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

#######################################################################
#
#                 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
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# 
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#  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.
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data_sjagain

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            NiCl3(PPh3)ClPPh3
_chemical_melting_point          'not measured'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H30 Cl4 Ni P2'
_chemical_formula_weight         725.05

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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   Pbca

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

_cell_length_a                   17.435(4)
_cell_length_b                   15.662(3)
_cell_length_c                   24.139(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6591(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7161
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      24.6755

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2976
_exptl_absorpt_coefficient_mu    1.036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9180
_exptl_absorpt_correction_T_max  0.9424
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 'Bruker D8 goniometer with CCD area detector' 
;

_diffrn_ambient_temperature      100(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            57380
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.10
_reflns_number_total             5858
_reflns_number_gt                4551
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_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 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)+(0.0266P)²+5.3335P] 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         5858
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0720
_refine_ls_wR_factor_gt          0.0649
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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 0.088080(18) 0.77572(2) 0.356472(13) 0.01856(9) Uani 1 1 d . . .
C21 C 0.00366(14) 0.57662(15) 0.37985(10) 0.0160(5) Uani 1 1 d . . .
C11 C -0.02500(13) 0.70276(16) 0.46538(10) 0.0162(5) Uani 1 1 d . . .
C31 C 0.12253(14) 0.62042(15) 0.45547(10) 0.0171(6) Uani 1 1 d . . .
C61 C -0.01057(14) 1.09641(16) 0.33568(10) 0.0178(6) Uani 1 1 d . . .
C36 C 0.11281(15) 0.59913(16) 0.51077(11) 0.0208(6) Uani 1 1 d . . .
H36 H 0.0674 0.6158 0.5296 0.025 Uiso 1 1 calc R . .
C52 C -0.20481(15) 0.93398(17) 0.31531(12) 0.0255(6) Uani 1 1 d . . .
H52 H -0.2194 0.9267 0.3529 0.031 Uiso 1 1 calc R . .
C26 C -0.04699(14) 0.58995(17) 0.33593(10) 0.0216(6) Uani 1 1 d . . .
H26 H -0.0598 0.6465 0.3251 0.026 Uiso 1 1 calc R . .
C22 C 0.02178(15) 0.49253(16) 0.39478(10) 0.0187(6) Uani 1 1 d . . .
H22 H 0.0553 0.4822 0.4251 0.022 Uiso 1 1 calc R . .
C44 C -0.27515(15) 1.24979(17) 0.41115(11) 0.0246(6) Uani 1 1 d . . .
H44 H -0.3122 1.2903 0.4231 0.029 Uiso 1 1 calc R . .
C12 C -0.08027(14) 0.64738(16) 0.48620(11) 0.0206(6) Uani 1 1 d . . .
H12 H -0.0831 0.5907 0.4724 0.025 Uiso 1 1 calc R . .
C43 C -0.21594(15) 1.22643(17) 0.44646(11) 0.0245(6) Uani 1 1 d . . .
H43 H -0.2125 1.2509 0.4824 0.029 Uiso 1 1 calc R . .
C16 C -0.02172(15) 0.78632(16) 0.48578(10) 0.0210(6) Uani 1 1 d . . .
H16 H 0.0153 0.8252 0.4716 0.025 Uiso 1 1 calc R . .
C42 C -0.16204(15) 1.16768(17) 0.42925(11) 0.0230(6) Uani 1 1 d . . .
H42 H -0.1208 1.1524 0.4529 0.028 Uiso 1 1 calc R . .
C51 C -0.14502(13) 0.98943(16) 0.30123(10) 0.0172(6) Uani 1 1 d . . .
C25 C -0.07873(15) 0.52122(17) 0.30801(11) 0.0237(6) Uani 1 1 d . . .
H25 H -0.1144 0.5309 0.2789 0.028 Uiso 1 1 calc R . .
C62 C 0.05621(15) 1.04883(17) 0.34330(10) 0.0218(6) Uani 1 1 d . . .
H62 H 0.0537 0.9923 0.3574 0.026 Uiso 1 1 calc R . .
C56 C -0.12452(15) 1.00102(16) 0.24636(11) 0.0205(6) Uani 1 1 d . . .
H56 H -0.0834 1.0381 0.2369 0.025 Uiso 1 1 calc R . .
C45 C -0.28078(15) 1.21494(16) 0.35910(11) 0.0236(6) Uani 1 1 d . . .
H45 H -0.3210 1.2323 0.3351 0.028 Uiso 1 1 calc R . .
C33 C 0.24602(15) 0.55307(17) 0.45671(12) 0.0266(6) Uani 1 1 d . . .
H33 H 0.2922 0.5379 0.4384 0.032 Uiso 1 1 calc R . .
C14 C -0.12679(15) 0.75631(18) 0.54711(11) 0.0252(6) Uani 1 1 d . . .
H14 H -0.1612 0.7745 0.5752 0.030 Uiso 1 1 calc R . .
C13 C -0.13131(15) 0.67377(18) 0.52680(11) 0.0238(6) Uani 1 1 d . . .
H13 H -0.1691 0.6355 0.5406 0.029 Uiso 1 1 calc R . .
C54 C -0.22281(15) 0.90226(17) 0.21904(11) 0.0239(6) Uani 1 1 d . . .
H54 H -0.2495 0.8723 0.1908 0.029 Uiso 1 1 calc R . .
C41 C -0.16856(14) 1.13084(16) 0.37674(11) 0.0177(6) Uani 1 1 d . . .
C23 C -0.00881(15) 0.42450(17) 0.36580(11) 0.0241(6) Uani 1 1 d . . .
H23 H 0.0045 0.3678 0.3758 0.029 Uiso 1 1 calc R . .
C35 C 0.16900(15) 0.55368(17) 0.53873(12) 0.0260(6) Uani 1 1 d . . .
H35 H 0.1621 0.5392 0.5766 0.031 Uiso 1 1 calc R . .
C53 C -0.24234(15) 0.89001(17) 0.27398(11) 0.0258(6) Uani 1 1 d . . .
H53 H -0.2820 0.8509 0.2833 0.031 Uiso 1 1 calc R . .
C24 C -0.05884(16) 0.43868(18) 0.32220(11) 0.0269(7) Uani 1 1 d . . .
H24 H -0.0794 0.3918 0.3021 0.032 Uiso 1 1 calc R . .
C65 C 0.06296(15) 1.21415(17) 0.30077(11) 0.0242(6) Uani 1 1 d . . .
H65 H 0.0656 1.2702 0.2859 0.029 Uiso 1 1 calc R . .
C66 C -0.00745(15) 1.17886(17) 0.31418(10) 0.0211(6) Uani 1 1 d . . .
H66 H -0.0533 1.2106 0.3088 0.025 Uiso 1 1 calc R . .
C63 C 0.12632(15) 1.08537(18) 0.32995(11) 0.0250(6) Uani 1 1 d . . .
H63 H 0.1723 1.0538 0.3351 0.030 Uiso 1 1 calc R . .
C32 C 0.19008(14) 0.59858(16) 0.42876(11) 0.0217(6) Uani 1 1 d . . .
H32 H 0.1980 0.6148 0.3913 0.026 Uiso 1 1 calc R . .
C46 C -0.22801(14) 1.15450(16) 0.34146(11) 0.0208(6) Uani 1 1 d . . .
H46 H -0.2324 1.1296 0.3057 0.025 Uiso 1 1 calc R . .
C64 C 0.12947(15) 1.16764(19) 0.30907(11) 0.0264(7) Uani 1 1 d . . .
H64 H 0.1777 1.1924 0.3004 0.032 Uiso 1 1 calc R . .
C34 C 0.23470(16) 0.52969(17) 0.51140(13) 0.0301(7) Uani 1 1 d . . .
H34 H 0.2725 0.4969 0.5301 0.036 Uiso 1 1 calc R . .
C55 C -0.16463(15) 0.95790(17) 0.20528(11) 0.0246(6) Uani 1 1 d . . .
H55 H -0.1519 0.9668 0.1675 0.030 Uiso 1 1 calc R . .
C15 C -0.07247(16) 0.81233(18) 0.52663(11) 0.0266(6) Uani 1 1 d . . .
H15 H -0.0699 0.8689 0.5406 0.032 Uiso 1 1 calc R . .
P1 P 0.04599(4) 0.66869(4) 0.41464(3) 0.01549(15) Uani 1 1 d . . .
P2 P -0.10146(4) 1.05178(4) 0.35419(3) 0.01757(15) Uani 1 1 d . . .
Cl4 Cl -0.08177(4) 0.97705(4) 0.41973(3) 0.02675(16) Uani 1 1 d . . .
Cl1 Cl 0.15453(4) 0.86154(4) 0.41368(3) 0.02944(17) Uani 1 1 d . . .
Cl2 Cl 0.15883(4) 0.70996(4) 0.29164(3) 0.02439(16) Uani 1 1 d . . .
Cl3 Cl -0.02129(4) 0.82685(4) 0.32201(3) 0.02856(17) 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 Cl3 2.2293(8) . ?
Ni1 Cl2 2.2431(8) . ?
Ni1 Cl1 2.2485(8) . ?
Ni1 P1 2.3065(8) . ?
C21 C26 1.395(3) . ?
C21 C22 1.401(3) . ?
C21 P1 1.825(3) . ?
C11 C12 1.391(3) . ?
C11 C16 1.399(3) . ?
C11 P1 1.821(2) . ?
C31 C32 1.386(4) . ?
C31 C36 1.386(4) . ?
C31 P1 1.823(3) . ?
C61 C66 1.393(4) . ?
C61 C62 1.395(4) . ?
C61 P2 1.789(3) . ?
C36 C35 1.386(4) . ?
C36 H36 0.9500 . ?
C52 C53 1.378(4) . ?
C52 C51 1.399(3) . ?
C52 H52 0.9500 . ?
C26 C25 1.385(4) . ?
C26 H26 0.9500 . ?
C22 C23 1.382(4) . ?
C22 H22 0.9500 . ?
C44 C45 1.373(4) . ?
C44 C43 1.388(4) . ?
C44 H44 0.9500 . ?
C12 C13 1.387(4) . ?
C12 H12 0.9500 . ?
C43 C42 1.379(4) . ?
C43 H43 0.9500 . ?
C16 C15 1.386(4) . ?
C16 H16 0.9500 . ?
C42 C41 1.397(4) . ?
C42 H42 0.9500 . ?
C51 C56 1.384(4) . ?
C51 P2 1.779(3) . ?
C25 C24 1.382(4) . ?
C25 H25 0.9500 . ?
C62 C63 1.388(4) . ?
C62 H62 0.9500 . ?
C56 C55 1.389(4) . ?
C56 H56 0.9500 . ?
C45 C46 1.387(4) . ?
C45 H45 0.9500 . ?
C33 C32 1.384(4) . ?
C33 C34 1.384(4) . ?
C33 H33 0.9500 . ?
C14 C15 1.382(4) . ?
C14 C13 1.385(4) . ?
C14 H14 0.9500 . ?
C13 H13 0.9500 . ?
C54 C55 1.378(4) . ?
C54 C53 1.382(4) . ?
C54 H54 0.9500 . ?
C41 C46 1.392(4) . ?
C41 P2 1.788(3) . ?
C23 C24 1.385(4) . ?
C23 H23 0.9500 . ?
C35 C34 1.374(4) . ?
C35 H35 0.9500 . ?
C53 H53 0.9500 . ?
C24 H24 0.9500 . ?
C65 C64 1.384(4) . ?
C65 C66 1.385(4) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C63 C64 1.385(4) . ?
C63 H63 0.9500 . ?
C32 H32 0.9500 . ?
C46 H46 0.9500 . ?
C64 H64 0.9500 . ?
C34 H34 0.9500 . ?
C55 H55 0.9500 . ?
C15 H15 0.9500 . ?
P2 Cl4 1.9977(10) . ?

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
Cl3 Ni1 Cl2 112.02(3) . . ?
Cl3 Ni1 Cl1 117.08(3) . . ?
Cl2 Ni1 Cl1 114.81(3) . . ?
Cl3 Ni1 P1 102.48(3) . . ?
Cl2 Ni1 P1 105.43(3) . . ?
Cl1 Ni1 P1 102.97(3) . . ?
C26 C21 C22 118.6(2) . . ?
C26 C21 P1 119.17(19) . . ?
C22 C21 P1 122.22(19) . . ?
C12 C11 C16 119.0(2) . . ?
C12 C11 P1 122.09(19) . . ?
C16 C11 P1 118.88(19) . . ?
C32 C31 C36 119.5(2) . . ?
C32 C31 P1 118.22(19) . . ?
C36 C31 P1 122.1(2) . . ?
C66 C61 C62 120.8(2) . . ?
C66 C61 P2 119.35(19) . . ?
C62 C61 P2 119.9(2) . . ?
C31 C36 C35 120.4(3) . . ?
C31 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C53 C52 C51 119.2(3) . . ?
C53 C52 H52 120.4 . . ?
C51 C52 H52 120.4 . . ?
C25 C26 C21 120.4(2) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C23 C22 C21 120.5(2) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C45 C44 C43 120.7(3) . . ?
C45 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
C13 C12 C11 120.9(2) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C42 C43 C44 119.9(3) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C15 C16 C11 119.9(3) . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
C43 C42 C41 119.6(2) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C56 C51 C52 120.4(2) . . ?
C56 C51 P2 120.38(19) . . ?
C52 C51 P2 119.0(2) . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C63 C62 C61 119.0(2) . . ?
C63 C62 H62 120.5 . . ?
C61 C62 H62 120.5 . . ?
C51 C56 C55 119.3(2) . . ?
C51 C56 H56 120.3 . . ?
C55 C56 H56 120.3 . . ?
C44 C45 C46 120.3(3) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C32 C33 C34 120.1(3) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C15 C14 C13 120.3(2) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C13 C12 119.5(3) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C55 C54 C53 120.0(3) . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
C46 C41 C42 120.4(2) . . ?
C46 C41 P2 119.0(2) . . ?
C42 C41 P2 120.6(2) . . ?
C22 C23 C24 120.3(2) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C34 C35 C36 119.7(3) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C52 C53 C54 120.6(3) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 H53 119.7 . . ?
C25 C24 C23 119.8(3) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C64 C65 C66 119.9(3) . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C65 C66 C61 119.5(2) . . ?
C65 C66 H66 120.3 . . ?
C61 C66 H66 120.3 . . ?
C64 C63 C62 120.2(3) . . ?
C64 C63 H63 119.9 . . ?
C62 C63 H63 119.9 . . ?
C33 C32 C31 119.9(3) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C45 C46 C41 119.2(2) . . ?
C45 C46 H46 120.4 . . ?
C41 C46 H46 120.4 . . ?
C65 C64 C63 120.6(3) . . ?
C65 C64 H64 119.7 . . ?
C63 C64 H64 119.7 . . ?
C35 C34 C33 120.3(3) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C54 C55 C56 120.4(3) . . ?
C54 C55 H55 119.8 . . ?
C56 C55 H55 119.8 . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C11 P1 C31 104.79(11) . . ?
C11 P1 C21 105.44(11) . . ?
C31 P1 C21 102.54(11) . . ?
C11 P1 Ni1 114.38(8) . . ?
C31 P1 Ni1 113.43(8) . . ?
C21 P1 Ni1 115.02(8) . . ?
C51 P2 C41 108.64(12) . . ?
C51 P2 C61 114.40(12) . . ?
C41 P2 C61 112.64(12) . . ?
C51 P2 Cl4 108.72(9) . . ?
C41 P2 Cl4 106.08(9) . . ?
C61 P2 Cl4 105.94(9) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.063
_database_code_depnum_ccdc_archive 'CCDC 992218'
#######################################################################
#
#                 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_sj2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Cl2P(PPh3)3
_chemical_melting_point          'not measured'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H15 Cl2 P'
_chemical_formula_weight         333.17

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   13.338(3)
_cell_length_b                   14.376(3)
_cell_length_c                   8.7454(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.53(3)
_cell_angle_gamma                90.00
_cell_volume                     1637.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7427
_cell_measurement_theta_min      2.775
_cell_measurement_theta_max      24.9975

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    0.484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8111
_exptl_absorpt_correction_T_max  0.9248
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 'Bruker D8 goniometer with CCD area detector' 
;

_diffrn_ambient_temperature      100(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            18333
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         25.01
_reflns_number_total             2874
_reflns_number_gt                2527
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_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 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)+(0.0303P)²+1.1255P] 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         2874
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0710
_refine_ls_wR_factor_gt          0.0677
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_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
C11 C 0.22238(13) 0.53306(13) -0.0840(2) 0.0182(4) Uani 1 1 d . . .
C12 C 0.24135(14) 0.62160(13) -0.1362(2) 0.0229(4) Uani 1 1 d . . .
H12 H 0.2766 0.6667 -0.0651 0.028 Uiso 1 1 calc R . .
C13 C 0.20772(16) 0.64273(15) -0.2943(2) 0.0318(5) Uani 1 1 d . . .
H13 H 0.2226 0.7019 -0.3323 0.038 Uiso 1 1 calc R . .
C14 C 0.15305(16) 0.57853(17) -0.3961(2) 0.0347(5) Uani 1 1 d . . .
H14 H 0.1278 0.5948 -0.5029 0.042 Uiso 1 1 calc R . .
C15 C 0.13467(16) 0.49106(16) -0.3446(2) 0.0329(5) Uani 1 1 d . . .
H15 H 0.0971 0.4471 -0.4156 0.039 Uiso 1 1 calc R . .
C16 C 0.17130(15) 0.46706(14) -0.1879(2) 0.0247(4) Uani 1 1 d . . .
H16 H 0.1613 0.4059 -0.1527 0.030 Uiso 1 1 calc R . .
C21 C 0.36166(13) 0.57025(12) 0.2477(2) 0.0179(4) Uani 1 1 d . . .
C22 C 0.35582(14) 0.58843(13) 0.4015(2) 0.0221(4) Uani 1 1 d . . .
H22 H 0.3005 0.5644 0.4419 0.026 Uiso 1 1 calc R . .
C23 C 0.43117(15) 0.64190(14) 0.4956(2) 0.0257(4) Uani 1 1 d . . .
H23 H 0.4285 0.6534 0.6016 0.031 Uiso 1 1 calc R . .
C24 C 0.51033(14) 0.67850(13) 0.4350(2) 0.0255(4) Uani 1 1 d . . .
H24 H 0.5601 0.7176 0.4982 0.031 Uiso 1 1 calc R . .
C25 C 0.51739(14) 0.65857(14) 0.2836(2) 0.0275(5) Uani 1 1 d . . .
H25 H 0.5729 0.6828 0.2438 0.033 Uiso 1 1 calc R . .
C26 C 0.44377(14) 0.60319(13) 0.1888(2) 0.0231(4) Uani 1 1 d . . .
H26 H 0.4495 0.5881 0.0853 0.028 Uiso 1 1 calc R . .
C31 C 0.19023(13) 0.41732(12) 0.2058(2) 0.0155(4) Uani 1 1 d . . .
C32 C 0.08837(13) 0.39790(12) 0.1364(2) 0.0170(4) Uani 1 1 d . . .
H32 H 0.0545 0.4310 0.0459 0.020 Uiso 1 1 calc R . .
C33 C 0.03664(14) 0.32956(13) 0.2009(2) 0.0198(4) Uani 1 1 d . . .
H33 H -0.0322 0.3144 0.1521 0.024 Uiso 1 1 calc R . .
C34 C 0.08458(14) 0.28356(13) 0.3354(2) 0.0233(4) Uani 1 1 d . . .
H34 H 0.0482 0.2378 0.3800 0.028 Uiso 1 1 calc R . .
C35 C 0.18552(15) 0.30398(13) 0.4055(2) 0.0257(4) Uani 1 1 d . . .
H35 H 0.2181 0.2725 0.4986 0.031 Uiso 1 1 calc R . .
C36 C 0.23911(14) 0.37027(13) 0.3402(2) 0.0226(4) Uani 1 1 d . . .
H36 H 0.3088 0.3834 0.3870 0.027 Uiso 1 1 calc R . .
Cl1 Cl 0.14271(3) 0.61325(3) 0.16899(5) 0.01696(12) Uani 1 1 d . . .
Cl2 Cl 0.37086(3) 0.39823(3) 0.07639(5) 0.02395(13) Uani 1 1 d . . .
P1 P 0.26018(3) 0.50460(3) 0.12233(5) 0.01519(12) 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
C11 C16 1.387(3) . ?
C11 C12 1.394(3) . ?
C11 P1 1.8116(18) . ?
C12 C13 1.392(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.377(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.394(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.388(3) . ?
C21 C26 1.391(3) . ?
C21 P1 1.8115(18) . ?
C22 C23 1.385(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.378(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.390(3) . ?
C31 C32 1.391(3) . ?
C31 P1 1.8092(17) . ?
C32 C33 1.389(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.384(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.387(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
Cl1 P1 2.3107(7) . ?
Cl2 P1 2.2218(7) . ?

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
C16 C11 C12 120.56(17) . . ?
C16 C11 P1 119.31(14) . . ?
C12 C11 P1 120.09(14) . . ?
C13 C12 C11 118.85(19) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C14 C13 C12 120.5(2) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C15 C14 C13 120.51(19) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.9(2) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C11 C16 C15 119.51(19) . . ?
C11 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C22 C21 C26 120.59(17) . . ?
C22 C21 P1 119.53(14) . . ?
C26 C21 P1 119.87(14) . . ?
C23 C22 C21 119.59(17) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C24 C23 C22 119.95(18) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 120.37(18) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 120.38(18) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 119.01(18) . . ?
C25 C26 H26 120.5 . . ?
C21 C26 H26 120.5 . . ?
C36 C31 C32 120.38(16) . . ?
C36 C31 P1 119.36(14) . . ?
C32 C31 P1 120.25(13) . . ?
C33 C32 C31 119.30(16) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C34 C33 C32 120.41(17) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 120.15(17) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C36 120.12(17) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 119.59(17) . . ?
C35 C36 H36 120.2 . . ?
C31 C36 H36 120.2 . . ?
C31 P1 C21 120.01(8) . . ?
C31 P1 C11 120.13(8) . . ?
C21 P1 C11 119.68(9) . . ?
C31 P1 Cl2 90.96(6) . . ?
C21 P1 Cl2 91.70(6) . . ?
C11 P1 Cl2 91.59(6) . . ?
C31 P1 Cl1 88.21(6) . . ?
C21 P1 Cl1 89.26(6) . . ?
C11 P1 Cl1 88.30(6) . . ?
Cl2 P1 Cl1 178.96(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.046
_database_code_depnum_ccdc_archive 'CCDC 992219'
#######################################################################
#
#                 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_sj

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ClPPh3OTf
_chemical_melting_point          'not measured'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H15 Cl F3 O3 P S'
_chemical_formula_weight         446.79

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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   11.255(2)
_cell_length_b                   9.1501(18)
_cell_length_c                   18.658(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.04(3)
_cell_angle_gamma                90.00
_cell_volume                     1918.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9118
_cell_measurement_theta_min      2.1655
_cell_measurement_theta_max      25.036

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9417
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 'Bruker D8 goniometer with CCD area detector' 
;

_diffrn_ambient_temperature      100(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            18058
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         25.04
_reflns_number_total             3392
_reflns_number_gt                2859
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_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 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)+(0.0280P)²+1.6150P] 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         3392
_refine_ls_number_parameters     308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0737
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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
F1A F 0.271(2) 0.0662(17) 0.1453(12) 0.036(3) Uani 0.679(2) 1 d P A 1
F2A F 0.3239(7) 0.0676(18) 0.0359(9) 0.0308(13) Uani 0.679(2) 1 d P A 1
F3A F 0.15785(16) 0.1655(2) 0.05803(11) 0.0398(6) Uani 0.679(2) 1 d P A 1
C41A C 0.2713(4) 0.1503(4) 0.0843(2) 0.0250(9) Uani 0.679(2) 1 d P A 1
S1A S 0.34008(12) 0.32752(10) 0.09975(5) 0.0185(2) Uani 0.679(2) 1 d P A 1
O1A O 0.2657(9) 0.3954(14) 0.1503(6) 0.0280(16) Uani 0.679(2) 1 d P A 1
O2A O 0.3327(5) 0.3908(7) 0.0278(3) 0.0260(9) Uani 0.679(2) 1 d P A 1
O3A O 0.45726(18) 0.2889(3) 0.12787(12) 0.0301(5) Uani 0.679(2) 1 d P A 1
F1B F 0.253(5) 0.064(4) 0.138(3) 0.037(7) Uani 0.321(2) 1 d P A 2
F2B F 0.3482(19) 0.070(4) 0.039(2) 0.0308(13) Uani 0.321(2) 1 d P A 2
F3B F 0.4420(3) 0.1257(5) 0.1319(2) 0.0387(12) Uani 0.321(2) 1 d P A 2
C41B C 0.3340(8) 0.1302(9) 0.1001(5) 0.0256(18) Uani 0.321(2) 1 d P A 2
S1B S 0.2782(3) 0.3171(2) 0.08889(11) 0.0220(5) Uani 0.321(2) 1 d P A 2
O1B O 0.291(2) 0.374(3) 0.1617(14) 0.026(3) Uani 0.321(2) 1 d P A 2
O2B O 0.3621(12) 0.3796(18) 0.0419(8) 0.0260(9) Uani 0.321(2) 1 d P A 2
O3B O 0.1589(4) 0.2966(6) 0.0621(3) 0.0301(5) Uani 0.321(2) 1 d P A 2
C11 C 0.93178(17) 1.0989(2) 0.25583(11) 0.0162(4) Uani 1 1 d . . .
C12 C 1.02145(17) 1.1897(2) 0.23177(11) 0.0194(4) Uani 1 1 d . . .
H12 H 1.0350 1.1961 0.1820 0.023 Uiso 1 1 calc R . .
C13 C 1.09015(18) 1.2698(2) 0.28126(11) 0.0223(5) Uani 1 1 d . . .
H13 H 1.1517 1.3311 0.2656 0.027 Uiso 1 1 calc R . .
C14 C 1.06943(18) 1.2610(2) 0.35354(12) 0.0244(5) Uani 1 1 d . . .
H14 H 1.1159 1.3180 0.3871 0.029 Uiso 1 1 calc R . .
C15 C 0.98165(19) 1.1699(2) 0.37755(12) 0.0237(5) Uani 1 1 d . . .
H15 H 0.9688 1.1637 0.4274 0.028 Uiso 1 1 calc R . .
C16 C 0.91270(18) 1.0879(2) 0.32882(11) 0.0194(4) Uani 1 1 d . . .
H16 H 0.8528 1.0246 0.3450 0.023 Uiso 1 1 calc R . .
C21 C 0.81241(17) 1.1054(2) 0.11216(10) 0.0168(4) Uani 1 1 d . . .
C22 C 0.89505(19) 1.1047(2) 0.05958(11) 0.0235(5) Uani 1 1 d . . .
H22 H 0.9617 1.0409 0.0635 0.028 Uiso 1 1 calc R . .
C23 C 0.8795(2) 1.1977(2) 0.00132(12) 0.0261(5) Uani 1 1 d . . .
H23 H 0.9365 1.1991 -0.0345 0.031 Uiso 1 1 calc R . .
C24 C 0.78164(18) 1.2886(2) -0.00505(11) 0.0211(5) Uani 1 1 d . . .
H24 H 0.7719 1.3527 -0.0450 0.025 Uiso 1 1 calc R . .
C25 C 0.69758(18) 1.2867(2) 0.04650(11) 0.0226(5) Uani 1 1 d . . .
H25 H 0.6295 1.3479 0.0413 0.027 Uiso 1 1 calc R . .
C26 C 0.71267(17) 1.1959(2) 0.10561(11) 0.0208(5) Uani 1 1 d . . .
H26 H 0.6556 1.1952 0.1414 0.025 Uiso 1 1 calc R . .
C31 C 0.91020(17) 0.8295(2) 0.16827(11) 0.0169(4) Uani 1 1 d . . .
C32 C 0.85264(18) 0.7427(2) 0.11516(11) 0.0201(4) Uani 1 1 d . . .
H32 H 0.7802 0.7743 0.0917 0.024 Uiso 1 1 calc R . .
C33 C 0.90240(19) 0.6106(2) 0.09734(12) 0.0236(5) Uani 1 1 d . . .
H33 H 0.8637 0.5504 0.0618 0.028 Uiso 1 1 calc R . .
C34 C 1.00860(19) 0.5658(2) 0.13122(12) 0.0254(5) Uani 1 1 d . . .
H34 H 1.0426 0.4751 0.1185 0.030 Uiso 1 1 calc R . .
C35 C 1.06565(19) 0.6516(2) 0.18336(12) 0.0245(5) Uani 1 1 d . . .
H35 H 1.1385 0.6195 0.2061 0.029 Uiso 1 1 calc R . .
C36 C 1.01710(18) 0.7845(2) 0.20268(11) 0.0206(4) Uani 1 1 d . . .
H36 H 1.0559 0.8437 0.2386 0.025 Uiso 1 1 calc R . .
P1 P 0.84357(4) 0.99832(5) 0.19080(3) 0.01562(13) Uani 1 1 d . . .
Cl1 Cl 0.68872(4) 0.95565(5) 0.23320(3) 0.02216(13) 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
F1A C41A 1.37(2) . ?
F2A C41A 1.340(16) . ?
F3A C41A 1.350(5) . ?
C41A S1A 1.813(4) . ?
S1A O1A 1.435(13) . ?
S1A O3A 1.437(2) . ?
S1A O2A 1.461(5) . ?
F1B C41B 1.33(4) . ?
F2B C41B 1.28(4) . ?
F3B C41B 1.324(10) . ?
C41B S1B 1.830(9) . ?
S1B O3B 1.420(6) . ?
S1B O2B 1.441(17) . ?
S1B O1B 1.45(3) . ?
C11 C16 1.394(3) . ?
C11 C12 1.399(3) . ?
C11 P1 1.782(2) . ?
C12 C13 1.383(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.387(3) . ?
C21 C26 1.395(3) . ?
C21 P1 1.784(2) . ?
C22 C23 1.385(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.380(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.396(3) . ?
C31 C32 1.402(3) . ?
C31 P1 1.777(2) . ?
C32 C33 1.380(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.384(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.389(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
P1 Cl1 1.9905(8) . ?

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
F2A C41A F3A 104.9(5) . . ?
F2A C41A F1A 105.2(10) . . ?
F3A C41A F1A 108.4(11) . . ?
F2A C41A S1A 114.3(6) . . ?
F3A C41A S1A 110.7(3) . . ?
F1A C41A S1A 112.9(10) . . ?
O1A S1A O3A 115.0(4) . . ?
O1A S1A O2A 115.2(4) . . ?
O3A S1A O2A 116.1(3) . . ?
O1A S1A C41A 103.4(6) . . ?
O3A S1A C41A 102.37(18) . . ?
O2A S1A C41A 101.9(3) . . ?
F2B C41B F3B 103.2(12) . . ?
F2B C41B F1B 113(2) . . ?
F3B C41B F1B 113(3) . . ?
F2B C41B S1B 111.0(18) . . ?
F3B C41B S1B 112.4(5) . . ?
F1B C41B S1B 104.4(17) . . ?
O3B S1B O2B 118.5(5) . . ?
O3B S1B O1B 115.1(10) . . ?
O2B S1B O1B 112.9(13) . . ?
O3B S1B C41B 103.2(4) . . ?
O2B S1B C41B 102.0(7) . . ?
O1B S1B C41B 102.0(8) . . ?
C16 C11 C12 120.50(18) . . ?
C16 C11 P1 121.25(15) . . ?
C12 C11 P1 118.25(15) . . ?
C13 C12 C11 119.21(19) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 120.2(2) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C15 120.7(2) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C16 C15 C14 119.9(2) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C15 C16 C11 119.50(19) . . ?
C15 C16 H16 120.2 . . ?
C11 C16 H16 120.2 . . ?
C22 C21 C26 120.50(19) . . ?
C22 C21 P1 117.98(15) . . ?
C26 C21 P1 121.35(16) . . ?
C23 C22 C21 119.38(19) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 120.30(19) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C26 C25 C24 120.10(19) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C21 119.36(19) . . ?
C25 C26 H26 120.3 . . ?
C21 C26 H26 120.3 . . ?
C36 C31 C32 120.83(18) . . ?
C36 C31 P1 120.81(15) . . ?
C32 C31 P1 118.36(15) . . ?
C33 C32 C31 119.25(19) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C32 C33 C34 120.1(2) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C35 C34 C33 120.7(2) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C34 C35 C36 120.4(2) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C31 118.73(19) . . ?
C35 C36 H36 120.6 . . ?
C31 C36 H36 120.6 . . ?
C31 P1 C11 112.52(9) . . ?
C31 P1 C21 110.48(9) . . ?
C11 P1 C21 110.75(9) . . ?
C31 P1 Cl1 108.24(7) . . ?
C11 P1 Cl1 107.37(7) . . ?
C21 P1 Cl1 107.26(7) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.049
_database_code_depnum_ccdc_archive 'CCDC 992220'
#######################################################################
#
#                 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_sj

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            NiCl4(PPh2(THF)2)2
_chemical_melting_point          'not measured'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H48 Cl4 Ni O4 P2'
_chemical_formula_weight         855.23

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   10.1261(8)
_cell_length_b                   23.4579(18)
_cell_length_c                   17.8192(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.3550(12)
_cell_angle_gamma                90.00
_cell_volume                     4061.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7748
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      25.02

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6370
_exptl_absorpt_correction_T_max  0.8191
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'

_exptl_special_details           
; 
 'Bruker D8 goniometer with CCD area detector' 
;

_diffrn_ambient_temperature      100(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            44051
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         25.10
_reflns_number_total             7212
_reflns_number_gt                5695
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_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 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. 
;
# start Validation Reply Form
_vrf_PLAT411_sj                  
;
PROBLEM: Short Inter H...H Contact H52 .. H82C .. 1.95 Ang. 
RESPONSE: H82C is one of the hydrogen atoms attached to the disordered carbon atom so this model is reasonable.
;
# end Validation Reply Form

_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)+(0.0281P)²+14.0724P] 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         7212
_refine_ls_number_parameters     448
_refine_ls_number_restraints     94
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1315
_refine_ls_wR_factor_gt          0.1234
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.131
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C -0.4952(4) 0.37018(19) -0.0756(2) 0.0223(9) Uani 1 1 d . . .
C12 C -0.4308(5) 0.41556(19) -0.1012(3) 0.0295(10) Uani 1 1 d . . .
H12 H -0.4613 0.4535 -0.0976 0.035 Uiso 1 1 calc R . .
C13 C -0.3230(5) 0.4051(2) -0.1317(3) 0.0349(11) Uani 1 1 d . . .
H13 H -0.2778 0.4362 -0.1483 0.042 Uiso 1 1 calc R . .
C14 C -0.2790(5) 0.3501(2) -0.1387(3) 0.0365(12) Uani 1 1 d . . .
H14 H -0.2049 0.3436 -0.1606 0.044 Uiso 1 1 calc R . .
C15 C -0.3431(5) 0.3042(2) -0.1138(3) 0.0334(11) Uani 1 1 d . . .
H15 H -0.3129 0.2664 -0.1181 0.040 Uiso 1 1 calc R . .
C16 C -0.4519(5) 0.31463(19) -0.0825(3) 0.0281(10) Uani 1 1 d . . .
H16 H -0.4971 0.2836 -0.0658 0.034 Uiso 1 1 calc R . .
C21 C -0.7631(4) 0.3299(2) -0.0629(3) 0.0293(10) Uani 1 1 d . . .
C22 C -0.8156(5) 0.3191(2) -0.1425(3) 0.0285(10) Uani 1 1 d . . .
H22 H -0.7770 0.3374 -0.1790 0.034 Uiso 1 1 calc R . .
C23 C -0.9245(5) 0.2815(2) -0.1683(3) 0.0359(11) Uani 1 1 d . . .
H23 H -0.9619 0.2747 -0.2227 0.043 Uiso 1 1 calc R . .
C24 C -0.9784(5) 0.2541(3) -0.1158(3) 0.0481(10) Uani 1 1 d . . .
H24 H -1.0511 0.2275 -0.1337 0.058 Uiso 1 1 calc R . .
C25 C -0.9274(5) 0.2652(3) -0.0377(3) 0.0481(10) Uani 1 1 d . . .
H25 H -0.9663 0.2461 -0.0019 0.058 Uiso 1 1 calc R . .
C26 C -0.8207(5) 0.3033(3) -0.0091(3) 0.0461(14) Uani 1 1 d . . .
H26 H -0.7876 0.3112 0.0453 0.055 Uiso 1 1 calc R . .
C31 C -0.5637(4) 0.3814(2) 0.0742(3) 0.0330(11) Uani 1 1 d D . .
H31 H -0.6398 0.3877 0.0989 0.040 Uiso 0.693(3) 1 calc PR A 1
H31A H -0.6433 0.3847 0.0968 0.040 Uiso 0.307(3) 1 calc PR A 2
C32 C -0.4826(9) 0.3302(3) 0.1089(5) 0.0273(6) Uani 0.693(3) 1 d PD A 1
H32A H -0.4326 0.3134 0.0738 0.033 Uiso 0.693(3) 1 calc PR A 1
H32B H -0.5402 0.3007 0.1240 0.033 Uiso 0.693(3) 1 calc PR A 1
C33 C -0.3833(7) 0.3601(3) 0.1818(4) 0.0273(6) Uani 0.693(3) 1 d PD A 1
H33A H -0.4310 0.3691 0.2217 0.033 Uiso 0.693(3) 1 calc PR A 1
H33B H -0.3020 0.3360 0.2056 0.033 Uiso 0.693(3) 1 calc PR A 1
C34 C -0.3425(6) 0.4137(3) 0.1471(4) 0.0273(6) Uani 0.693(3) 1 d PD A 1
H34A H -0.3097 0.4431 0.1880 0.033 Uiso 0.693(3) 1 calc PR A 1
H34B H -0.2682 0.4056 0.1225 0.033 Uiso 0.693(3) 1 calc PR A 1
O1 O -0.4696(5) 0.4336(2) 0.0872(3) 0.0273(6) Uani 0.693(3) 1 d PD A 1
C32A C -0.4995(19) 0.3221(5) 0.0956(11) 0.0273(6) Uani 0.307(3) 1 d PD A 2
H32C H -0.5675 0.2960 0.1077 0.033 Uiso 0.307(3) 1 calc PR A 2
H32D H -0.4710 0.3061 0.0512 0.033 Uiso 0.307(3) 1 calc PR A 2
C33A C -0.3766(13) 0.3282(6) 0.1658(8) 0.0273(6) Uani 0.307(3) 1 d PD A 2
H33C H -0.2899 0.3219 0.1517 0.033 Uiso 0.307(3) 1 calc PR A 2
H33D H -0.3812 0.3010 0.2075 0.033 Uiso 0.307(3) 1 calc PR A 2
C34A C -0.3868(14) 0.3894(6) 0.1917(7) 0.0273(6) Uani 0.307(3) 1 d PD A 2
H34C H -0.2943 0.4057 0.2158 0.033 Uiso 0.307(3) 1 calc PR A 2
H34D H -0.4415 0.3917 0.2297 0.033 Uiso 0.307(3) 1 calc PR A 2
O1A O -0.4600(11) 0.4211(4) 0.1150(6) 0.0273(6) Uani 0.307(3) 1 d PD A 2
C41 C -0.7064(5) 0.4530(2) -0.0584(3) 0.0360(11) Uani 1 1 d D . .
H41 H -0.6326 0.4824 -0.0405 0.043 Uiso 0.693(3) 1 calc PR A 1
H41A H -0.6326 0.4824 -0.0405 0.043 Uiso 0.307(3) 1 calc PR A 2
O2 O -0.7568(3) 0.45498(15) -0.14201(18) 0.0397(8) Uani 1 1 d D A .
C42 C -0.8244(8) 0.4674(5) -0.0256(4) 0.0544(11) Uani 0.693(3) 1 d PD A 1
H42A H -0.8728 0.4325 -0.0167 0.065 Uiso 0.693(3) 1 calc PR A 1
H42B H -0.7915 0.4884 0.0244 0.065 Uiso 0.693(3) 1 calc PR A 1
C43 C -0.9150(8) 0.5033(4) -0.0861(4) 0.0544(11) Uani 0.693(3) 1 d PD A 1
H43A H -0.8836 0.5435 -0.0817 0.065 Uiso 0.693(3) 1 calc PR A 1
H43B H -1.0115 0.5017 -0.0838 0.065 Uiso 0.693(3) 1 calc PR A 1
C44 C -0.8988(9) 0.4754(5) -0.1597(6) 0.0544(11) Uani 0.693(3) 1 d PD A 1
H44A H -0.9638 0.4431 -0.1753 0.065 Uiso 0.693(3) 1 calc PR A 1
H44B H -0.9177 0.5032 -0.2032 0.065 Uiso 0.693(3) 1 calc PR A 1
C42A C -0.8239(13) 0.4673(10) -0.0255(7) 0.0544(11) Uani 0.307(3) 1 d PD A 2
H42C H -0.8196 0.5077 -0.0088 0.065 Uiso 0.307(3) 1 calc PR A 2
H42D H -0.8229 0.4426 0.0197 0.065 Uiso 0.307(3) 1 calc PR A 2
C43A C -0.9507(11) 0.4563(9) -0.0928(7) 0.0544(11) Uani 0.307(3) 1 d PD A 2
H43C H -1.0244 0.4838 -0.0919 0.065 Uiso 0.307(3) 1 calc PR A 2
H43D H -0.9855 0.4172 -0.0898 0.065 Uiso 0.307(3) 1 calc PR A 2
C44A C -0.9033(16) 0.4641(13) -0.1711(15) 0.0544(11) Uani 0.307(3) 1 d PD A 2
H44C H -0.9472 0.4355 -0.2112 0.065 Uiso 0.307(3) 1 calc PR A 2
H44D H -0.9246 0.5028 -0.1933 0.065 Uiso 0.307(3) 1 calc PR A 2
P1 P -0.63153(11) 0.38233(5) -0.03134(6) 0.0243(3) Uani 1 1 d . A .
C51 C -1.0271(4) 0.38913(17) -0.3843(2) 0.0217(9) Uani 1 1 d . A .
C52 C -1.0621(5) 0.44547(19) -0.3743(3) 0.0291(10) Uani 1 1 d . . .
H52 H -1.0083 0.4755 -0.3861 0.035 Uiso 1 1 calc R . .
C53 C -1.1745(5) 0.4583(2) -0.3473(3) 0.0330(11) Uani 1 1 d . . .
H53 H -1.1990 0.4968 -0.3414 0.040 Uiso 1 1 calc R . .
C54 C -1.2498(5) 0.4142(2) -0.3290(3) 0.0356(12) Uani 1 1 d . . .
H54 H -1.3263 0.4225 -0.3099 0.043 Uiso 1 1 calc R . .
C55 C -1.2157(5) 0.3581(2) -0.3381(3) 0.0364(12) Uani 1 1 d . . .
H55 H -1.2689 0.3282 -0.3254 0.044 Uiso 1 1 calc R . .
C56 C -1.1044(5) 0.34533(19) -0.3655(3) 0.0286(10) Uani 1 1 d . . .
H56 H -1.0809 0.3067 -0.3716 0.034 Uiso 1 1 calc R . .
C61 C -0.7635(4) 0.42914(18) -0.4017(3) 0.0234(9) Uani 1 1 d . A .
C62 C -0.7048(5) 0.44186(19) -0.3228(3) 0.0315(11) Uani 1 1 d . . .
H62 H -0.7371 0.4235 -0.2839 0.038 Uiso 1 1 calc R . .
C63 C -0.5999(5) 0.4812(2) -0.3016(3) 0.0372(12) Uani 1 1 d . . .
H63 H -0.5583 0.4891 -0.2479 0.045 Uiso 1 1 calc R . .
C64 C -0.5545(5) 0.5094(2) -0.3580(3) 0.0381(12) Uani 1 1 d . . .
H64 H -0.4820 0.5364 -0.3431 0.046 Uiso 1 1 calc R . .
C65 C -0.6158(5) 0.4978(2) -0.4363(3) 0.0373(12) Uani 1 1 d . . .
H65 H -0.5865 0.5179 -0.4750 0.045 Uiso 1 1 calc R . .
C66 C -0.7185(5) 0.45761(19) -0.4588(3) 0.0294(10) Uani 1 1 d . . .
H66 H -0.7583 0.4493 -0.5126 0.035 Uiso 1 1 calc R . .
C71 C -0.8133(5) 0.30532(18) -0.3954(3) 0.0269(10) Uani 1 1 d . A .
H71 H -0.8861 0.2753 -0.4100 0.032 Uiso 1 1 calc R . .
C72 C -0.6959(5) 0.2892(2) -0.4289(3) 0.0310(11) Uani 1 1 d . . .
H72A H -0.6983 0.2481 -0.4419 0.037 Uiso 0.693(3) 1 calc PR A 1
H72B H -0.6991 0.3118 -0.4764 0.037 Uiso 0.693(3) 1 calc PR A 1
H72C H -0.7306 0.2676 -0.4783 0.037 Uiso 0.307(3) 1 calc PR A 2
H72D H -0.6473 0.3237 -0.4392 0.037 Uiso 0.307(3) 1 calc PR A 2
C73 C -0.5702(7) 0.3038(3) -0.3629(5) 0.0419(17) Uani 0.693(3) 1 d P A 1
H73A H -0.4909 0.2796 -0.3643 0.050 Uiso 0.693(3) 1 calc PR A 1
H73B H -0.5446 0.3444 -0.3649 0.050 Uiso 0.693(3) 1 calc PR A 1
C73A C -0.6041(16) 0.2536(8) -0.3681(10) 0.0419(17) Uani 0.307(3) 1 d P A 2
H73C H -0.5090 0.2525 -0.3727 0.050 Uiso 0.307(3) 1 calc PR A 2
H73D H -0.6395 0.2143 -0.3676 0.050 Uiso 0.307(3) 1 calc PR A 2
C74 C -0.6164(6) 0.2916(3) -0.2917(3) 0.0527(15) Uani 1 1 d . . .
H74A H -0.6042 0.2508 -0.2776 0.063 Uiso 0.693(3) 1 calc PR A 1
H74B H -0.5632 0.3146 -0.2468 0.063 Uiso 0.693(3) 1 calc PR A 1
H74C H -0.5907 0.2686 -0.2432 0.063 Uiso 0.307(3) 1 calc PR A 2
H74D H -0.5571 0.3259 -0.2844 0.063 Uiso 0.307(3) 1 calc PR A 2
C81 C -0.9650(9) 0.3703(3) -0.5340(5) 0.0301(6) Uani 0.693(3) 1 d PD A 1
H81 H -0.8899 0.3708 -0.5604 0.036 Uiso 0.693(3) 1 calc PR A 1
C82 C -1.0716(7) 0.4135(3) -0.5701(4) 0.0301(6) Uani 0.693(3) 1 d PD A 1
H82A H -1.0599 0.4273 -0.6204 0.036 Uiso 0.693(3) 1 calc PR A 1
H82B H -1.0668 0.4465 -0.5348 0.036 Uiso 0.693(3) 1 calc PR A 1
C83 C -1.2099(7) 0.3812(3) -0.5832(5) 0.0301(6) Uani 0.693(3) 1 d PD A 1
H83A H -1.2802 0.3953 -0.6301 0.036 Uiso 0.693(3) 1 calc PR A 1
H83B H -1.2457 0.3842 -0.5371 0.036 Uiso 0.693(3) 1 calc PR A 1
C84 C -1.1640(6) 0.3194(3) -0.5949(4) 0.0301(6) Uani 0.693(3) 1 d PD A 1
H84A H -1.2295 0.2914 -0.5841 0.036 Uiso 0.693(3) 1 calc PR A 1
H84B H -1.1592 0.3139 -0.6491 0.036 Uiso 0.693(3) 1 calc PR A 1
O4 O -1.0241(5) 0.31255(19) -0.5376(3) 0.0301(6) Uani 0.693(3) 1 d PD A 1
C81A C -0.9622(19) 0.3680(7) -0.5333(9) 0.0301(6) Uani 0.307(3) 1 d PD A 2
H81A H -0.8868 0.3575 -0.5568 0.036 Uiso 0.307(3) 1 calc PR A 2
C82A C -1.0129(14) 0.4261(6) -0.5601(9) 0.0301(6) Uani 0.307(3) 1 d PD A 2
H82C H -0.9476 0.4453 -0.5840 0.036 Uiso 0.307(3) 1 calc PR A 2
H82D H -1.0211 0.4492 -0.5152 0.036 Uiso 0.307(3) 1 calc PR A 2
C83A C -1.1500(13) 0.4202(5) -0.6188(8) 0.0301(6) Uani 0.307(3) 1 d PD A 2
H83C H -1.1410 0.4165 -0.6725 0.036 Uiso 0.307(3) 1 calc PR A 2
H83D H -1.2104 0.4530 -0.6167 0.036 Uiso 0.307(3) 1 calc PR A 2
C84A C -1.2043(14) 0.3647(5) -0.5918(11) 0.0301(6) Uani 0.307(3) 1 d PD A 2
H84C H -1.2706 0.3457 -0.6364 0.036 Uiso 0.307(3) 1 calc PR A 2
H84D H -1.2509 0.3728 -0.5510 0.036 Uiso 0.307(3) 1 calc PR A 2
O4A O -1.0752(11) 0.3262(4) -0.5583(7) 0.0301(6) Uani 0.307(3) 1 d PD A 2
O3 O -0.7604(4) 0.30708(14) -0.31279(19) 0.0372(8) Uani 1 1 d . A .
P2 P -0.89137(11) 0.37474(5) -0.42772(6) 0.0217(2) Uani 1 1 d D . .
Cl1A Cl -0.0196(2) 0.3741(3) 0.2455(5) 0.0539(10) Uani 0.693(3) 1 d PD A 1
Cl1B Cl -0.0137(9) 0.3608(14) 0.2569(19) 0.0539(10) Uani 0.193(6) 1 d PD A 2
Cl1C Cl -0.0230(5) 0.3579(8) 0.2054(11) 0.0539(10) Uani 0.114(5) 1 d PD A 3
Cl2 Cl 0.26752(12) 0.28909(5) 0.20479(6) 0.0314(3) Uani 1 1 d . A .
Cl3 Cl 0.32503(12) 0.37486(5) 0.38395(6) 0.0327(3) Uani 1 1 d . A .
Cl4 Cl 0.26238(11) 0.44933(5) 0.19691(6) 0.0296(3) Uani 1 1 d . A .
Ni1 Ni 0.20631(5) 0.37026(2) 0.25511(3) 0.02505(15) Uani 1 1 d 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
C11 C12 1.391(6) . ?
C11 C16 1.391(6) . ?
C11 P1 1.794(4) . ?
C12 C13 1.372(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.393(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.391(6) . ?
C21 C26 1.400(6) . ?
C21 P1 1.784(5) . ?
C22 C23 1.385(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.369(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.366(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 O1A 1.438(10) . ?
C31 C32 1.487(8) . ?
C31 O1 1.528(6) . ?
C31 C32A 1.536(12) . ?
C31 P1 1.812(4) . ?
C31 H31 1.0000 . ?
C31 H31A 1.0000 . ?
C32 C33 1.566(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.509(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 O1 1.497(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C32A C33A 1.503(13) . ?
C32A H32C 0.9900 . ?
C32A H32D 0.9900 . ?
C33A C34A 1.520(15) . ?
C33A H33C 0.9900 . ?
C33A H33D 0.9900 . ?
C34A O1A 1.549(12) . ?
C34A H34C 0.9900 . ?
C34A H34D 0.9900 . ?
C41 O2 1.434(5) . ?
C41 C42A 1.505(12) . ?
C41 C42 1.509(8) . ?
C41 P1 1.829(5) . ?
C41 H41 1.0000 . ?
C41 H41A 1.0000 . ?
O2 C44A 1.443(14) . ?
O2 C44 1.463(8) . ?
C42 C43 1.468(11) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.517(10) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C42A C43A 1.512(15) . ?
C42A H42C 0.9900 . ?
C42A H42D 0.9900 . ?
C43A C44A 1.61(3) . ?
C43A H43C 0.9900 . ?
C43A H43D 0.9900 . ?
C44A H44C 0.9900 . ?
C44A H44D 0.9900 . ?
C51 C56 1.389(6) . ?
C51 C52 1.393(6) . ?
C51 P2 1.788(4) . ?
C52 C53 1.388(6) . ?
C52 H52 0.9500 . ?
C53 C54 1.377(7) . ?
C53 H53 0.9500 . ?
C54 C55 1.383(7) . ?
C54 H54 0.9500 . ?
C55 C56 1.382(6) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C61 C62 1.395(6) . ?
C61 C66 1.397(6) . ?
C61 P2 1.784(4) . ?
C62 C63 1.377(7) . ?
C62 H62 0.9500 . ?
C63 C64 1.384(7) . ?
C63 H63 0.9500 . ?
C64 C65 1.384(7) . ?
C64 H64 0.9500 . ?
C65 C66 1.377(6) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C71 O3 1.419(5) . ?
C71 C72 1.520(6) . ?
C71 P2 1.831(4) . ?
C71 H71 1.0000 . ?
C72 C73A 1.473(17) . ?
C72 C73 1.509(9) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C72 H72C 0.9900 . ?
C72 H72D 0.9900 . ?
C73 C74 1.497(9) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C73A C74 1.662(18) . ?
C73A H73C 0.9900 . ?
C73A H73D 0.9900 . ?
C74 O3 1.446(6) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 H74C 0.9900 . ?
C74 H74D 0.9900 . ?
C81 O4 1.474(8) . ?
C81 C82 1.489(9) . ?
C81 P2 1.832(8) . ?
C81 H81 1.0000 . ?
C82 C83 1.551(9) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 C84 1.554(8) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 O4 1.504(7) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C81A O4A 1.477(13) . ?
C81A C82A 1.485(14) . ?
C81A P2 1.822(15) . ?
C81A H81A 1.0000 . ?
C82A C83A 1.490(13) . ?
C82A H82C 0.9900 . ?
C82A H82D 0.9900 . ?
C83A C84A 1.542(16) . ?
C83A H83C 0.9900 . ?
C83A H83D 0.9900 . ?
C84A O4A 1.562(13) . ?
C84A H84C 0.9900 . ?
C84A H84D 0.9900 . ?
Cl1A Ni1 2.2466(19) . ?
Cl1B Ni1 2.249(4) . ?
Cl1C Ni1 2.258(5) . ?
Cl2 Ni1 2.2643(12) . ?
Cl3 Ni1 2.2745(12) . ?
Cl4 Ni1 2.2737(12) . ?

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
C12 C11 C16 119.9(4) . . ?
C12 C11 P1 120.8(3) . . ?
C16 C11 P1 119.2(3) . . ?
C13 C12 C11 119.5(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 121.0(4) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C15 120.1(4) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 119.1(4) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C11 120.4(4) . . ?
C15 C16 H16 119.8 . . ?
C11 C16 H16 119.8 . . ?
C22 C21 C26 120.3(4) . . ?
C22 C21 P1 118.9(3) . . ?
C26 C21 P1 120.6(4) . . ?
C23 C22 C21 119.6(4) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C24 C23 C22 120.4(5) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 119.9(5) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 121.9(5) . . ?
C24 C25 H25 119.0 . . ?
C26 C25 H25 119.0 . . ?
C25 C26 C21 117.9(5) . . ?
C25 C26 H26 121.0 . . ?
C21 C26 H26 121.0 . . ?
O1A C31 C32 94.3(5) . . ?
O1A C31 O1 21.5(4) . . ?
C32 C31 O1 109.7(4) . . ?
O1A C31 C32A 105.3(7) . . ?
C32 C31 C32A 11.7(6) . . ?
O1 C31 C32A 119.0(7) . . ?
O1A C31 P1 121.7(5) . . ?
C32 C31 P1 116.4(4) . . ?
O1 C31 P1 100.7(3) . . ?
C32A C31 P1 106.2(7) . . ?
O1A C31 H31 103.1 . . ?
C32 C31 H31 109.9 . . ?
O1 C31 H31 109.9 . . ?
C32A C31 H31 110.4 . . ?
P1 C31 H31 109.9 . . ?
O1A C31 H31A 107.6 . . ?
C32 C31 H31A 108.0 . . ?
O1 C31 H31A 114.6 . . ?
C32A C31 H31A 107.6 . . ?
P1 C31 H31A 107.6 . . ?
H31 C31 H31A 4.7 . . ?
C31 C32 C33 97.7(5) . . ?
C31 C32 H32A 112.2 . . ?
C33 C32 H32A 112.2 . . ?
C31 C32 H32B 112.2 . . ?
C33 C32 H32B 112.2 . . ?
H32A C32 H32B 109.8 . . ?
C34 C33 C32 102.7(5) . . ?
C34 C33 H33A 111.2 . . ?
C32 C33 H33A 111.2 . . ?
C34 C33 H33B 111.2 . . ?
C32 C33 H33B 111.2 . . ?
H33A C33 H33B 109.1 . . ?
O1 C34 C33 105.8(5) . . ?
O1 C34 H34A 110.6 . . ?
C33 C34 H34A 110.6 . . ?
O1 C34 H34B 110.6 . . ?
C33 C34 H34B 110.6 . . ?
H34A C34 H34B 108.7 . . ?
C34 O1 C31 103.5(4) . . ?
C33A C32A C31 108.3(9) . . ?
C33A C32A H32C 110.0 . . ?
C31 C32A H32C 110.0 . . ?
C33A C32A H32D 110.0 . . ?
C31 C32A H32D 110.0 . . ?
H32C C32A H32D 108.4 . . ?
C32A C33A C34A 103.4(9) . . ?
C32A C33A H33C 111.1 . . ?
C34A C33A H33C 111.1 . . ?
C32A C33A H33D 111.1 . . ?
C34A C33A H33D 111.1 . . ?
H33C C33A H33D 109.1 . . ?
C33A C34A O1A 104.0(8) . . ?
C33A C34A H34C 111.0 . . ?
O1A C34A H34C 111.0 . . ?
C33A C34A H34D 111.0 . . ?
O1A C34A H34D 111.0 . . ?
H34C C34A H34D 109.0 . . ?
C31 O1A C34A 103.5(8) . . ?
O2 C41 C42A 107.9(5) . . ?
O2 C41 C42 107.8(4) . . ?
C42A C41 C42 0.1(10) . . ?
O2 C41 P1 107.6(3) . . ?
C42A C41 P1 114.5(9) . . ?
C42 C41 P1 114.6(5) . . ?
O2 C41 H41 108.9 . . ?
C42A C41 H41 108.9 . . ?
C42 C41 H41 108.9 . . ?
P1 C41 H41 108.9 . . ?
O2 C41 H41A 108.9 . . ?
C42A C41 H41A 108.9 . . ?
C42 C41 H41A 108.9 . . ?
P1 C41 H41A 108.9 . . ?
H41 C41 H41A 0.0 . . ?
C41 O2 C44A 114.0(11) . . ?
C41 O2 C44 106.0(5) . . ?
C44A O2 C44 13.0(12) . . ?
C43 C42 C41 104.1(6) . . ?
C43 C42 H42A 110.9 . . ?
C41 C42 H42A 110.9 . . ?
C43 C42 H42B 110.9 . . ?
C41 C42 H42B 110.9 . . ?
H42A C42 H42B 109.0 . . ?
C42 C43 C44 100.9(7) . . ?
C42 C43 H43A 111.6 . . ?
C44 C43 H43A 111.6 . . ?
C42 C43 H43B 111.6 . . ?
C44 C43 H43B 111.6 . . ?
H43A C43 H43B 109.4 . . ?
O2 C44 C43 107.1(6) . . ?
O2 C44 H44A 110.3 . . ?
C43 C44 H44A 110.3 . . ?
O2 C44 H44B 110.3 . . ?
C43 C44 H44B 110.3 . . ?
H44A C44 H44B 108.5 . . ?
C41 C42A C43A 103.9(9) . . ?
C41 C42A H42C 111.0 . . ?
C43A C42A H42C 111.0 . . ?
C41 C42A H42D 111.0 . . ?
C43A C42A H42D 111.0 . . ?
H42C C42A H42D 109.0 . . ?
C42A C43A C44A 105.9(10) . . ?
C42A C43A H43C 110.5 . . ?
C44A C43A H43C 110.5 . . ?
C42A C43A H43D 110.5 . . ?
C44A C43A H43D 110.5 . . ?
H43C C43A H43D 108.7 . . ?
O2 C44A C43A 101.5(16) . . ?
O2 C44A H44C 111.5 . . ?
C43A C44A H44C 111.5 . . ?
O2 C44A H44D 111.5 . . ?
C43A C44A H44D 111.5 . . ?
H44C C44A H44D 109.3 . . ?
C21 P1 C11 110.5(2) . . ?
C21 P1 C31 110.5(2) . . ?
C11 P1 C31 109.88(19) . . ?
C21 P1 C41 109.0(2) . . ?
C11 P1 C41 109.9(2) . . ?
C31 P1 C41 107.0(2) . . ?
C56 C51 C52 119.4(4) . . ?
C56 C51 P2 121.2(3) . . ?
C52 C51 P2 119.3(3) . . ?
C53 C52 C51 120.9(4) . . ?
C53 C52 H52 119.6 . . ?
C51 C52 H52 119.6 . . ?
C54 C53 C52 118.8(4) . . ?
C54 C53 H53 120.6 . . ?
C52 C53 H53 120.6 . . ?
C53 C54 C55 121.0(4) . . ?
C53 C54 H54 119.5 . . ?
C55 C54 H54 119.5 . . ?
C56 C55 C54 120.2(4) . . ?
C56 C55 H55 119.9 . . ?
C54 C55 H55 119.9 . . ?
C55 C56 C51 119.8(4) . . ?
C55 C56 H56 120.1 . . ?
C51 C56 H56 120.1 . . ?
C62 C61 C66 119.9(4) . . ?
C62 C61 P2 119.2(3) . . ?
C66 C61 P2 121.0(3) . . ?
C63 C62 C61 119.8(4) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C62 C63 C64 120.6(5) . . ?
C62 C63 H63 119.7 . . ?
C64 C63 H63 119.7 . . ?
C65 C64 C63 119.4(4) . . ?
C65 C64 H64 120.3 . . ?
C63 C64 H64 120.3 . . ?
C66 C65 C64 121.0(5) . . ?
C66 C65 H65 119.5 . . ?
C64 C65 H65 119.5 . . ?
C65 C66 C61 119.3(4) . . ?
C65 C66 H66 120.3 . . ?
C61 C66 H66 120.3 . . ?
O3 C71 C72 107.8(4) . . ?
O3 C71 P2 107.7(3) . . ?
C72 C71 P2 114.4(3) . . ?
O3 C71 H71 108.9 . . ?
C72 C71 H71 108.9 . . ?
P2 C71 H71 108.9 . . ?
C73A C72 C73 48.4(7) . . ?
C73A C72 C71 104.7(7) . . ?
C73 C72 C71 102.6(4) . . ?
C73A C72 H72A 65.7 . . ?
C73 C72 H72A 111.2 . . ?
C71 C72 H72A 111.2 . . ?
C73A C72 H72B 142.5 . . ?
C73 C72 H72B 111.2 . . ?
C71 C72 H72B 111.2 . . ?
H72A C72 H72B 109.2 . . ?
C73A C72 H72C 110.8 . . ?
C73 C72 H72C 145.0 . . ?
C71 C72 H72C 110.8 . . ?
H72A C72 H72C 46.8 . . ?
H72B C72 H72C 66.2 . . ?
C73A C72 H72D 110.8 . . ?
C73 C72 H72D 66.7 . . ?
C71 C72 H72D 110.8 . . ?
H72A C72 H72D 137.1 . . ?
H72B C72 H72D 45.9 . . ?
H72C C72 H72D 108.9 . . ?
C74 C73 C72 102.8(5) . . ?
C74 C73 H73A 111.2 . . ?
C72 C73 H73A 111.2 . . ?
C74 C73 H73B 111.2 . . ?
C72 C73 H73B 111.2 . . ?
H73A C73 H73B 109.1 . . ?
C72 C73A C74 96.9(9) . . ?
C72 C73A H73C 112.4 . . ?
C74 C73A H73C 112.4 . . ?
C72 C73A H73D 112.4 . . ?
C74 C73A H73D 112.4 . . ?
H73C C73A H73D 109.9 . . ?
O3 C74 C73 105.4(4) . . ?
O3 C74 C73A 103.0(6) . . ?
C73 C74 C73A 45.2(7) . . ?
O3 C74 H74A 110.7 . . ?
C73 C74 H74A 110.7 . . ?
C73A C74 H74A 69.8 . . ?
O3 C74 H74B 110.7 . . ?
C73 C74 H74B 110.7 . . ?
C73A C74 H74B 143.8 . . ?
H74A C74 H74B 108.8 . . ?
O3 C74 H74C 111.2 . . ?
C73 C74 H74C 140.9 . . ?
C73A C74 H74C 111.2 . . ?
H74A C74 H74C 42.9 . . ?
H74B C74 H74C 68.9 . . ?
O3 C74 H74D 111.2 . . ?
C73 C74 H74D 68.5 . . ?
C73A C74 H74D 111.2 . . ?
H74A C74 H74D 136.5 . . ?
H74B C74 H74D 43.9 . . ?
H74C C74 H74D 109.1 . . ?
O4 C81 C82 111.8(6) . . ?
O4 C81 P2 98.0(5) . . ?
C82 C81 P2 116.3(7) . . ?
O4 C81 H81 110.1 . . ?
C82 C81 H81 110.1 . . ?
P2 C81 H81 110.1 . . ?
C81 C82 C83 104.3(6) . . ?
C81 C82 H82A 110.9 . . ?
C83 C82 H82A 110.9 . . ?
C81 C82 H82B 110.9 . . ?
C83 C82 H82B 110.9 . . ?
H82A C82 H82B 108.9 . . ?
C82 C83 C84 100.6(5) . . ?
C82 C83 H83A 111.6 . . ?
C84 C83 H83A 111.6 . . ?
C82 C83 H83B 111.6 . . ?
C84 C83 H83B 111.6 . . ?
H83A C83 H83B 109.4 . . ?
O4 C84 C83 105.6(5) . . ?
O4 C84 H84A 110.6 . . ?
C83 C84 H84A 110.6 . . ?
O4 C84 H84B 110.6 . . ?
C83 C84 H84B 110.6 . . ?
H84A C84 H84B 108.7 . . ?
C81 O4 C84 103.0(5) . . ?
O4A C81A C82A 110.1(12) . . ?
O4A C81A P2 114.5(12) . . ?
C82A C81A P2 104.6(11) . . ?
O4A C81A H81A 109.1 . . ?
C82A C81A H81A 109.1 . . ?
P2 C81A H81A 109.1 . . ?
C81A C82A C83A 108.1(10) . . ?
C81A C82A H82C 110.1 . . ?
C83A C82A H82C 110.1 . . ?
C81A C82A H82D 110.1 . . ?
C83A C82A H82D 110.1 . . ?
H82C C82A H82D 108.4 . . ?
C82A C83A C84A 101.7(10) . . ?
C82A C83A H83C 111.4 . . ?
C84A C83A H83C 111.4 . . ?
C82A C83A H83D 111.4 . . ?
C84A C83A H83D 111.4 . . ?
H83C C83A H83D 109.3 . . ?
C83A C84A O4A 105.8(9) . . ?
C83A C84A H84C 110.6 . . ?
O4A C84A H84C 110.6 . . ?
C83A C84A H84D 110.6 . . ?
O4A C84A H84D 110.6 . . ?
H84C C84A H84D 108.7 . . ?
C81A O4A C84A 103.0(10) . . ?
C71 O3 C74 108.7(3) . . ?
C61 P2 C51 110.0(2) . . ?
C61 P2 C81A 112.1(6) . . ?
C51 P2 C81A 109.6(7) . . ?
C61 P2 C71 109.7(2) . . ?
C51 P2 C71 110.4(2) . . ?
C81A P2 C71 104.9(6) . . ?
C61 P2 C81 111.3(3) . . ?
C51 P2 C81 108.6(4) . . ?
C81A P2 C81 1.8(8) . . ?
C71 P2 C81 106.7(3) . . ?
Cl1A Ni1 Cl1B 9.4(6) . . ?
Cl1A Ni1 Cl1C 20.5(5) . . ?
Cl1B Ni1 Cl1C 23.0(11) . . ?
Cl1A Ni1 Cl2 112.9(3) . . ?
Cl1B Ni1 Cl2 107.8(10) . . ?
Cl1C Ni1 Cl2 95.9(5) . . ?
Cl1A Ni1 Cl4 108.17(13) . . ?
Cl1B Ni1 Cl4 117.6(5) . . ?
Cl1C Ni1 Cl4 106.7(4) . . ?
Cl2 Ni1 Cl4 111.97(4) . . ?
Cl1A Ni1 Cl3 108.2(2) . . ?
Cl1B Ni1 Cl3 103.6(9) . . ?
Cl1C Ni1 Cl3 126.5(5) . . ?
Cl2 Ni1 Cl3 108.29(5) . . ?
Cl4 Ni1 Cl3 107.03(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.080
_database_code_depnum_ccdc_archive 'CCDC 992221'
