# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_miller041_b
_database_code_depnum_ccdc_archive 'CCDC 1448783'
_audit_update_record             
;
2016-01-21 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;
_audit_creation_date             2014-10-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        Ni(dmpbz)2(BF4)2
_chemical_formula_moiety         'C20 H32 Ni P4, 2(B F4)'
_chemical_formula_sum            'C20 H32 B2 F8 Ni P4'
_chemical_formula_weight         628.66
_chemical_melting_point          ?
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
'x-1/2, y-1/2, -z-1/2'

_cell_length_a                   16.0457(14)
_cell_length_b                   9.2602(8)
_cell_length_c                   17.5605(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2609.3(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2670
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0578 before and 0.0474 after correction.
The Ratio of minimum to maximum transmission is 0.7837.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19719
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         2.320
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1731
_reflns_number_total             2971
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         2971
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0548
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0650P)²+5.6613P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1561
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C5A)
Uanis(C6) = Uanis(C6A)
Uanis(C7) = Uanis(C7A)
Uanis(C8) = Uanis(C8A)
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
3. Others
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(P2A)=Sof(C10A)=Sof(C9A)=Sof(H9A)=Sof(C8A)=Sof(H8A)=Sof(C7A)=Sof(H7A)=
 Sof(C6A)=Sof(H6A)=Sof(C5A)=1-FVAR(1)
 Sof(P2)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=
 Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=
 Sof(C10)=FVAR(1)
 Sof(F7A)=Sof(F3A)=Sof(F2A)=1-FVAR(2)
 Sof(F2)=Sof(F3)=Sof(F7)=FVAR(2)
 Sof(F1A)=1-FVAR(3)
 Sof(F1)=FVAR(3)
4.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C9A(H9A), C8A(H8A), C7A(H7A), C6A(H6A)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C2A(H2AA,
 H2AB,H2AC), C1A(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.5000 0.5000 0.0292(2) Uani 1 2 d S T P A .
P1 P 0.60700(8) 0.49325(14) 0.42253(7) 0.0385(3) Uani 1 1 d . . . . .
P2 P 0.4507(3) 0.3042(5) 0.4486(2) 0.0270(7) Uani 0.635(7) 1 d . . . A 1
C1 C 0.3702(6) 0.3380(13) 0.3790(5) 0.054(3) Uani 0.635(7) 1 d . . . A 1
H1A H 0.3237 0.3889 0.4032 0.081 Uiso 0.635(7) 1 calc GR . . A 1
H1B H 0.3504 0.2459 0.3582 0.081 Uiso 0.635(7) 1 calc GR . . A 1
H1C H 0.3928 0.3974 0.3377 0.081 Uiso 0.635(7) 1 calc GR . . A 1
C2 C 0.4136(7) 0.1563(10) 0.5055(6) 0.051(3) Uani 0.635(7) 1 d . . . A 1
H2A H 0.4550 0.1331 0.5447 0.076 Uiso 0.635(7) 1 calc GR . . A 1
H2B H 0.4047 0.0717 0.4730 0.076 Uiso 0.635(7) 1 calc GR . . A 1
H2C H 0.3610 0.1834 0.5299 0.076 Uiso 0.635(7) 1 calc GR . . A 1
C3 C 0.7116(3) 0.5137(6) 0.4603(3) 0.0499(13) Uani 1 1 d . . . . .
H3A H 0.7191 0.6126 0.4789 0.075 Uiso 1 1 calc GR . . . .
H3B H 0.7523 0.4939 0.4200 0.075 Uiso 1 1 calc GR . . . .
H3C H 0.7199 0.4456 0.5023 0.075 Uiso 1 1 calc GR . . . .
C4 C 0.5996(4) 0.6211(6) 0.3437(3) 0.0642(18) Uani 1 1 d . . . . .
H4A H 0.5463 0.6078 0.3173 0.096 Uiso 1 1 calc GR . . . .
H4B H 0.6455 0.6041 0.3079 0.096 Uiso 1 1 calc GR . . . .
H4C H 0.6031 0.7199 0.3634 0.096 Uiso 1 1 calc GR . . . .
C5 C 0.6013(6) 0.3138(14) 0.3790(7) 0.0252(19) Uani 0.635(7) 1 d . . . A 1
C6 C 0.6648(6) 0.2644(11) 0.3268(6) 0.0345(18) Uani 0.635(7) 1 d . . . A 1
H6 H 0.7119 0.3234 0.3165 0.041 Uiso 0.635(7) 1 calc R . . A 1
C7 C 0.6571(7) 0.1337(14) 0.2925(5) 0.040(3) Uani 0.635(7) 1 d . . . A 1
H7 H 0.6997 0.1027 0.2587 0.048 Uiso 0.635(7) 1 calc R . . A 1
C8 C 0.5895(7) 0.0440(12) 0.3050(5) 0.037(2) Uani 0.635(7) 1 d . . . A 1
H8 H 0.5852 -0.0467 0.2801 0.044 Uiso 0.635(7) 1 calc R . . A 1
C9 C 0.5277(7) 0.0912(14) 0.3555(6) 0.036(2) Uani 0.635(7) 1 d . . . A 1
H9 H 0.4817 0.0300 0.3663 0.043 Uiso 0.635(7) 1 calc R . . A 1
C10 C 0.5324(6) 0.2244(12) 0.3898(6) 0.0235(19) Uani 0.635(7) 1 d . . . A 1
C2A C 0.4187(13) 0.160(2) 0.4667(10) 0.051(3) Uani 0.365(7) 1 d . . . A 2
H2AA H 0.4555 0.1181 0.5054 0.076 Uiso 0.365(7) 1 calc GR . . A 2
H2AB H 0.4074 0.0875 0.4272 0.076 Uiso 0.365(7) 1 calc GR . . A 2
H2AC H 0.3662 0.1894 0.4905 0.076 Uiso 0.365(7) 1 calc GR . . A 2
C1A C 0.3986(10) 0.374(3) 0.3482(10) 0.054(3) Uani 0.365(7) 1 d . . . A 2
H1AA H 0.3488 0.4182 0.3703 0.081 Uiso 0.365(7) 1 calc GR . . A 2
H1AB H 0.3823 0.2907 0.3170 0.081 Uiso 0.365(7) 1 calc GR . . A 2
H1AC H 0.4278 0.4445 0.3165 0.081 Uiso 0.365(7) 1 calc GR . . A 2
P2A P 0.4678(4) 0.3130(8) 0.4248(4) 0.0248(13) Uani 0.365(7) 1 d . . . A 2
C10A C 0.5585(13) 0.247(3) 0.3780(12) 0.0235(19) Uani 0.365(7) 1 d . . . A 2
C9A C 0.5562(14) 0.112(3) 0.3382(13) 0.036(2) Uani 0.365(7) 1 d . . . A 2
H9A H 0.5083 0.0521 0.3389 0.043 Uiso 0.365(7) 1 calc R . . A 2
C8A C 0.6262(14) 0.075(3) 0.2991(12) 0.037(2) Uani 0.365(7) 1 d . . . A 2
H8A H 0.6269 -0.0186 0.2768 0.044 Uiso 0.365(7) 1 calc R . . A 2
C7A C 0.6954(11) 0.158(2) 0.2890(11) 0.040(3) Uani 0.365(7) 1 d . . . A 2
H7A H 0.7407 0.1282 0.2580 0.048 Uiso 0.365(7) 1 calc R . . A 2
C6A C 0.6952(10) 0.299(2) 0.3299(11) 0.0345(18) Uani 0.365(7) 1 d . . . A 2
H6A H 0.7416 0.3629 0.3284 0.041 Uiso 0.365(7) 1 calc R . . A 2
C5A C 0.6280(13) 0.330(3) 0.3676(14) 0.0252(19) Uani 0.365(7) 1 d . . . A 2
F1 F 0.1641(3) 0.4277(4) 0.3657(3) 0.0597(16) Uani 0.716(7) 1 d . . . B 1
F2 F 0.1881(4) 0.2178(9) 0.3243(4) 0.094(3) Uani 0.598(8) 1 d . . . B 1
F3 F 0.1634(6) 0.2817(7) 0.4425(3) 0.087(3) Uani 0.598(8) 1 d . . . B 1
B4 B 0.1404(4) 0.2761(7) 0.3744(3) 0.0430(14) Uani 1 1 d . . . . .
F7 F 0.0646(5) 0.3177(13) 0.3465(8) 0.163(5) Uani 0.598(8) 1 d . . . B 1
F7A F 0.0941(5) 0.2519(9) 0.4370(4) 0.046(2) Uani 0.402(8) 1 d . . . B 2
F3A F 0.2228(5) 0.2107(8) 0.3971(5) 0.055(3) Uani 0.402(8) 1 d . . . B 2
F2A F 0.1179(7) 0.2268(10) 0.3130(4) 0.068(4) Uani 0.402(8) 1 d . . . B 2
F1A F 0.0927(7) 0.1213(12) 0.3812(7) 0.060(4) Uani 0.284(7) 1 d . . . B 2


_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 P1 2.1915(14) 5_666 ?
Ni1 P1 2.1915(14) . ?
Ni1 P2 2.174(5) 5_666 ?
Ni1 P2 2.174(5) . ?
Ni1 P2A 2.238(7) . ?
Ni1 P2A 2.238(7) 5_666 ?
P1 C3 1.814(5) . ?
P1 C4 1.825(5) . ?
P1 C5 1.832(14) . ?
P1 C5A 1.83(3) . ?
P2 C1 1.807(10) . ?
P2 C2 1.796(10) . ?
P2 C10 1.825(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.445(13) . ?
C5 C10 1.393(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.358(17) . ?
C7 H7 0.9500 . ?
C7 C8 1.383(13) . ?
C8 H8 0.9500 . ?
C8 C9 1.400(15) . ?
C9 H9 0.9500 . ?
C9 C10 1.375(17) . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2A P2A 1.782(17) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C1A P2A 1.83(2) . ?
P2A C10A 1.78(2) . ?
C10A C9A 1.43(4) . ?
C10A C5A 1.367(18) . ?
C9A H9A 0.9500 . ?
C9A C8A 1.36(3) . ?
C8A H8A 0.9500 . ?
C8A C7A 1.36(2) . ?
C7A H7A 0.9500 . ?
C7A C6A 1.49(3) . ?
C6A H6A 0.9500 . ?
C6A C5A 1.30(2) . ?
F1 B4 1.462(7) . ?
F2 B4 1.285(8) . ?
F3 B4 1.253(8) . ?
B4 F7 1.367(9) . ?
B4 F7A 1.345(9) . ?
B4 F3A 1.508(9) . ?
B4 F2A 1.225(9) . ?
B4 F1A 1.630(12) . ?
F7A F1A 1.557(14) . ?
F2A F1A 1.598(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Ni1 P1 180.0 . 5_666 ?
P1 Ni1 P2A 101.99(18) 5_666 . ?
P1 Ni1 P2A 101.99(18) . 5_666 ?
P1 Ni1 P2A 78.01(18) . . ?
P1 Ni1 P2A 78.01(18) 5_666 5_666 ?
P2 Ni1 P1 90.22(10) . . ?
P2 Ni1 P1 89.78(10) . 5_666 ?
P2 Ni1 P1 90.22(10) 5_666 5_666 ?
P2 Ni1 P1 89.78(10) 5_666 . ?
P2 Ni1 P2 180.0 . 5_666 ?
P2A Ni1 P2A 180.0(3) 5_666 . ?
C3 P1 Ni1 119.67(19) . . ?
C3 P1 C4 105.6(3) . . ?
C3 P1 C5 107.1(4) . . ?
C3 P1 C5A 96.2(8) . . ?
C4 P1 Ni1 113.7(2) . . ?
C4 P1 C5 105.6(4) . . ?
C5 P1 Ni1 104.2(3) . . ?
C5A P1 Ni1 119.8(5) . . ?
C5A P1 C4 98.5(7) . . ?
C1 P2 Ni1 113.4(4) . . ?
C1 P2 C10 101.6(5) . . ?
C2 P2 Ni1 121.7(3) . . ?
C2 P2 C1 105.8(5) . . ?
C2 P2 C10 104.1(5) . . ?
C10 P2 Ni1 108.1(3) . . ?
P2 C1 H1A 109.5 . . ?
P2 C1 H1B 109.5 . . ?
P2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
P2 C2 H2A 109.5 . . ?
P2 C2 H2B 109.5 . . ?
P2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
P1 C3 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
P1 C4 H4A 109.5 . . ?
P1 C4 H4B 109.5 . . ?
P1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 P1 121.1(6) . . ?
C10 C5 P1 121.4(8) . . ?
C10 C5 C6 117.3(11) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 119.9(8) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 118.8 . . ?
C6 C7 C8 122.4(9) . . ?
C8 C7 H7 118.8 . . ?
C7 C8 H8 121.0 . . ?
C7 C8 C9 117.9(10) . . ?
C9 C8 H8 121.0 . . ?
C8 C9 H9 119.4 . . ?
C10 C9 C8 121.2(8) . . ?
C10 C9 H9 119.4 . . ?
C5 C10 P2 114.0(9) . . ?
C9 C10 P2 124.9(6) . . ?
C9 C10 C5 121.1(9) . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
P2A C2A H2AA 109.5 . . ?
P2A C2A H2AB 109.5 . . ?
P2A C2A H2AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
P2A C1A H1AA 109.5 . . ?
P2A C1A H1AB 109.5 . . ?
P2A C1A H1AC 109.5 . . ?
C2A P2A Ni1 118.3(6) . . ?
C2A P2A C1A 106.2(10) . . ?
C1A P2A Ni1 109.6(7) . . ?
C10A P2A Ni1 110.5(8) . . ?
C10A P2A C2A 106.2(10) . . ?
C10A P2A C1A 105.2(9) . . ?
C9A C10A P2A 120.3(14) . . ?
C5A C10A P2A 122.4(19) . . ?
C5A C10A C9A 116(2) . . ?
C10A C9A H9A 121.7 . . ?
C8A C9A C10A 116.6(17) . . ?
C8A C9A H9A 121.7 . . ?
C9A C8A H8A 116.8 . . ?
C9A C8A C7A 126(2) . . ?
C7A C8A H8A 116.8 . . ?
C8A C7A H7A 122.2 . . ?
C8A C7A C6A 115.5(18) . . ?
C6A C7A H7A 122.2 . . ?
C7A C6A H6A 121.9 . . ?
C5A C6A C7A 116.1(17) . . ?
C5A C6A H6A 121.9 . . ?
C10A C5A P1 104.1(15) . . ?
C6A C5A P1 127.3(18) . . ?
C6A C5A C10A 129(3) . . ?
F2 B4 F1 100.2(6) . . ?
F2 B4 F7 113.8(8) . . ?
F3 B4 F1 89.0(6) . . ?
F3 B4 F2 119.7(7) . . ?
F3 B4 F7 126.4(8) . . ?
F7 B4 F1 85.6(6) . . ?
F7A B4 F3A 101.6(6) . . ?
F7A B4 F1A 62.3(6) . . ?
F3A B4 F1A 92.2(6) . . ?
F2A B4 F7A 119.6(8) . . ?
F2A B4 F3A 110.0(8) . . ?
F2A B4 F1A 66.3(7) . . ?
B4 F7A F1A 67.9(6) . . ?
B4 F2A F1A 69.1(6) . . ?
F7A F1A B4 49.9(5) . . ?
F7A F1A F2A 89.6(7) . . ?
F2A F1A B4 44.6(4) . . ?

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
Ni1 P1 C5 C6 -176.5(8) . . . . ?
Ni1 P1 C5 C10 8.8(11) . . . . ?
Ni1 P1 C5A C10A 10(2) . . . . ?
Ni1 P1 C5A C6A -167.3(18) . . . . ?
Ni1 P2 C10 C5 -10.6(10) . . . . ?
Ni1 P2 C10 C9 172.0(10) . . . . ?
Ni1 P2A C10A C9A 168.5(17) . . . . ?
Ni1 P2A C10A C5A -22(2) . . . . ?
P1 C5 C6 C7 -176.9(8) . . . . ?
P1 C5 C10 P2 1.0(14) . . . . ?
P1 C5 C10 C9 178.5(10) . . . . ?
C1 P2 C10 C5 108.9(10) . . . . ?
C1 P2 C10 C9 -68.4(12) . . . . ?
C2 P2 C10 C5 -141.4(9) . . . . ?
C2 P2 C10 C9 41.3(12) . . . . ?
C3 P1 C5 C6 -48.8(10) . . . . ?
C3 P1 C5 C10 136.6(10) . . . . ?
C3 P1 C5A C10A 140.0(17) . . . . ?
C3 P1 C5A C6A -38(2) . . . . ?
C4 P1 C5 C6 63.4(10) . . . . ?
C4 P1 C5 C10 -111.2(10) . . . . ?
C4 P1 C5A C10A -113.1(17) . . . . ?
C4 P1 C5A C6A 69(2) . . . . ?
C5 P1 C5A C10A 5(3) . . . . ?
C5 P1 C5A C6A -173(6) . . . . ?
C5 C6 C7 C8 0.5(14) . . . . ?
C6 C5 C10 P2 -173.8(8) . . . . ?
C6 C5 C10 C9 3.6(18) . . . . ?
C6 C7 C8 C9 -0.5(15) . . . . ?
C7 C8 C9 C10 2.1(17) . . . . ?
C8 C9 C10 P2 173.4(9) . . . . ?
C8 C9 C10 C5 -3.8(19) . . . . ?
C10 C5 C6 C7 -2.0(16) . . . . ?
C2A P2A C10A C9A 39(2) . . . . ?
C2A P2A C10A C5A -152(2) . . . . ?
C1A P2A C10A C9A -73(2) . . . . ?
C1A P2A C10A C5A 96(2) . . . . ?
P2A C10A C9A C8A 175.2(18) . . . . ?
P2A C10A C5A P1 8(3) . . . . ?
P2A C10A C5A C6A -174(2) . . . . ?
C10A C9A C8A C7A -6(4) . . . . ?
C9A C10A C5A P1 177.6(18) . . . . ?
C9A C10A C5A C6A -5(4) . . . . ?
C9A C8A C7A C6A 5(3) . . . . ?
C8A C7A C6A C5A -3(3) . . . . ?
C7A C6A C5A P1 -179.3(16) . . . . ?
C7A C6A C5A C10A 3(4) . . . . ?
C5A P1 C5 C6 -1(4) . . . . ?
C5A P1 C5 C10 -176(5) . . . . ?
C5A C10A C9A C8A 5(3) . . . . ?
F1 B4 F7A F1A 166.6(7) . . . . ?
F1 B4 F2A F1A -166.5(7) . . . . ?
F1 B4 F1A F7A -71(3) . . . . ?
F1 B4 F1A F2A 76(3) . . . . ?
F2 B4 F7A F1A -34.3(13) . . . . ?
F2 B4 F2A F1A 105.2(8) . . . . ?
F2 B4 F1A F7A 161.1(7) . . . . ?
F2 B4 F1A F2A -51.7(7) . . . . ?
F3 B4 F7A F1A -123.8(8) . . . . ?
F3 B4 F2A F1A 27(3) . . . . ?
F3 B4 F1A F7A 41.5(6) . . . . ?
F3 B4 F1A F2A -171.3(9) . . . . ?
B4 F7A F1A F2A -22.4(6) . . . . ?
B4 F2A F1A F7A 24.5(7) . . . . ?
F7 B4 F7A F1A 85.2(8) . . . . ?
F7 B4 F2A F1A -93.3(8) . . . . ?
F7 B4 F1A F7A -84.5(8) . . . . ?
F7 B4 F1A F2A 62.7(8) . . . . ?
F7A B4 F2A F1A -33.5(9) . . . . ?
F7A B4 F1A F2A 147.2(9) . . . . ?
F3A B4 F7A F1A -86.4(7) . . . . ?
F3A B4 F2A F1A 83.5(7) . . . . ?
F3A B4 F1A F7A 101.9(7) . . . . ?
F3A B4 F1A F2A -110.8(8) . . . . ?
F2A B4 F7A F1A 34.8(9) . . . . ?
F2A B4 F1A F7A -147.2(9) . . . . ?

_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_original_sample_id Miller041
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sjc009_0m
_database_code_depnum_ccdc_archive 'CCDC 1468872'
_audit_update_record             
;
2016-03-15 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            Ni(dmpe)2(H)(BF4)
_chemical_name_systematic        
;Nickel(II) bis(dimethylphosphinoethane) hydride tetrafluoroborate
;
_chemical_formula_moiety         'C20 H32 Ni P4, B F4'
_chemical_formula_sum            'C20 H32 B F4 Ni P4'
_chemical_formula_weight         541.85
_chemical_melting_point          ?

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'

_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+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   12.354(3)
_cell_length_b                   19.109(3)
_cell_length_c                   20.927(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4940.2(19)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3411
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.720
_cell_measurement_theta_min      2.888

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_F_000             2248
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.081
_shelx_estimated_absorpt_T_min   0.938
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6989
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0557 before and 0.0461 after correction.
The Ratio of minimum to maximum transmission is 0.9376.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13187
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.191
_diffrn_reflns_theta_max         26.445
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             1258
_reflns_number_gt                977
_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       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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)+(0.0343P)²+7.4839P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         1258
_refine_ls_number_parameters     92
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0743
_refine_ls_wR_factor_gt          0.0687
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.65794(5) 0.1250 0.1250 0.0175(2) Uani 0.5 2 d S T P A 1
P01 P 0.6916(8) 0.1990(5) 0.1817(6) 0.0268(13) Uani 0.5 1 d . . P B 2
F1 F 0.81101(12) 0.33359(7) 0.33713(8) 0.0583(5) Uani 1 1 d . . . . .
C3 C 0.66132(16) 0.28829(10) 0.15029(9) 0.0212(4) Uani 1 1 d . . . . .
C4 C 0.69791(17) 0.35152(11) 0.17539(10) 0.0276(5) Uani 1 1 d . . . . .
H4A H 0.7478 0.3518 0.2099 0.033 Uiso 1 1 calc R U . . .
C5 C 0.66153(19) 0.41379(10) 0.14993(10) 0.0344(5) Uani 1 1 d . . . . .
H5A H 0.6869 0.4569 0.1668 0.041 Uiso 1 1 calc R U . . .
C2 C 0.66347(19) 0.21187(11) 0.26633(10) 0.0298(5) Uani 1 1 d . . . . .
H2D H 0.5850 0.2135 0.2731 0.045 Uiso 0.5 1 calc R U P B 2
H2E H 0.6944 0.1731 0.2909 0.045 Uiso 0.5 1 calc R U P B 2
H2F H 0.6959 0.2560 0.2805 0.045 Uiso 0.5 1 calc R U P B 2
H2A H 0.6873 0.1700 0.2894 0.045 Uiso 0.5 1 calc R U P B 1
H2B H 0.6924 0.2537 0.2874 0.045 Uiso 0.5 1 calc R U P B 1
H2C H 0.5842 0.2139 0.2663 0.045 Uiso 0.5 1 calc R U P B 1
B1 B 0.8750 0.3750 0.3750 0.0232(10) Uani 1 4 d S T P . .
C01 C 0.8358(6) 0.1981(4) 0.1828(4) 0.0339(17) Uani 0.5 1 d . . P B 2
H01A H 0.8623 0.2384 0.2072 0.051 Uiso 0.5 1 calc R U P B 2
H01B H 0.8632 0.2005 0.1390 0.051 Uiso 0.5 1 calc R U P B 2
H01C H 0.8611 0.1548 0.2030 0.051 Uiso 0.5 1 calc R U P B 2
P1 P 0.7130(7) 0.2082(5) 0.1837(5) 0.0198(9) Uani 0.5 1 d . . P A 1
C1 C 0.8595(6) 0.2230(3) 0.1911(4) 0.0231(14) Uani 0.5 1 d . . P A 1
H1C H 0.8905 0.2314 0.1486 0.035 Uiso 0.5 1 calc R U P A 1
H1B H 0.8936 0.1817 0.2102 0.035 Uiso 0.5 1 calc R U P A 1
H1A H 0.8725 0.2639 0.2183 0.035 Uiso 0.5 1 calc R U P A 1


_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 Ni1 0.8139(12) 14_545 ?
Ni1 P1 2.121(9) 8_544 ?
Ni1 P1 2.121(9) . ?
Ni1 P1 2.504(8) 14_545 ?
Ni1 P1 2.504(8) 11_554 ?
P01 C01 1.781(12) . ?
P01 C2 1.821(12) . ?
P01 C3 1.867(12) . ?
F1 B1 1.3709(13) . ?
C3 C3 1.388(4) 11_554 ?
C3 C4 1.393(3) . ?
C3 P1 1.799(11) . ?
C4 C5 1.379(3) . ?
C4 H4A 0.9500 . ?
C5 C5 1.380(5) 11_554 ?
C5 H5A 0.9500 . ?
C2 P1 1.836(11) . ?
C2 H2D 0.9800 . ?
C2 H2E 0.9800 . ?
C2 H2F 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
B1 F1 1.3710(13) 4 ?
B1 F1 1.3710(13) 3_655 ?
B1 F1 1.3710(13) 2_655 ?
C01 H01A 0.9800 . ?
C01 H01B 0.9800 . ?
C01 H01C 0.9800 . ?
P1 C1 1.838(11) . ?
P1 Ni1 2.504(8) 14_545 ?
C1 H1C 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1A 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ni1 Ni1 P1 108.7(3) 14_545 8_544 ?
Ni1 Ni1 P1 108.7(3) 14_545 . ?
P1 Ni1 P1 142.6(6) 8_544 . ?
Ni1 Ni1 P1 53.4(2) 14_545 14_545 ?
P1 Ni1 P1 89.9(6) 8_544 14_545 ?
P1 Ni1 P1 112.6(5) . 14_545 ?
Ni1 Ni1 P1 53.4(2) 14_545 11_554 ?
P1 Ni1 P1 112.6(5) 8_544 11_554 ?
P1 Ni1 P1 89.9(6) . 11_554 ?
P1 Ni1 P1 106.7(5) 14_545 11_554 ?
C01 P01 C2 100.3(6) . . ?
C01 P01 C3 102.3(5) . . ?
C2 P01 C3 100.4(5) . . ?
C3 C3 C4 119.83(12) 11_554 . ?
C3 C3 P1 121.7(3) 11_554 . ?
C4 C3 P1 118.4(3) . . ?
C3 C3 P01 113.5(3) 11_554 . ?
C4 C3 P01 126.5(3) . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
C4 C5 C5 120.36(13) . 11_554 ?
C4 C5 H5A 119.8 . . ?
C5 C5 H5A 119.8 11_554 . ?
P01 C2 H2D 109.5 . . ?
P01 C2 H2E 109.5 . . ?
H2D C2 H2E 109.5 . . ?
P01 C2 H2F 109.5 . . ?
H2D C2 H2F 109.5 . . ?
H2E C2 H2F 109.5 . . ?
P1 C2 H2A 109.5 . . ?
P1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
P1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
F1 B1 F1 109.57(14) . 4 ?
F1 B1 F1 109.49(12) . 3_655 ?
F1 B1 F1 109.36(14) 4 3_655 ?
F1 B1 F1 109.36(14) . 2_655 ?
F1 B1 F1 109.48(12) 4 2_655 ?
F1 B1 F1 109.57(14) 3_655 2_655 ?
P01 C01 H01A 109.5 . . ?
P01 C01 H01B 109.5 . . ?
H01A C01 H01B 109.5 . . ?
P01 C01 H01C 109.5 . . ?
H01A C01 H01C 109.5 . . ?
H01B C01 H01C 109.5 . . ?
C3 P1 C2 102.4(5) . . ?
C3 P1 C1 104.6(5) . . ?
C2 P1 C1 104.0(5) . . ?
C3 P1 Ni1 107.4(5) . . ?
C2 P1 Ni1 117.8(4) . . ?
C1 P1 Ni1 118.7(6) . . ?
C3 P1 Ni1 97.9(4) . 14_545 ?
C2 P1 Ni1 106.7(4) . 14_545 ?
C1 P1 Ni1 136.6(6) . 14_545 ?
Ni1 P1 Ni1 17.93(7) . 14_545 ?
P1 C1 H1C 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1C C1 H1B 109.5 . . ?
P1 C1 H1A 109.5 . . ?
H1C C1 H1A 109.5 . . ?
H1B C1 H1A 109.5 . . ?

_refine_diff_density_max         0.335
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.053


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'acetonitrile, diethyl ether'
