uani 1 1 d . U . . .
H13A H 0.3904 0.6037 0.4588 0.090 Uiso 1 1 calc R U . . .
H13B H 0.5645 0.6384 0.4273 0.090 Uiso 1 1 calc R U . . .
H13C H 0.4552 0.5539 0.3503 0.090 Uiso 1 1 calc R U . . .
C14 C 0.403(3) 0.858(2) 0.4333(15) 0.066(7) Uani 1 1 d . U . . .
H14A H 0.3523 0.8304 0.4959 0.099 Uiso 1 1 calc R U . . .
H14B H 0.3468 0.9322 0.4061 0.099 Uiso 1 1 calc R U . . .
H14C H 0.5108 0.8832 0.4494 0.099 Uiso 1 1 calc R U . . .
C15 C 0.722(2) 0.788(2) 0.2523(14) 0.043(4) Uani 1 1 d . U . . .
C16 C 0.783(2) 0.649(2) 0.2455(19) 0.066(6) Uani 1 1 d . U . . .
H16A H 0.7594 0.6117 0.1769 0.099 Uiso 1 1 calc R U . . .
H16B H 0.7325 0.5976 0.2974 0.099 Uiso 1 1 calc R U . . .
H16C H 0.8958 0.6497 0.2577 0.099 Uiso 1 1 calc R U . . .
C17 C 0.777(2) 0.849(2) 0.3573(14) 0.059(6) Uani 1 1 d . U . . .
H17A H 0.8906 0.8449 0.3632 0.089 Uiso 1 1 calc R U . . .
H17B H 0.7305 0.8019 0.4133 0.089 Uiso 1 1 calc R U . . .
H17C H 0.7441 0.9392 0.3616 0.089 Uiso 1 1 calc R U . . .
C18 C 0.794(2) 0.862(2) 0.1673(15) 0.057(6) Uani 1 1 d . U . . .
H18A H 0.7614 0.9520 0.1728 0.086 Uiso 1 1 calc R U . . .
H18B H 0.7594 0.8245 0.1007 0.086 Uiso 1 1 calc R U . . .
H18C H 0.9075 0.8573 0.1732 0.086 Uiso 1 1 calc R U . . .
C19 C 0.998(5) 0.816(3) 0.597(2) 0.115(12) Uani 1 1 d . U . . .
H19A H 1.0936 0.8679 0.5868 0.139 Uiso 1 1 calc R U . . .
H19B H 0.9087 0.8639 0.5694 0.139 Uiso 1 1 calc R U . . .
C20 C 0.980(4) 0.801(3) 0.698(2) 0.096(9) Uani 1 1 d . U . . .
H20A H 0.8911 0.8521 0.7237 0.115 Uiso 1 1 calc R U . . .
H20B H 1.0750 0.8269 0.7376 0.115 Uiso 1 1 calc R U . . .
C21 C 0.947(5) 0.654(3) 0.708(2) 0.133(14) Uani 1 1 d . U . . .
H21A H 1.0344 0.6095 0.7417 0.160 Uiso 1 1 calc R U . . .
H21B H 0.8495 0.6372 0.7443 0.160 Uiso 1 1 calc R U . . .
C22 C 0.934(5) 0.621(3) 0.607(2) 0.145(16) Uani 1 1 d . U . . .
H22A H 0.8226 0.6188 0.5866 0.174 Uiso 1 1 calc R U . . .
H22B H 0.9751 0.5325 0.5963 0.174 Uiso 1 1 calc R U . . .
N1 N 0.2866(16) 0.8280(14) 0.0771(11) 0.033(3) Uani 1 1 d . U . . .
Ni1 Ni 0.4035(3) 0.9597(2) 0.16391(18) 0.0327(8) Uani 1 1 d . U . . .
O1 O 0.3111(15) 1.0970(12) 0.0963(9) 0.041(3) Uani 1 1 d . U . . .
O2 O 0.3291(18) 1.3135(12) 0.0812(10) 0.055(4) Uani 1 1 d . U . . .
O3 O 1.010(3) 0.7005(19) 0.5453(14) 0.127(9) Uani 1 1 d . U . . .
P1 P 0.5057(5) 0.7980(5) 0.2361(3) 0.0329(13) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.20(2) . ?
C1 O1 1.352(19) . ?
C1 C2 1.56(3) . ?
C2 C3 1.37(3) . ?
C2 C4 1.49(3) . ?
C2 H2 1.0000 . ?
C3 Ni1 1.939(19) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.37(2) . ?
C5 N1 1.39(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.41(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.38(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.36(2) . ?
C8 H8 0.9500 . ?
C9 N1 1.33(2) . ?
C9 C10 1.47(2) . ?
C10 P1 1.869(17) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C13 1.52(3) . ?
C11 C14 1.54(2) . ?
C11 C12 1.56(3) . ?
C11 P1 1.869(17) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
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 C18 1.51(3) . ?
C15 C17 1.55(2) . ?
C15 C16 1.53(3) . ?
C15 P1 1.872(18) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.34(3) . ?
C19 O3 1.37(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.56(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.35(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 O3 1.35(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
N1 Ni1 2.002(14) . ?
Ni1 O1 1.872(13) . ?
Ni1 P1 2.136(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 125(2) . . ?
O2 C1 C2 127(2) . . ?
O1 C1 C2 108.3(16) . . ?
C3 C2 C4 118(2) . . ?
C3 C2 C1 111(2) . . ?
C4 C2 C1 110(2) . . ?
C3 C2 H2 105.9 . . ?
C4 C2 H2 105.9 . . ?
C1 C2 H2 105.9 . . ?
C2 C3 Ni1 106.3(16) . . ?
C2 C3 H3A 110.5 . . ?
Ni1 C3 H3A 110.5 . . ?
C2 C3 H3B 110.5 . . ?
Ni1 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N1 120.2(17) . . ?
C6 C5 H5 119.9 . . ?
N1 C5 H5 119.9 . . ?
C5 C6 C7 119.3(19) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C8 C7 C6 118.3(19) . . ?
C8 C7 H7 120.9 . . ?
C6 C7 H7 120.9 . . ?
C9 C8 C7 121.0(19) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
N1 C9 C8 120.9(18) . . ?
N1 C9 C10 115.7(17) . . ?
C8 C9 C10 123.4(18) . . ?
C9 C10 P1 109.5(13) . . ?
C9 C10 H10A 109.8 . . ?
P1 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
P1 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C13 C11 C14 109.3(15) . . ?
C13 C11 C12 105.3(16) . . ?
C14 C11 C12 109.4(17) . . ?
C13 C11 P1 115.9(14) . . ?
C14 C11 P1 109.3(13) . . ?
C12 C11 P1 107.4(11) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
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 . . ?
C18 C15 C17 108.7(17) . . ?
C18 C15 C16 108.1(17) . . ?
C17 C15 C16 108.2(17) . . ?
C18 C15 P1 107.5(13) . . ?
C17 C15 P1 110.9(13) . . ?
C16 C15 P1 113.3(14) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 O3 112(3) . . ?
C20 C19 H19A 109.3 . . ?
O3 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
O3 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 C21 104(2) . . ?
C19 C20 H20A 110.9 . . ?
C21 C20 H20A 110.9 . . ?
C19 C20 H20B 110.9 . . ?
C21 C20 H20B 110.9 . . ?
H20A C20 H20B 108.9 . . ?
C22 C21 C20 99(3) . . ?
C22 C21 H21A 112.0 . . ?
C20 C21 H21A 112.0 . . ?
C22 C21 H21B 112.0 . . ?
C20 C21 H21B 112.0 . . ?
H21A C21 H21B 109.6 . . ?
C21 C22 O3 114(3) . . ?
C21 C22 H22A 108.8 . . ?
O3 C22 H22A 108.8 . . ?
C21 C22 H22B 108.8 . . ?
O3 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C9 N1 C5 120.2(16) . . ?
C9 N1 Ni1 122.5(13) . . ?
C5 N1 Ni1 117.0(12) . . ?
O1 Ni1 C3 84.2(8) . . ?
O1 Ni1 N1 92.7(6) . . ?
C3 Ni1 N1 174.9(9) . . ?
O1 Ni1 P1 177.7(4) . . ?
C3 Ni1 P1 98.1(7) . . ?
N1 Ni1 P1 85.0(5) . . ?
C1 O1 Ni1 116.1(11) . . ?
C22 O3 C19 102(2) . . ?
C11 P1 C10 105.2(8) . . ?
C11 P1 C15 112.7(8) . . ?
C10 P1 C15 102.5(8) . . ?
C11 P1 Ni1 113.4(7) . . ?
C10 P1 Ni1 100.0(6) . . ?
C15 P1 Ni1 120.2(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C3 152(2) . . . . ?
O1 C1 C2 C3 -30(2) . . . . ?
O2 C1 C2 C4 21(3) . . . . ?
O1 C1 C2 C4 -161.5(19) . . . . ?
C4 C2 C3 Ni1 168.1(19) . . . . ?
C1 C2 C3 Ni1 41(2) . . . . ?
N1 C5 C6 C7 2(2) . . . . ?
C5 C6 C7 C8 -3(3) . . . . ?
C6 C7 C8 C9 2(3) . . . . ?
C7 C8 C9 N1 0(3) . . . . ?
C7 C8 C9 C10 179.8(17) . . . . ?
N1 C9 C10 P1 23.7(19) . . . . ?
C8 C9 C10 P1 -155.8(14) . . . . ?
O3 C19 C20 C21 -11(4) . . . . ?
C19 C20 C21 C22 -8(4) . . . . ?
C20 C21 C22 O3 25(5) . . . . ?
C8 C9 N1 C5 -1(3) . . . . ?
C10 C9 N1 C5 179.3(14) . . . . ?
C8 C9 N1 Ni1 172.6(12) . . . . ?
C10 C9 N1 Ni1 -7(2) . . . . ?
C6 C5 N1 C9 0(2) . . . . ?
C6 C5 N1 Ni1 -174.0(12) . . . . ?
O2 C1 O1 Ni1 -179.0(15) . . . . ?
C2 C1 O1 Ni1 3.3(18) . . . . ?
C3 Ni1 O1 C1 15.3(13) . . . . ?
N1 Ni1 O1 C1 -168.8(11) . . . . ?
C21 C22 O3 C19 -32(5) . . . . ?
C20 C19 O3 C22 25(4) . . . . ?
C13 C11 P1 C10 66.3(16) . . . . ?
C14 C11 P1 C10 -169.6(14) . . . . ?
C12 C11 P1 C10 -51.1(16) . . . . ?
C13 C11 P1 C15 -44.6(17) . . . . ?
C14 C11 P1 C15 79.4(16) . . . . ?
C12 C11 P1 C15 -162.0(14) . . . . ?
C13 C11 P1 Ni1 174.5(12) . . . . ?
C14 C11 P1 Ni1 -61.4(14) . . . . ?
C12 C11 P1 Ni1 57.2(15) . . . . ?
C9 C10 P1 C11 90.0(14) . . . . ?
C9 C10 P1 C15 -151.9(13) . . . . ?
C9 C10 P1 Ni1 -27.7(13) . . . . ?
C18 C15 P1 C11 -165.5(13) . . . . ?
C17 C15 P1 C11 -46.9(17) . . . . ?
C16 C15 P1 C11 75.1(16) . . . . ?
C18 C15 P1 C10 81.9(15) . . . . ?
C17 C15 P1 C10 -159.4(14) . . . . ?
C16 C15 P1 C10 -37.5(16) . . . . ?
C18 C15 P1 Ni1 -27.6(16) . . . . ?
C17 C15 P1 Ni1 91.0(14) . . . . ?
C16 C15 P1 Ni1 -147.0(13) . . . . ?

_refine_diff_density_max         0.864
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.159

_shelxl_version_number           2013-3

_database_code_depnum_ccdc_archive 'CCDC 997719'
