# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_dd81hs
_database_code_depnum_ccdc_archive 'CCDC 1834874'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
? 
;
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_moiety         'C38 H32 N2 Ni O2 P2, 2(B F4)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C38 H32 B2 F8 N2 Ni O2 P2'
_chemical_formula_weight         842.92
_chemical_absolute_configuration ad
_chemical_compound_source        ?
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   22.8739(7)
_cell_length_b                   30.4914(9)
_cell_length_c                   10.5514(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7359.2(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    19784
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   0.925
_shelx_estimated_absorpt_T_min   0.844
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/7 (Krause et al., 2015)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3440
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 1.00 0.00 0.0560
3.00 -1.00 1.00 0.0360
-2.00 -1.00 -1.00 0.0690
-3.00 1.00 -1.00 0.0580
2.00 -2.00 3.00 0.0790
0.00 -1.00 0.00 0.0820
-2.00 2.00 -3.00 0.0890
2.00 2.00 -3.00 0.1200
-2.00 -2.00 3.00 0.1040
2.00 3.00 -1.00 0.1090
0.00 2.00 1.00 0.0980
1.00 1.00 0.00 0.0960
3.00 0.00 -1.00 0.1210

_exptl_crystal_id                dd81hsa
_exptl_crystal_preparation       
;
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1 -1 -4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.114
_exptl_special_details           
;
One distinct cell was identified using APEX3 (Bruker, 2016). 
Five frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by 
the multi-scan method using SADABS v2014/7 (Krause et al., 2015). 
No decay correction was applied. 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24395
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.358
_diffrn_reflns_theta_min         2.228
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dd81hsa
_diffrn_source                   ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4148
_reflns_number_total             4571
_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 V8.37A (Bruker, 2014)'
_computing_data_collection       'APEX3 V2016.9-0 (Bruker, 2016)'
_computing_data_reduction        
;
SAINT V8.34A, XPREP v2014/2, SADABS V2014/7 (Krause et al., 2015), 
;
_computing_molecular_graphics    
;
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2015)'
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack (1983), 2152 Friedels'
_refine_ls_abs_structure_Flack   0.006(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4571
_refine_ls_number_restraints     523
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0507
_refine_ls_restrained_S_all      1.077
_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)+(0.0412P)²+43.0782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1197
_refine_special_details          
;
Structure was phased by direct methods (Sheldrick, 2015).  Systematic 
conditions suggested the unambiguous space group. The space group choice was 
confirmed by successful convergence of the full-matrix least-squares 
refinement on F². The highest peaks in the final difference Fourier map were 
in the vicinity of atom Ni1; the final map had no other significant features. 
A final analysis of variance between observed and calculated structure factors 
showed some dependence on amplitude and little dependence on resolution. 
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.62406(7) 0.0257(2) Uani 1 2 d S T P A .
P1 P 0.50537(6) 0.55357(4) 0.48554(11) 0.0274(3) Uani 1 1 d D . . . .
O1 O 0.55998(18) 0.51958(14) 0.8507(3) 0.0362(9) Uani 1 1 d . . . . .
H1 H 0.583(3) 0.497(3) 0.820(7) 0.054 Uiso 1 1 d . U . . .
N1 N 0.52917(19) 0.54024(15) 0.7542(4) 0.0283(9) Uani 1 1 d . . . . .
C1 C 0.4817(2) 0.60405(18) 0.5638(5) 0.0296(11) Uani 1 1 d . . . . .
C2 C 0.4957(2) 0.61212(19) 0.6914(5) 0.0318(11) Uani 1 1 d . . . . .
C3 C 0.4805(3) 0.6536(2) 0.7437(6) 0.0435(14) Uani 1 1 d . . . . .
H3A H 0.4899 0.6598 0.8296 0.052 Uiso 1 1 calc R U . . .
C4 C 0.4530(3) 0.6845(2) 0.6738(6) 0.0509(17) Uani 1 1 d . . . . .
H4A H 0.4426 0.7117 0.7113 0.061 Uiso 1 1 calc R U . . .
C5 C 0.4399(3) 0.6768(2) 0.5489(6) 0.0476(16) Uani 1 1 d . . . . .
H5A H 0.4210 0.6986 0.4996 0.057 Uiso 1 1 calc R U . . .
C6 C 0.4546(2) 0.63672(19) 0.4951(5) 0.0376(12) Uani 1 1 d . . . . .
H6A H 0.4457 0.6317 0.4083 0.045 Uiso 1 1 calc R U . . .
C7 C 0.5249(2) 0.58163(18) 0.7737(5) 0.0312(11) Uani 1 1 d . . . . .
H7A H 0.5423 0.5930 0.8485 0.037 Uiso 1 1 calc R U . . .
C8 C 0.4526(5) 0.5500(6) 0.3554(9) 0.034(2) Uani 0.60(2) 1 d DG U P A 1
C9 C 0.4691(5) 0.5427(5) 0.2303(10) 0.041(3) Uani 0.60(2) 1 d G U P A 1
H9A H 0.5093 0.5415 0.2084 0.049 Uiso 0.60(2) 1 calc R U P A 1
C10 C 0.4267(7) 0.5372(4) 0.1374(9) 0.046(3) Uani 0.60(2) 1 d G U P A 1
H10A H 0.4379 0.5322 0.0519 0.055 Uiso 0.60(2) 1 calc R U P A 1
C11 C 0.3678(6) 0.5389(3) 0.1695(11) 0.048(3) Uani 0.60(2) 1 d G U P A 1
H11A H 0.3388 0.5351 0.1060 0.057 Uiso 0.60(2) 1 calc R U P A 1
C12 C 0.3513(5) 0.5462(4) 0.2946(12) 0.047(3) Uani 0.60(2) 1 d G U P A 1
H12A H 0.3111 0.5474 0.3165 0.056 Uiso 0.60(2) 1 calc R U P A 1
C13 C 0.3938(6) 0.5517(5) 0.3875(9) 0.037(2) Uani 0.60(2) 1 d G U P A 1
H13A H 0.3825 0.5567 0.4730 0.045 Uiso 0.60(2) 1 calc R U P A 1
C8B C 0.4612(9) 0.5498(10) 0.3451(14) 0.038(3) Uani 0.40(2) 1 d DG U P A 2
C9B C 0.4860(8) 0.5478(9) 0.2249(18) 0.044(3) Uani 0.40(2) 1 d G U P A 2
H9B H 0.5272 0.5499 0.2151 0.052 Uiso 0.40(2) 1 calc R U P A 2
C10B C 0.4505(10) 0.5426(7) 0.1191(13) 0.049(3) Uani 0.40(2) 1 d G U P A 2
H10B H 0.4674 0.5412 0.0369 0.059 Uiso 0.40(2) 1 calc R U P A 2
C11B C 0.3902(9) 0.5395(6) 0.1334(14) 0.050(3) Uani 0.40(2) 1 d G U P A 2
H11B H 0.3659 0.5359 0.0611 0.060 Uiso 0.40(2) 1 calc R U P A 2
C12B C 0.3655(7) 0.5415(6) 0.2536(18) 0.046(3) Uani 0.40(2) 1 d G U P A 2
H12B H 0.3243 0.5394 0.2634 0.056 Uiso 0.40(2) 1 calc R U P A 2
C13B C 0.4010(9) 0.5467(8) 0.3594(13) 0.042(3) Uani 0.40(2) 1 d G U P A 2
H13B H 0.3841 0.5481 0.4416 0.050 Uiso 0.40(2) 1 calc R U P A 2
C14 C 0.5769(5) 0.5652(6) 0.4226(18) 0.027(2) Uani 0.57(4) 1 d DG U P A 1
C15 C 0.6263(6) 0.5472(6) 0.4787(18) 0.032(2) Uani 0.57(4) 1 d G U P A 1
H15 H 0.6222 0.5264 0.5453 0.038 Uiso 0.57(4) 1 calc R U P A 1
C16 C 0.6816(5) 0.5595(6) 0.4375(18) 0.032(2) Uani 0.57(4) 1 d G U P A 1
H16 H 0.7154 0.5471 0.4759 0.038 Uiso 0.57(4) 1 calc R U P A 1
C17 C 0.6875(5) 0.5899(5) 0.3402(18) 0.037(3) Uani 0.57(4) 1 d G U P A 1
H17 H 0.7253 0.5983 0.3120 0.044 Uiso 0.57(4) 1 calc R U P A 1
C18 C 0.6381(7) 0.6079(4) 0.2840(18) 0.039(3) Uani 0.57(4) 1 d G U P A 1
H18 H 0.6421 0.6287 0.2175 0.046 Uiso 0.57(4) 1 calc R U P A 1
C19 C 0.5828(6) 0.5956(6) 0.3252(18) 0.035(3) Uani 0.57(4) 1 d G U P A 1
H19 H 0.5490 0.6080 0.2869 0.042 Uiso 0.57(4) 1 calc R U P A 1
C14B C 0.5800(5) 0.5677(8) 0.440(2) 0.032(3) Uani 0.43(4) 1 d DG U P A 2
C15B C 0.6247(9) 0.5430(8) 0.494(3) 0.031(3) Uani 0.43(4) 1 d G U P A 2
H15B H 0.6158 0.5207 0.5538 0.037 Uiso 0.43(4) 1 calc R U P A 2
C16B C 0.6825(7) 0.5509(8) 0.460(2) 0.037(3) Uani 0.43(4) 1 d G U P A 2
H16B H 0.7130 0.5340 0.4966 0.044 Uiso 0.43(4) 1 calc R U P A 2
C17B C 0.6956(6) 0.5835(7) 0.373(2) 0.037(3) Uani 0.43(4) 1 d G U P A 2
H17B H 0.7350 0.5889 0.3493 0.045 Uiso 0.43(4) 1 calc R U P A 2
C18B C 0.6509(9) 0.6083(6) 0.319(2) 0.041(3) Uani 0.43(4) 1 d G U P A 2
H18B H 0.6598 0.6306 0.2592 0.049 Uiso 0.43(4) 1 calc R U P A 2
C19B C 0.5931(7) 0.6003(8) 0.353(2) 0.037(3) Uani 0.43(4) 1 d G U P A 2
H19B H 0.5626 0.6172 0.3164 0.044 Uiso 0.43(4) 1 calc R U P A 2
B1 B 0.6622(4) 0.4452(3) 0.7488(8) 0.0410(19) Uani 0.822(9) 1 d D U P B 1
F1 F 0.6055(2) 0.45773(18) 0.7064(6) 0.0609(17) Uani 0.822(9) 1 d D U P B 1
F2 F 0.6687(4) 0.4565(4) 0.8725(8) 0.068(2) Uani 0.822(9) 1 d D U P B 1
F3 F 0.7004(3) 0.46929(16) 0.6742(5) 0.0552(14) Uani 0.822(9) 1 d D U P B 1
F4 F 0.6700(4) 0.4010(2) 0.7279(10) 0.051(2) Uani 0.822(9) 1 d D U P B 1
B1B B 0.6554(9) 0.4353(10) 0.775(3) 0.054(5) Uani 0.178(9) 1 d D U P B 2
F1B F 0.5956(7) 0.4376(6) 0.810(2) 0.046(5) Uani 0.178(9) 1 d D U P B 2
F2B F 0.6868(12) 0.4532(14) 0.871(3) 0.044(6) Uani 0.178(9) 1 d D U P B 2
F3B F 0.6588(14) 0.4612(9) 0.667(2) 0.072(6) Uani 0.178(9) 1 d D U P B 2
F4B F 0.6710(18) 0.3928(9) 0.750(4) 0.054(8) Uani 0.178(9) 1 d D U P 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 2.1952(14) 2_665 ?
Ni1 P1 2.1952(14) . ?
Ni1 N1 1.958(4) . ?
Ni1 N1 1.958(4) 2_665 ?
P1 C1 1.829(5) . ?
P1 C8 1.831(6) . ?
P1 C8B 1.797(8) . ?
P1 C14 1.800(7) . ?
P1 C14B 1.825(9) . ?
O1 H1 0.93(8) . ?
O1 N1 1.389(5) . ?
N1 C7 1.282(7) . ?
C1 C2 1.405(7) . ?
C1 C6 1.379(8) . ?
C2 C3 1.424(8) . ?
C2 C7 1.437(8) . ?
C3 H3A 0.9500 . ?
C3 C4 1.351(9) . ?
C4 H4A 0.9500 . ?
C4 C5 1.371(9) . ?
C5 H5A 0.9500 . ?
C5 C6 1.388(8) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C9 1.3900 . ?
C8 C13 1.3900 . ?
C9 H9A 0.9500 . ?
C9 C10 1.3900 . ?
C10 H10A 0.9500 . ?
C10 C11 1.3900 . ?
C11 H11A 0.9500 . ?
C11 C12 1.3900 . ?
C12 H12A 0.9500 . ?
C12 C13 1.3900 . ?
C13 H13A 0.9500 . ?
C8B C9B 1.3900 . ?
C8B C13B 1.3900 . ?
C9B H9B 0.9500 . ?
C9B C10B 1.3900 . ?
C10B H10B 0.9500 . ?
C10B C11B 1.3900 . ?
C11B H11B 0.9500 . ?
C11B C12B 1.3900 . ?
C12B H12B 0.9500 . ?
C12B C13B 1.3900 . ?
C13B H13B 0.9500 . ?
C14 C15 1.3900 . ?
C14 C19 1.3900 . ?
C15 H15 0.9500 . ?
C15 C16 1.3900 . ?
C16 H16 0.9500 . ?
C16 C17 1.3900 . ?
C17 H17 0.9500 . ?
C17 C18 1.3900 . ?
C18 H18 0.9500 . ?
C18 C19 1.3900 . ?
C19 H19 0.9500 . ?
C14B C15B 1.3900 . ?
C14B C19B 1.3900 . ?
C15B H15B 0.9500 . ?
C15B C16B 1.3900 . ?
C16B H16B 0.9500 . ?
C16B C17B 1.3900 . ?
C17B H17B 0.9500 . ?
C17B C18B 1.3900 . ?
C18B H18B 0.9500 . ?
C18B C19B 1.3900 . ?
C19B H19B 0.9500 . ?
B1 F1 1.426(9) . ?
B1 F2 1.358(10) . ?
B1 F3 1.386(11) . ?
B1 F4 1.375(10) . ?
B1B F1B 1.422(16) . ?
B1B F2B 1.356(16) . ?
B1B F3B 1.385(17) . ?
B1B F4B 1.371(16) . ?

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 96.51(7) . 2_665 ?
N1 Ni1 P1 162.16(14) . 2_665 ?
N1 Ni1 P1 162.16(14) 2_665 . ?
N1 Ni1 P1 88.94(13) 2_665 2_665 ?
N1 Ni1 P1 88.94(13) . . ?
N1 Ni1 N1 91.0(2) 2_665 . ?
C1 P1 Ni1 107.98(18) . . ?
C1 P1 C8 101.2(6) . . ?
C8 P1 Ni1 114.7(5) . . ?
C8B P1 Ni1 118.1(9) . . ?
C8B P1 C1 105.0(9) . . ?
C8B P1 C14B 109.0(11) . . ?
C14 P1 Ni1 116.3(6) . . ?
C14 P1 C1 105.6(6) . . ?
C14 P1 C8 109.5(8) . . ?
C14B P1 Ni1 113.7(8) . . ?
C14B P1 C1 101.3(9) . . ?
N1 O1 H1 112(5) . . ?
O1 N1 Ni1 113.7(3) . . ?
C7 N1 Ni1 134.7(4) . . ?
C7 N1 O1 111.5(4) . . ?
C2 C1 P1 120.8(4) . . ?
C6 C1 P1 120.2(4) . . ?
C6 C1 C2 118.7(5) . . ?
C1 C2 C3 118.1(5) . . ?
C1 C2 C7 124.9(5) . . ?
C3 C2 C7 117.0(5) . . ?
C2 C3 H3A 119.3 . . ?
C4 C3 C2 121.4(5) . . ?
C4 C3 H3A 119.3 . . ?
C3 C4 H4A 119.8 . . ?
C3 C4 C5 120.4(6) . . ?
C5 C4 H4A 119.8 . . ?
C4 C5 H5A 120.3 . . ?
C4 C5 C6 119.5(6) . . ?
C6 C5 H5A 120.3 . . ?
C1 C6 C5 121.9(5) . . ?
C1 C6 H6A 119.1 . . ?
C5 C6 H6A 119.1 . . ?
N1 C7 C2 125.1(5) . . ?
N1 C7 H7A 117.4 . . ?
C2 C7 H7A 117.4 . . ?
C9 C8 P1 122.9(7) . . ?
C9 C8 C13 120.0 . . ?
C13 C8 P1 117.0(7) . . ?
C8 C9 H9A 120.0 . . ?
C10 C9 C8 120.0 . . ?
C10 C9 H9A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C9 C10 C11 120.0 . . ?
C11 C10 H10A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C11 C12 C13 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C8 C13 H13A 120.0 . . ?
C12 C13 C8 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C9B C8B P1 121.8(12) . . ?
C9B C8B C13B 120.0 . . ?
C13B C8B P1 118.1(12) . . ?
C8B C9B H9B 120.0 . . ?
C10B C9B C8B 120.0 . . ?
C10B C9B H9B 120.0 . . ?
C9B C10B H10B 120.0 . . ?
C11B C10B C9B 120.0 . . ?
C11B C10B H10B 120.0 . . ?
C10B C11B H11B 120.0 . . ?
C10B C11B C12B 120.0 . . ?
C12B C11B H11B 120.0 . . ?
C11B C12B H12B 120.0 . . ?
C13B C12B C11B 120.0 . . ?
C13B C12B H12B 120.0 . . ?
C8B C13B H13B 120.0 . . ?
C12B C13B C8B 120.0 . . ?
C12B C13B H13B 120.0 . . ?
C15 C14 P1 120.2(9) . . ?
C15 C14 C19 120.0 . . ?
C19 C14 P1 119.5(9) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C14 C19 H19 120.0 . . ?
C18 C19 C14 120.0 . . ?
C18 C19 H19 120.0 . . ?
C15B C14B P1 117.0(13) . . ?
C15B C14B C19B 120.0 . . ?
C19B C14B P1 122.9(13) . . ?
C14B C15B H15B 120.0 . . ?
C16B C15B C14B 120.0 . . ?
C16B C15B H15B 120.0 . . ?
C15B C16B H16B 120.0 . . ?
C15B C16B C17B 120.0 . . ?
C17B C16B H16B 120.0 . . ?
C16B C17B H17B 120.0 . . ?
C18B C17B C16B 120.0 . . ?
C18B C17B H17B 120.0 . . ?
C17B C18B H18B 120.0 . . ?
C17B C18B C19B 120.0 . . ?
C19B C18B H18B 120.0 . . ?
C14B C19B H19B 120.0 . . ?
C18B C19B C14B 120.0 . . ?
C18B C19B H19B 120.0 . . ?
F2 B1 F1 109.4(7) . . ?
F2 B1 F3 110.1(8) . . ?
F2 B1 F4 112.8(9) . . ?
F3 B1 F1 104.7(7) . . ?
F4 B1 F1 109.3(7) . . ?
F4 B1 F3 110.3(7) . . ?
F2B B1B F1B 107.1(17) . . ?
F2B B1B F3B 111(2) . . ?
F2B B1B F4B 113(2) . . ?
F3B B1B F1B 104.0(18) . . ?
F4B B1B F1B 110.3(19) . . ?
F4B B1B F3B 111.5(19) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 F1 0.93(8) 1.77(8) 2.638(7) 155(7) .
O1 H1 F2 0.93(8) 2.38(8) 3.152(10) 141(6) .
O1 H1 F1B 0.93(8) 1.84(8) 2.664(19) 147(7) .

####################################################################### 
# 
# 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_twin4_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1834876'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
? 
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C57 H45 N3 Ni3 O4 P3, B F4, 0.5(H2 O)'
_chemical_formula_sum            'C57 H46 B F4 N3 Ni3 O4.50 P3'
_chemical_formula_structural     ?
_chemical_formula_weight         1200.82

_chemical_absolute_configuration ?
_chemical_formula_iupac          ?
_chemical_formula_analytical     ?
_chemical_compound_source        ?

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.4858(13)
_cell_length_b                   14.8932(13)
_cell_length_c                   15.1803(12)
_cell_angle_alpha                91.309(3)
_cell_angle_beta                 108.166(3)
_cell_angle_gamma                118.187(3)
_cell_volume                     2685.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    51757
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      25.55
_exptl_crystal_description       plate-like
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_F_000             1230
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.042
_exptl_crystal_id                twin4_a_sq

_exptl_crystal_preparation       
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 2 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_absorpt_coefficient_mu    1.195
_shelx_estimated_absorpt_T_min   0.717
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.642095
_exptl_absorpt_correction_T_max  0.745209
_exptl_absorpt_process_details   'TWINABS V2014/5 (Bruker, 2014)'

_exptl_absorpt_special_details   ?
_exptl_special_details           
; 
All crystals examined exhibited non-merohedral twinning (which 
consists of a 4° rotation roughly about the a axis). 
One distinct cell was identified using APEX2 (Bruker, 2014) and 
Cell_Now (Sheldrick, 2008). Ten frame series were integrated and 
filtered for statistical outliers using SAINT (Bruker, 2014) then corrected 
for absorption by the multi-scan method using TWINABS v2014/5 (Bruker, 2014). 
Combined unit cell parameters were determined from both components using SAINT 
(Bruker, 2013).  The twin law by rows was (0.994 -0.000 -0.016), 
(0.028 1.012 0072), (-0.026 -0.078 0.988). Averaged reflections from only the 
primary orientation were used for phasing and refinement. Refinement against 
both orientations was attempted but led to higher R factors and less 
satisfactory placement of the water hydrogen atoms. 
No decay correction was applied. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  twin4_a_sq
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source                   ?
_diffrn_standards_number         ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_time  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18684

_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.349
_diffrn_reflns_theta_max         25.540
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9844
_reflns_number_gt                8288
_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. 
 
 Structure factors included contributions from the .fab file. 
 
 _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       'APEX2 V2014.9-0 (Bruker, 2014)'

_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.34A, XPREP v2014/2, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_structure_solution    'SHELXT-2014-4 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by intrinsic methods (Sheldrick, 2015b). 
Systematic conditions suggested the ambiguous space group. 
The space group choice was confirmed by successful convergence of the 
full-matrix least-squares refinement on F².  The highest peaks in 
the final difference Fourier map were in the vicinity of the disordered water 
molecule; the final map had no other significant features.  A final analysis 
of variance between observed and calculated structure factors showed some 
dependence on amplitude and little dependence on resolution. 
 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0166P)²+10.2153P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9844
_refine_ls_number_parameters     688
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1080
_refine_ls_wR_factor_gt          0.1021
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_ls_abs_structure_details ?
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 0.37727(4) 0.42054(4) 0.21983(3) 0.00998(12) Uani 1 1 d . . . . .
Ni2 Ni 0.29799(4) 0.56601(4) 0.28614(3) 0.00918(12) Uani 1 1 d . . . . .
Ni3 Ni 0.52907(4) 0.66307(4) 0.25988(3) 0.00996(12) Uani 1 1 d . . . . .
P1 P 0.34673(8) 0.26350(8) 0.19144(7) 0.0107(2) Uani 1 1 d . . . . .
P2 P 0.18470(8) 0.57802(8) 0.34496(7) 0.0100(2) Uani 1 1 d . . . . .
P3 P 0.69863(8) 0.79192(8) 0.30027(7) 0.0109(2) Uani 1 1 d . . . . .
O1 O 0.5808(2) 0.5799(2) 0.2296(2) 0.0163(6) Uani 1 1 d . . . . .
O2 O 0.2628(2) 0.3679(2) 0.2674(2) 0.0163(6) Uani 1 1 d . . . . .
O3 O 0.3895(2) 0.7075(2) 0.31754(19) 0.0144(6) Uani 1 1 d . . . . .
O4 O 0.3874(2) 0.5498(2) 0.23068(18) 0.0121(6) Uani 1 1 d . . . . .
N1 N 0.5040(3) 0.4775(2) 0.1865(2) 0.0114(7) Uani 1 1 d . . . . .
N2 N 0.2060(3) 0.4226(3) 0.2572(2) 0.0123(7) Uani 1 1 d . . . . .
N3 N 0.4793(2) 0.7515(2) 0.2878(2) 0.0116(7) Uani 1 1 d . . . . .
C1 C 0.3999(3) 0.2457(3) 0.1035(3) 0.0137(8) Uani 1 1 d . . . . .
C2 C 0.4879(3) 0.3328(3) 0.0873(3) 0.0126(8) Uani 1 1 d . . . . .
C3 C 0.5349(3) 0.3158(3) 0.0252(3) 0.0164(9) Uani 1 1 d . . . . .
H3 H 0.5936 0.3737 0.0138 0.020 Uiso 1 1 calc R U . . .
C4 C 0.4972(3) 0.2158(3) -0.0200(3) 0.0203(9) Uani 1 1 d . . . . .
H4 H 0.5310 0.2056 -0.0609 0.024 Uiso 1 1 calc R U . . .
C5 C 0.4108(3) 0.1317(3) -0.0050(3) 0.0199(9) Uani 1 1 d . . . . .
H5 H 0.3844 0.0635 -0.0363 0.024 Uiso 1 1 calc R U . . .
C6 C 0.3618(3) 0.1462(3) 0.0557(3) 0.0168(9) Uani 1 1 d . . . . .
H6 H 0.3016 0.0875 0.0647 0.020 Uiso 1 1 calc R U . . .
C7 C 0.5382(3) 0.4403(3) 0.1342(3) 0.0144(8) Uani 1 1 d . . . . .
H7 H 0.6046 0.4893 0.1251 0.017 Uiso 1 1 calc R U . . .
C8 C 0.4122(3) 0.2247(3) 0.2948(3) 0.0126(8) Uani 1 1 d . . . . .
C9 C 0.4737(3) 0.1759(3) 0.2943(3) 0.0199(9) Uani 1 1 d . . . . .
H9 H 0.4865 0.1636 0.2387 0.024 Uiso 1 1 calc R U . . .
C10 C 0.5164(4) 0.1452(3) 0.3762(3) 0.0239(10) Uani 1 1 d . . . . .
H10 H 0.5579 0.1114 0.3758 0.029 Uiso 1 1 calc R U . . .
C11 C 0.4994(3) 0.1634(3) 0.4569(3) 0.0211(9) Uani 1 1 d . . . . .
H11 H 0.5296 0.1427 0.5123 0.025 Uiso 1 1 calc R U . . .
C12 C 0.4380(3) 0.2119(3) 0.4581(3) 0.0216(10) Uani 1 1 d . . . . .
H12 H 0.4257 0.2239 0.5141 0.026 Uiso 1 1 calc R U . . .
C13 C 0.3948(3) 0.2428(3) 0.3773(3) 0.0187(9) Uani 1 1 d . . . . .
H13 H 0.3532 0.2764 0.3782 0.022 Uiso 1 1 calc R U . . .
C14 C 0.1986(3) 0.1651(3) 0.1507(3) 0.0126(8) Uani 1 1 d . . . . .
C15 C 0.1619(3) 0.0690(3) 0.1771(3) 0.0201(9) Uani 1 1 d . . . . .
H15 H 0.2154 0.0518 0.2139 0.024 Uiso 1 1 calc R U . . .
C16 C 0.0473(4) -0.0024(3) 0.1500(3) 0.0261(10) Uani 1 1 d . . . . .
H16 H 0.0227 -0.0684 0.1676 0.031 Uiso 1 1 calc R U . . .
C17 C -0.0309(4) 0.0235(4) 0.0971(3) 0.0289(11) Uani 1 1 d . . . . .
H17 H -0.1090 -0.0239 0.0802 0.035 Uiso 1 1 calc R U . . .
C18 C 0.0049(3) 0.1181(4) 0.0690(3) 0.0243(10) Uani 1 1 d . . . . .
H18 H -0.0489 0.1345 0.0312 0.029 Uiso 1 1 calc R U . . .
C19 C 0.1187(3) 0.1889(3) 0.0957(3) 0.0148(8) Uani 1 1 d . . . . .
H19 H 0.1427 0.2539 0.0765 0.018 Uiso 1 1 calc R U . . .
C20 C 0.0423(3) 0.4936(3) 0.2621(3) 0.0120(8) Uani 1 1 d . . . . .
C21 C 0.0163(3) 0.3969(3) 0.2159(3) 0.0122(8) Uani 1 1 d . . . . .
C22 C -0.0937(3) 0.3286(3) 0.1538(3) 0.0155(8) Uani 1 1 d . . . . .
H22 H -0.1125 0.2625 0.1234 0.019 Uiso 1 1 calc R U . . .
C23 C -0.1759(3) 0.3560(3) 0.1359(3) 0.0210(9) Uani 1 1 d . . . . .
H23 H -0.2503 0.3092 0.0930 0.025 Uiso 1 1 calc R U . . .
C24 C -0.1497(3) 0.4513(3) 0.1803(3) 0.0250(10) Uani 1 1 d . . . . .
H24 H -0.2060 0.4702 0.1675 0.030 Uiso 1 1 calc R U . . .
C25 C -0.0408(3) 0.5203(3) 0.2440(3) 0.0178(9) Uani 1 1 d . . . . .
H25 H -0.0235 0.5854 0.2751 0.021 Uiso 1 1 calc R U . . .
C26 C 0.0977(3) 0.3621(3) 0.2285(3) 0.0132(8) Uani 1 1 d . . . . .
H26 H 0.0690 0.2893 0.2145 0.016 Uiso 1 1 calc R U . . .
C27 C 0.1890(3) 0.5275(3) 0.4531(3) 0.0122(8) Uani 1 1 d . . . . .
C28 C 0.0931(3) 0.4576(3) 0.4692(3) 0.0184(9) Uani 1 1 d . . . . .
H28 H 0.0207 0.4329 0.4221 0.022 Uiso 1 1 calc R U . . .
C29 C 0.1033(4) 0.4241(4) 0.5543(3) 0.0244(10) Uani 1 1 d . . . . .
H29 H 0.0378 0.3752 0.5647 0.029 Uiso 1 1 calc R U . . .
C30 C 0.2082(4) 0.4612(3) 0.6242(3) 0.0216(9) Uani 1 1 d . . . . .
H30 H 0.2148 0.4390 0.6830 0.026 Uiso 1 1 calc R U . . .
C31 C 0.3036(3) 0.5310(3) 0.6079(3) 0.0212(9) Uani 1 1 d . . . . .
H31 H 0.3759 0.5568 0.6557 0.025 Uiso 1 1 calc R U . . .
C32 C 0.2945(3) 0.5632(3) 0.5231(3) 0.0171(9) Uani 1 1 d . . . . .
H32 H 0.3605 0.6100 0.5121 0.021 Uiso 1 1 calc R U . . .
C33 C 0.2022(3) 0.7060(3) 0.3738(3) 0.0132(8) Uani 1 1 d . . . . .
C34 C 0.2262(3) 0.7735(3) 0.3113(3) 0.0155(9) Uani 1 1 d . . . . .
H34 H 0.2266 0.7503 0.2526 0.019 Uiso 1 1 calc R U . . .
C35 C 0.2495(3) 0.8747(3) 0.3349(3) 0.0228(10) Uani 1 1 d . . . . .
H35 H 0.2666 0.9210 0.2928 0.027 Uiso 1 1 calc R U . . .
C36 C 0.2477(3) 0.9080(3) 0.4207(3) 0.0260(11) Uani 1 1 d . . . . .
H36 H 0.2650 0.9775 0.4375 0.031 Uiso 1 1 calc R U . . .
C37 C 0.2212(3) 0.8410(3) 0.4809(3) 0.0226(10) Uani 1 1 d . . . . .
H37 H 0.2178 0.8637 0.5382 0.027 Uiso 1 1 calc R U . . .
C38 C 0.1991(3) 0.7397(3) 0.4587(3) 0.0151(8) Uani 1 1 d . . . . .
H38 H 0.1820 0.6939 0.5012 0.018 Uiso 1 1 calc R U . . .
C39 C 0.7017(3) 0.9093(3) 0.2693(3) 0.0124(8) Uani 1 1 d . . . . .
C40 C 0.6081(3) 0.9208(3) 0.2606(3) 0.0119(8) Uani 1 1 d . . . . .
C41 C 0.6095(3) 1.0108(3) 0.2336(3) 0.0166(9) Uani 1 1 d . . . . .
H41 H 0.5469 1.0194 0.2270 0.020 Uiso 1 1 calc R U . . .
C42 C 0.7007(4) 1.0873(3) 0.2162(3) 0.0199(9) Uani 1 1 d . . . . .
H42 H 0.7000 1.1475 0.1975 0.024 Uiso 1 1 calc R U . . .
C43 C 0.7931(3) 1.0759(3) 0.2261(3) 0.0215(9) Uani 1 1 d . . . . .
H43 H 0.8561 1.1287 0.2153 0.026 Uiso 1 1 calc R U . . .
C44 C 0.7928(3) 0.9867(3) 0.2521(3) 0.0166(9) Uani 1 1 d . . . . .
H44 H 0.8557 0.9787 0.2580 0.020 Uiso 1 1 calc R U . . .
C45 C 0.5096(3) 0.8471(3) 0.2802(3) 0.0128(8) Uani 1 1 d . . . . .
H45 H 0.4625 0.8719 0.2882 0.015 Uiso 1 1 calc R U . . .
C46 C 0.7728(3) 0.8199(3) 0.4270(3) 0.0119(8) Uani 1 1 d . . . . .
C47 C 0.8411(3) 0.9197(3) 0.4835(3) 0.0179(9) Uani 1 1 d . . . . .
H47 H 0.8498 0.9786 0.4561 0.021 Uiso 1 1 calc R U . . .
C48 C 0.8959(3) 0.9326(3) 0.5793(3) 0.0222(10) Uani 1 1 d . . . . .
H48 H 0.9412 1.0005 0.6179 0.027 Uiso 1 1 calc R U . . .
C49 C 0.8857(3) 0.8474(3) 0.6200(3) 0.0195(9) Uani 1 1 d . . . . .
H49 H 0.9249 0.8571 0.6858 0.023 Uiso 1 1 calc R U . . .
C50 C 0.8183(3) 0.7482(3) 0.5643(3) 0.0205(9) Uani 1 1 d . . . . .
H50 H 0.8113 0.6898 0.5919 0.025 Uiso 1 1 calc R U . . .
C51 C 0.7609(3) 0.7340(3) 0.4686(3) 0.0175(9) Uani 1 1 d . . . . .
H51 H 0.7132 0.6657 0.4309 0.021 Uiso 1 1 calc R U . . .
C52 C 0.7850(3) 0.7708(3) 0.2474(3) 0.0122(8) Uani 1 1 d . . . . .
C53 C 0.7424(3) 0.7345(3) 0.1500(3) 0.0176(9) Uani 1 1 d . . . . .
H53 H 0.6723 0.7271 0.1121 0.021 Uiso 1 1 calc R U . . .
C54 C 0.8012(4) 0.7091(3) 0.1077(3) 0.0216(9) Uani 1 1 d . . . . .
H54 H 0.7709 0.6833 0.0414 0.026 Uiso 1 1 calc R U . . .
C55 C 0.9049(4) 0.7214(3) 0.1627(3) 0.0230(10) Uani 1 1 d . . . . .
H55 H 0.9454 0.7039 0.1339 0.028 Uiso 1 1 calc R U . . .
C56 C 0.9487(3) 0.7589(3) 0.2588(3) 0.0204(9) Uani 1 1 d . . . . .
H56 H 1.0202 0.7684 0.2958 0.024 Uiso 1 1 calc R U . . .
C57 C 0.8895(3) 0.7831(3) 0.3025(3) 0.0146(8) Uani 1 1 d . . . . .
H57 H 0.9196 0.8076 0.3691 0.018 Uiso 1 1 calc R U . . .
B1 B 0.2648(4) 0.8570(4) 0.0842(4) 0.0257(12) Uani 1 1 d . . . . .
F1 F 0.3076(3) 0.7909(2) 0.0932(2) 0.0461(8) Uani 1 1 d . . . . .
F2 F 0.3343(2) 0.9432(2) 0.15947(19) 0.0375(7) Uani 1 1 d . . . . .
F3 F 0.2547(3) 0.8894(2) -0.00059(19) 0.0482(8) Uani 1 1 d . . . . .
F4 F 0.1577(2) 0.8032(3) 0.0885(2) 0.0468(8) Uani 1 1 d . . . . .
O5 O 0.4937(5) 0.5169(5) 0.4550(5) 0.0288(15) Uani 0.5 1 d G . P A -1
H5A H 0.5283 0.5017 0.4170 0.043 Uiso 0.5 1 d G U P A -1
H5B H 0.4147 0.4691 0.4232 0.043 Uiso 0.5 1 d G 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 O2 1.852(3) . ?
Ni1 O4 1.859(3) . ?
Ni1 N1 1.863(3) . ?
Ni1 P1 2.1700(11) . ?
Ni2 O3 1.829(3) . ?
Ni2 O4 1.848(3) . ?
Ni2 N2 1.853(3) . ?
Ni2 P2 2.1693(11) . ?
Ni3 O1 1.836(3) . ?
Ni3 O4 1.839(3) . ?
Ni3 N3 1.871(3) . ?
Ni3 P3 2.1553(11) . ?
P1 C1 1.806(4) . ?
P1 C14 1.816(4) . ?
P1 C8 1.823(4) . ?
P2 C20 1.810(4) . ?
P2 C27 1.817(4) . ?
P2 C33 1.823(4) . ?
P3 C39 1.805(4) . ?
P3 C46 1.812(4) . ?
P3 C52 1.815(4) . ?
O1 N1 1.375(4) . ?
O2 N2 1.388(4) . ?
O3 N3 1.377(4) . ?
N1 C7 1.291(5) . ?
N2 C26 1.297(5) . ?
N3 C45 1.297(5) . ?
C1 C6 1.399(6) . ?
C1 C2 1.420(6) . ?
C2 C3 1.402(5) . ?
C2 C7 1.458(6) . ?
C3 C4 1.392(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.391(5) . ?
C8 C13 1.398(6) . ?
C9 C10 1.397(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.368(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.388(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.390(6) . ?
C14 C19 1.401(5) . ?
C15 C16 1.394(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.392(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(6) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C25 1.390(5) . ?
C20 C21 1.409(5) . ?
C21 C22 1.398(5) . ?
C21 C26 1.461(5) . ?
C22 C23 1.386(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.397(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.389(5) . ?
C27 C32 1.394(5) . ?
C28 C29 1.385(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.384(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.386(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.374(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.394(6) . ?
C33 C34 1.397(5) . ?
C34 C35 1.391(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.395(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.370(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.395(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C44 1.390(5) . ?
C39 C40 1.412(5) . ?
C40 C41 1.404(5) . ?
C40 C45 1.459(5) . ?
C41 C42 1.386(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.391(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.392(6) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.395(6) . ?
C46 C51 1.400(5) . ?
C47 C48 1.381(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.388(6) . ?
C48 H48 0.9500 . ?
C49 C50 1.384(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.384(6) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.393(6) . ?
C52 C57 1.402(5) . ?
C53 C54 1.384(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.392(6) . ?
C54 H54 0.9500 . ?
C55 C56 1.377(6) . ?
C55 H55 0.9500 . ?
C56 C57 1.393(6) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
B1 F3 1.374(6) . ?
B1 F1 1.380(6) . ?
B1 F4 1.394(6) . ?
B1 F2 1.400(6) . ?
O5 H5A 0.9584 . ?
O5 H5B 0.9584 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O4 90.82(11) . . ?
O2 Ni1 N1 173.31(13) . . ?
O4 Ni1 N1 89.36(12) . . ?
O2 Ni1 P1 87.60(9) . . ?
O4 Ni1 P1 172.82(9) . . ?
N1 Ni1 P1 93.03(10) . . ?
O3 Ni2 O4 92.25(11) . . ?
O3 Ni2 N2 178.74(13) . . ?
O4 Ni2 N2 88.33(12) . . ?
O3 Ni2 P2 90.32(8) . . ?
O4 Ni2 P2 176.76(9) . . ?
N2 Ni2 P2 89.13(10) . . ?
O1 Ni3 O4 91.14(11) . . ?
O1 Ni3 N3 177.64(13) . . ?
O4 Ni3 N3 90.47(12) . . ?
O1 Ni3 P3 87.31(9) . . ?
O4 Ni3 P3 176.74(9) . . ?
N3 Ni3 P3 91.17(10) . . ?
C1 P1 C14 107.17(18) . . ?
C1 P1 C8 105.36(17) . . ?
C14 P1 C8 104.14(18) . . ?
C1 P1 Ni1 112.41(14) . . ?
C14 P1 Ni1 113.11(13) . . ?
C8 P1 Ni1 113.93(13) . . ?
C20 P2 C27 104.78(18) . . ?
C20 P2 C33 107.88(17) . . ?
C27 P2 C33 105.16(18) . . ?
C20 P2 Ni2 107.76(13) . . ?
C27 P2 Ni2 111.94(12) . . ?
C33 P2 Ni2 118.45(13) . . ?
C39 P3 C46 107.18(18) . . ?
C39 P3 C52 106.33(17) . . ?
C46 P3 C52 105.47(18) . . ?
C39 P3 Ni3 111.96(13) . . ?
C46 P3 Ni3 110.88(13) . . ?
C52 P3 Ni3 114.53(13) . . ?
N1 O1 Ni3 118.5(2) . . ?
N2 O2 Ni1 113.8(2) . . ?
N3 O3 Ni2 118.3(2) . . ?
Ni3 O4 Ni2 115.69(14) . . ?
Ni3 O4 Ni1 115.82(13) . . ?
Ni2 O4 Ni1 117.11(13) . . ?
C7 N1 O1 112.1(3) . . ?
C7 N1 Ni1 133.8(3) . . ?
O1 N1 Ni1 114.0(2) . . ?
C26 N2 O2 112.7(3) . . ?
C26 N2 Ni2 132.7(3) . . ?
O2 N2 Ni2 114.6(2) . . ?
C45 N3 O3 112.1(3) . . ?
C45 N3 Ni3 132.1(3) . . ?
O3 N3 Ni3 115.7(2) . . ?
C6 C1 C2 118.8(4) . . ?
C6 C1 P1 121.0(3) . . ?
C2 C1 P1 120.0(3) . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 C7 116.4(4) . . ?
C1 C2 C7 124.7(3) . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.4(4) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 121.0(4) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
N1 C7 C2 128.4(4) . . ?
N1 C7 H7 115.8 . . ?
C2 C7 H7 115.8 . . ?
C9 C8 C13 119.5(4) . . ?
C9 C8 P1 123.9(3) . . ?
C13 C8 P1 116.6(3) . . ?
C8 C9 C10 119.5(4) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 120.8(4) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 120.2(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 119.8(4) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C8 120.2(4) . . ?
C12 C13 H13 119.9 . . ?
C8 C13 H13 119.9 . . ?
C15 C14 C19 119.0(4) . . ?
C15 C14 P1 121.9(3) . . ?
C19 C14 P1 119.0(3) . . ?
C14 C15 C16 120.6(4) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 119.5(4) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C18 C17 C16 120.3(4) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 120.2(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C18 C19 C14 120.4(4) . . ?
C18 C19 H19 119.8 . . ?
C14 C19 H19 119.8 . . ?
C25 C20 C21 119.8(4) . . ?
C25 C20 P2 122.6(3) . . ?
C21 C20 P2 117.6(3) . . ?
C22 C21 C20 119.0(3) . . ?
C22 C21 C26 116.8(4) . . ?
C20 C21 C26 124.2(3) . . ?
C23 C22 C21 120.8(4) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C24 C23 C22 120.0(4) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 120.4(4) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C20 C25 C24 120.1(4) . . ?
C20 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
N2 C26 C21 125.3(4) . . ?
N2 C26 H26 117.4 . . ?
C21 C26 H26 117.4 . . ?
C28 C27 C32 119.4(4) . . ?
C28 C27 P2 123.3(3) . . ?
C32 C27 P2 117.3(3) . . ?
C29 C28 C27 119.8(4) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C30 C29 C28 120.6(4) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C29 C30 C31 119.4(4) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
C32 C31 C30 120.5(4) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C31 C32 C27 120.3(4) . . ?
C31 C32 H32 119.8 . . ?
C27 C32 H32 119.8 . . ?
C38 C33 C34 119.8(4) . . ?
C38 C33 P2 121.6(3) . . ?
C34 C33 P2 118.5(3) . . ?
C35 C34 C33 120.0(4) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 119.7(4) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C37 C36 C35 120.4(4) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C38 120.5(4) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C33 C38 C37 119.7(4) . . ?
C33 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C44 C39 C40 120.0(4) . . ?
C44 C39 P3 121.3(3) . . ?
C40 C39 P3 118.8(3) . . ?
C41 C40 C39 118.5(4) . . ?
C41 C40 C45 116.4(3) . . ?
C39 C40 C45 125.1(3) . . ?
C42 C41 C40 121.1(4) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C43 120.0(4) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C42 C43 C44 119.8(4) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C39 C44 C43 120.7(4) . . ?
C39 C44 H44 119.7 . . ?
C43 C44 H44 119.7 . . ?
N3 C45 C40 127.1(3) . . ?
N3 C45 H45 116.5 . . ?
C40 C45 H45 116.5 . . ?
C47 C46 C51 119.4(4) . . ?
C47 C46 P3 124.4(3) . . ?
C51 C46 P3 116.2(3) . . ?
C48 C47 C46 119.7(4) . . ?
C48 C47 H47 120.1 . . ?
C46 C47 H47 120.1 . . ?
C47 C48 C49 120.8(4) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 H48 119.6 . . ?
C50 C49 C48 119.7(4) . . ?
C50 C49 H49 120.1 . . ?
C48 C49 H49 120.1 . . ?
C51 C50 C49 120.1(4) . . ?
C51 C50 H50 119.9 . . ?
C49 C50 H50 119.9 . . ?
C50 C51 C46 120.3(4) . . ?
C50 C51 H51 119.9 . . ?
C46 C51 H51 119.9 . . ?
C53 C52 C57 119.3(4) . . ?
C53 C52 P3 118.7(3) . . ?
C57 C52 P3 121.9(3) . . ?
C54 C53 C52 120.7(4) . . ?
C54 C53 H53 119.7 . . ?
C52 C53 H53 119.7 . . ?
C53 C54 C55 119.9(4) . . ?
C53 C54 H54 120.1 . . ?
C55 C54 H54 120.1 . . ?
C56 C55 C54 119.9(4) . . ?
C56 C55 H55 120.1 . . ?
C54 C55 H55 120.1 . . ?
C55 C56 C57 120.8(4) . . ?
C55 C56 H56 119.6 . . ?
C57 C56 H56 119.6 . . ?
C56 C57 C52 119.4(4) . . ?
C56 C57 H57 120.3 . . ?
C52 C57 H57 120.3 . . ?
F3 B1 F1 112.4(4) . . ?
F3 B1 F4 108.0(4) . . ?
F1 B1 F4 107.9(4) . . ?
F3 B1 F2 110.0(4) . . ?
F1 B1 F2 109.1(4) . . ?
F4 B1 F2 109.3(4) . . ?
H5A O5 H5B 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Ni3 O1 N1 9.2(3) . . . . ?
P3 Ni3 O1 N1 -173.7(2) . . . . ?
O4 Ni1 O2 N2 22.5(2) . . . . ?
P1 Ni1 O2 N2 -150.5(2) . . . . ?
O4 Ni2 O3 N3 4.1(2) . . . . ?
P2 Ni2 O3 N3 -173.9(2) . . . . ?
O1 Ni3 O4 Ni2 157.71(15) . . . . ?
N3 Ni3 O4 Ni2 -24.01(16) . . . . ?
O1 Ni3 O4 Ni1 15.11(16) . . . . ?
N3 Ni3 O4 Ni1 -166.61(16) . . . . ?
O3 Ni2 O4 Ni3 15.55(16) . . . . ?
N2 Ni2 O4 Ni3 -163.33(16) . . . . ?
O3 Ni2 O4 Ni1 157.66(15) . . . . ?
N2 Ni2 O4 Ni1 -21.22(16) . . . . ?
O2 Ni1 O4 Ni3 146.47(15) . . . . ?
N1 Ni1 O4 Ni3 -26.85(16) . . . . ?
O2 Ni1 O4 Ni2 4.41(16) . . . . ?
N1 Ni1 O4 Ni2 -168.90(16) . . . . ?
Ni3 O1 N1 C7 152.4(3) . . . . ?
Ni3 O1 N1 Ni1 -30.2(3) . . . . ?
O4 Ni1 N1 C7 -150.4(4) . . . . ?
P1 Ni1 N1 C7 22.9(4) . . . . ?
O4 Ni1 N1 O1 33.0(2) . . . . ?
P1 Ni1 N1 O1 -153.8(2) . . . . ?
Ni1 O2 N2 C26 136.4(3) . . . . ?
Ni1 O2 N2 Ni2 -43.4(3) . . . . ?
O4 Ni2 N2 C26 -141.5(4) . . . . ?
P2 Ni2 N2 C26 36.4(4) . . . . ?
O4 Ni2 N2 O2 38.1(2) . . . . ?
P2 Ni2 N2 O2 -143.9(2) . . . . ?
Ni2 O3 N3 C45 154.6(3) . . . . ?
Ni2 O3 N3 Ni3 -22.2(3) . . . . ?
O4 Ni3 N3 C45 -148.8(4) . . . . ?
P3 Ni3 N3 C45 34.0(4) . . . . ?
O4 Ni3 N3 O3 27.2(2) . . . . ?
P3 Ni3 N3 O3 -150.0(2) . . . . ?
C14 P1 C1 C6 -36.6(4) . . . . ?
C8 P1 C1 C6 73.9(3) . . . . ?
Ni1 P1 C1 C6 -161.5(3) . . . . ?
C14 P1 C1 C2 148.4(3) . . . . ?
C8 P1 C1 C2 -101.1(3) . . . . ?
Ni1 P1 C1 C2 23.5(3) . . . . ?
C6 C1 C2 C3 -1.1(5) . . . . ?
P1 C1 C2 C3 174.0(3) . . . . ?
C6 C1 C2 C7 -178.0(3) . . . . ?
P1 C1 C2 C7 -2.9(5) . . . . ?
C1 C2 C3 C4 -0.3(6) . . . . ?
C7 C2 C3 C4 176.9(4) . . . . ?
C2 C3 C4 C5 1.2(6) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C4 C5 C6 C1 -0.8(6) . . . . ?
C2 C1 C6 C5 1.6(6) . . . . ?
P1 C1 C6 C5 -173.4(3) . . . . ?
O1 N1 C7 C2 171.6(3) . . . . ?
Ni1 N1 C7 C2 -5.1(6) . . . . ?
C3 C2 C7 N1 172.5(4) . . . . ?
C1 C2 C7 N1 -10.5(6) . . . . ?
C1 P1 C8 C9 -9.5(4) . . . . ?
C14 P1 C8 C9 103.1(4) . . . . ?
Ni1 P1 C8 C9 -133.2(3) . . . . ?
C1 P1 C8 C13 172.7(3) . . . . ?
C14 P1 C8 C13 -74.6(3) . . . . ?
Ni1 P1 C8 C13 49.1(3) . . . . ?
C13 C8 C9 C10 0.4(6) . . . . ?
P1 C8 C9 C10 -177.3(3) . . . . ?
C8 C9 C10 C11 -0.6(7) . . . . ?
C9 C10 C11 C12 0.6(7) . . . . ?
C10 C11 C12 C13 -0.5(6) . . . . ?
C11 C12 C13 C8 0.4(6) . . . . ?
C9 C8 C13 C12 -0.3(6) . . . . ?
P1 C8 C13 C12 177.5(3) . . . . ?
C1 P1 C14 C15 92.2(4) . . . . ?
C8 P1 C14 C15 -19.1(4) . . . . ?
Ni1 P1 C14 C15 -143.3(3) . . . . ?
C1 P1 C14 C19 -91.5(3) . . . . ?
C8 P1 C14 C19 157.2(3) . . . . ?
Ni1 P1 C14 C19 32.9(3) . . . . ?
C19 C14 C15 C16 -0.6(6) . . . . ?
P1 C14 C15 C16 175.6(3) . . . . ?
C14 C15 C16 C17 -0.8(7) . . . . ?
C15 C16 C17 C18 2.0(7) . . . . ?
C16 C17 C18 C19 -1.9(7) . . . . ?
C17 C18 C19 C14 0.5(6) . . . . ?
C15 C14 C19 C18 0.8(6) . . . . ?
P1 C14 C19 C18 -175.6(3) . . . . ?
C27 P2 C20 C25 98.7(4) . . . . ?
C33 P2 C20 C25 -12.9(4) . . . . ?
Ni2 P2 C20 C25 -141.9(3) . . . . ?
C27 P2 C20 C21 -80.3(3) . . . . ?
C33 P2 C20 C21 168.0(3) . . . . ?
Ni2 P2 C20 C21 39.0(3) . . . . ?
C25 C20 C21 C22 -1.1(6) . . . . ?
P2 C20 C21 C22 178.0(3) . . . . ?
C25 C20 C21 C26 178.9(4) . . . . ?
P2 C20 C21 C26 -2.1(5) . . . . ?
C20 C21 C22 C23 1.4(6) . . . . ?
C26 C21 C22 C23 -178.5(4) . . . . ?
C21 C22 C23 C24 -0.6(6) . . . . ?
C22 C23 C24 C25 -0.6(7) . . . . ?
C21 C20 C25 C24 0.0(6) . . . . ?
P2 C20 C25 C24 -179.1(3) . . . . ?
C23 C24 C25 C20 0.9(7) . . . . ?
O2 N2 C26 C21 176.7(3) . . . . ?
Ni2 N2 C26 C21 -3.6(6) . . . . ?
C22 C21 C26 N2 157.1(4) . . . . ?
C20 C21 C26 N2 -22.9(6) . . . . ?
C20 P2 C27 C28 -14.6(4) . . . . ?
C33 P2 C27 C28 99.0(4) . . . . ?
Ni2 P2 C27 C28 -131.1(3) . . . . ?
C20 P2 C27 C32 166.6(3) . . . . ?
C33 P2 C27 C32 -79.8(3) . . . . ?
Ni2 P2 C27 C32 50.1(3) . . . . ?
C32 C27 C28 C29 -0.1(6) . . . . ?
P2 C27 C28 C29 -178.9(3) . . . . ?
C27 C28 C29 C30 1.3(7) . . . . ?
C28 C29 C30 C31 -1.3(7) . . . . ?
C29 C30 C31 C32 0.0(7) . . . . ?
C30 C31 C32 C27 1.2(6) . . . . ?
C28 C27 C32 C31 -1.2(6) . . . . ?
P2 C27 C32 C31 177.7(3) . . . . ?
C20 P2 C33 C38 102.1(3) . . . . ?
C27 P2 C33 C38 -9.3(3) . . . . ?
Ni2 P2 C33 C38 -135.3(3) . . . . ?
C20 P2 C33 C34 -81.9(3) . . . . ?
C27 P2 C33 C34 166.7(3) . . . . ?
Ni2 P2 C33 C34 40.7(3) . . . . ?
C38 C33 C34 C35 1.5(5) . . . . ?
P2 C33 C34 C35 -174.5(3) . . . . ?
C33 C34 C35 C36 -0.6(6) . . . . ?
C34 C35 C36 C37 -1.2(6) . . . . ?
C35 C36 C37 C38 2.0(6) . . . . ?
C34 C33 C38 C37 -0.7(5) . . . . ?
P2 C33 C38 C37 175.3(3) . . . . ?
C36 C37 C38 C33 -1.1(6) . . . . ?
C46 P3 C39 C44 84.9(4) . . . . ?
C52 P3 C39 C44 -27.5(4) . . . . ?
Ni3 P3 C39 C44 -153.3(3) . . . . ?
C46 P3 C39 C40 -96.5(3) . . . . ?
C52 P3 C39 C40 151.0(3) . . . . ?
Ni3 P3 C39 C40 25.3(3) . . . . ?
C44 C39 C40 C41 0.6(6) . . . . ?
P3 C39 C40 C41 -178.0(3) . . . . ?
C44 C39 C40 C45 -177.6(4) . . . . ?
P3 C39 C40 C45 3.8(5) . . . . ?
C39 C40 C41 C42 -0.4(6) . . . . ?
C45 C40 C41 C42 178.0(4) . . . . ?
C40 C41 C42 C43 -0.4(6) . . . . ?
C41 C42 C43 C44 1.0(7) . . . . ?
C40 C39 C44 C43 0.0(6) . . . . ?
P3 C39 C44 C43 178.5(3) . . . . ?
C42 C43 C44 C39 -0.8(7) . . . . ?
O3 N3 C45 C40 172.9(3) . . . . ?
Ni3 N3 C45 C40 -11.1(6) . . . . ?
C41 C40 C45 N3 165.4(4) . . . . ?
C39 C40 C45 N3 -16.4(6) . . . . ?
C39 P3 C46 C47 -13.9(4) . . . . ?
C52 P3 C46 C47 99.2(4) . . . . ?
Ni3 P3 C46 C47 -136.3(3) . . . . ?
C39 P3 C46 C51 167.5(3) . . . . ?
C52 P3 C46 C51 -79.5(3) . . . . ?
Ni3 P3 C46 C51 45.1(3) . . . . ?
C51 C46 C47 C48 0.0(6) . . . . ?
P3 C46 C47 C48 -178.5(3) . . . . ?
C46 C47 C48 C49 1.3(6) . . . . ?
C47 C48 C49 C50 -1.2(6) . . . . ?
C48 C49 C50 C51 -0.2(6) . . . . ?
C49 C50 C51 C46 1.5(6) . . . . ?
C47 C46 C51 C50 -1.4(6) . . . . ?
P3 C46 C51 C50 177.3(3) . . . . ?
C39 P3 C52 C53 -74.5(3) . . . . ?
C46 P3 C52 C53 171.9(3) . . . . ?
Ni3 P3 C52 C53 49.7(3) . . . . ?
C39 P3 C52 C57 110.0(3) . . . . ?
C46 P3 C52 C57 -3.6(4) . . . . ?
Ni3 P3 C52 C57 -125.8(3) . . . . ?
C57 C52 C53 C54 1.0(6) . . . . ?
P3 C52 C53 C54 -174.6(3) . . . . ?
C52 C53 C54 C55 -1.1(6) . . . . ?
C53 C54 C55 C56 -0.1(6) . . . . ?
C54 C55 C56 C57 1.2(6) . . . . ?
C55 C56 C57 C52 -1.3(6) . . . . ?
C53 C52 C57 C56 0.1(6) . . . . ?
P3 C52 C57 C56 175.6(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5B O2 0.96 2.48 3.314(6) 145.0 .

_refine_diff_density_max         0.700
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.104




loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 -1.00 0.00 0.0180
-1.00 1.00 0.00 0.0160
-1.00 -1.00 0.00 0.0250
-1.00 -2.00 2.00 0.0960
1.00 0.00 -2.00 0.1240
0.00 0.00 1.00 0.1320
2.00 1.00 0.00 0.0150

# SQUEEZE RESULTS (Version = 120716) 
# Note: Data are Listed for all Voids in the P1 Unit Cell 
# i.e. Centre of Gravity, Solvent Accessible Volume, 
# Recovered number of Electrons in the Void and 
# Details about the Squeezed Material 
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 133 49 ' '
2 0.051 0.790 0.580 14 0 ' '
3 0.257 0.693 0.700 25 1 ' '
4 0.743 0.307 0.300 25 1 ' '
5 0.948 0.209 0.420 14 0 ' '
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 1.714
-1 1 0 1.645
0 1 0 1.584
0 -1 1 1.913
-1 0 1 1.791
0 0 1 1.442
-1 1 1 1.976
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
; 
One void space containing significant electron density was identified 
by SQUEEZE. The electron density removed from this void space is consistent 
with two methanol solvate molecules, making the most probable solution one 
that consists of one methanol molecule per target molecule.
;
####################################################################### 
# 
# 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_dd21h1s
_database_code_depnum_ccdc_archive 'CCDC 1834875'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
? 
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
; 
 C50 H30 F10 N2 Ni2 O2 P2, 0.364(C5 H12), 1.136(C H2 Cl2) 
;
_chemical_formula_sum            'C52.96 H36.64 Cl2.27 F10 N2 Ni2 O2 P2'
_chemical_formula_structural     ?
_chemical_formula_weight         1182.83

_chemical_absolute_configuration ?
_chemical_formula_iupac          ?
_chemical_formula_analytical     ?
_chemical_compound_source        ?

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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.3092(4)
_cell_length_b                   14.2034(5)
_cell_length_c                   16.4001(6)
_cell_angle_alpha                90.3120(10)
_cell_angle_beta                 100.8350(10)
_cell_angle_gamma                108.0310(10)
_cell_volume                     2454.58(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16097
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      25.37
_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_F_000             1198
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.063
_exptl_crystal_id                dd21h1s

_exptl_crystal_preparation       
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (3 3 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_absorpt_coefficient_mu    1.039
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS V2014/7 (Krause et al., 2015)'

_exptl_absorpt_special_details   ?
_exptl_special_details           
; 
One distinct cell was identified using APEX3 (Bruker, 2016).  Six 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by 
multi-scan methods SADABS v2014/7 (Krause et al., 2015). 
No decay correction was applied. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dd21h1s
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source                   ?
_diffrn_standards_number         ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_time  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45651

_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.250
_diffrn_reflns_theta_max         25.381
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9000
_reflns_number_gt                6964
_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       'APEX3 V2016.9-0 (Bruker, 2016)'

_computing_cell_refinement       'SAINT V8.37A (Bruker, 2014)'
_computing_data_reduction        
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/7 (Krause et al., 2015), 
;
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by intrinsic phasing methods (Sheldrick, 
2015).  Systematic conditions suggested the ambiguous space group. 
The space group choice was confirmed by successful convergence of the 
full-matrix least-squares refinement on F².  The highest peaks in 
the final difference Fourier map were in the vicinity of the full 
occupied disordered dichloromethane site; the 
final map had no other significant features.  A final analysis of 
variance between observed and calculated structure factors showed little 
dependence on amplitude or resolution. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0316P)²+6.9453P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9000
_refine_ls_number_parameters     714
_refine_ls_number_restraints     127
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.0986
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_ls_abs_structure_details ?
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 0.55404(4) 0.87284(3) 0.29412(3) 0.01246(12) Uani 1 1 d . . . . .
Ni2 Ni 0.45786(4) 0.63124(3) 0.28035(3) 0.01147(12) Uani 1 1 d . . . . .
P1 P 0.45660(9) 0.97390(7) 0.24744(6) 0.0144(2) Uani 1 1 d . . . . .
P2 P 0.55122(9) 0.52490(7) 0.26520(6) 0.0127(2) Uani 1 1 d . . . . .
F1 F 0.8039(2) 1.04177(19) 0.37096(15) 0.0358(6) Uani 1 1 d . . . . .
F2 F 1.0025(2) 1.1379(2) 0.30194(17) 0.0426(7) Uani 1 1 d . . . . .
F3 F 1.0053(2) 1.08968(17) 0.14198(16) 0.0312(6) Uani 1 1 d . . . . .
F4 F 0.8078(2) 0.94219(18) 0.05186(14) 0.0312(6) Uani 1 1 d . . . . .
F5 F 0.6072(2) 0.84774(16) 0.11812(13) 0.0234(5) Uani 1 1 d . . . . .
F6 F 0.4292(2) 0.63847(17) 0.08832(14) 0.0256(5) Uani 1 1 d . . . . .
F7 F 0.2390(2) 0.53725(18) -0.03476(14) 0.0336(6) Uani 1 1 d . . . . .
F8 F 0.0256(2) 0.40609(18) 0.00062(16) 0.0334(6) Uani 1 1 d . . . . .
F9 F 0.0031(2) 0.37921(19) 0.16202(17) 0.0376(7) Uani 1 1 d . . . . .
F10 F 0.1909(2) 0.48025(18) 0.28616(14) 0.0282(6) Uani 1 1 d . . . . .
O1 O 0.3587(2) 0.70440(17) 0.31319(16) 0.0157(6) Uani 1 1 d . . . . .
O2 O 0.6518(2) 0.79892(17) 0.35322(16) 0.0165(6) Uani 1 1 d . . . . .
N1 N 0.4057(3) 0.8032(2) 0.33402(18) 0.0131(7) Uani 1 1 d . . . . .
N2 N 0.6034(3) 0.7003(2) 0.36178(18) 0.0124(6) Uani 1 1 d . . . . .
C1 C 0.4039(3) 1.0138(3) 0.3358(2) 0.0166(8) Uani 1 1 d . . . . .
C2 C 0.3602(4) 0.9431(3) 0.3923(2) 0.0168(8) Uani 1 1 d . . . . .
C3 C 0.3185(4) 0.9727(3) 0.4600(2) 0.0207(9) Uani 1 1 d . . . . .
H3 H 0.2888 0.9255 0.4984 0.025 Uiso 1 1 calc R U . . .
C4 C 0.3194(4) 1.0688(3) 0.4723(3) 0.0260(10) Uani 1 1 d . . . . .
H4 H 0.2931 1.0879 0.5197 0.031 Uiso 1 1 calc R U . . .
C5 C 0.3587(4) 1.1378(3) 0.4156(3) 0.0282(10) Uani 1 1 d . . . . .
H5 H 0.3568 1.2036 0.4231 0.034 Uiso 1 1 calc R U . . .
C6 C 0.4009(4) 1.1101(3) 0.3479(3) 0.0237(9) Uani 1 1 d . . . . .
H6 H 0.4281 1.1577 0.3092 0.028 Uiso 1 1 calc R U . . .
C7 C 0.3426(4) 0.8374(3) 0.3774(2) 0.0148(8) Uani 1 1 d . . . . .
H7 H 0.2805 0.7911 0.4015 0.018 Uiso 1 1 calc R U . . .
C8 C 0.5422(4) 1.0857(3) 0.2029(3) 0.0202(9) Uani 1 1 d . . . . .
C9 C 0.6400(4) 1.1590(3) 0.2538(3) 0.0278(10) Uani 1 1 d . . . . .
H9 H 0.6552 1.1547 0.3125 0.033 Uiso 1 1 calc R U . . .
C10 C 0.7158(4) 1.2389(3) 0.2184(4) 0.0375(12) Uani 1 1 d . . . . .
H10 H 0.7817 1.2898 0.2529 0.045 Uiso 1 1 calc R U . . .
C11 C 0.6945(5) 1.2434(4) 0.1333(4) 0.0439(14) Uani 1 1 d . . . . .
H11 H 0.7468 1.2973 0.1093 0.053 Uiso 1 1 calc R U . . .
C12 C 0.5992(4) 1.1714(4) 0.0829(3) 0.0399(13) Uani 1 1 d . . . . .
H12 H 0.5856 1.1756 0.0243 0.048 Uiso 1 1 calc R U . . .
C13 C 0.5222(4) 1.0920(3) 0.1171(3) 0.0266(10) Uani 1 1 d . . . . .
H13 H 0.4559 1.0420 0.0819 0.032 Uiso 1 1 calc R U . . .
C14 C 0.3148(4) 0.9156(3) 0.1701(2) 0.0145(8) Uani 1 1 d . . . . .
C15 C 0.2210(4) 0.9608(3) 0.1471(3) 0.0214(9) Uani 1 1 d . . . . .
H15 H 0.2290 1.0223 0.1743 0.026 Uiso 1 1 calc R U . . .
C16 C 0.1164(4) 0.9165(3) 0.0848(3) 0.0246(9) Uani 1 1 d . . . . .
H16 H 0.0530 0.9476 0.0695 0.030 Uiso 1 1 calc R U . . .
C17 C 0.1040(4) 0.8273(3) 0.0449(3) 0.0235(9) Uani 1 1 d . . . . .
H17 H 0.0324 0.7971 0.0020 0.028 Uiso 1 1 calc R U . . .
C18 C 0.1969(4) 0.7818(3) 0.0679(3) 0.0234(9) Uani 1 1 d . . . . .
H18 H 0.1885 0.7203 0.0404 0.028 Uiso 1 1 calc R U . . .
C19 C 0.3005(4) 0.8252(3) 0.1298(2) 0.0189(9) Uani 1 1 d . . . . .
H19 H 0.3629 0.7931 0.1454 0.023 Uiso 1 1 calc R U . . .
C20 C 0.6982(3) 0.9402(3) 0.2477(2) 0.0142(8) Uani 1 1 d . . . . .
C21 C 0.8021(4) 1.0138(3) 0.2909(2) 0.0218(9) Uani 1 1 d . . . . .
C22 C 0.9041(4) 1.0648(3) 0.2574(3) 0.0248(10) Uani 1 1 d . . . . .
C23 C 0.9056(4) 1.0411(3) 0.1765(3) 0.0206(9) Uani 1 1 d . . . . .
C24 C 0.8055(4) 0.9671(3) 0.1311(2) 0.0179(8) Uani 1 1 d . . . . .
C25 C 0.7048(3) 0.9189(3) 0.1671(2) 0.0153(8) Uani 1 1 d . . . . .
C26 C 0.3183(4) 0.5653(3) 0.1929(2) 0.0155(8) Uani 1 1 d . . . . .
C27 C 0.3236(4) 0.5755(3) 0.1098(2) 0.0173(8) Uani 1 1 d . . . . .
C28 C 0.2281(4) 0.5241(3) 0.0453(2) 0.0220(9) Uani 1 1 d . . . . .
C29 C 0.1199(4) 0.4583(3) 0.0629(3) 0.0225(9) Uani 1 1 d . . . . .
C30 C 0.1085(4) 0.4457(3) 0.1446(3) 0.0225(9) Uani 1 1 d . . . . .
C31 C 0.2064(4) 0.4994(3) 0.2068(2) 0.0188(9) Uani 1 1 d . . . . .
C32 C 0.5929(3) 0.4869(3) 0.3700(2) 0.0155(8) Uani 1 1 d . . . . .
C33 C 0.6423(3) 0.5613(3) 0.4357(2) 0.0135(8) Uani 1 1 d . . . . .
C34 C 0.6822(4) 0.5347(3) 0.5157(2) 0.0199(9) Uani 1 1 d . . . . .
H34 H 0.7179 0.5846 0.5601 0.024 Uiso 1 1 calc R U . . .
C35 C 0.6704(4) 0.4370(3) 0.5310(3) 0.0249(10) Uani 1 1 d . . . . .
H35 H 0.6964 0.4199 0.5859 0.030 Uiso 1 1 calc R U . . .
C36 C 0.6208(4) 0.3643(3) 0.4666(3) 0.0257(10) Uani 1 1 d . . . . .
H36 H 0.6121 0.2970 0.4772 0.031 Uiso 1 1 calc R U . . .
C37 C 0.5836(4) 0.3892(3) 0.3860(3) 0.0210(9) Uani 1 1 d . . . . .
H37 H 0.5516 0.3391 0.3416 0.025 Uiso 1 1 calc R U . . .
C38 C 0.6647(3) 0.6669(3) 0.4231(2) 0.0141(8) Uani 1 1 d . . . . .
H38 H 0.7283 0.7138 0.4626 0.017 Uiso 1 1 calc R U . . .
C39 C 0.7024(4) 0.5729(3) 0.2328(2) 0.0153(8) Uani 1 1 d . . . . .
C40 C 0.7231(4) 0.6530(3) 0.1827(3) 0.0252(10) Uani 1 1 d . . . . .
H40 H 0.6580 0.6818 0.1649 0.030 Uiso 1 1 calc R U . . .
C41 C 0.8392(4) 0.6904(3) 0.1590(3) 0.0328(11) Uani 1 1 d . . . . .
H41 H 0.8527 0.7441 0.1238 0.039 Uiso 1 1 calc R U . . .
C42 C 0.9358(4) 0.6505(3) 0.1859(3) 0.0311(11) Uani 1 1 d . . . . .
H42 H 1.0159 0.6778 0.1707 0.037 Uiso 1 1 calc R U . . .
C43 C 0.9148(4) 0.5707(3) 0.2351(3) 0.0283(10) Uani 1 1 d . . . . .
H43 H 0.9806 0.5426 0.2534 0.034 Uiso 1 1 calc R U . . .
C44 C 0.7985(4) 0.5313(3) 0.2580(3) 0.0249(10) Uani 1 1 d . . . . .
H44 H 0.7842 0.4756 0.2910 0.030 Uiso 1 1 calc R U . . .
C45 C 0.4609(4) 0.4115(3) 0.2013(2) 0.0175(8) Uani 1 1 d . . . . .
C46 C 0.4851(4) 0.3943(3) 0.1235(3) 0.0253(10) Uani 1 1 d . . . . .
H46 H 0.5563 0.4378 0.1053 0.030 Uiso 1 1 calc R U . . .
C47 C 0.4034(5) 0.3122(3) 0.0723(3) 0.0368(12) Uani 1 1 d . . . . .
H47 H 0.4185 0.3006 0.0187 0.044 Uiso 1 1 calc R U . . .
C48 C 0.3015(4) 0.2480(3) 0.0985(3) 0.0344(11) Uani 1 1 d . . . . .
H48 H 0.2472 0.1922 0.0632 0.041 Uiso 1 1 calc R U . . .
C49 C 0.2777(4) 0.2643(3) 0.1758(3) 0.0304(11) Uani 1 1 d . . . . .
H49 H 0.2076 0.2195 0.1941 0.036 Uiso 1 1 calc R U . . .
C50 C 0.3566(4) 0.3464(3) 0.2268(3) 0.0206(9) Uani 1 1 d . . . . .
H50 H 0.3393 0.3584 0.2797 0.025 Uiso 1 1 calc R U . . .
Cl1 Cl 1.04819(12) 0.88464(10) 0.29619(9) 0.0464(3) Uani 1 1 d . . . . .
Cl2 Cl 0.97865(19) 0.8761(2) 0.45612(14) 0.0672(10) Uani 0.699(5) 1 d D U P A 1
Cl2B Cl 1.0082(5) 0.7722(6) 0.4495(5) 0.102(3) Uani 0.301(5) 1 d D U P A 2
C51 C 0.9432(6) 0.8197(5) 0.3575(4) 0.0656(18) Uani 1 1 d D . . . .
H51A H 0.8556 0.8156 0.3307 0.079 Uiso 0.699(5) 1 calc R U P A 1
H51B H 0.9473 0.7512 0.3613 0.079 Uiso 0.699(5) 1 calc R U P A 1
H51C H 0.8789 0.7632 0.3224 0.079 Uiso 0.301(5) 1 calc R U P A 2
H51D H 0.8982 0.8642 0.3739 0.079 Uiso 0.301(5) 1 calc R U P A 2
C52 C 1.0599(19) 0.6810(15) 0.5444(13) 0.082(5) Uani 0.364(5) 1 d G U P B -1
H52A H 1.1465 0.7200 0.5715 0.123 Uiso 0.364(5) 1 calc R U P B -1
H52B H 0.9990 0.7027 0.5686 0.123 Uiso 0.364(5) 1 calc R U P B -1
H52C H 1.0475 0.6910 0.4847 0.123 Uiso 0.364(5) 1 calc R U P B -1
C53 C 1.039(3) 0.5709(15) 0.5574(8) 0.080(5) Uani 0.364(5) 1 d G U P B -1
H53A H 0.9788 0.5486 0.5951 0.097 Uiso 0.364(5) 1 calc R U P B -1
H53B H 1.1210 0.5626 0.5849 0.097 Uiso 0.364(5) 1 calc R U P B -1
C54 C 0.9886(16) 0.5047(15) 0.4762(8) 0.079(4) Uani 0.364(5) 1 d G U P B -1
H54A H 1.0493 0.5272 0.4385 0.095 Uiso 0.364(5) 1 calc R U P B -1
H54B H 0.9072 0.5133 0.4487 0.095 Uiso 0.364(5) 1 calc R U P B -1
C55 C 0.968(3) 0.3942(15) 0.4883(12) 0.092(4) Uani 0.364(5) 1 d G U P B -1
H55A H 1.0490 0.3855 0.5157 0.110 Uiso 0.364(5) 1 calc R U P B -1
H55B H 0.9068 0.3716 0.5259 0.110 Uiso 0.364(5) 1 calc R U P B -1
C56 C 0.917(2) 0.3290(16) 0.4067(15) 0.110(6) Uani 0.364(5) 1 d G U P B -1
H56A H 0.9142 0.2607 0.4177 0.165 Uiso 0.364(5) 1 calc R U P B -1
H56B H 0.9728 0.3544 0.3674 0.165 Uiso 0.364(5) 1 calc R U P B -1
H56C H 0.8312 0.3303 0.3829 0.165 Uiso 0.364(5) 1 calc R U P B -1
Cl3 Cl 0.978(3) 0.3766(18) 0.4961(17) 0.120(5) Uani 0.136(5) 1 d G U P B -2
Cl4 Cl 1.0287(17) 0.5768(16) 0.5706(10) 0.072(4) Uani 0.136(5) 1 d G U P B -2
C57 C 0.976(6) 0.498(2) 0.4788(12) 0.085(5) Uani 0.136(5) 1 d G U P B -2
H57A H 0.8887 0.4961 0.4535 0.102 Uiso 0.136(5) 1 calc R U P B -2
H57B H 1.0311 0.5263 0.4387 0.102 Uiso 0.136(5) 1 calc R U P 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 O2 1.895(2) . ?
Ni1 N1 1.901(3) . ?
Ni1 C20 1.914(4) . ?
Ni1 P1 2.1295(11) . ?
Ni2 O1 1.890(2) . ?
Ni2 N2 1.901(3) . ?
Ni2 C26 1.909(4) . ?
Ni2 P2 2.1307(10) . ?
P1 C14 1.808(4) . ?
P1 C1 1.817(4) . ?
P1 C8 1.821(4) . ?
P2 C39 1.815(4) . ?
P2 C45 1.816(4) . ?
P2 C32 1.825(4) . ?
F1 C21 1.364(4) . ?
F2 C22 1.350(5) . ?
F3 C23 1.353(4) . ?
F4 C24 1.352(4) . ?
F5 C25 1.361(4) . ?
F6 C27 1.360(4) . ?
F7 C28 1.351(4) . ?
F8 C29 1.350(4) . ?
F9 C30 1.352(5) . ?
F10 C31 1.363(4) . ?
O1 N1 1.354(4) . ?
O2 N2 1.355(4) . ?
N1 C7 1.286(5) . ?
N2 C38 1.290(5) . ?
C1 C6 1.394(5) . ?
C1 C2 1.409(5) . ?
C2 C3 1.396(5) . ?
C2 C7 1.464(5) . ?
C3 C4 1.375(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.391(6) . ?
C8 C9 1.391(6) . ?
C9 C10 1.397(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.376(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.365(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.390(5) . ?
C14 C15 1.398(5) . ?
C15 C16 1.384(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.392(6) . ?
C17 H17 0.9500 . ?
C18 C19 1.373(6) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C25 1.376(5) . ?
C20 C21 1.376(5) . ?
C21 C22 1.373(6) . ?
C22 C23 1.371(6) . ?
C23 C24 1.370(5) . ?
C24 C25 1.375(5) . ?
C26 C31 1.382(5) . ?
C26 C27 1.382(5) . ?
C27 C28 1.375(6) . ?
C28 C29 1.371(6) . ?
C29 C30 1.378(6) . ?
C30 C31 1.375(6) . ?
C32 C37 1.390(5) . ?
C32 C33 1.408(5) . ?
C33 C34 1.398(5) . ?
C33 C38 1.465(5) . ?
C34 C35 1.382(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.380(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.392(6) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C44 1.389(5) . ?
C39 C40 1.394(5) . ?
C40 C41 1.386(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.384(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.381(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.384(6) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C46 1.390(6) . ?
C45 C50 1.392(5) . ?
C46 C47 1.396(6) . ?
C46 H46 0.9500 . ?
C47 C48 1.372(7) . ?
C47 H47 0.9500 . ?
C48 C49 1.377(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.385(6) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
Cl1 C51 1.747(6) . ?
Cl2 C51 1.721(7) . ?
Cl2B C51 1.780(8) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 H51C 0.9900 . ?
C51 H51D 0.9900 . ?
C52 C53 1.5312 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.5331 . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.5333 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.5314 . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
Cl3 C57 1.7600 . ?
Cl4 C57 1.7604 . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 N1 93.37(12) . . ?
O2 Ni1 C20 88.19(13) . . ?
N1 Ni1 C20 176.76(15) . . ?
O2 Ni1 P1 169.58(9) . . ?
N1 Ni1 P1 86.85(9) . . ?
C20 Ni1 P1 92.13(11) . . ?
O1 Ni2 N2 93.06(12) . . ?
O1 Ni2 C26 88.82(14) . . ?
N2 Ni2 C26 176.06(15) . . ?
O1 Ni2 P2 165.92(8) . . ?
N2 Ni2 P2 87.22(9) . . ?
C26 Ni2 P2 91.80(11) . . ?
C14 P1 C1 106.24(17) . . ?
C14 P1 C8 105.64(18) . . ?
C1 P1 C8 107.02(18) . . ?
C14 P1 Ni1 112.79(12) . . ?
C1 P1 Ni1 105.34(13) . . ?
C8 P1 Ni1 119.04(13) . . ?
C39 P2 C45 107.37(18) . . ?
C39 P2 C32 104.05(17) . . ?
C45 P2 C32 106.06(18) . . ?
C39 P2 Ni2 115.54(13) . . ?
C45 P2 Ni2 117.94(13) . . ?
C32 P2 Ni2 104.51(12) . . ?
N1 O1 Ni2 122.5(2) . . ?
N2 O2 Ni1 122.5(2) . . ?
C7 N1 O1 115.3(3) . . ?
C7 N1 Ni1 128.8(3) . . ?
O1 N1 Ni1 115.9(2) . . ?
C38 N2 O2 115.0(3) . . ?
C38 N2 Ni2 129.6(3) . . ?
O2 N2 Ni2 115.4(2) . . ?
C6 C1 C2 119.1(4) . . ?
C6 C1 P1 122.6(3) . . ?
C2 C1 P1 118.3(3) . . ?
C3 C2 C1 118.8(3) . . ?
C3 C2 C7 118.4(3) . . ?
C1 C2 C7 122.5(3) . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.1(4) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.6(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 121.0(4) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
N1 C7 C2 124.3(3) . . ?
N1 C7 H7 117.9 . . ?
C2 C7 H7 117.9 . . ?
C13 C8 C9 119.6(4) . . ?
C13 C8 P1 120.2(3) . . ?
C9 C8 P1 119.7(3) . . ?
C8 C9 C10 119.7(4) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 119.7(5) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C12 C11 C10 120.9(4) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 120.2(5) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C8 119.9(4) . . ?
C12 C13 H13 120.0 . . ?
C8 C13 H13 120.0 . . ?
C19 C14 C15 118.8(4) . . ?
C19 C14 P1 119.4(3) . . ?
C15 C14 P1 121.8(3) . . ?
C16 C15 C14 120.4(4) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 120.2(4) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 119.7(4) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 120.4(4) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C14 120.5(4) . . ?
C18 C19 H19 119.7 . . ?
C14 C19 H19 119.7 . . ?
C25 C20 C21 114.6(3) . . ?
C25 C20 Ni1 121.9(3) . . ?
C21 C20 Ni1 123.5(3) . . ?
F1 C21 C22 116.8(4) . . ?
F1 C21 C20 119.2(3) . . ?
C22 C21 C20 123.9(4) . . ?
F2 C22 C23 119.3(4) . . ?
F2 C22 C21 121.6(4) . . ?
C23 C22 C21 119.1(4) . . ?
F3 C23 C24 120.3(4) . . ?
F3 C23 C22 120.4(4) . . ?
C24 C23 C22 119.3(3) . . ?
F4 C24 C23 119.5(3) . . ?
F4 C24 C25 121.0(3) . . ?
C23 C24 C25 119.5(4) . . ?
F5 C25 C24 116.6(3) . . ?
F5 C25 C20 119.9(3) . . ?
C24 C25 C20 123.5(3) . . ?
C31 C26 C27 114.2(3) . . ?
C31 C26 Ni2 123.2(3) . . ?
C27 C26 Ni2 122.6(3) . . ?
F6 C27 C28 116.4(3) . . ?
F6 C27 C26 119.5(3) . . ?
C28 C27 C26 124.0(4) . . ?
F7 C28 C29 119.6(4) . . ?
F7 C28 C27 121.2(4) . . ?
C29 C28 C27 119.2(4) . . ?
F8 C29 C28 120.3(4) . . ?
F8 C29 C30 120.3(4) . . ?
C28 C29 C30 119.4(4) . . ?
F9 C30 C31 121.5(4) . . ?
F9 C30 C29 119.5(4) . . ?
C31 C30 C29 119.1(4) . . ?
F10 C31 C30 115.9(3) . . ?
F10 C31 C26 120.0(3) . . ?
C30 C31 C26 124.0(4) . . ?
C37 C32 C33 119.6(3) . . ?
C37 C32 P2 122.4(3) . . ?
C33 C32 P2 117.9(3) . . ?
C34 C33 C32 118.9(3) . . ?
C34 C33 C38 117.9(3) . . ?
C32 C33 C38 123.0(3) . . ?
C35 C34 C33 120.9(4) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C36 C35 C34 120.0(4) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C37 120.2(4) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C32 C37 C36 120.4(4) . . ?
C32 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
N2 C38 C33 124.0(3) . . ?
N2 C38 H38 118.0 . . ?
C33 C38 H38 118.0 . . ?
C44 C39 C40 119.5(4) . . ?
C44 C39 P2 120.8(3) . . ?
C40 C39 P2 119.7(3) . . ?
C41 C40 C39 119.7(4) . . ?
C41 C40 H40 120.2 . . ?
C39 C40 H40 120.2 . . ?
C42 C41 C40 120.7(4) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C43 C42 C41 119.6(4) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C42 C43 C44 120.3(4) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C43 C44 C39 120.3(4) . . ?
C43 C44 H44 119.9 . . ?
C39 C44 H44 119.9 . . ?
C46 C45 C50 119.5(4) . . ?
C46 C45 P2 121.2(3) . . ?
C50 C45 P2 118.9(3) . . ?
C45 C46 C47 119.1(4) . . ?
C45 C46 H46 120.5 . . ?
C47 C46 H46 120.5 . . ?
C48 C47 C46 120.9(4) . . ?
C48 C47 H47 119.6 . . ?
C46 C47 H47 119.6 . . ?
C47 C48 C49 120.3(4) . . ?
C47 C48 H48 119.9 . . ?
C49 C48 H48 119.9 . . ?
C48 C49 C50 119.6(4) . . ?
C48 C49 H49 120.2 . . ?
C50 C49 H49 120.2 . . ?
C49 C50 C45 120.7(4) . . ?
C49 C50 H50 119.7 . . ?
C45 C50 H50 119.7 . . ?
Cl2 C51 Cl1 111.6(4) . . ?
Cl1 C51 Cl2B 117.5(4) . . ?
Cl2 C51 H51A 109.3 . . ?
Cl1 C51 H51A 109.3 . . ?
Cl2 C51 H51B 109.3 . . ?
Cl1 C51 H51B 109.3 . . ?
H51A C51 H51B 108.0 . . ?
Cl1 C51 H51C 107.9 . . ?
Cl2B C51 H51C 107.9 . . ?
Cl1 C51 H51D 107.9 . . ?
Cl2B C51 H51D 107.9 . . ?
H51C C51 H51D 107.2 . . ?
C53 C52 H52A 109.5 . . ?
C53 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C53 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C52 C53 C54 113.3 . . ?
C52 C53 H53A 108.9 . . ?
C54 C53 H53A 108.9 . . ?
C52 C53 H53B 108.9 . . ?
C54 C53 H53B 108.9 . . ?
H53A C53 H53B 107.7 . . ?
C53 C54 C55 113.8 . . ?
C53 C54 H54A 108.8 . . ?
C55 C54 H54A 108.8 . . ?
C53 C54 H54B 108.8 . . ?
C55 C54 H54B 108.8 . . ?
H54A C54 H54B 107.7 . . ?
C56 C55 C54 113.3 . . ?
C56 C55 H55A 108.9 . . ?
C54 C55 H55A 108.9 . . ?
C56 C55 H55B 108.9 . . ?
C54 C55 H55B 108.9 . . ?
H55A C55 H55B 107.7 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
Cl3 C57 Cl4 112.9 . . ?
Cl3 C57 H57A 109.0 . . ?
Cl4 C57 H57A 109.0 . . ?
Cl3 C57 H57B 109.0 . . ?
Cl4 C57 H57B 109.0 . . ?
H57A C57 H57B 107.8 . . ?

_refine_diff_density_max         0.739
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.091


loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 2.00 2.00 0.0420
2.00 2.00 -1.00 0.0520
-2.00 -2.00 1.00 0.0230
0.00 0.00 -1.00 0.0480
2.00 0.00 1.00 0.0300
-2.00 0.00 -1.00 0.0070
-1.00 1.00 2.00 0.0430
1.00 -1.00 -2.00 0.0560
0.00 -1.00 -2.00 0.0450
-1.00 0.00 2.00 0.0320
0.00 3.00 -2.00 0.0530
####################################################################### 
# 
# 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_dm96csa
_database_code_depnum_ccdc_archive 'CCDC 1834880'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
? 
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C38 H32 Cl2 N2 Ni O2 P2, C H2 Cl1.68, C H2 Cl2, 0.321(Cl)'
_chemical_formula_sum            'C40 H36 Cl6 N2 Ni O2 P2'
_chemical_formula_structural     ?
_chemical_formula_weight         910.06

_chemical_absolute_configuration ?
_chemical_formula_iupac          ?
_chemical_formula_analytical     ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   14.1984(3)
_cell_length_b                   14.3857(3)
_cell_length_c                   20.3796(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.7539(10)
_cell_angle_gamma                90
_cell_volume                     4006.25(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9953
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      28.40
_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.173
_exptl_crystal_id                dm96csa

_exptl_crystal_preparation       
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (3 -1 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_absorpt_coefficient_mu    1.003
_shelx_estimated_absorpt_T_min   0.738
_shelx_estimated_absorpt_T_max   0.846
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.7989
_exptl_absorpt_correction_T_max  0.9357
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker, 2014)'

_exptl_absorpt_special_details   ?
_exptl_special_details           
; 
One distinct cell was identified using APEX2 (Bruker, 2014). 
Eleven frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by 
integration using SADABS v2014/5 (Bruker, 2014). 
No decay correction was applied. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dm96csa
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_source                   ?
_diffrn_standards_number         ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_time  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            118162

_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.514
_diffrn_reflns_theta_max         28.433
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10070
_reflns_number_gt                8826
_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       'APEX2 V2014.9-0 (Bruker, 2014)'

_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/5, 
(Bruker, 2012 & 2014) 
;
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by direct methods (Sheldrick, 2015). 
Systematic conditions suggested the unambiguous space group. 
The space group choice was confirmed by successful convergence of the 
full-matrix least-squares refinement on F².  The highest peaks in 
the final difference Fourier map were in the vicinity of atoms Cl6 and 
Cl4B; the final map had no other significant features.  A final analysis of 
variance between observed and calculated structure factors showed little 
dependence on amplitude or resolution. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0271P)²+4.6165P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10070
_refine_ls_number_parameters     491
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0731
_refine_ls_wR_factor_gt          0.0690
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_ls_abs_structure_details ?
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 0.32207(2) 0.05933(2) 0.28564(2) 0.00924(5) Uani 1 1 d . . . . .
P1 P 0.23518(3) -0.08202(3) 0.29628(2) 0.01022(8) Uani 1 1 d . . . . .
P2 P 0.21748(3) 0.13561(3) 0.18744(2) 0.00968(8) Uani 1 1 d . . . . .
Cl1 Cl 0.42149(3) -0.03420(3) 0.22971(2) 0.01338(8) Uani 1 1 d . . . . .
Cl2 Cl 0.25343(3) 0.16477(3) 0.35300(2) 0.01392(8) Uani 1 1 d . . . . .
O1 O 0.52027(8) 0.13766(9) 0.29856(6) 0.0167(2) Uani 1 1 d . . . . .
H1 H 0.5165(17) 0.0845(17) 0.2886(12) 0.025 Uiso 1 1 d . U . . .
O2 O 0.44901(9) 0.09161(9) 0.42639(6) 0.0182(2) Uani 1 1 d . . . . .
H2 H 0.4074(18) 0.1292(17) 0.4146(12) 0.027 Uiso 1 1 d . U . . .
N1 N 0.41095(10) 0.01756(10) 0.38174(7) 0.0136(3) Uani 1 1 d . . . . .
N2 N 0.42146(9) 0.16471(10) 0.27784(7) 0.0128(3) Uani 1 1 d . . . . .
C1 C 0.33046(11) -0.17125(11) 0.32373(8) 0.0126(3) Uani 1 1 d . . . . .
C2 C 0.41797(12) -0.15101(11) 0.37451(8) 0.0136(3) Uani 1 1 d . . . . .
C3 C 0.48647(13) -0.22187(12) 0.39808(9) 0.0182(3) Uani 1 1 d . . . . .
H3A H 0.5442 -0.2087 0.4333 0.022 Uiso 1 1 calc R U . . .
C4 C 0.47185(13) -0.31075(12) 0.37114(10) 0.0207(4) Uani 1 1 d . . . . .
H4A H 0.5194 -0.3579 0.3872 0.025 Uiso 1 1 calc R U . . .
C5 C 0.38714(13) -0.33003(12) 0.32054(10) 0.0203(4) Uani 1 1 d . . . . .
H5A H 0.3768 -0.3906 0.3014 0.024 Uiso 1 1 calc R U . . .
C6 C 0.31677(12) -0.26109(12) 0.29742(9) 0.0162(3) Uani 1 1 d . . . . .
H6A H 0.2585 -0.2757 0.2631 0.019 Uiso 1 1 calc R U . . .
C7 C 0.44379(12) -0.06073(12) 0.40760(8) 0.0152(3) Uani 1 1 d . . . . .
H7A H 0.4885 -0.0603 0.4518 0.018 Uiso 1 1 calc R U . . .
C8 C 0.16569(12) -0.09614(12) 0.35929(8) 0.0132(3) Uani 1 1 d . . . . .
C9 C 0.15343(12) -0.18388(12) 0.38544(8) 0.0158(3) Uani 1 1 d . . . . .
H9A H 0.1851 -0.2364 0.3728 0.019 Uiso 1 1 calc R U . . .
C10 C 0.09523(13) -0.19479(13) 0.42983(9) 0.0191(3) Uani 1 1 d . . . . .
H10A H 0.0870 -0.2547 0.4471 0.023 Uiso 1 1 calc R U . . .
C11 C 0.04931(14) -0.11864(14) 0.44889(9) 0.0236(4) Uani 1 1 d . . . . .
H11A H 0.0097 -0.1261 0.4794 0.028 Uiso 1 1 calc R U . . .
C12 C 0.06114(15) -0.03161(14) 0.42350(10) 0.0258(4) Uani 1 1 d . . . . .
H12A H 0.0296 0.0206 0.4367 0.031 Uiso 1 1 calc R U . . .
C13 C 0.11895(13) -0.01983(13) 0.37869(9) 0.0194(3) Uani 1 1 d . . . . .
H13A H 0.1265 0.0402 0.3614 0.023 Uiso 1 1 calc R U . . .
C14 C 0.15249(11) -0.12918(11) 0.21865(8) 0.0120(3) Uani 1 1 d . . . . .
C15 C 0.05521(12) -0.15144(12) 0.21399(9) 0.0164(3) Uani 1 1 d . . . . .
H15A H 0.0312 -0.1460 0.2530 0.020 Uiso 1 1 calc R U . . .
C16 C -0.00690(13) -0.18159(13) 0.15246(9) 0.0208(4) Uani 1 1 d . . . . .
H16A H -0.0729 -0.1971 0.1498 0.025 Uiso 1 1 calc R U . . .
C17 C 0.02722(13) -0.18904(13) 0.09517(9) 0.0210(4) Uani 1 1 d . . . . .
H17A H -0.0154 -0.2092 0.0531 0.025 Uiso 1 1 calc R U . . .
C18 C 0.12376(13) -0.16694(13) 0.09932(9) 0.0208(4) Uani 1 1 d . . . . .
H18A H 0.1473 -0.1722 0.0601 0.025 Uiso 1 1 calc R U . . .
C19 C 0.18606(12) -0.13718(12) 0.16053(9) 0.0170(3) Uani 1 1 d . . . . .
H19A H 0.2521 -0.1221 0.1629 0.020 Uiso 1 1 calc R U . . .
C20 C 0.22663(11) 0.25921(11) 0.21073(8) 0.0116(3) Uani 1 1 d . . . . .
C21 C 0.31854(11) 0.29986(11) 0.24123(8) 0.0125(3) Uani 1 1 d . . . . .
C22 C 0.32409(12) 0.39522(12) 0.25518(9) 0.0168(3) Uani 1 1 d . . . . .
H22A H 0.3861 0.4232 0.2741 0.020 Uiso 1 1 calc R U . . .
C23 C 0.24024(13) 0.44945(12) 0.24182(10) 0.0202(3) Uani 1 1 d . . . . .
H23A H 0.2448 0.5138 0.2527 0.024 Uiso 1 1 calc R U . . .
C24 C 0.15013(13) 0.40955(12) 0.21257(9) 0.0188(3) Uani 1 1 d . . . . .
H24A H 0.0925 0.4464 0.2035 0.023 Uiso 1 1 calc R U . . .
C25 C 0.14383(12) 0.31540(11) 0.19633(8) 0.0149(3) Uani 1 1 d . . . . .
H25A H 0.0817 0.2890 0.1750 0.018 Uiso 1 1 calc R U . . .
C26 C 0.41250(11) 0.25053(11) 0.26117(8) 0.0132(3) Uani 1 1 d . . . . .
H26A H 0.4701 0.2845 0.2617 0.016 Uiso 1 1 calc R U . . .
C27 C 0.08672(11) 0.10988(11) 0.16778(8) 0.0119(3) Uani 1 1 d . . . . .
C28 C 0.03724(12) 0.12380(11) 0.21774(8) 0.0149(3) Uani 1 1 d . . . . .
H28A H 0.0712 0.1489 0.2608 0.018 Uiso 1 1 calc R U . . .
C29 C -0.06125(12) 0.10116(12) 0.20472(9) 0.0182(3) Uani 1 1 d . . . . .
H29A H -0.0947 0.1120 0.2386 0.022 Uiso 1 1 calc R U . . .
C30 C -0.11091(12) 0.06287(13) 0.14251(10) 0.0204(4) Uani 1 1 d . . . . .
H30A H -0.1782 0.0471 0.1339 0.025 Uiso 1 1 calc R U . . .
C31 C -0.06235(13) 0.04759(13) 0.09296(9) 0.0202(3) Uani 1 1 d . . . . .
H31A H -0.0963 0.0209 0.0505 0.024 Uiso 1 1 calc R U . . .
C32 C 0.03614(12) 0.07126(11) 0.10531(9) 0.0155(3) Uani 1 1 d . . . . .
H32A H 0.0690 0.0611 0.0711 0.019 Uiso 1 1 calc R U . . .
C33 C 0.23986(11) 0.13952(11) 0.10324(8) 0.0121(3) Uani 1 1 d . . . . .
C34 C 0.21558(13) 0.21862(12) 0.06244(9) 0.0181(3) Uani 1 1 d . . . . .
H34A H 0.1904 0.2719 0.0795 0.022 Uiso 1 1 calc R U . . .
C35 C 0.22803(14) 0.21999(13) -0.00295(9) 0.0213(4) Uani 1 1 d . . . . .
H35A H 0.2116 0.2742 -0.0303 0.026 Uiso 1 1 calc R U . . .
C36 C 0.26439(13) 0.14254(13) -0.02822(9) 0.0197(3) Uani 1 1 d . . . . .
H36A H 0.2724 0.1434 -0.0730 0.024 Uiso 1 1 calc R U . . .
C37 C 0.28907(13) 0.06366(13) 0.01191(9) 0.0197(3) Uani 1 1 d . . . . .
H37A H 0.3141 0.0105 -0.0054 0.024 Uiso 1 1 calc R U . . .
C38 C 0.27721(12) 0.06223(12) 0.07769(8) 0.0165(3) Uani 1 1 d . . . . .
H38A H 0.2947 0.0083 0.1052 0.020 Uiso 1 1 calc R U . . .
Cl3 Cl 0.32382(4) 0.80135(4) 0.00667(3) 0.03205(11) Uani 1 1 d D . . . .
C39 C 0.4142(3) 0.8117(6) 0.0847(2) 0.0254(8) Uani 0.6783(13) 1 d D . P A 1
H39A H 0.4198 0.7527 0.1104 0.030 Uiso 0.6783(13) 1 calc R U P A 1
H39B H 0.3960 0.8615 0.1125 0.030 Uiso 0.6783(13) 1 calc R U P A 1
Cl4 Cl 0.52687(6) 0.83862(8) .06848(4) .0440(2) Uani 0.6783(13) 1 d D . P A 1
C39B C 0.4278(9) 0.8189(13) 0.0766(5) 0.0254(8) Uani 0.3217(13) 1 d D . P A 2
H39C H 0.4052 0.8346 0.1172 0.030 Uiso 0.3217(13) 1 calc R U P A 2
H39D H 0.4645 0.7597 0.0864 0.030 Uiso 0.3217(13) 1 calc R U P A 2
Cl4B Cl .50832(13) .90651(18) .06514(10) .0440(2) Uani 0.321(1) 1 d D . P A 2
Cl5 Cl 0.23827(4) 0.62189(4) 0.11179(3) 0.03539(12) Uani 1 1 d . . . . .
Cl6 Cl 0.29558(5) 0.44536(4) 0.06412(4) 0.04604(15) Uani 1 1 d . . . . .
C40 C 0.29881(16) 0.56726(14) 0.05751(11) 0.0291(4) Uani 1 1 d . . . . .
H40A H 0.3678 0.5883 0.0693 0.035 Uiso 1 1 calc R U . . .
H40B H 0.2674 0.5859 0.0098 0.035 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.1064(14) . ?
Ni1 N1 2.1089(14) . ?
Ni1 P2 2.4085(4) . ?
Ni1 P1 2.4184(4) . ?
Ni1 Cl2 2.4211(4) . ?
Ni1 Cl1 2.4446(4) . ?
P1 C14 1.8256(16) . ?
P1 C8 1.8308(16) . ?
P1 C1 1.8384(16) . ?
P2 C27 1.8277(16) . ?
P2 C33 1.8289(16) . ?
P2 C20 1.8358(16) . ?
O1 N2 1.4058(17) . ?
O1 H1 0.79(2) . ?
O2 N1 1.4099(17) . ?
O2 H2 0.79(2) . ?
N1 C7 1.277(2) . ?
N2 C26 1.278(2) . ?
C1 C6 1.392(2) . ?
C1 C2 1.415(2) . ?
C2 C3 1.401(2) . ?
C2 C7 1.463(2) . ?
C3 C4 1.385(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.383(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.396(2) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C13 1.395(2) . ?
C8 C9 1.399(2) . ?
C9 C10 1.390(2) . ?
C9 H9A 0.9500 . ?
C10 C11 1.383(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.382(3) . ?
C11 H11A 0.9500 . ?
C12 C13 1.394(2) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C15 1.396(2) . ?
C14 C19 1.396(2) . ?
C15 C16 1.392(2) . ?
C15 H15A 0.9500 . ?
C16 C17 1.384(3) . ?
C16 H16A 0.9500 . ?
C17 C18 1.387(3) . ?
C17 H17A 0.9500 . ?
C18 C19 1.387(2) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 C25 1.391(2) . ?
C20 C21 1.411(2) . ?
C21 C22 1.399(2) . ?
C21 C26 1.468(2) . ?
C22 C23 1.387(2) . ?
C22 H22A 0.9500 . ?
C23 C24 1.381(2) . ?
C23 H23A 0.9500 . ?
C24 C25 1.391(2) . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 C32 1.396(2) . ?
C27 C28 1.400(2) . ?
C28 C29 1.389(2) . ?
C28 H28A 0.9500 . ?
C29 C30 1.387(3) . ?
C29 H29A 0.9500 . ?
C30 C31 1.386(3) . ?
C30 H30A 0.9500 . ?
C31 C32 1.394(2) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C33 C38 1.392(2) . ?
C33 C34 1.396(2) . ?
C34 C35 1.391(2) . ?
C34 H34A 0.9500 . ?
C35 C36 1.385(3) . ?
C35 H35A 0.9500 . ?
C36 C37 1.387(3) . ?
C36 H36A 0.9500 . ?
C37 C38 1.396(2) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
Cl3 C39 1.757(4) . ?
Cl3 C39B 1.770(7) . ?
C39 Cl4 1.763(4) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39B Cl4B 1.760(7) . ?
C39B H39C 0.9900 . ?
C39B H39D 0.9900 . ?
Cl5 C40 1.760(2) . ?
Cl6 C40 1.760(2) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?

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
N2 Ni1 N1 91.77(5) . . ?
N2 Ni1 P2 83.34(4) . . ?
N1 Ni1 P2 168.52(4) . . ?
N2 Ni1 P1 168.64(4) . . ?
N1 Ni1 P1 82.44(4) . . ?
P2 Ni1 P1 104.073(15) . . ?
N2 Ni1 Cl2 88.45(4) . . ?
N1 Ni1 Cl2 83.31(4) . . ?
P2 Ni1 Cl2 86.177(15) . . ?
P1 Ni1 Cl2 100.505(15) . . ?
N2 Ni1 Cl1 82.96(4) . . ?
N1 Ni1 Cl1 90.03(4) . . ?
P2 Ni1 Cl1 99.622(15) . . ?
P1 Ni1 Cl1 87.263(15) . . ?
Cl2 Ni1 Cl1 168.966(16) . . ?
C14 P1 C8 102.96(7) . . ?
C14 P1 C1 104.55(7) . . ?
C8 P1 C1 101.60(7) . . ?
C14 P1 Ni1 117.29(5) . . ?
C8 P1 Ni1 122.78(5) . . ?
C1 P1 Ni1 105.27(5) . . ?
C27 P2 C33 103.03(7) . . ?
C27 P2 C20 104.44(7) . . ?
C33 P2 C20 101.22(7) . . ?
C27 P2 Ni1 116.76(5) . . ?
C33 P2 Ni1 124.65(5) . . ?
C20 P2 Ni1 104.01(5) . . ?
N2 O1 H1 101.4(17) . . ?
N1 O2 H2 101.4(18) . . ?
C7 N1 O2 111.54(13) . . ?
C7 N1 Ni1 133.95(11) . . ?
O2 N1 Ni1 114.33(10) . . ?
C26 N2 O1 111.50(13) . . ?
C26 N2 Ni1 134.04(11) . . ?
O1 N2 Ni1 114.37(10) . . ?
C6 C1 C2 118.41(15) . . ?
C6 C1 P1 121.10(12) . . ?
C2 C1 P1 120.43(12) . . ?
C3 C2 C1 119.42(15) . . ?
C3 C2 C7 115.09(15) . . ?
C1 C2 C7 125.46(15) . . ?
C4 C3 C2 121.37(16) . . ?
C4 C3 H3A 119.3 . . ?
C2 C3 H3A 119.3 . . ?
C5 C4 C3 119.15(16) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
C4 C5 C6 120.46(16) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
C1 C6 C5 121.14(16) . . ?
C1 C6 H6A 119.4 . . ?
C5 C6 H6A 119.4 . . ?
N1 C7 C2 125.09(15) . . ?
N1 C7 H7A 117.5 . . ?
C2 C7 H7A 117.5 . . ?
C13 C8 C9 118.96(15) . . ?
C13 C8 P1 120.01(13) . . ?
C9 C8 P1 120.92(13) . . ?
C10 C9 C8 120.48(16) . . ?
C10 C9 H9A 119.8 . . ?
C8 C9 H9A 119.8 . . ?
C11 C10 C9 120.14(17) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C12 C11 C10 119.85(16) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C11 C12 C13 120.55(17) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C12 C13 C8 120.01(17) . . ?
C12 C13 H13A 120.0 . . ?
C8 C13 H13A 120.0 . . ?
C15 C14 C19 118.87(15) . . ?
C15 C14 P1 122.41(12) . . ?
C19 C14 P1 118.58(12) . . ?
C16 C15 C14 120.39(16) . . ?
C16 C15 H15A 119.8 . . ?
C14 C15 H15A 119.8 . . ?
C17 C16 C15 120.18(16) . . ?
C17 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
C16 C17 C18 119.81(16) . . ?
C16 C17 H17A 120.1 . . ?
C18 C17 H17A 120.1 . . ?
C19 C18 C17 120.27(16) . . ?
C19 C18 H18A 119.9 . . ?
C17 C18 H18A 119.9 . . ?
C18 C19 C14 120.48(16) . . ?
C18 C19 H19A 119.8 . . ?
C14 C19 H19A 119.8 . . ?
C25 C20 C21 118.67(14) . . ?
C25 C20 P2 120.79(12) . . ?
C21 C20 P2 120.50(12) . . ?
C22 C21 C20 119.37(15) . . ?
C22 C21 C26 114.90(14) . . ?
C20 C21 C26 125.73(14) . . ?
C23 C22 C21 120.91(15) . . ?
C23 C22 H22A 119.5 . . ?
C21 C22 H22A 119.5 . . ?
C24 C23 C22 119.74(16) . . ?
C24 C23 H23A 120.1 . . ?
C22 C23 H23A 120.1 . . ?
C23 C24 C25 119.96(16) . . ?
C23 C24 H24A 120.0 . . ?
C25 C24 H24A 120.0 . . ?
C20 C25 C24 121.30(15) . . ?
C20 C25 H25A 119.4 . . ?
C24 C25 H25A 119.4 . . ?
N2 C26 C21 123.94(14) . . ?
N2 C26 H26A 118.0 . . ?
C21 C26 H26A 118.0 . . ?
C32 C27 C28 119.01(15) . . ?
C32 C27 P2 121.40(12) . . ?
C28 C27 P2 119.48(12) . . ?
C29 C28 C27 120.37(15) . . ?
C29 C28 H28A 119.8 . . ?
C27 C28 H28A 119.8 . . ?
C30 C29 C28 120.22(16) . . ?
C30 C29 H29A 119.9 . . ?
C28 C29 H29A 119.9 . . ?
C31 C30 C29 119.93(16) . . ?
C31 C30 H30A 120.0 . . ?
C29 C30 H30A 120.0 . . ?
C30 C31 C32 120.18(16) . . ?
C30 C31 H31A 119.9 . . ?
C32 C31 H31A 119.9 . . ?
C31 C32 C27 120.28(16) . . ?
C31 C32 H32A 119.9 . . ?
C27 C32 H32A 119.9 . . ?
C38 C33 C34 119.06(15) . . ?
C38 C33 P2 120.48(12) . . ?
C34 C33 P2 120.40(13) . . ?
C35 C34 C33 120.46(16) . . ?
C35 C34 H34A 119.8 . . ?
C33 C34 H34A 119.8 . . ?
C36 C35 C34 120.13(17) . . ?
C36 C35 H35A 119.9 . . ?
C34 C35 H35A 119.9 . . ?
C35 C36 C37 119.94(16) . . ?
C35 C36 H36A 120.0 . . ?
C37 C36 H36A 120.0 . . ?
C36 C37 C38 120.09(17) . . ?
C36 C37 H37A 120.0 . . ?
C38 C37 H37A 120.0 . . ?
C33 C38 C37 120.33(16) . . ?
C33 C38 H38A 119.8 . . ?
C37 C38 H38A 119.8 . . ?
Cl3 C39 Cl4 109.0(2) . . ?
Cl3 C39 H39A 109.9 . . ?
Cl4 C39 H39A 109.9 . . ?
Cl3 C39 H39B 109.9 . . ?
Cl4 C39 H39B 109.9 . . ?
H39A C39 H39B 108.3 . . ?
Cl4B C39B Cl3 115.1(5) . . ?
Cl4B C39B H39C 108.5 . . ?
Cl3 C39B H39C 108.5 . . ?
Cl4B C39B H39D 108.5 . . ?
Cl3 C39B H39D 108.5 . . ?
H39C C39B H39D 107.5 . . ?
Cl5 C40 Cl6 111.69(12) . . ?
Cl5 C40 H40A 109.3 . . ?
Cl6 C40 H40A 109.3 . . ?
Cl5 C40 H40B 109.3 . . ?
Cl6 C40 H40B 109.3 . . ?
H40A C40 H40B 107.9 . . ?

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
C14 P1 C1 C6 -15.64(15) . . . . ?
C8 P1 C1 C6 91.21(14) . . . . ?
Ni1 P1 C1 C6 -139.82(12) . . . . ?
C14 P1 C1 C2 167.12(13) . . . . ?
C8 P1 C1 C2 -86.03(14) . . . . ?
Ni1 P1 C1 C2 42.94(13) . . . . ?
C6 C1 C2 C3 -1.8(2) . . . . ?
P1 C1 C2 C3 175.50(12) . . . . ?
C6 C1 C2 C7 -179.79(15) . . . . ?
P1 C1 C2 C7 -2.5(2) . . . . ?
C1 C2 C3 C4 2.1(3) . . . . ?
C7 C2 C3 C4 -179.68(16) . . . . ?
C2 C3 C4 C5 -0.9(3) . . . . ?
C3 C4 C5 C6 -0.7(3) . . . . ?
C2 C1 C6 C5 0.3(2) . . . . ?
P1 C1 C6 C5 -176.99(13) . . . . ?
C4 C5 C6 C1 1.0(3) . . . . ?
O2 N1 C7 C2 179.53(15) . . . . ?
Ni1 N1 C7 C2 -5.8(3) . . . . ?
C3 C2 C7 N1 156.88(17) . . . . ?
C1 C2 C7 N1 -25.1(3) . . . . ?
C14 P1 C8 C13 -102.48(14) . . . . ?
C1 P1 C8 C13 149.43(14) . . . . ?
Ni1 P1 C8 C13 32.57(16) . . . . ?
C14 P1 C8 C9 73.49(14) . . . . ?
C1 P1 C8 C9 -34.60(15) . . . . ?
Ni1 P1 C8 C9 -151.46(11) . . . . ?
C13 C8 C9 C10 0.3(2) . . . . ?
P1 C8 C9 C10 -175.75(13) . . . . ?
C8 C9 C10 C11 -0.4(3) . . . . ?
C9 C10 C11 C12 0.2(3) . . . . ?
C10 C11 C12 C13 0.1(3) . . . . ?
C11 C12 C13 C8 -0.2(3) . . . . ?
C9 C8 C13 C12 0.0(3) . . . . ?
P1 C8 C13 C12 176.09(14) . . . . ?
C8 P1 C14 C15 10.19(16) . . . . ?
C1 P1 C14 C15 116.04(14) . . . . ?
Ni1 P1 C14 C15 -127.86(13) . . . . ?
C8 P1 C14 C19 -174.31(13) . . . . ?
C1 P1 C14 C19 -68.47(14) . . . . ?
Ni1 P1 C14 C19 47.63(15) . . . . ?
C19 C14 C15 C16 0.4(3) . . . . ?
P1 C14 C15 C16 175.85(14) . . . . ?
C14 C15 C16 C17 -0.5(3) . . . . ?
C15 C16 C17 C18 0.4(3) . . . . ?
C16 C17 C18 C19 -0.2(3) . . . . ?
C17 C18 C19 C14 0.1(3) . . . . ?
C15 C14 C19 C18 -0.1(3) . . . . ?
P1 C14 C19 C18 -175.80(14) . . . . ?
C27 P2 C20 C25 -14.26(15) . . . . ?
C33 P2 C20 C25 92.50(14) . . . . ?
Ni1 P2 C20 C25 -137.18(12) . . . . ?
C27 P2 C20 C21 168.24(13) . . . . ?
C33 P2 C20 C21 -84.99(13) . . . . ?
Ni1 P2 C20 C21 45.32(13) . . . . ?
C25 C20 C21 C22 -0.9(2) . . . . ?
P2 C20 C21 C22 176.64(12) . . . . ?
C25 C20 C21 C26 178.50(15) . . . . ?
P2 C20 C21 C26 -4.0(2) . . . . ?
C20 C21 C22 C23 2.4(2) . . . . ?
C26 C21 C22 C23 -177.03(16) . . . . ?
C21 C22 C23 C24 -1.8(3) . . . . ?
C22 C23 C24 C25 -0.3(3) . . . . ?
C21 C20 C25 C24 -1.2(2) . . . . ?
P2 C20 C25 C24 -178.76(13) . . . . ?
C23 C24 C25 C20 1.9(3) . . . . ?
O1 N2 C26 C21 -176.33(14) . . . . ?
Ni1 N2 C26 C21 -0.2(3) . . . . ?
C22 C21 C26 N2 151.68(16) . . . . ?
C20 C21 C26 N2 -27.8(3) . . . . ?
C33 P2 C27 C32 19.58(15) . . . . ?
C20 P2 C27 C32 125.00(14) . . . . ?
Ni1 P2 C27 C32 -120.81(12) . . . . ?
C33 P2 C27 C28 -164.35(13) . . . . ?
C20 P2 C27 C28 -58.93(14) . . . . ?
Ni1 P2 C27 C28 55.26(14) . . . . ?
C32 C27 C28 C29 -1.3(2) . . . . ?
P2 C27 C28 C29 -177.42(13) . . . . ?
C27 C28 C29 C30 1.2(3) . . . . ?
C28 C29 C30 C31 -0.4(3) . . . . ?
C29 C30 C31 C32 -0.5(3) . . . . ?
C30 C31 C32 C27 0.5(3) . . . . ?
C28 C27 C32 C31 0.4(2) . . . . ?
P2 C27 C32 C31 176.50(13) . . . . ?
C27 P2 C33 C38 -97.48(14) . . . . ?
C20 P2 C33 C38 154.66(13) . . . . ?
Ni1 P2 C33 C38 38.73(15) . . . . ?
C27 P2 C33 C34 79.62(14) . . . . ?
C20 P2 C33 C34 -28.25(15) . . . . ?
Ni1 P2 C33 C34 -144.17(11) . . . . ?
C38 C33 C34 C35 0.4(3) . . . . ?
P2 C33 C34 C35 -176.78(13) . . . . ?
C33 C34 C35 C36 0.2(3) . . . . ?
C34 C35 C36 C37 -0.4(3) . . . . ?
C35 C36 C37 C38 0.1(3) . . . . ?
C34 C33 C38 C37 -0.7(2) . . . . ?
P2 C33 C38 C37 176.41(13) . . . . ?
C36 C37 C38 C33 0.5(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 Cl1 0.79(2) 2.30(2) 2.9966(13) 147(2) .
O2 H2 Cl2 0.79(2) 2.26(2) 2.9667(13) 149(2) .

_refine_diff_density_max         1.191
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.066


loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2.00 -2.00 1.00 0.1020
-1.00 1.00 1.00 0.1630
1.00 -1.00 -1.00 0.1000
1.00 -2.00 1.00 0.1560
-1.00 2.00 -1.00 0.1320
1.00 4.00 -3.00 0.0220
-1.00 0.00 -1.00 0.1360
1.00 1.00 4.00 0.1230
2.00 -3.00 -4.00 0.0940
-2.00 3.00 4.00 0.1630
0.00 -2.00 -3.00 0.1140
-1.00 -2.00 1.00 0.0880
1.00 2.00 -1.00 0.0250
3.00 4.00 -4.00 0.0200
-2.00 -3.00 3.00 0.0900
####################################################################### 
# 
# 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_dd49fs
_database_code_depnum_ccdc_archive 'CCDC 1834878'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
? 
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H32 Cl4 N2 Ni2 O2 P2'
_chemical_formula_sum            'C38 H32 Cl4 N2 Ni2 O2 P2'
_chemical_formula_structural     ?
_chemical_formula_weight         869.81

_chemical_absolute_configuration ?
_chemical_formula_iupac          ?
_chemical_formula_analytical     ?
_chemical_compound_source        ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9955(7)
_cell_length_b                   10.6309(5)
_cell_length_c                   13.5275(7)
_cell_angle_alpha                90
_cell_angle_beta                 91.069(2)
_cell_angle_gamma                90
_cell_volume                     1868.55(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    15364
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      25.38
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.054
_exptl_crystal_id                dd49fs

_exptl_crystal_preparation       
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 5 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_absorpt_coefficient_mu    1.416
_shelx_estimated_absorpt_T_min   0.812
_shelx_estimated_absorpt_T_max   0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6887
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS V2014/7 (Krause et al., 2015)'

_exptl_absorpt_special_details   ?
_exptl_special_details           
; 
One distinct cell was identified using APEX3 (Bruker, 2016). 
Six frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by 
the multi-scan method using SADABS v2014/7 (Krause et al., 2015). 
No decay correction was applied. 
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dd49fs
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source                   ?
_diffrn_standards_number         ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_time  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25454

_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.437
_diffrn_reflns_theta_max         25.386
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3434
_reflns_number_gt                3098
_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       'APEX3 V2016.9-0 (Bruker, 2016)'

_computing_cell_refinement       'SAINT V8.34A (Bruker, 2014)'
_computing_data_reduction        
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/7 (Krause et al., 2015), 
;
_computing_structure_solution    'SHELXT-2014-7 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by intrinsic methods (Sheldrick, 2015b). 
Systematic conditions suggested the unambiguous space group. 
The space group choice was confirmed by successful convergence of the 
full-matrix least-squares refinement on F².  The highest peaks in 
the final difference Fourier map were in the vicinity of atom O1; the 
final map had no other significant features.  A final analysis of 
variance between observed and calculated structure factors showed little 
dependence on amplitude or resolution. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+2.1280P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3434
_refine_ls_number_parameters     227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0675
_refine_ls_wR_factor_gt          0.0650
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_ls_abs_structure_details ?
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 0.46794(2) 0.54058(2) 0.61968(2) 0.01440(9) Uani 1 1 d . . . . .
Cl1 Cl 0.40503(4) 0.39230(5) 0.72754(4) 0.02265(13) Uani 1 1 d . . . . .
Cl2 Cl 0.42934(4) 0.61328(5) 0.46094(4) 0.01672(12) Uani 1 1 d . . . . .
P1 P 0.59514(4) 0.67772(5) 0.67283(4) 0.01302(12) Uani 1 1 d . . . . .
O1 O 0.26934(13) 0.61419(17) 0.70304(14) 0.0319(4) Uani 1 1 d . . . . .
H1 H 0.2776 0.5375 0.7157 0.048 Uiso 1 1 calc R U . . .
N1 N 0.36381(14) 0.66740(18) 0.67756(13) 0.0205(4) Uani 1 1 d . . . . .
C1 C 0.36218(17) 0.7875(2) 0.68467(15) 0.0203(5) Uani 1 1 d . . . . .
H1A H 0.3008 0.8249 0.7079 0.024 Uiso 1 1 calc R U . . .
C2 C 0.44642(17) 0.8720(2) 0.66020(15) 0.0175(4) Uani 1 1 d . . . . .
C3 C 0.55063(16) 0.83779(19) 0.64738(14) 0.0148(4) Uani 1 1 d . . . . .
C4 C 0.62010(17) 0.9297(2) 0.61902(15) 0.0188(4) Uani 1 1 d . . . . .
H4 H 0.6899 0.9073 0.6091 0.023 Uiso 1 1 calc R U . . .
C5 C 0.58964(19) 1.0539(2) 0.60485(16) 0.0224(5) Uani 1 1 d . . . . .
H5 H 0.6380 1.1149 0.5839 0.027 Uiso 1 1 calc R U . . .
C6 C 0.48926(19) 1.0885(2) 0.62118(16) 0.0246(5) Uani 1 1 d . . . . .
H6 H 0.4688 1.1738 0.6139 0.030 Uiso 1 1 calc R U . . .
C7 C 0.41797(18) 0.9977(2) 0.64834(16) 0.0228(5) Uani 1 1 d . . . . .
H7 H 0.3487 1.0218 0.6590 0.027 Uiso 1 1 calc R U . . .
C8 C 0.62048(15) 0.6767(2) 0.80542(15) 0.0178(4) Uani 1 1 d . . . . .
C9 C 0.60637(18) 0.5644(2) 0.85749(18) 0.0271(5) Uani 1 1 d . . . . .
H9 H 0.5853 0.4902 0.8236 0.033 Uiso 1 1 calc R U . . .
C10 C 0.62340(19) 0.5625(3) 0.95921(19) 0.0385(7) Uani 1 1 d . . . . .
H10 H 0.6138 0.4866 0.9950 0.046 Uiso 1 1 calc R U . . .
C11 C 0.65428(18) 0.6703(3) 1.00860(18) 0.0405(7) Uani 1 1 d . . . . .
H11 H 0.6642 0.6684 1.0783 0.049 Uiso 1 1 calc R U . . .
C12 C 0.67081(18) 0.7808(3) 0.95760(17) 0.0321(6) Uani 1 1 d . . . . .
H12 H 0.6938 0.8538 0.9919 0.039 Uiso 1 1 calc R U . . .
C13 C 0.65364(17) 0.7846(2) 0.85600(16) 0.0226(5) Uani 1 1 d . . . . .
H13 H 0.6644 0.8606 0.8208 0.027 Uiso 1 1 calc R U . . .
C14 C 0.71915(16) 0.67003(19) 0.61379(15) 0.0167(4) Uani 1 1 d . . . . .
C15 C 0.81214(18) 0.6681(2) 0.66637(17) 0.0279(5) Uani 1 1 d . . . . .
H15 H 0.8125 0.6697 0.7366 0.033 Uiso 1 1 calc R U . . .
C16 C 0.9045(2) 0.6637(3) 0.6162(2) 0.0394(7) Uani 1 1 d . . . . .
H16 H 0.9679 0.6629 0.6523 0.047 Uiso 1 1 calc R U . . .
C17 C 0.9044(2) 0.6606(3) 0.5145(2) 0.0412(7) Uani 1 1 d . . . . .
H17 H 0.9676 0.6559 0.4805 0.049 Uiso 1 1 calc R U . . .
C18 C 0.8116(2) 0.6645(3) 0.46166(19) 0.0352(6) Uani 1 1 d . . . . .
H18 H 0.8116 0.6642 0.3914 0.042 Uiso 1 1 calc R U . . .
C19 C 0.71934(18) 0.6686(2) 0.51102(16) 0.0241(5) Uani 1 1 d . . . . .
H19 H 0.6561 0.6705 0.4747 0.029 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.0740(19) . ?
Ni1 Cl1 2.3079(6) . ?
Ni1 P1 2.3089(6) . ?
Ni1 Cl2 2.3280(5) . ?
Ni1 Cl2 2.3877(5) 3_666 ?
Cl2 Ni1 2.3877(5) 3_666 ?
P1 C14 1.814(2) . ?
P1 C8 1.817(2) . ?
P1 C3 1.828(2) . ?
O1 N1 1.401(2) . ?
O1 H1 0.8400 . ?
N1 C1 1.281(3) . ?
C1 C2 1.459(3) . ?
C1 H1A 0.9500 . ?
C2 C7 1.395(3) . ?
C2 C3 1.416(3) . ?
C3 C4 1.390(3) . ?
C4 C5 1.390(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.377(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.392(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.399(3) . ?
C8 C9 1.400(3) . ?
C9 C10 1.390(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.390(3) . ?
C14 C15 1.391(3) . ?
C15 C16 1.391(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.384(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 Cl1 87.94(5) . . ?
N1 Ni1 P1 86.58(5) . . ?
Cl1 Ni1 P1 119.63(2) . . ?
N1 Ni1 Cl2 90.09(5) . . ?
Cl1 Ni1 Cl2 137.49(2) . . ?
P1 Ni1 Cl2 102.61(2) . . ?
N1 Ni1 Cl2 172.76(5) . 3_666 ?
Cl1 Ni1 Cl2 91.64(2) . 3_666 ?
P1 Ni1 Cl2 99.89(2) . 3_666 ?
Cl2 Ni1 Cl2 85.342(19) . 3_666 ?
Ni1 Cl2 Ni1 94.658(19) . 3_666 ?
C14 P1 C8 106.75(9) . . ?
C14 P1 C3 103.86(10) . . ?
C8 P1 C3 104.01(10) . . ?
C14 P1 Ni1 118.11(7) . . ?
C8 P1 Ni1 114.78(7) . . ?
C3 P1 Ni1 107.88(7) . . ?
N1 O1 H1 109.5 . . ?
C1 N1 O1 111.61(19) . . ?
C1 N1 Ni1 133.50(16) . . ?
O1 N1 Ni1 114.29(13) . . ?
N1 C1 C2 125.7(2) . . ?
N1 C1 H1A 117.2 . . ?
C2 C1 H1A 117.2 . . ?
C7 C2 C3 118.9(2) . . ?
C7 C2 C1 114.7(2) . . ?
C3 C2 C1 126.40(19) . . ?
C4 C3 C2 118.75(19) . . ?
C4 C3 P1 120.14(16) . . ?
C2 C3 P1 121.06(16) . . ?
C3 C4 C5 121.4(2) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C6 C5 C4 120.0(2) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 119.6(2) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C2 121.2(2) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
C13 C8 C9 119.7(2) . . ?
C13 C8 P1 121.76(17) . . ?
C9 C8 P1 118.58(17) . . ?
C10 C9 C8 119.4(2) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 120.4(2) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C10 120.7(2) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 119.7(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C8 120.2(2) . . ?
C12 C13 H13 119.9 . . ?
C8 C13 H13 119.9 . . ?
C19 C14 C15 119.6(2) . . ?
C19 C14 P1 117.32(16) . . ?
C15 C14 P1 123.10(17) . . ?
C16 C15 C14 120.1(2) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C17 C16 C15 120.2(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 119.9(2) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 120.2(2) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C14 120.0(2) . . ?
C18 C19 H19 120.0 . . ?
C14 C19 H19 120.0 . . ?

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
O1 N1 C1 C2 -177.65(19) . . . . ?
Ni1 N1 C1 C2 -7.3(3) . . . . ?
N1 C1 C2 C7 163.5(2) . . . . ?
N1 C1 C2 C3 -16.1(3) . . . . ?
C7 C2 C3 C4 -2.9(3) . . . . ?
C1 C2 C3 C4 176.68(19) . . . . ?
C7 C2 C3 P1 174.37(16) . . . . ?
C1 C2 C3 P1 -6.1(3) . . . . ?
C14 P1 C3 C4 -18.26(19) . . . . ?
C8 P1 C3 C4 93.30(17) . . . . ?
Ni1 P1 C3 C4 -144.39(15) . . . . ?
C14 P1 C3 C2 164.53(16) . . . . ?
C8 P1 C3 C2 -83.91(17) . . . . ?
Ni1 P1 C3 C2 38.40(17) . . . . ?
C2 C3 C4 C5 1.1(3) . . . . ?
P1 C3 C4 C5 -176.15(16) . . . . ?
C3 C4 C5 C6 1.5(3) . . . . ?
C4 C5 C6 C7 -2.3(3) . . . . ?
C5 C6 C7 C2 0.5(3) . . . . ?
C3 C2 C7 C6 2.1(3) . . . . ?
C1 C2 C7 C6 -177.51(19) . . . . ?
C14 P1 C8 C13 78.13(19) . . . . ?
C3 P1 C8 C13 -31.3(2) . . . . ?
Ni1 P1 C8 C13 -148.95(16) . . . . ?
C14 P1 C8 C9 -101.73(18) . . . . ?
C3 P1 C8 C9 148.82(18) . . . . ?
Ni1 P1 C8 C9 31.19(19) . . . . ?
C13 C8 C9 C10 1.4(3) . . . . ?
P1 C8 C9 C10 -178.74(18) . . . . ?
C8 C9 C10 C11 -0.2(4) . . . . ?
C9 C10 C11 C12 -1.4(4) . . . . ?
C10 C11 C12 C13 1.7(4) . . . . ?
C11 C12 C13 C8 -0.5(3) . . . . ?
C9 C8 C13 C12 -1.1(3) . . . . ?
P1 C8 C13 C12 179.07(17) . . . . ?
C8 P1 C14 C19 179.50(17) . . . . ?
C3 P1 C14 C19 -70.94(19) . . . . ?
Ni1 P1 C14 C19 48.43(19) . . . . ?
C8 P1 C14 C15 -1.8(2) . . . . ?
C3 P1 C14 C15 107.8(2) . . . . ?
Ni1 P1 C14 C15 -132.86(18) . . . . ?
C19 C14 C15 C16 -0.5(4) . . . . ?
P1 C14 C15 C16 -179.2(2) . . . . ?
C14 C15 C16 C17 -0.4(4) . . . . ?
C15 C16 C17 C18 1.3(5) . . . . ?
C16 C17 C18 C19 -1.4(5) . . . . ?
C17 C18 C19 C14 0.5(4) . . . . ?
C15 C14 C19 C18 0.4(4) . . . . ?
P1 C14 C19 C18 179.2(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 Cl1 0.84 2.27 2.9600(19) 140.0 .

_refine_diff_density_max         0.923
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.064


loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 -1.00 0.0310
-1.00 0.00 1.00 0.0200
1.00 0.00 1.00 0.0740
-1.00 0.00 -1.00 0.0260
1.00 7.00 0.00 0.0250
-1.00 -7.00 0.00 0.0250
####################################################################### 
# 
# 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_dd67ms
_database_code_depnum_ccdc_archive 'CCDC 1838219'
_audit_update_record             
;
2018-04-18 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
? 
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
; 
C38 H30 B F2 N2 Ni O2 P2, B F4, C H2 Cl2 
;
_chemical_formula_sum            'C39 H32 B2 Cl2 F6 N2 Ni O2 P2'
_chemical_formula_structural     ?
_chemical_formula_weight         887.83

_chemical_absolute_configuration ?
_chemical_formula_iupac          ?
_chemical_formula_analytical     ?
_chemical_compound_source        ?

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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+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                   18.2498(6)
_cell_length_b                   18.0627(6)
_cell_length_c                   23.1305(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7624.8(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    65605
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      28.30
_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_F_000             3616
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.464
_exptl_crystal_size_mid          0.249
_exptl_crystal_size_min          0.172
_exptl_crystal_id                dd67ms

_exptl_crystal_preparation       
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 0.3 mm 
cryo-loop (Hampton Research) with the (-4 4 -3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_absorpt_coefficient_mu    0.802
_shelx_estimated_absorpt_T_min   0.707
_shelx_estimated_absorpt_T_max   0.874
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6713
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS V2014/7 (Krause et al., 2015)'

_exptl_absorpt_special_details   ?
_exptl_special_details           
; 
One distinct cell was identified using APEX3 (Bruker, 2016). Five frame series 
were integrated and filtered for statistical outliers using SAINT 
(Bruker, 2014) then corrected for absorption by the multi-scan method using 
SADABS v2014/7 (Krause et al., 2015). No decay correction was applied. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dd67ms
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source                   ?
_diffrn_standards_number         ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_time  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            118020

_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.085
_diffrn_reflns_theta_max         28.338
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9471
_reflns_number_gt                8153
_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       'APEX3 V2016.9-0 (Bruker, 2016)'

_computing_cell_refinement       'SAINT V8.37A (Bruker, 2014)'
_computing_data_reduction        
; 
SAINT V8.34A, XPREP v2014/2, (Bruker, 2014) SADABS V2014/7 
(Krause et al., 2015) 
;
_computing_structure_solution    'SHELXT-2014-4 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2014-7 (Sheldrick, 2015a)'
_computing_molecular_graphics    
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by intrinsic methods (Sheldrick, 2015b). Systematic 
conditions suggested the unambiguous space group. The space group choice was 
confirmed by successful convergence of the full-matrix least-squares 
refinement on F². The final difference Fourier map had no significant 
features. A final analysis of variance between observed and calculated 
structure factors showed a slight dependence on amplitude and little dependence 
on resolution. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0547P)²+16.0184P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9471
_refine_ls_number_parameters     545
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1147
_refine_ls_wR_factor_gt          0.1073
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_refine_ls_abs_structure_details ?
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 0.64999(2) 0.63120(2) 0.64696(2) 0.00960(7) Uani 1 1 d . . . . .
P1 P 0.72211(3) 0.61771(3) 0.72200(2) 0.01040(11) Uani 1 1 d . . . . .
P2 P 0.72202(3) 0.57482(3) 0.58499(2) 0.01019(11) Uani 1 1 d . . . . .
F1 F 0.42457(7) 0.68478(7) 0.61320(6) 0.0190(3) Uani 1 1 d . . . . .
F2 F 0.47430(7) 0.78742(7) 0.65519(6) 0.0181(3) Uani 1 1 d . . . . .
O1 O 0.51028(8) 0.66496(8) 0.68269(6) 0.0134(3) Uani 1 1 d . . . . .
O2 O 0.54736(8) 0.72378(8) 0.59288(6) 0.0143(3) Uani 1 1 d . . . . .
N1 N 0.58289(9) 0.67981(10) 0.69899(7) 0.0118(3) Uani 1 1 d . . . . .
N2 N 0.58513(9) 0.65696(10) 0.58293(7) 0.0123(3) Uani 1 1 d . . . . .
C1 C 0.58746(11) 0.72279(11) 0.74299(9) 0.0130(4) Uani 1 1 d . . . . .
H1 H 0.5433 0.7427 0.7582 0.016 Uiso 1 1 calc R U . . .
C2 C 0.65610(11) 0.74317(12) 0.77136(9) 0.0146(4) Uani 1 1 d . . . . .
C3 C 0.72180(12) 0.70333(11) 0.76379(9) 0.0139(4) Uani 1 1 d . . . . .
C4 C 0.78405(12) 0.72563(12) 0.79413(10) 0.0183(4) Uani 1 1 d . . . . .
H4 H 0.8286 0.6989 0.7897 0.022 Uiso 1 1 calc R U . . .
C5 C 0.78146(14) 0.78695(14) 0.83095(11) 0.0246(5) Uani 1 1 d . . . . .
H5 H 0.8242 0.8017 0.8514 0.030 Uiso 1 1 calc R U . . .
C6 C 0.71690(14) 0.82623(15) 0.83781(12) 0.0276(5) Uani 1 1 d . . . . .
H6 H 0.7156 0.8683 0.8624 0.033 Uiso 1 1 calc R U . . .
C7 C 0.65416(13) 0.80423(13) 0.80878(11) 0.0217(5) Uani 1 1 d . . . . .
H7 H 0.6097 0.8306 0.8142 0.026 Uiso 1 1 calc R U . . .
C8 C 0.68260(11) 0.55018(11) 0.77096(9) 0.0130(4) Uani 1 1 d . . . . .
C9 C 0.63651(12) 0.49437(12) 0.75045(9) 0.0150(4) Uani 1 1 d . . . . .
H9 H 0.6257 0.4912 0.7103 0.018 Uiso 1 1 calc R U . . .
C10 C 0.60632(12) 0.44330(12) 0.78877(10) 0.0188(4) Uani 1 1 d . . . . .
H10 H 0.5761 0.4044 0.7747 0.023 Uiso 1 1 calc R U . . .
C11 C 0.62051(13) 0.44933(13) 0.84742(10) 0.0213(5) Uani 1 1 d . . . . .
H11 H 0.5992 0.4150 0.8736 0.026 Uiso 1 1 calc R U . . .
C12 C 0.66557(15) 0.50494(15) 0.86817(11) 0.0257(5) Uani 1 1 d . . . . .
H12 H 0.6749 0.5087 0.9085 0.031 Uiso 1 1 calc R U . . .
C13 C 0.69721(14) 0.55522(13) 0.83022(10) 0.0211(5) Uani 1 1 d . . . . .
H13 H 0.7287 0.5929 0.8445 0.025 Uiso 1 1 calc R U . . .
C14 C 0.81900(11) 0.59882(11) 0.71475(9) 0.0126(4) Uani 1 1 d . . . . .
C15 C 0.85252(12) 0.53740(12) 0.74035(9) 0.0158(4) Uani 1 1 d . . . . .
H15 H 0.8240 0.5023 0.7612 0.019 Uiso 1 1 calc R U . . .
C16 C 0.92809(13) 0.52801(13) 0.73510(10) 0.0205(5) Uani 1 1 d . . . . .
H16 H 0.9514 0.4869 0.7529 0.025 Uiso 1 1 calc R U . . .
C17 C 0.96933(12) 0.57880(13) 0.70387(10) 0.0201(5) Uani 1 1 d . . . . .
H17 H 1.0206 0.5715 0.6996 0.024 Uiso 1 1 calc R U . . .
C18 C 0.93624(12) 0.64025(13) 0.67882(10) 0.0185(4) Uani 1 1 d . . . . .
H18 H 0.9649 0.6750 0.6579 0.022 Uiso 1 1 calc R U . . .
C19 C 0.86112(12) 0.65059(12) 0.68456(9) 0.0149(4) Uani 1 1 d . . . . .
H19 H 0.8384 0.6929 0.6680 0.018 Uiso 1 1 calc R U . . .
C20 C 0.57167(12) 0.63114(11) 0.53241(9) 0.0139(4) Uani 1 1 d . . . . .
H20 H 0.5360 0.6566 0.5101 0.017 Uiso 1 1 calc R U . . .
C21 C 0.60567(12) 0.56656(12) 0.50584(9) 0.0148(4) Uani 1 1 d . . . . .
C22 C 0.67036(11) 0.53291(11) 0.52613(9) 0.0125(4) Uani 1 1 d . . . . .
C23 C 0.69764(12) 0.47081(12) 0.49714(9) 0.0154(4) Uani 1 1 d . . . . .
H23 H 0.7410 0.4474 0.5106 0.019 Uiso 1 1 calc R U . . .
C24 C 0.66150(13) 0.44294(12) 0.44850(9) 0.0175(4) Uani 1 1 d . . . . .
H24 H 0.6802 0.4005 0.4292 0.021 Uiso 1 1 calc R U . . .
C25 C 0.59839(13) 0.47706(13) 0.42823(10) 0.0199(4) Uani 1 1 d . . . . .
H25 H 0.5741 0.4582 0.3950 0.024 Uiso 1 1 calc R U . . .
C26 C 0.57101(13) 0.53863(13) 0.45658(9) 0.0184(4) Uani 1 1 d . . . . .
H26 H 0.5281 0.5622 0.4424 0.022 Uiso 1 1 calc R U . . .
C27 C 0.78141(11) 0.49976(11) 0.60796(9) 0.0121(4) Uani 1 1 d . . . . .
C28 C 0.74724(12) 0.43995(11) 0.63552(9) 0.0146(4) Uani 1 1 d . . . . .
H28 H 0.6958 0.4404 0.6416 0.018 Uiso 1 1 calc R U . . .
C29 C 0.78868(13) 0.38011(12) 0.65399(10) 0.0185(4) Uani 1 1 d . . . . .
H29 H 0.7658 0.3403 0.6738 0.022 Uiso 1 1 calc R U . . .
C30 C 0.86365(14) 0.37826(13) 0.64364(10) 0.0216(5) Uani 1 1 d . . . . .
H30 H 0.8918 0.3368 0.6558 0.026 Uiso 1 1 calc R U . . .
C31 C 0.89740(13) 0.43691(13) 0.61554(10) 0.0205(5) Uani 1 1 d . . . . .
H31 H 0.9486 0.4353 0.6083 0.025 Uiso 1 1 calc R U . . .
C32 C 0.85677(12) 0.49828(12) 0.59788(9) 0.0158(4) Uani 1 1 d . . . . .
H32 H 0.8802 0.5387 0.5792 0.019 Uiso 1 1 calc R U . . .
C33 C 0.77618(11) 0.64594(11) 0.54988(9) 0.0121(4) Uani 1 1 d . . . . .
C34 C 0.77004(12) 0.71895(12) 0.56957(9) 0.0148(4) Uani 1 1 d . . . . .
H34 H 0.7362 0.7305 0.5994 0.018 Uiso 1 1 calc R U . . .
C35 C 0.81296(13) 0.77459(12) 0.54585(10) 0.0185(4) Uani 1 1 d . . . . .
H35 H 0.8090 0.8239 0.5597 0.022 Uiso 1 1 calc R U . . .
C36 C 0.86186(13) 0.75771(13) 0.50170(10) 0.0194(4) Uani 1 1 d . . . . .
H36 H 0.8923 0.7954 0.4861 0.023 Uiso 1 1 calc R U . . .
C37 C 0.86646(13) 0.68598(13) 0.48036(10) 0.0203(5) Uani 1 1 d . . . . .
H37 H 0.8990 0.6751 0.4495 0.024 Uiso 1 1 calc R U . . .
C38 C 0.82345(13) 0.62989(12) 0.50406(9) 0.0174(4) Uani 1 1 d . . . . .
H38 H 0.8263 0.5810 0.4891 0.021 Uiso 1 1 calc R U . . .
B1 B 0.48770(13) 0.71551(13) 0.63628(10) 0.0137(4) Uani 1 1 d . . . . .
F3 F 0.3899(7) 0.8220(8) 0.8297(7) 0.030(2) Uani 0.66(3) 1 d D . P A 1
F4 F 0.4832(7) 0.8140(6) 0.8966(5) 0.0309(15) Uani 0.66(3) 1 d D . P A 1
F5 F 0.4303(4) 0.9260(4) 0.8778(5) 0.0347(18) Uani 0.66(3) 1 d D . P A 1
F6 F 0.4953(3) 0.8686(8) 0.8073(4) 0.0415(19) Uani 0.66(3) 1 d D . P A 1
B2 B 0.4492(5) 0.8575(3) 0.8546(3) 0.0223(6) Uani 0.66(3) 1 d D U P A 1
F3A F 0.3820(12) 0.8270(15) 0.8376(12) 0.024(3) Uani 0.34(3) 1 d D U P A 2
F4A F 0.4875(13) 0.8013(11) 0.8873(10) 0.031(3) Uani 0.34(3) 1 d D U P A 2
F5A F 0.4216(4) 0.9067(10) 0.8993(8) 0.031(2) Uani 0.34(3) 1 d D U P A 2
F6A F 0.4973(5) 0.8932(7) 0.8235(7) 0.029(2) Uani 0.34(3) 1 d D U P A 2
B2A B 0.4474(9) 0.8559(6) 0.8587(6) 0.0223(6) Uani 0.34(3) 1 d D . P A 2
Cl1 Cl 0.53197(5) 0.58051(5) 0.96601(4) 0.0470(2) Uani 1 1 d . . . B 1
Cl2 Cl 0.65083(6) 0.68889(7) 0.95805(6) 0.0716(3) Uani 1 1 d . . . B 1
C39 C 0.55726(19) 0.67396(18) 0.97387(15) 0.0420(7) Uani 1 1 d . . . B 1
H39A H 0.5473 0.6899 1.0140 0.050 Uiso 1 1 calc R U . B 1
H39B H 0.5269 0.7047 0.9477 0.050 Uiso 1 1 calc R U . B 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 N1 1.9285(18) . ?
Ni1 N2 1.9522(18) . ?
Ni1 P1 2.1919(6) . ?
Ni1 P2 2.1954(6) . ?
P1 C14 1.809(2) . ?
P1 C8 1.814(2) . ?
P1 C3 1.824(2) . ?
P2 C33 1.813(2) . ?
P2 C27 1.815(2) . ?
P2 C22 1.821(2) . ?
F1 B1 1.386(3) . ?
F2 B1 1.392(3) . ?
O1 N1 1.403(2) . ?
O1 B1 1.468(3) . ?
O2 N2 1.409(2) . ?
O2 B1 1.488(3) . ?
N1 C1 1.283(3) . ?
N2 C20 1.282(3) . ?
C1 C2 1.461(3) . ?
C1 H1 0.9500 . ?
C2 C7 1.402(3) . ?
C2 C3 1.409(3) . ?
C3 C4 1.395(3) . ?
C4 C5 1.398(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.385(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.386(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.396(3) . ?
C8 C13 1.399(3) . ?
C9 C10 1.393(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.398(3) . ?
C14 C15 1.399(3) . ?
C15 C16 1.395(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.390(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.457(3) . ?
C20 H20 0.9500 . ?
C21 C26 1.397(3) . ?
C21 C22 1.408(3) . ?
C22 C23 1.399(3) . ?
C23 C24 1.398(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.395(3) . ?
C27 C28 1.401(3) . ?
C28 C29 1.387(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.389(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.387(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.395(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.397(3) . ?
C33 C34 1.400(3) . ?
C34 C35 1.387(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.389(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.394(3) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
F3 B2 1.382(5) . ?
F4 B2 1.395(5) . ?
F5 B2 1.393(5) . ?
F6 B2 1.394(5) . ?
F3A B2A 1.390(7) . ?
F4A B2A 1.396(7) . ?
F5A B2A 1.396(7) . ?
F6A B2A 1.395(7) . ?
Cl1 C39 1.759(3) . ?
Cl2 C39 1.767(4) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 88.85(7) . . ?
N1 Ni1 P1 86.43(5) . . ?
N2 Ni1 P1 172.45(6) . . ?
N1 Ni1 P2 177.30(5) . . ?
N2 Ni1 P2 88.76(5) . . ?
P1 Ni1 P2 96.08(2) . . ?
C14 P1 C8 108.64(10) . . ?
C14 P1 C3 102.25(10) . . ?
C8 P1 C3 103.78(10) . . ?
C14 P1 Ni1 122.32(7) . . ?
C8 P1 Ni1 109.30(7) . . ?
C3 P1 Ni1 108.88(7) . . ?
C33 P2 C27 109.56(10) . . ?
C33 P2 C22 104.00(9) . . ?
C27 P2 C22 102.57(9) . . ?
C33 P2 Ni1 106.87(7) . . ?
C27 P2 Ni1 120.85(7) . . ?
C22 P2 Ni1 111.78(7) . . ?
N1 O1 B1 110.03(15) . . ?
N2 O2 B1 112.46(15) . . ?
C1 N1 O1 112.97(17) . . ?
C1 N1 Ni1 136.83(15) . . ?
O1 N1 Ni1 110.17(12) . . ?
C20 N2 O2 111.52(17) . . ?
C20 N2 Ni1 136.14(15) . . ?
O2 N2 Ni1 112.14(12) . . ?
N1 C1 C2 124.38(19) . . ?
N1 C1 H1 117.8 . . ?
C2 C1 H1 117.8 . . ?
C7 C2 C3 120.0(2) . . ?
C7 C2 C1 116.98(19) . . ?
C3 C2 C1 123.02(19) . . ?
C4 C3 C2 118.88(19) . . ?
C4 C3 P1 120.61(16) . . ?
C2 C3 P1 120.10(16) . . ?
C3 C4 C5 120.5(2) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 120.3(2) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.0(2) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C2 120.3(2) . . ?
C6 C7 H7 119.9 . . ?
C2 C7 H7 119.9 . . ?
C9 C8 C13 119.7(2) . . ?
C9 C8 P1 120.86(16) . . ?
C13 C8 P1 119.47(17) . . ?
C10 C9 C8 120.0(2) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 119.8(2) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C12 C11 C10 120.5(2) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 120.2(2) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C8 119.8(2) . . ?
C12 C13 H13 120.1 . . ?
C8 C13 H13 120.1 . . ?
C19 C14 C15 120.12(19) . . ?
C19 C14 P1 117.24(16) . . ?
C15 C14 P1 122.55(16) . . ?
C16 C15 C14 119.5(2) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C17 C16 C15 120.0(2) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 120.6(2) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C17 C18 C19 119.7(2) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C14 120.0(2) . . ?
C18 C19 H19 120.0 . . ?
C14 C19 H19 120.0 . . ?
N2 C20 C21 126.45(19) . . ?
N2 C20 H20 116.8 . . ?
C21 C20 H20 116.8 . . ?
C26 C21 C22 119.7(2) . . ?
C26 C21 C20 116.11(19) . . ?
C22 C21 C20 124.19(19) . . ?
C23 C22 C21 119.00(19) . . ?
C23 C22 P2 120.50(16) . . ?
C21 C22 P2 120.26(16) . . ?
C24 C23 C22 120.4(2) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 120.2(2) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C26 C25 C24 119.8(2) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C21 120.9(2) . . ?
C25 C26 H26 119.6 . . ?
C21 C26 H26 119.6 . . ?
C32 C27 C28 120.01(19) . . ?
C32 C27 P2 123.63(17) . . ?
C28 C27 P2 116.32(16) . . ?
C29 C28 C27 119.9(2) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 120.2(2) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C31 C30 C29 120.0(2) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C32 120.5(2) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C27 119.4(2) . . ?
C31 C32 H32 120.3 . . ?
C27 C32 H32 120.3 . . ?
C38 C33 C34 119.47(19) . . ?
C38 C33 P2 121.97(16) . . ?
C34 C33 P2 118.56(16) . . ?
C35 C34 C33 120.6(2) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C34 C35 C36 119.6(2) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
C37 C36 C35 120.3(2) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C38 120.3(2) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C37 C38 C33 119.7(2) . . ?
C37 C38 H38 120.2 . . ?
C33 C38 H38 120.2 . . ?
F1 B1 F2 110.41(18) . . ?
F1 B1 O1 105.41(17) . . ?
F2 B1 O1 113.55(18) . . ?
F1 B1 O2 112.87(18) . . ?
F2 B1 O2 104.29(17) . . ?
O1 B1 O2 110.50(17) . . ?
F3 B2 F5 112.3(9) . . ?
F3 B2 F6 102.2(11) . . ?
F5 B2 F6 108.9(5) . . ?
F3 B2 F4 112.2(6) . . ?
F5 B2 F4 110.0(5) . . ?
F6 B2 F4 111.0(9) . . ?
F3A B2A F6A 122.5(18) . . ?
F3A B2A F5A 101.2(15) . . ?
F6A B2A F5A 107.2(7) . . ?
F3A B2A F4A 110.6(10) . . ?
F6A B2A F4A 106.0(17) . . ?
F5A B2A F4A 108.7(9) . . ?
Cl1 C39 Cl2 112.25(18) . . ?
Cl1 C39 H39A 109.2 . . ?
Cl2 C39 H39A 109.2 . . ?
Cl1 C39 H39B 109.2 . . ?
Cl2 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?

_refine_diff_density_max         0.568
_refine_diff_density_min         -1.343
_refine_diff_density_rms         0.090


loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 -3.00 0.0730
1.00 0.00 3.00 0.0830
-2.00 1.00 -1.00 0.1310
1.00 3.00 0.00 0.1990
-1.00 -3.00 0.00 0.2270
-1.00 0.00 -1.00 0.1200
2.00 -1.00 3.00 0.0870
-2.00 3.00 2.00 0.1480
0.00 1.00 2.00 0.0980
1.00 0.00 1.00 0.0860
1.00 -2.00 -2.00 0.1610
3.00 0.00 -2.00 0.0860
-3.00 0.00 2.00 0.1480
-1.00 -1.00 1.00 0.1990
1.00 1.00 -1.00 0.1610
-3.00 1.00 3.00 0.1140
3.00 -1.00 -3.00 0.0740
-1.00 0.00 2.00 0.1070
-1.00 1.00 3.00 0.0850
####################################################################### 
# 
# 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_dd37dsa
_database_code_depnum_ccdc_archive 'CCDC 1834879'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
? 
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H30 N2 Ni O2 P2'
_chemical_formula_sum            'C38 H30 N2 Ni O2 P2'
_chemical_formula_structural     ?
_chemical_formula_weight         667.29

_chemical_formula_iupac          ?
_chemical_formula_analytical     ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

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

_cell_length_a                   23.4743(8)
_cell_length_b                   13.0781(4)
_cell_length_c                   20.2265(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6209.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    90686
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      26.41
_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_F_000             2768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.066
_exptl_crystal_id                dd37dsa

_exptl_crystal_preparation       
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 -1 4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_absorpt_coefficient_mu    0.767
_shelx_estimated_absorpt_T_min   0.821
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.8248
_exptl_absorpt_correction_T_max  0.9633
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker, 2014)'

_exptl_absorpt_special_details   ?
_exptl_special_details           
; 
One distinct cell was identified using APEX2 (Bruker, 2014). 
Seven frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2014) then corrected for absorption by 
integration using SADABS v2014/5 (Bruker, 2014). 
No decay correction was applied. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dd37dsa
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source                   ?
_diffrn_standards_number         ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_time  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            161076

_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.332
_diffrn_reflns_theta_max         26.415
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12698
_reflns_number_gt                12158
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.999

_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       'APEX2 V2014.9-0 (Bruker, 2014)'

_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/5 (Bruker, 2012 & 2014) 
;
_computing_structure_solution    'SHELXT-2014-7 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_molecular_graphics    
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by intrinsic methods (Sheldrick, 2015b). 
Systematic conditions suggested the ambiguous space group. 
The space group choice was confirmed by successful convergence of the 
full-matrix least-squares refinement on F². The final difference Fourier 
map had no significant features. A final analysis of variance between observed 
and calculated structure factors showed little dependence on amplitude or 
resolution. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0299P)²+4.0914P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 'Flack (1983),  6162 Friedels'
_refine_ls_abs_structure_Flack   0.329(9)
_chemical_absolute_configuration ad
_chemical_compound_source        ?

_refine_ls_number_reflns         12698
_refine_ls_number_parameters     812
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0627
_refine_ls_wR_factor_gt          0.0611
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.71785(2) 0.54324(3) 0.62355(2) 0.00874(8) Uani 1 1 d . . . . .
P1 P 0.62934(3) 0.49247(6) 0.61336(4) 0.00994(15) Uani 1 1 d . . . . .
P2 P 0.80627(3) 0.53234(6) 0.59057(4) 0.00927(15) Uani 1 1 d . . . . .
O1 O 0.75942(10) 0.49914(19) 0.73788(11) 0.0189(5) Uani 1 1 d . . . . .
O2 O 0.67671(9) 0.72198(16) 0.60839(11) 0.0148(5) Uani 1 1 d . . . . .
N1 N 0.72792(11) 0.4525(2) 0.69402(13) 0.0119(5) Uani 1 1 d . . . . .
N2 N 0.70829(11) 0.6600(2) 0.57279(13) 0.0110(5) Uani 1 1 d . . . . .
C1 C 0.63310(12) 0.3536(2) 0.61490(16) 0.0118(6) Uani 1 1 d . . . . .
C2 C 0.67059(13) 0.3056(2) 0.66048(15) 0.0122(6) Uani 1 1 d . . . . .
C3 C 0.66915(14) 0.1985(3) 0.66540(17) 0.0164(7) Uani 1 1 d . . . . .
H3A H 0.6935 0.1651 0.6960 0.020 Uiso 1 1 calc R U . . .
C4 C 0.63272(14) 0.1403(2) 0.62627(18) 0.0176(6) Uani 1 1 d . . . . .
H4A H 0.6316 0.0681 0.6313 0.021 Uiso 1 1 calc R U . . .
C5 C 0.59809(15) 0.1877(2) 0.58000(17) 0.0180(7) Uani 1 1 d . . . . .
H5A H 0.5742 0.1478 0.5522 0.022 Uiso 1 1 calc R U . . .
C6 C 0.59842(14) 0.2938(3) 0.57432(17) 0.0167(7) Uani 1 1 d . . . . .
H6A H 0.5747 0.3259 0.5424 0.020 Uiso 1 1 calc R U . . .
C7 C 0.70902(14) 0.3602(3) 0.70447(16) 0.0142(7) Uani 1 1 d . . . . .
H7A H 0.7212 0.3262 0.7435 0.017 Uiso 1 1 calc R U . . .
C8 C 0.57868(13) 0.5236(2) 0.67859(16) 0.0124(6) Uani 1 1 d . . . . .
C9 C 0.58154(14) 0.6196(3) 0.70777(16) 0.0168(7) Uani 1 1 d . . . . .
H9A H 0.6121 0.6643 0.6973 0.020 Uiso 1 1 calc R U . . .
C10 C 0.53962(15) 0.6507(3) 0.75239(17) 0.0217(7) Uani 1 1 d . . . . .
H10A H 0.5414 0.7168 0.7718 0.026 Uiso 1 1 calc R U . . .
C11 C 0.49523(15) 0.5846(3) 0.76840(17) 0.0221(8) Uani 1 1 d . . . . .
H11A H 0.4666 0.6056 0.7987 0.027 Uiso 1 1 calc R U . . .
C12 C 0.49278(14) 0.4881(3) 0.74017(17) 0.0215(7) Uani 1 1 d . . . . .
H12A H 0.4626 0.4430 0.7515 0.026 Uiso 1 1 calc R U . . .
C13 C 0.53431(14) 0.4570(3) 0.69526(17) 0.0165(7) Uani 1 1 d . . . . .
H13A H 0.5325 0.3908 0.6760 0.020 Uiso 1 1 calc R U . . .
C14 C 0.59212(13) 0.5258(2) 0.53735(16) 0.0122(6) Uani 1 1 d . . . . .
C15 C 0.62129(14) 0.5175(2) 0.47706(16) 0.0147(7) Uani 1 1 d . . . . .
H15A H 0.6591 0.4914 0.4764 0.018 Uiso 1 1 calc R U . . .
C16 C 0.59543(16) 0.5471(3) 0.41808(17) 0.0205(7) Uani 1 1 d . . . . .
H16A H 0.6154 0.5409 0.3774 0.025 Uiso 1 1 calc R U . . .
C17 C 0.54001(16) 0.5858(3) 0.41898(17) 0.0220(7) Uani 1 1 d . . . . .
H17A H 0.5223 0.6066 0.3790 0.026 Uiso 1 1 calc R U . . .
C18 C 0.51090(15) 0.5938(3) 0.47851(19) 0.0209(7) Uani 1 1 d . . . . .
H18A H 0.4731 0.6197 0.4790 0.025 Uiso 1 1 calc R U . . .
C19 C 0.53652(14) 0.5642(3) 0.53745(18) 0.0174(7) Uani 1 1 d . . . . .
H19A H 0.5162 0.5701 0.5779 0.021 Uiso 1 1 calc R U . . .
C20 C 0.80517(13) 0.5535(2) 0.50142(15) 0.0101(6) Uani 1 1 d . . . . .
C21 C 0.76683(12) 0.6265(2) 0.47514(15) 0.0113(6) Uani 1 1 d . . . . .
C22 C 0.76689(13) 0.6448(2) 0.40661(16) 0.0153(6) Uani 1 1 d . . . . .
H22A H 0.7415 0.6940 0.3885 0.018 Uiso 1 1 calc R U . . .
C23 C 0.80359(14) 0.5917(3) 0.36506(16) 0.0176(7) Uani 1 1 d . . . . .
H23A H 0.8030 0.6045 0.3188 0.021 Uiso 1 1 calc R U . . .
C24 C 0.84120(14) 0.5201(2) 0.39091(16) 0.0163(7) Uani 1 1 d . . . . .
H24A H 0.8664 0.4841 0.3625 0.020 Uiso 1 1 calc R U . . .
C25 C 0.84186(13) 0.5012(2) 0.45878(16) 0.0129(6) Uani 1 1 d . . . . .
H25A H 0.8676 0.4521 0.4763 0.015 Uiso 1 1 calc R U . . .
C26 C 0.72788(13) 0.6883(2) 0.51526(15) 0.0112(6) Uani 1 1 d . . . . .
H26A H 0.7162 0.7528 0.4984 0.013 Uiso 1 1 calc R U . . .
C27 C 0.85807(12) 0.6236(2) 0.62266(17) 0.0125(6) Uani 1 1 d . . . . .
C28 C 0.85327(14) 0.6571(3) 0.68819(17) 0.0161(7) Uani 1 1 d . . . . .
H28A H 0.8239 0.6306 0.7156 0.019 Uiso 1 1 calc R U . . .
C29 C 0.89122(14) 0.7289(3) 0.71329(18) 0.0199(7) Uani 1 1 d . . . . .
H29A H 0.8880 0.7513 0.7578 0.024 Uiso 1 1 calc R U . . .
C30 C 0.93408(15) 0.7680(3) 0.67252(19) 0.0202(7) Uani 1 1 d . . . . .
H30A H 0.9598 0.8176 0.6894 0.024 Uiso 1 1 calc R U . . .
C31 C 0.93929(14) 0.7350(2) 0.60781(17) 0.0195(7) Uani 1 1 d . . . . .
H31A H 0.9688 0.7615 0.5807 0.023 Uiso 1 1 calc R U . . .
C32 C 0.90150(13) 0.6631(2) 0.58221(17) 0.0154(6) Uani 1 1 d . . . . .
H32A H 0.9050 0.6409 0.5377 0.019 Uiso 1 1 calc R U . . .
C33 C 0.83699(13) 0.4054(2) 0.59933(15) 0.0109(6) Uani 1 1 d . . . . .
C34 C 0.80238(14) 0.3219(2) 0.58298(16) 0.0138(6) Uani 1 1 d . . . . .
H34A H 0.7643 0.3331 0.5689 0.017 Uiso 1 1 calc R U . . .
C35 C 0.82346(14) 0.2229(3) 0.58724(16) 0.0177(7) Uani 1 1 d . . . . .
H35A H 0.8000 0.1665 0.5757 0.021 Uiso 1 1 calc R U . . .
C36 C 0.87913(15) 0.2065(3) 0.60852(16) 0.0202(7) Uani 1 1 d . . . . .
H36A H 0.8936 0.1388 0.6117 0.024 Uiso 1 1 calc R U . . .
C37 C 0.91344(14) 0.2889(3) 0.62512(18) 0.0218(7) Uani 1 1 d . . . . .
H37A H 0.9514 0.2774 0.6396 0.026 Uiso 1 1 calc R U . . .
C38 C 0.89251(13) 0.3883(3) 0.62069(17) 0.0169(6) Uani 1 1 d . . . . .
H38A H 0.9162 0.4445 0.6323 0.020 Uiso 1 1 calc R U . . .
Ni2 Ni 0.61171(2) 0.95289(3) 0.37531(2) 0.00905(8) Uani 1 1 d . . . . .
P3 P 0.52490(3) 0.97295(6) 0.41285(4) 0.00950(15) Uani 1 1 d . . . . .
P4 P 0.70167(3) 0.99705(6) 0.38485(4) 0.00910(15) Uani 1 1 d . . . . .
O3 O 0.64646(9) 0.77123(16) 0.38781(11) 0.0167(5) Uani 1 1 d . . . . .
O4 O 0.57241(11) 0.9933(2) 0.25900(12) 0.0243(6) Uani 1 1 d . . . . .
N3 N 0.61801(10) 0.8349(2) 0.42610(13) 0.0104(5) Uani 1 1 d . . . . .
N4 N 0.60494(12) 1.0398(2) 0.30234(14) 0.0144(6) Uani 1 1 d . . . . .
C39 C 0.52749(13) 0.9492(2) 0.50172(15) 0.0100(6) Uani 1 1 d . . . . .
C40 C 0.56319(12) 0.8706(2) 0.52582(15) 0.0110(6) Uani 1 1 d . . . . .
C41 C 0.56125(13) 0.8473(2) 0.59347(16) 0.0140(6) Uani 1 1 d . . . . .
H41A H 0.5845 0.7937 0.6102 0.017 Uiso 1 1 calc R U . . .
C42 C 0.52607(13) 0.9008(3) 0.63664(16) 0.0151(6) Uani 1 1 d . . . . .
H42A H 0.5257 0.8842 0.6824 0.018 Uiso 1 1 calc R U . . .
C43 C 0.49135(13) 0.9787(2) 0.61279(16) 0.0147(6) Uani 1 1 d . . . . .
H43A H 0.4673 1.0156 0.6421 0.018 Uiso 1 1 calc R U . . .
C44 C 0.49201(13) 1.0024(2) 0.54594(16) 0.0130(6) Uani 1 1 d . . . . .
H44A H 0.4681 1.0554 0.5298 0.016 Uiso 1 1 calc R U . . .
C45 C 0.59961(13) 0.8072(2) 0.48369(15) 0.0113(6) Uani 1 1 d . . . . .
H45A H 0.6104 0.7417 0.4996 0.014 Uiso 1 1 calc R U . . .
C46 C 0.47006(12) 0.8850(2) 0.38428(16) 0.0120(6) Uani 1 1 d . . . . .
C47 C 0.47075(15) 0.8562(3) 0.31777(18) 0.0177(7) Uani 1 1 d . . . . .
H47A H 0.4983 0.8845 0.2887 0.021 Uiso 1 1 calc R U . . .
C48 C 0.43102(16) 0.7859(3) 0.29413(18) 0.0241(8) Uani 1 1 d . . . . .
H48A H 0.4313 0.7666 0.2488 0.029 Uiso 1 1 calc R U . . .
C49 C 0.39096(15) 0.7440(3) 0.3369(2) 0.0232(8) Uani 1 1 d . . . . .
H49A H 0.3639 0.6961 0.3207 0.028 Uiso 1 1 calc R U . . .
C50 C 0.39027(15) 0.7716(3) 0.40244(19) 0.0218(8) Uani 1 1 d . . . . .
H50A H 0.3628 0.7426 0.4313 0.026 Uiso 1 1 calc R U . . .
C51 C 0.42983(14) 0.8424(3) 0.42704(17) 0.0168(7) Uani 1 1 d . . . . .
H51A H 0.4293 0.8612 0.4724 0.020 Uiso 1 1 calc R U . . .
C52 C 0.49640(13) 1.1018(2) 0.40783(15) 0.0119(6) Uani 1 1 d . . . . .
C53 C 0.53465(14) 1.1828(2) 0.41812(15) 0.0139(6) Uani 1 1 d . . . . .
H53A H 0.5742 1.1694 0.4229 0.017 Uiso 1 1 calc R U . . .
C54 C 0.51461(15) 1.2825(2) 0.42124(16) 0.0167(7) Uani 1 1 d . . . . .
H54A H 0.5404 1.3372 0.4288 0.020 Uiso 1 1 calc R U . . .
C55 C 0.45700(15) 1.3024(3) 0.41329(17) 0.0203(7) Uani 1 1 d . . . . .
H55A H 0.4435 1.3708 0.4158 0.024 Uiso 1 1 calc R U . . .
C56 C 0.41901(14) 1.2235(3) 0.40175(17) 0.0204(7) Uani 1 1 d . . . . .
H56A H 0.3797 1.2378 0.3959 0.025 Uiso 1 1 calc R U . . .
C57 C 0.43854(13) 1.1229(2) 0.39871(16) 0.0161(7) Uani 1 1 d . . . . .
H57A H 0.4125 1.0687 0.3905 0.019 Uiso 1 1 calc R U . . .
C58 C 0.70094(12) 1.1358(2) 0.38064(17) 0.0117(6) Uani 1 1 d . . . . .
C59 C 0.66721(13) 1.1834(2) 0.33118(15) 0.0131(6) Uani 1 1 d . . . . .
C60 C 0.67177(14) 1.2888(3) 0.32211(17) 0.0174(7) Uani 1 1 d . . . . .
H60A H 0.6509 1.3206 0.2875 0.021 Uiso 1 1 calc R U . . .
C61 C 0.70618(14) 1.3484(2) 0.36262(17) 0.0172(7) Uani 1 1 d . . . . .
H61A H 0.7088 1.4201 0.3556 0.021 Uiso 1 1 calc R U . . .
C62 C 0.73673(14) 1.3024(3) 0.41346(17) 0.0182(7) Uani 1 1 d . . . . .
H62A H 0.7591 1.3431 0.4425 0.022 Uiso 1 1 calc R U . . .
C63 C 0.73469(14) 1.1972(3) 0.42190(16) 0.0147(6) Uani 1 1 d . . . . .
H63A H 0.7565 1.1663 0.4561 0.018 Uiso 1 1 calc R U . . .
C64 C 0.62815(14) 1.1280(3) 0.28760(16) 0.0164(7) Uani 1 1 d . . . . .
H64A H 0.6191 1.1578 0.2461 0.020 Uiso 1 1 calc R U . . .
C65 C 0.75132(13) 0.9574(2) 0.32032(15) 0.0115(6) Uani 1 1 d . . . . .
C66 C 0.74047(14) 0.8658(2) 0.28740(15) 0.0142(6) Uani 1 1 d . . . . .
H66A H 0.7062 0.8294 0.2956 0.017 Uiso 1 1 calc R U . . .
C67 C 0.78011(14) 0.8279(3) 0.24235(17) 0.0192(7) Uani 1 1 d . . . . .
H67A H 0.7725 0.7663 0.2191 0.023 Uiso 1 1 calc R U . . .
C68 C 0.83073(14) 0.8801(3) 0.23157(16) 0.0173(7) Uani 1 1 d . . . . .
H68A H 0.8581 0.8530 0.2018 0.021 Uiso 1 1 calc R U . . .
C69 C 0.84161(14) 0.9714(3) 0.26386(16) 0.0162(7) Uani 1 1 d . . . . .
H69A H 0.8763 1.0070 0.2561 0.019 Uiso 1 1 calc R U . . .
C70 C 0.80150(14) 1.0112(2) 0.30786(16) 0.0140(6) Uani 1 1 d . . . . .
H70A H 0.8084 1.0746 0.3293 0.017 Uiso 1 1 calc R U . . .
C71 C 0.73896(13) 0.9651(2) 0.46125(16) 0.0112(6) Uani 1 1 d . . . . .
C72 C 0.71101(14) 0.9812(3) 0.52152(17) 0.0166(7) Uani 1 1 d . . . . .
H72A H 0.6736 1.0089 0.5219 0.020 Uiso 1 1 calc R U . . .
C73 C 0.73767(15) 0.9569(3) 0.58079(17) 0.0202(7) Uani 1 1 d . . . . .
H73A H 0.7185 0.9689 0.6215 0.024 Uiso 1 1 calc R U . . .
C74 C 0.79236(15) 0.9150(3) 0.58101(17) 0.0211(7) Uani 1 1 d . . . . .
H74A H 0.8106 0.8986 0.6216 0.025 Uiso 1 1 calc R U . . .
C75 C 0.81972(15) 0.8978(3) 0.52160(18) 0.0205(7) Uani 1 1 d . . . . .
H75A H 0.8567 0.8685 0.5214 0.025 Uiso 1 1 calc R U . . .
C76 C 0.79353(14) 0.9231(3) 0.46182(16) 0.0163(7) Uani 1 1 d . . . . .
H76A H 0.8130 0.9117 0.4213 0.020 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.854(3) . ?
Ni1 N1 1.870(3) . ?
Ni1 P2 2.1849(8) . ?
Ni1 P1 2.1909(8) . ?
P1 C1 1.819(3) . ?
P1 C14 1.821(3) . ?
P1 C8 1.822(3) . ?
P2 C33 1.818(3) . ?
P2 C27 1.823(3) . ?
P2 C20 1.825(3) . ?
O1 N1 1.306(3) . ?
O2 N2 1.313(3) . ?
N1 C7 1.303(4) . ?
N2 C26 1.305(4) . ?
C1 C6 1.396(5) . ?
C1 C2 1.421(4) . ?
C2 C3 1.405(5) . ?
C2 C7 1.454(5) . ?
C3 C4 1.391(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.386(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.392(5) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C9 1.389(5) . ?
C8 C13 1.399(4) . ?
C9 C10 1.396(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.393(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.386(5) . ?
C11 H11A 0.9500 . ?
C12 C13 1.393(5) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C19 1.398(5) . ?
C14 C15 1.403(5) . ?
C15 C16 1.393(5) . ?
C15 H15A 0.9500 . ?
C16 C17 1.396(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.388(5) . ?
C17 H17A 0.9500 . ?
C18 C19 1.390(5) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 C25 1.397(4) . ?
C20 C21 1.415(4) . ?
C21 C22 1.407(5) . ?
C21 C26 1.466(4) . ?
C22 C23 1.389(5) . ?
C22 H22A 0.9500 . ?
C23 C24 1.390(5) . ?
C23 H23A 0.9500 . ?
C24 C25 1.395(5) . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 C28 1.401(5) . ?
C27 C32 1.405(4) . ?
C28 C29 1.391(5) . ?
C28 H28A 0.9500 . ?
C29 C30 1.398(5) . ?
C29 H29A 0.9500 . ?
C30 C31 1.384(5) . ?
C30 H30A 0.9500 . ?
C31 C32 1.392(5) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C33 C38 1.391(4) . ?
C33 C34 1.400(4) . ?
C34 C35 1.390(5) . ?
C34 H34A 0.9500 . ?
C35 C36 1.392(5) . ?
C35 H35A 0.9500 . ?
C36 C37 1.386(5) . ?
C36 H36A 0.9500 . ?
C37 C38 1.394(5) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
Ni2 N3 1.860(3) . ?
Ni2 N4 1.870(3) . ?
Ni2 P3 2.1905(8) . ?
Ni2 P4 2.1977(8) . ?
P3 C52 1.816(3) . ?
P3 C46 1.820(3) . ?
P3 C39 1.825(3) . ?
P4 C58 1.817(3) . ?
P4 C71 1.825(3) . ?
P4 C65 1.825(3) . ?
O3 N3 1.319(3) . ?
O4 N4 1.312(4) . ?
N3 C45 1.294(4) . ?
N4 C64 1.310(4) . ?
C39 C44 1.406(4) . ?
C39 C40 1.413(4) . ?
C40 C41 1.403(5) . ?
C40 C45 1.464(4) . ?
C41 C42 1.391(5) . ?
C41 H41A 0.9500 . ?
C42 C43 1.391(5) . ?
C42 H42A 0.9500 . ?
C43 C44 1.387(5) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 H45A 0.9500 . ?
C46 C51 1.397(5) . ?
C46 C47 1.397(5) . ?
C47 C48 1.394(5) . ?
C47 H47A 0.9500 . ?
C48 C49 1.390(5) . ?
C48 H48A 0.9500 . ?
C49 C50 1.374(5) . ?
C49 H49A 0.9500 . ?
C50 C51 1.402(5) . ?
C50 H50A 0.9500 . ?
C51 H51A 0.9500 . ?
C52 C57 1.398(4) . ?
C52 C53 1.404(4) . ?
C53 C54 1.387(5) . ?
C53 H53A 0.9500 . ?
C54 C55 1.387(5) . ?
C54 H54A 0.9500 . ?
C55 C56 1.384(5) . ?
C55 H55A 0.9500 . ?
C56 C57 1.395(5) . ?
C56 H56A 0.9500 . ?
C57 H57A 0.9500 . ?
C58 C63 1.403(4) . ?
C58 C59 1.419(4) . ?
C59 C60 1.395(5) . ?
C59 C64 1.464(5) . ?
C60 C61 1.390(5) . ?
C60 H60A 0.9500 . ?
C61 C62 1.391(5) . ?
C61 H61A 0.9500 . ?
C62 C63 1.387(5) . ?
C62 H62A 0.9500 . ?
C63 H63A 0.9500 . ?
C64 H64A 0.9500 . ?
C65 C66 1.394(4) . ?
C65 C70 1.395(5) . ?
C66 C67 1.394(5) . ?
C66 H66A 0.9500 . ?
C67 C68 1.388(5) . ?
C67 H67A 0.9500 . ?
C68 C69 1.385(5) . ?
C68 H68A 0.9500 . ?
C69 C70 1.396(5) . ?
C69 H69A 0.9500 . ?
C70 H70A 0.9500 . ?
C71 C76 1.394(4) . ?
C71 C72 1.400(5) . ?
C72 C73 1.389(5) . ?
C72 H72A 0.9500 . ?
C73 C74 1.396(5) . ?
C73 H73A 0.9500 . ?
C74 C75 1.381(5) . ?
C74 H74A 0.9500 . ?
C75 C76 1.396(5) . ?
C75 H75A 0.9500 . ?
C76 H76A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N1 163.82(12) . . ?
N2 Ni1 P2 89.98(8) . . ?
N1 Ni1 P2 94.09(9) . . ?
N2 Ni1 P1 94.75(8) . . ?
N1 Ni1 P1 89.96(8) . . ?
P2 Ni1 P1 148.47(4) . . ?
C1 P1 C14 106.08(15) . . ?
C1 P1 C8 104.04(15) . . ?
C14 P1 C8 104.16(15) . . ?
C1 P1 Ni1 104.78(10) . . ?
C14 P1 Ni1 117.50(11) . . ?
C8 P1 Ni1 118.87(11) . . ?
C33 P2 C27 107.36(14) . . ?
C33 P2 C20 103.91(14) . . ?
C27 P2 C20 105.18(15) . . ?
C33 P2 Ni1 113.99(10) . . ?
C27 P2 Ni1 118.82(10) . . ?
C20 P2 Ni1 106.17(10) . . ?
C7 N1 O1 121.0(3) . . ?
C7 N1 Ni1 132.0(2) . . ?
O1 N1 Ni1 107.0(2) . . ?
C26 N2 O2 120.9(3) . . ?
C26 N2 Ni1 133.2(2) . . ?
O2 N2 Ni1 105.83(19) . . ?
C6 C1 C2 119.7(3) . . ?
C6 C1 P1 121.4(2) . . ?
C2 C1 P1 118.8(2) . . ?
C3 C2 C1 118.1(3) . . ?
C3 C2 C7 117.5(3) . . ?
C1 C2 C7 124.4(3) . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 H3A 119.4 . . ?
C2 C3 H3A 119.4 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5A 120.1 . . ?
C6 C5 H5A 120.1 . . ?
C5 C6 C1 120.9(3) . . ?
C5 C6 H6A 119.6 . . ?
C1 C6 H6A 119.6 . . ?
N1 C7 C2 124.5(3) . . ?
N1 C7 H7A 117.7 . . ?
C2 C7 H7A 117.7 . . ?
C9 C8 C13 119.8(3) . . ?
C9 C8 P1 118.6(2) . . ?
C13 C8 P1 121.4(3) . . ?
C8 C9 C10 120.3(3) . . ?
C8 C9 H9A 119.9 . . ?
C10 C9 H9A 119.9 . . ?
C11 C10 C9 119.8(3) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 H11A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C11 C12 C13 120.4(3) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
C12 C13 C8 119.7(3) . . ?
C12 C13 H13A 120.1 . . ?
C8 C13 H13A 120.1 . . ?
C19 C14 C15 119.0(3) . . ?
C19 C14 P1 122.2(3) . . ?
C15 C14 P1 118.7(2) . . ?
C16 C15 C14 120.7(3) . . ?
C16 C15 H15A 119.7 . . ?
C14 C15 H15A 119.7 . . ?
C15 C16 C17 119.7(3) . . ?
C15 C16 H16A 120.1 . . ?
C17 C16 H16A 120.1 . . ?
C18 C17 C16 119.8(3) . . ?
C18 C17 H17A 120.1 . . ?
C16 C17 H17A 120.1 . . ?
C17 C18 C19 120.7(3) . . ?
C17 C18 H18A 119.7 . . ?
C19 C18 H18A 119.7 . . ?
C18 C19 C14 120.2(3) . . ?
C18 C19 H19A 119.9 . . ?
C14 C19 H19A 119.9 . . ?
C25 C20 C21 119.3(3) . . ?
C25 C20 P2 121.8(2) . . ?
C21 C20 P2 118.8(2) . . ?
C22 C21 C20 118.9(3) . . ?
C22 C21 C26 116.9(3) . . ?
C20 C21 C26 124.1(3) . . ?
C23 C22 C21 120.8(3) . . ?
C23 C22 H22A 119.6 . . ?
C21 C22 H22A 119.6 . . ?
C22 C23 C24 120.2(3) . . ?
C22 C23 H23A 119.9 . . ?
C24 C23 H23A 119.9 . . ?
C23 C24 C25 119.8(3) . . ?
C23 C24 H24A 120.1 . . ?
C25 C24 H24A 120.1 . . ?
C24 C25 C20 120.9(3) . . ?
C24 C25 H25A 119.5 . . ?
C20 C25 H25A 119.5 . . ?
N2 C26 C21 123.8(3) . . ?
N2 C26 H26A 118.1 . . ?
C21 C26 H26A 118.1 . . ?
C28 C27 C32 119.6(3) . . ?
C28 C27 P2 119.2(2) . . ?
C32 C27 P2 121.1(3) . . ?
C29 C28 C27 120.4(3) . . ?
C29 C28 H28A 119.8 . . ?
C27 C28 H28A 119.8 . . ?
C28 C29 C30 119.5(3) . . ?
C28 C29 H29A 120.2 . . ?
C30 C29 H29A 120.2 . . ?
C31 C30 C29 120.5(3) . . ?
C31 C30 H30A 119.7 . . ?
C29 C30 H30A 119.7 . . ?
C30 C31 C32 120.4(3) . . ?
C30 C31 H31A 119.8 . . ?
C32 C31 H31A 119.8 . . ?
C31 C32 C27 119.6(3) . . ?
C31 C32 H32A 120.2 . . ?
C27 C32 H32A 120.2 . . ?
C38 C33 C34 119.5(3) . . ?
C38 C33 P2 123.2(2) . . ?
C34 C33 P2 117.3(2) . . ?
C35 C34 C33 120.4(3) . . ?
C35 C34 H34A 119.8 . . ?
C33 C34 H34A 119.8 . . ?
C34 C35 C36 119.8(3) . . ?
C34 C35 H35A 120.1 . . ?
C36 C35 H35A 120.1 . . ?
C37 C36 C35 120.1(3) . . ?
C37 C36 H36A 120.0 . . ?
C35 C36 H36A 120.0 . . ?
C36 C37 C38 120.3(3) . . ?
C36 C37 H37A 119.8 . . ?
C38 C37 H37A 119.8 . . ?
C33 C38 C37 120.0(3) . . ?
C33 C38 H38A 120.0 . . ?
C37 C38 H38A 120.0 . . ?
N3 Ni2 N4 161.31(12) . . ?
N3 Ni2 P3 88.96(8) . . ?
N4 Ni2 P3 96.99(9) . . ?
N3 Ni2 P4 95.35(8) . . ?
N4 Ni2 P4 89.50(9) . . ?
P3 Ni2 P4 146.31(4) . . ?
C52 P3 C46 107.94(14) . . ?
C52 P3 C39 103.03(14) . . ?
C46 P3 C39 103.21(14) . . ?
C52 P3 Ni2 115.74(10) . . ?
C46 P3 Ni2 118.18(10) . . ?
C39 P3 Ni2 106.86(10) . . ?
C58 P4 C71 105.86(15) . . ?
C58 P4 C65 104.84(14) . . ?
C71 P4 C65 103.54(15) . . ?
C58 P4 Ni2 104.44(10) . . ?
C71 P4 Ni2 118.36(11) . . ?
C65 P4 Ni2 118.44(11) . . ?
C45 N3 O3 121.4(3) . . ?
C45 N3 Ni2 134.6(2) . . ?
O3 N3 Ni2 103.88(19) . . ?
C64 N4 O4 119.9(3) . . ?
C64 N4 Ni2 132.8(2) . . ?
O4 N4 Ni2 107.1(2) . . ?
C44 C39 C40 119.5(3) . . ?
C44 C39 P3 121.5(2) . . ?
C40 C39 P3 118.9(2) . . ?
C41 C40 C39 118.4(3) . . ?
C41 C40 C45 117.6(3) . . ?
C39 C40 C45 123.9(3) . . ?
C42 C41 C40 121.5(3) . . ?
C42 C41 H41A 119.3 . . ?
C40 C41 H41A 119.3 . . ?
C43 C42 C41 119.9(3) . . ?
C43 C42 H42A 120.0 . . ?
C41 C42 H42A 120.0 . . ?
C44 C43 C42 119.7(3) . . ?
C44 C43 H43A 120.2 . . ?
C42 C43 H43A 120.2 . . ?
C43 C44 C39 121.1(3) . . ?
C43 C44 H44A 119.5 . . ?
C39 C44 H44A 119.5 . . ?
N3 C45 C40 124.1(3) . . ?
N3 C45 H45A 117.9 . . ?
C40 C45 H45A 117.9 . . ?
C51 C46 C47 119.8(3) . . ?
C51 C46 P3 122.3(3) . . ?
C47 C46 P3 117.9(2) . . ?
C48 C47 C46 120.0(3) . . ?
C48 C47 H47A 120.0 . . ?
C46 C47 H47A 120.0 . . ?
C49 C48 C47 119.9(3) . . ?
C49 C48 H48A 120.0 . . ?
C47 C48 H48A 120.0 . . ?
C50 C49 C48 120.3(3) . . ?
C50 C49 H49A 119.8 . . ?
C48 C49 H49A 119.8 . . ?
C49 C50 C51 120.5(3) . . ?
C49 C50 H50A 119.7 . . ?
C51 C50 H50A 119.7 . . ?
C46 C51 C50 119.4(3) . . ?
C46 C51 H51A 120.3 . . ?
C50 C51 H51A 120.3 . . ?
C57 C52 C53 119.5(3) . . ?
C57 C52 P3 123.2(2) . . ?
C53 C52 P3 117.1(2) . . ?
C54 C53 C52 119.9(3) . . ?
C54 C53 H53A 120.0 . . ?
C52 C53 H53A 120.0 . . ?
C55 C54 C53 120.2(3) . . ?
C55 C54 H54A 119.9 . . ?
C53 C54 H54A 119.9 . . ?
C56 C55 C54 120.5(3) . . ?
C56 C55 H55A 119.8 . . ?
C54 C55 H55A 119.8 . . ?
C55 C56 C57 120.0(3) . . ?
C55 C56 H56A 120.0 . . ?
C57 C56 H56A 120.0 . . ?
C56 C57 C52 120.0(3) . . ?
C56 C57 H57A 120.0 . . ?
C52 C57 H57A 120.0 . . ?
C63 C58 C59 118.9(3) . . ?
C63 C58 P4 122.6(2) . . ?
C59 C58 P4 118.4(2) . . ?
C60 C59 C58 118.9(3) . . ?
C60 C59 C64 117.3(3) . . ?
C58 C59 C64 123.8(3) . . ?
C61 C60 C59 121.4(3) . . ?
C61 C60 H60A 119.3 . . ?
C59 C60 H60A 119.3 . . ?
C60 C61 C62 119.6(3) . . ?
C60 C61 H61A 120.2 . . ?
C62 C61 H61A 120.2 . . ?
C63 C62 C61 120.2(3) . . ?
C63 C62 H62A 119.9 . . ?
C61 C62 H62A 119.9 . . ?
C62 C63 C58 120.9(3) . . ?
C62 C63 H63A 119.5 . . ?
C58 C63 H63A 119.5 . . ?
N4 C64 C59 124.0(3) . . ?
N4 C64 H64A 118.0 . . ?
C59 C64 H64A 118.0 . . ?
C66 C65 C70 120.1(3) . . ?
C66 C65 P4 118.0(2) . . ?
C70 C65 P4 121.7(2) . . ?
C67 C66 C65 119.8(3) . . ?
C67 C66 H66A 120.1 . . ?
C65 C66 H66A 120.1 . . ?
C68 C67 C66 119.9(3) . . ?
C68 C67 H67A 120.0 . . ?
C66 C67 H67A 120.0 . . ?
C69 C68 C67 120.5(3) . . ?
C69 C68 H68A 119.7 . . ?
C67 C68 H68A 119.7 . . ?
C68 C69 C70 119.8(3) . . ?
C68 C69 H69A 120.1 . . ?
C70 C69 H69A 120.1 . . ?
C65 C70 C69 119.8(3) . . ?
C65 C70 H70A 120.1 . . ?
C69 C70 H70A 120.1 . . ?
C76 C71 C72 118.9(3) . . ?
C76 C71 P4 122.6(3) . . ?
C72 C71 P4 118.6(2) . . ?
C73 C72 C71 120.4(3) . . ?
C73 C72 H72A 119.8 . . ?
C71 C72 H72A 119.8 . . ?
C72 C73 C74 120.4(3) . . ?
C72 C73 H73A 119.8 . . ?
C74 C73 H73A 119.8 . . ?
C75 C74 C73 119.3(3) . . ?
C75 C74 H74A 120.4 . . ?
C73 C74 H74A 120.4 . . ?
C74 C75 C76 120.7(3) . . ?
C74 C75 H75A 119.7 . . ?
C76 C75 H75A 119.7 . . ?
C71 C76 C75 120.3(3) . . ?
C71 C76 H76A 119.8 . . ?
C75 C76 H76A 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ni1 N1 C7 144.9(4) . . . . ?
P2 Ni1 N1 C7 -110.9(3) . . . . ?
P1 Ni1 N1 C7 37.8(3) . . . . ?
N2 Ni1 N1 O1 -33.8(5) . . . . ?
P2 Ni1 N1 O1 70.34(19) . . . . ?
P1 Ni1 N1 O1 -140.96(19) . . . . ?
N1 Ni1 N2 C26 140.9(4) . . . . ?
P2 Ni1 N2 C26 36.1(3) . . . . ?
P1 Ni1 N2 C26 -112.6(3) . . . . ?
N1 Ni1 N2 O2 -35.9(5) . . . . ?
P2 Ni1 N2 O2 -140.66(17) . . . . ?
P1 Ni1 N2 O2 70.55(17) . . . . ?
C14 P1 C1 C6 -16.5(3) . . . . ?
C8 P1 C1 C6 93.0(3) . . . . ?
Ni1 P1 C1 C6 -141.5(3) . . . . ?
C14 P1 C1 C2 166.1(2) . . . . ?
C8 P1 C1 C2 -84.3(3) . . . . ?
Ni1 P1 C1 C2 41.2(3) . . . . ?
C6 C1 C2 C3 -3.3(5) . . . . ?
P1 C1 C2 C3 174.2(2) . . . . ?
C6 C1 C2 C7 179.2(3) . . . . ?
P1 C1 C2 C7 -3.3(4) . . . . ?
C1 C2 C3 C4 0.9(5) . . . . ?
C7 C2 C3 C4 178.5(3) . . . . ?
C2 C3 C4 C5 1.9(5) . . . . ?
C3 C4 C5 C6 -2.2(5) . . . . ?
C4 C5 C6 C1 -0.2(5) . . . . ?
C2 C1 C6 C5 3.0(5) . . . . ?
P1 C1 C6 C5 -174.4(3) . . . . ?
O1 N1 C7 C2 175.5(3) . . . . ?
Ni1 N1 C7 C2 -3.1(5) . . . . ?
C3 C2 C7 N1 158.9(3) . . . . ?
C1 C2 C7 N1 -23.6(5) . . . . ?
C1 P1 C8 C9 155.8(3) . . . . ?
C14 P1 C8 C9 -93.2(3) . . . . ?
Ni1 P1 C8 C9 39.8(3) . . . . ?
C1 P1 C8 C13 -30.1(3) . . . . ?
C14 P1 C8 C13 80.8(3) . . . . ?
Ni1 P1 C8 C13 -146.1(2) . . . . ?
C13 C8 C9 C10 -1.5(5) . . . . ?
P1 C8 C9 C10 172.7(3) . . . . ?
C8 C9 C10 C11 0.9(5) . . . . ?
C9 C10 C11 C12 0.1(5) . . . . ?
C10 C11 C12 C13 -0.5(6) . . . . ?
C11 C12 C13 C8 -0.1(5) . . . . ?
C9 C8 C13 C12 1.1(5) . . . . ?
P1 C8 C13 C12 -172.9(3) . . . . ?
C1 P1 C14 C19 108.4(3) . . . . ?
C8 P1 C14 C19 -1.1(3) . . . . ?
Ni1 P1 C14 C19 -134.9(2) . . . . ?
C1 P1 C14 C15 -74.9(3) . . . . ?
C8 P1 C14 C15 175.7(3) . . . . ?
Ni1 P1 C14 C15 41.8(3) . . . . ?
C19 C14 C15 C16 0.1(5) . . . . ?
P1 C14 C15 C16 -176.8(3) . . . . ?
C14 C15 C16 C17 0.3(5) . . . . ?
C15 C16 C17 C18 -0.5(5) . . . . ?
C16 C17 C18 C19 0.4(5) . . . . ?
C17 C18 C19 C14 -0.1(5) . . . . ?
C15 C14 C19 C18 -0.2(5) . . . . ?
P1 C14 C19 C18 176.6(3) . . . . ?
C33 P2 C20 C25 -23.3(3) . . . . ?
C27 P2 C20 C25 89.4(3) . . . . ?
Ni1 P2 C20 C25 -143.8(2) . . . . ?
C33 P2 C20 C21 158.0(2) . . . . ?
C27 P2 C20 C21 -89.3(3) . . . . ?
Ni1 P2 C20 C21 37.5(3) . . . . ?
C25 C20 C21 C22 -0.3(4) . . . . ?
P2 C20 C21 C22 178.4(2) . . . . ?
C25 C20 C21 C26 -177.8(3) . . . . ?
P2 C20 C21 C26 0.9(4) . . . . ?
C20 C21 C22 C23 0.5(5) . . . . ?
C26 C21 C22 C23 178.2(3) . . . . ?
C21 C22 C23 C24 -0.5(5) . . . . ?
C22 C23 C24 C25 0.3(5) . . . . ?
C23 C24 C25 C20 -0.1(5) . . . . ?
C21 C20 C25 C24 0.1(5) . . . . ?
P2 C20 C25 C24 -178.6(2) . . . . ?
O2 N2 C26 C21 175.2(3) . . . . ?
Ni1 N2 C26 C21 -1.3(5) . . . . ?
C22 C21 C26 N2 155.8(3) . . . . ?
C20 C21 C26 N2 -26.7(5) . . . . ?
C33 P2 C27 C28 -95.5(3) . . . . ?
C20 P2 C27 C28 154.3(2) . . . . ?
Ni1 P2 C27 C28 35.7(3) . . . . ?
C33 P2 C27 C32 86.5(3) . . . . ?
C20 P2 C27 C32 -23.7(3) . . . . ?
Ni1 P2 C27 C32 -142.3(2) . . . . ?
C32 C27 C28 C29 -0.1(5) . . . . ?
P2 C27 C28 C29 -178.1(3) . . . . ?
C27 C28 C29 C30 0.4(5) . . . . ?
C28 C29 C30 C31 -0.7(5) . . . . ?
C29 C30 C31 C32 0.7(5) . . . . ?
C30 C31 C32 C27 -0.4(5) . . . . ?
C28 C27 C32 C31 0.1(5) . . . . ?
P2 C27 C32 C31 178.1(2) . . . . ?
C27 P2 C33 C38 -5.9(3) . . . . ?
C20 P2 C33 C38 105.2(3) . . . . ?
Ni1 P2 C33 C38 -139.7(2) . . . . ?
C27 P2 C33 C34 174.6(2) . . . . ?
C20 P2 C33 C34 -74.3(3) . . . . ?
Ni1 P2 C33 C34 40.8(3) . . . . ?
C38 C33 C34 C35 -0.8(5) . . . . ?
P2 C33 C34 C35 178.7(3) . . . . ?
C33 C34 C35 C36 0.6(5) . . . . ?
C34 C35 C36 C37 -0.3(5) . . . . ?
C35 C36 C37 C38 0.1(5) . . . . ?
C34 C33 C38 C37 0.6(5) . . . . ?
P2 C33 C38 C37 -178.9(3) . . . . ?
C36 C37 C38 C33 -0.2(5) . . . . ?
N4 Ni2 N3 C45 -144.9(4) . . . . ?
P3 Ni2 N3 C45 -35.9(3) . . . . ?
P4 Ni2 N3 C45 110.6(3) . . . . ?
N4 Ni2 N3 O3 32.0(4) . . . . ?
P3 Ni2 N3 O3 141.02(17) . . . . ?
P4 Ni2 N3 O3 -72.45(17) . . . . ?
N3 Ni2 N4 C64 -139.8(4) . . . . ?
P3 Ni2 N4 C64 112.4(3) . . . . ?
P4 Ni2 N4 C64 -34.4(3) . . . . ?
N3 Ni2 N4 O4 35.6(5) . . . . ?
P3 Ni2 N4 O4 -72.2(2) . . . . ?
P4 Ni2 N4 O4 141.0(2) . . . . ?
C52 P3 C39 C44 23.9(3) . . . . ?
C46 P3 C39 C44 -88.4(3) . . . . ?
Ni2 P3 C39 C44 146.3(2) . . . . ?
C52 P3 C39 C40 -160.5(2) . . . . ?
C46 P3 C39 C40 87.2(3) . . . . ?
Ni2 P3 C39 C40 -38.1(3) . . . . ?
C44 C39 C40 C41 1.0(4) . . . . ?
P3 C39 C40 C41 -174.7(2) . . . . ?
C44 C39 C40 C45 176.9(3) . . . . ?
P3 C39 C40 C45 1.2(4) . . . . ?
C39 C40 C41 C42 -1.2(4) . . . . ?
C45 C40 C41 C42 -177.4(3) . . . . ?
C40 C41 C42 C43 0.7(5) . . . . ?
C41 C42 C43 C44 0.1(5) . . . . ?
C42 C43 C44 C39 -0.3(5) . . . . ?
C40 C39 C44 C43 -0.2(5) . . . . ?
P3 C39 C44 C43 175.4(2) . . . . ?
O3 N3 C45 C40 -173.8(3) . . . . ?
Ni2 N3 C45 C40 2.6(5) . . . . ?
C41 C40 C45 N3 -160.1(3) . . . . ?
C39 C40 C45 N3 23.9(5) . . . . ?
C52 P3 C46 C51 -89.4(3) . . . . ?
C39 P3 C46 C51 19.2(3) . . . . ?
Ni2 P3 C46 C51 136.8(2) . . . . ?
C52 P3 C46 C47 93.9(3) . . . . ?
C39 P3 C46 C47 -157.5(3) . . . . ?
Ni2 P3 C46 C47 -39.9(3) . . . . ?
C51 C46 C47 C48 0.7(5) . . . . ?
P3 C46 C47 C48 177.5(3) . . . . ?
C46 C47 C48 C49 -0.4(5) . . . . ?
C47 C48 C49 C50 0.1(6) . . . . ?
C48 C49 C50 C51 0.1(6) . . . . ?
C47 C46 C51 C50 -0.5(5) . . . . ?
P3 C46 C51 C50 -177.2(3) . . . . ?
C49 C50 C51 C46 0.2(5) . . . . ?
C46 P3 C52 C57 13.7(3) . . . . ?
C39 P3 C52 C57 -95.1(3) . . . . ?
Ni2 P3 C52 C57 148.7(2) . . . . ?
C46 P3 C52 C53 -170.6(2) . . . . ?
C39 P3 C52 C53 80.6(3) . . . . ?
Ni2 P3 C52 C53 -35.6(3) . . . . ?
C57 C52 C53 C54 2.0(5) . . . . ?
P3 C52 C53 C54 -173.8(2) . . . . ?
C52 C53 C54 C55 -0.9(5) . . . . ?
C53 C54 C55 C56 -0.4(5) . . . . ?
C54 C55 C56 C57 0.6(5) . . . . ?
C55 C56 C57 C52 0.5(5) . . . . ?
C53 C52 C57 C56 -1.8(5) . . . . ?
P3 C52 C57 C56 173.8(3) . . . . ?
C71 P4 C58 C63 12.8(3) . . . . ?
C65 P4 C58 C63 -96.3(3) . . . . ?
Ni2 P4 C58 C63 138.5(2) . . . . ?
C71 P4 C58 C59 -170.7(2) . . . . ?
C65 P4 C58 C59 80.2(3) . . . . ?
Ni2 P4 C58 C59 -45.1(3) . . . . ?
C63 C58 C59 C60 4.5(4) . . . . ?
P4 C58 C59 C60 -172.1(2) . . . . ?
C63 C58 C59 C64 -176.7(3) . . . . ?
P4 C58 C59 C64 6.7(4) . . . . ?
C58 C59 C60 C61 -3.5(5) . . . . ?
C64 C59 C60 C61 177.7(3) . . . . ?
C59 C60 C61 C62 -0.1(5) . . . . ?
C60 C61 C62 C63 2.7(5) . . . . ?
C61 C62 C63 C58 -1.5(5) . . . . ?
C59 C58 C63 C62 -2.1(5) . . . . ?
P4 C58 C63 C62 174.4(3) . . . . ?
O4 N4 C64 C59 -176.9(3) . . . . ?
Ni2 N4 C64 C59 -2.0(5) . . . . ?
C60 C59 C64 N4 -156.5(3) . . . . ?
C58 C59 C64 N4 24.7(5) . . . . ?
C58 P4 C65 C66 -146.8(3) . . . . ?
C71 P4 C65 C66 102.5(3) . . . . ?
Ni2 P4 C65 C66 -30.9(3) . . . . ?
C58 P4 C65 C70 39.1(3) . . . . ?
C71 P4 C65 C70 -71.7(3) . . . . ?
Ni2 P4 C65 C70 155.0(2) . . . . ?
C70 C65 C66 C67 0.4(5) . . . . ?
P4 C65 C66 C67 -173.8(3) . . . . ?
C65 C66 C67 C68 1.5(5) . . . . ?
C66 C67 C68 C69 -1.8(5) . . . . ?
C67 C68 C69 C70 0.3(5) . . . . ?
C66 C65 C70 C69 -2.0(5) . . . . ?
P4 C65 C70 C69 172.1(2) . . . . ?
C68 C69 C70 C65 1.6(5) . . . . ?
C58 P4 C71 C76 -108.3(3) . . . . ?
C65 P4 C71 C76 1.7(3) . . . . ?
Ni2 P4 C71 C76 135.1(2) . . . . ?
C58 P4 C71 C72 73.2(3) . . . . ?
C65 P4 C71 C72 -176.8(3) . . . . ?
Ni2 P4 C71 C72 -43.4(3) . . . . ?
C76 C71 C72 C73 0.8(5) . . . . ?
P4 C71 C72 C73 179.4(3) . . . . ?
C71 C72 C73 C74 -0.8(5) . . . . ?
C72 C73 C74 C75 -0.1(5) . . . . ?
C73 C74 C75 C76 0.9(6) . . . . ?
C72 C71 C76 C75 0.0(5) . . . . ?
P4 C71 C76 C75 -178.5(3) . . . . ?
C74 C75 C76 C71 -0.8(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C9 H9A O2 0.95 2.47 3.290(4) 144.5 .
C28 H28A O1 0.95 2.34 3.183(4) 148.3 .
C47 H47A O4 0.95 2.33 3.213(4) 155.2 .
C66 H66A O3 0.95 2.45 3.244(4) 140.6 .

_refine_diff_density_max         0.558
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.051


loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.1210
0.00 -1.00 0.00 0.1340
0.00 0.00 1.00 0.0270
0.00 0.00 -1.00 0.0330
1.00 0.00 0.00 0.0580
####################################################################### 
# 
# 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_dd74ks
_database_code_depnum_ccdc_archive 'CCDC 1834877'
_audit_update_record             
;
2018-04-04 deposited with the CCDC.
2018-05-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7

_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
; 
? 
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
; 
C57 H44 B F4 N3 Ni2 O2 P3, B F4, 5(C H2 Cl2) 
;
_chemical_formula_sum            'C62 H54 B2 Cl10 F8 N3 Ni2 O2 P3'
_chemical_formula_structural     ?
_chemical_formula_weight         1611.53

_chemical_absolute_configuration ?
_chemical_formula_iupac          ?
_chemical_formula_analytical     ?
_chemical_compound_source        ?

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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

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

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

_cell_length_a                   13.1695(5)
_cell_length_b                   17.5545(7)
_cell_length_c                   17.7200(7)
_cell_angle_alpha                114.3978(10)
_cell_angle_beta                 108.0799(10)
_cell_angle_gamma                95.4562(10)
_cell_volume                     3426.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    56928
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      28.36
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_F_000             1632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.531
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.302
_exptl_crystal_id                dd74ks

_exptl_crystal_preparation       
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (3 -4 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_absorpt_coefficient_mu    1.077
_shelx_estimated_absorpt_T_min   0.599
_shelx_estimated_absorpt_T_max   0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6306
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS V2014/7 (Krause et al., 2015)'

_exptl_absorpt_special_details   ?
_exptl_special_details           
; 
One distinct cell was identified using APEX3 (Bruker, 2016). Eight frame series 
were integrated and filtered for statistical outliers using SAINT 
(Bruker, 2014) then corrected for absorption by the multi-scan method using 
SADABS v2014/7 (Krause et al., 2015). No decay correction was applied. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dd74ks
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_source                   ?
_diffrn_standards_number         ?
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_time  ?

_diffrn_measurement_device_type  ?
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            109093

_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.283
_diffrn_reflns_theta_max         28.373
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             17107
_reflns_number_gt                14510
_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       'APEX3 V2016.9-0 (Bruker, 2016)'

_computing_cell_refinement       'SAINT V8.37A (Bruker, 2014)'
_computing_data_reduction        
; 
SAINT V8.34A, XPREP v2014/2, (Bruker, 2014) SADABS V2014/7 
(Krause et al., 2015) 
;
_computing_structure_solution    'SHELXT-2014-4 (Sheldrick, 2015b)'
_computing_structure_refinement  'SHELXL-2014-7 (Sheldrick, 2015a)'
_computing_molecular_graphics    
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Structure was phased by intrinsic methods (Sheldrick, 2015b). Systematic 
conditions suggested the ambiguous space group. The space group choice was 
confirmed by successful convergence of the full-matrix least-squares refinement 
on F². The final difference Fourier map had no significant features. A final 
analysis of variance between observed and calculated structure factors showed 
a slight dependence on amplitude and little dependence on resolution. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0213P)²+3.2103P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         17107
_refine_ls_number_parameters     903
_refine_ls_number_restraints     252
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0714
_refine_ls_wR_factor_gt          0.0665
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

_refine_ls_abs_structure_details ?
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 0.67314(2) 0.16800(2) 0.37743(2) 0.00999(5) Uani 1 1 d . . . . .
Ni2 Ni 0.53945(2) -0.03130(2) 0.25500(2) 0.01088(5) Uani 1 1 d . . . . .
Cl1 Cl 0.2017(5) 0.0930(2) 0.2542(2) 0.0442(6) Uani 0.77(2) 1 d D U P A 1
Cl2 Cl 0.1858(5) 0.2572(4) 0.3819(3) 0.0511(8) Uani 0.77(2) 1 d D U P A 1
Cl1A Cl 0.2399(16) 0.0942(6) 0.2625(8) 0.0412(18) Uani 0.23(2) 1 d D U P A 2
Cl2A Cl 0.1578(10) 0.2307(11) 0.3640(11) 0.0441(17) Uani 0.23(2) 1 d D U P A 2
Cl3 Cl 0.20866(6) 0.15610(4) 0.70712(5) 0.04915(16) Uani 1 1 d . . . . .
Cl4 Cl 0.31600(5) 0.24003(4) 0.63050(4) 0.03624(12) Uani 1 1 d . . . . .
Cl5 Cl 0.59382(5) 0.51486(4) 0.25568(4) 0.03889(13) Uani 1 1 d . . . . .
Cl6 Cl 0.45830(6) 0.57569(4) 0.13991(4) 0.04235(14) Uani 1 1 d . . . . .
Cl7 Cl 0.73285(5) 0.51574(4) 0.10333(4) 0.03693(12) Uani 1 1 d . . . . .
Cl8 Cl 0.88413(5) 0.67144(4) 0.14244(4) 0.04454(14) Uani 1 1 d . . . . .
Cl9 Cl 0.07470(5) 0.16987(5) 0.09397(4) 0.04729(16) Uani 1 1 d . . . . .
Cl10 Cl -0.00462(5) 0.11159(4) -0.09897(4) 0.04104(14) Uani 1 1 d . . . . .
P1 P 0.82689(3) 0.18477(3) 0.48132(3) 0.01037(8) Uani 1 1 d . . . . .
P2 P 0.69585(3) 0.29121(3) 0.37402(3) 0.01110(8) Uani 1 1 d . . . . .
P3 P 0.43855(3) -0.13660(3) 0.12341(3) 0.01288(8) Uani 1 1 d . . . . .
O1 O 0.56472(10) 0.03583(7) 0.20292(8) 0.0149(2) Uani 1 1 d . . . . .
O2 O 0.58834(10) -0.04990(7) 0.40576(8) 0.0149(2) Uani 1 1 d . . . . .
N1 N 0.63082(11) 0.05741(8) 0.37011(9) 0.0114(3) Uani 1 1 d . . . . .
N2 N 0.56201(11) 0.11952(9) 0.25626(9) 0.0128(3) Uani 1 1 d . . . . .
N3 N 0.51675(11) -0.09282(9) 0.31294(9) 0.0130(3) Uani 1 1 d . . . . .
C1 C 0.64341(13) 0.03224(10) 0.42909(11) 0.0119(3) Uani 1 1 d . . . . .
C2 C 0.71446(13) 0.07711(10) 0.52551(11) 0.0119(3) Uani 1 1 d . . . . .
C3 C 0.69522(14) 0.04676(11) 0.58278(11) 0.0147(3) Uani 1 1 d . . . . .
H3 H 0.6353 -0.0018 0.5599 0.018 Uiso 1 1 calc R U . . .
C4 C 0.76384(14) 0.08777(11) 0.67301(12) 0.0162(3) Uani 1 1 d . . . . .
H4 H 0.7494 0.0685 0.7124 0.019 Uiso 1 1 calc R U . . .
C5 C 0.85362(14) 0.15699(11) 0.70596(12) 0.0162(3) Uani 1 1 d . . . . .
H5 H 0.9009 0.1846 0.7677 0.019 Uiso 1 1 calc R U . . .
C6 C 0.87460(14) 0.18608(11) 0.64895(11) 0.0147(3) Uani 1 1 d . . . . .
H6 H 0.9374 0.2324 0.6717 0.018 Uiso 1 1 calc R U . . .
C7 C 0.80424(13) 0.14773(10) 0.55868(11) 0.0123(3) Uani 1 1 d . . . . .
C8 C 0.89401(13) 0.10884(10) 0.42184(11) 0.0133(3) Uani 1 1 d . . . . .
C9 C 0.98877(15) 0.09326(11) 0.46958(12) 0.0185(3) Uani 1 1 d . . . . .
H9 H 1.0143 0.1179 0.5331 0.022 Uiso 1 1 calc R U . . .
C10 C 1.04568(16) 0.04172(13) 0.42431(14) 0.0243(4) Uani 1 1 d . . . . .
H10 H 1.1106 0.0317 0.4569 0.029 Uiso 1 1 calc R U . . .
C11 C 1.00770(18) 0.00498(13) 0.33167(14) 0.0274(4) Uani 1 1 d . . . . .
H11 H 1.0477 -0.0293 0.3009 0.033 Uiso 1 1 calc R U . . .
C12 C 0.91212(17) 0.01779(13) 0.28357(13) 0.0247(4) Uani 1 1 d . . . . .
H12 H 0.8855 -0.0090 0.2199 0.030 Uiso 1 1 calc R U . . .
C13 C 0.85488(15) 0.06975(11) 0.32819(12) 0.0170(3) Uani 1 1 d . . . . .
H13 H 0.7893 0.0787 0.2951 0.020 Uiso 1 1 calc R U . . .
C14 C 0.93573(13) 0.28463(10) 0.55196(11) 0.0129(3) Uani 1 1 d . . . . .
C15 C 0.92652(14) 0.35080(11) 0.62655(12) 0.0160(3) Uani 1 1 d . . . . .
H15 H 0.8629 0.3436 0.6399 0.019 Uiso 1 1 calc R U . . .
C16 C 1.01045(16) 0.42686(11) 0.68086(12) 0.0208(4) Uani 1 1 d . . . . .
H16 H 1.0043 0.4715 0.7315 0.025 Uiso 1 1 calc R U . . .
C17 C 1.10329(16) 0.43772(12) 0.66126(13) 0.0241(4) Uani 1 1 d . . . . .
H17 H 1.1609 0.4896 0.6990 0.029 Uiso 1 1 calc R U . . .
C18 C 1.11254(15) 0.37329(12) 0.58700(13) 0.0216(4) Uani 1 1 d . . . . .
H18 H 1.1760 0.3813 0.5736 0.026 Uiso 1 1 calc R U . . .
C19 C 1.02878(14) 0.29685(11) 0.53202(12) 0.0162(3) Uani 1 1 d . . . . .
H19 H 1.0349 0.2529 0.4809 0.019 Uiso 1 1 calc R U . . .
C20 C 0.48977(14) 0.14717(11) 0.21418(12) 0.0161(3) Uani 1 1 d . . . . .
H20 H 0.4429 0.1084 0.1536 0.019 Uiso 1 1 calc R U . . .
C21 C 0.47501(14) 0.23419(12) 0.25343(12) 0.0169(3) Uani 1 1 d . . . . .
C22 C 0.37228(15) 0.24631(13) 0.21405(14) 0.0240(4) Uani 1 1 d . . . . .
H22 H 0.3167 0.1990 0.1625 0.029 Uiso 1 1 calc R U . . .
C23 C 0.35069(16) 0.32682(14) 0.24949(15) 0.0294(5) Uani 1 1 d . . . . .
H23 H 0.2801 0.3343 0.2234 0.035 Uiso 1 1 calc R U . . .
C24 C 0.43247(17) 0.39577(14) 0.32280(15) 0.0281(4) Uani 1 1 d . . . . .
H24 H 0.4178 0.4509 0.3471 0.034 Uiso 1 1 calc R U . . .
C25 C 0.53642(15) 0.38575(12) 0.36173(13) 0.0209(4) Uani 1 1 d . . . . .
H25 H 0.5923 0.4341 0.4117 0.025 Uiso 1 1 calc R U . . .
C26 C 0.55863(14) 0.30501(11) 0.32761(12) 0.0151(3) Uani 1 1 d . . . . .
C27 C 0.75894(13) 0.29188(10) 0.29635(11) 0.0131(3) Uani 1 1 d . . . . .
C28 C 0.85250(14) 0.26061(11) 0.29781(12) 0.0161(3) Uani 1 1 d . . . . .
H28 H 0.8798 0.2363 0.3366 0.019 Uiso 1 1 calc R U . . .
C29 C 0.90619(15) 0.26479(12) 0.24286(12) 0.0207(4) Uani 1 1 d . . . . .
H29 H 0.9693 0.2426 0.2435 0.025 Uiso 1 1 calc R U . . .
C30 C 0.86754(15) 0.30136(12) 0.18706(12) 0.0215(4) Uani 1 1 d . . . . .
H30 H 0.9055 0.3058 0.1508 0.026 Uiso 1 1 calc R U . . .
C31 C 0.77356(16) 0.33141(11) 0.18423(12) 0.0198(4) Uani 1 1 d . . . . .
H31 H 0.7466 0.3556 0.1452 0.024 Uiso 1 1 calc R U . . .
C32 C 0.71846(15) 0.32637(11) 0.23811(12) 0.0170(3) Uani 1 1 d . . . . .
H32 H 0.6535 0.3463 0.2353 0.020 Uiso 1 1 calc R U . . .
C33 C 0.76392(13) 0.39321(10) 0.47508(11) 0.0131(3) Uani 1 1 d . . . . .
C34 C 0.72658(14) 0.41103(11) 0.54491(12) 0.0160(3) Uani 1 1 d . . . . .
H34 H 0.6710 0.3684 0.5398 0.019 Uiso 1 1 calc R U . . .
C35 C 0.77021(15) 0.49027(11) 0.62117(12) 0.0185(3) Uani 1 1 d . . . . .
H35 H 0.7448 0.5020 0.6685 0.022 Uiso 1 1 calc R U . . .
C36 C 0.85135(15) 0.55296(11) 0.62884(13) 0.0208(4) Uani 1 1 d . . . . .
H36 H 0.8812 0.6075 0.6813 0.025 Uiso 1 1 calc R U . . .
C37 C 0.88864(15) 0.53580(11) 0.55989(13) 0.0216(4) Uani 1 1 d . . . . .
H37 H 0.9442 0.5787 0.5654 0.026 Uiso 1 1 calc R U . . .
C38 C 0.84536(14) 0.45627(11) 0.48282(12) 0.0171(3) Uani 1 1 d . . . . .
H38 H 0.8710 0.4448 0.4356 0.021 Uiso 1 1 calc R U . . .
C39 C 0.45246(14) -0.16321(10) 0.29497(11) 0.0143(3) Uani 1 1 d . . . . .
H39 H 0.4632 -0.1784 0.3419 0.017 Uiso 1 1 calc R U . . .
C40 C 0.36455(14) -0.22140(10) 0.20822(12) 0.0148(3) Uani 1 1 d . . . . .
C41 C 0.29222(15) -0.28614(11) 0.20735(13) 0.0192(4) Uani 1 1 d . . . . .
H41 H 0.3068 -0.2929 0.2599 0.023 Uiso 1 1 calc R U . . .
C42 C 0.19959(15) -0.34042(11) 0.13055(14) 0.0227(4) Uani 1 1 d . . . . .
H42 H 0.1509 -0.3837 0.1309 0.027 Uiso 1 1 calc R U . . .
C43 C 0.17805(15) -0.33153(12) 0.05353(13) 0.0233(4) Uani 1 1 d . . . . .
H43 H 0.1140 -0.3681 0.0012 0.028 Uiso 1 1 calc R U . . .
C44 C 0.25032(15) -0.26892(11) 0.05275(12) 0.0199(4) Uani 1 1 d . . . . .
H44 H 0.2356 -0.2637 -0.0007 0.024 Uiso 1 1 calc R U . . .
C45 C 0.34395(14) -0.21368(10) 0.12908(12) 0.0150(3) Uani 1 1 d . . . . .
C46 C 0.52195(14) -0.19674(11) 0.06915(11) 0.0169(3) Uani 1 1 d . . . . .
C47 C 0.61403(17) -0.15032(13) 0.06949(15) 0.0302(5) Uani 1 1 d . . . . .
H47 H 0.6314 -0.0889 0.0975 0.036 Uiso 1 1 calc R U . . .
C48 C 0.68038(19) -0.19367(15) 0.02895(17) 0.0393(6) Uani 1 1 d . . . . .
H48 H 0.7419 -0.1620 0.0276 0.047 Uiso 1 1 calc R U . . .
C49 C 0.65711(19) -0.28310(15) -0.00959(16) 0.0351(5) Uani 1 1 d . . . . .
H49 H 0.7034 -0.3127 -0.0363 0.042 Uiso 1 1 calc R U . . .
C50 C 0.5668(2) -0.32912(14) -0.00908(16) 0.0351(5) Uani 1 1 d . . . . .
H50 H 0.5510 -0.3905 -0.0357 0.042 Uiso 1 1 calc R U . . .
C51 C 0.49861(17) -0.28664(12) 0.02996(14) 0.0255(4) Uani 1 1 d . . . . .
H51 H 0.4363 -0.3188 0.0299 0.031 Uiso 1 1 calc R U . . .
C52 C 0.35312(14) -0.10105(11) 0.04939(11) 0.0158(3) Uani 1 1 d . . . . .
C53 C 0.27222(16) -0.06290(13) 0.07341(13) 0.0237(4) Uani 1 1 d . . . . .
H53 H 0.2609 -0.0596 0.1250 0.028 Uiso 1 1 calc R U . . .
C54 C 0.20819(16) -0.02977(14) 0.02231(14) 0.0278(4) Uani 1 1 d . . . . .
H54 H 0.1527 -0.0043 0.0384 0.033 Uiso 1 1 calc R U . . .
C55 C 0.22555(17) -0.03397(13) -0.05199(14) 0.0278(4) Uani 1 1 d . . . . .
H55 H 0.1817 -0.0113 -0.0870 0.033 Uiso 1 1 calc R U . . .
C56 C 0.30607(18) -0.07081(13) -0.07602(14) 0.0281(4) Uani 1 1 d . . . . .
H56 H 0.3177 -0.0731 -0.1271 0.034 Uiso 1 1 calc R U . . .
C57 C 0.37018(16) -0.10464(12) -0.02528(12) 0.0212(4) Uani 1 1 d . . . . .
H57 H 0.4255 -0.1301 -0.0418 0.025 Uiso 1 1 calc R U . . .
C58 C 0.2648(6) 0.1822(5) 0.3631(4) 0.0303(15) Uani 0.77(2) 1 d D U P A 1
H58A H 0.2758 0.1611 0.4082 0.036 Uiso 0.77(2) 1 calc R U P A 1
H58B H 0.3384 0.2112 0.3710 0.036 Uiso 0.77(2) 1 calc R U P A 1
C58A C 0.261(2) 0.175(2) 0.3705(11) 0.031(4) Uani 0.23(2) 1 d D U P A 2
H58C H 0.2597 0.1481 0.4096 0.037 Uiso 0.23(2) 1 calc R U P A 2
H58D H 0.3346 0.2160 0.3972 0.037 Uiso 0.23(2) 1 calc R U P A 2
C59 C 0.2564(2) 0.25514(15) 0.71020(19) 0.0420(6) Uani 1 1 d . . . . .
H59A H 0.1939 0.2813 0.6979 0.050 Uiso 1 1 calc R U . . .
H59B H 0.3120 0.2956 0.7710 0.050 Uiso 1 1 calc R U . . .
C60 C 0.47514(18) 0.55384(16) 0.23128(15) 0.0338(5) Uani 1 1 d . . . . .
H60A H 0.4090 0.5101 0.2164 0.041 Uiso 1 1 calc R U . . .
H60B H 0.4826 0.6074 0.2848 0.041 Uiso 1 1 calc R U . . .
C61 C 0.8367(2) 0.55745(14) 0.07695(17) 0.0357(5) Uani 1 1 d . . . . .
H61A H 0.8068 0.5420 0.0124 0.043 Uiso 1 1 calc R U . . .
H61B H 0.8993 0.5312 0.0883 0.043 Uiso 1 1 calc R U . . .
C62 C 0.0186(2) 0.1971(2) 0.00749(16) 0.0517(8) Uani 1 1 d . . . . .
H62A H 0.0699 0.2491 0.0186 0.062 Uiso 1 1 calc R U . . .
H62B H -0.0522 0.2114 0.0079 0.062 Uiso 1 1 calc R U . . .
B1 B 0.52658(17) 0.22916(14) 0.52068(14) 0.0196(4) Uani 1 1 d D . . . .
F1 F 0.46671(12) 0.15290(9) 0.50814(9) 0.0441(4) Uani 1 1 d D . . . .
F2 F 0.47736(11) 0.29562(9) 0.55308(9) 0.0420(3) Uani 1 1 d D . . . .
F3 F 0.63381(9) 0.25081(8) 0.58255(8) 0.0301(3) Uani 1 1 d D . . . .
F4 F 0.52842(9) 0.21909(7) 0.43919(7) 0.0230(2) Uani 1 1 d D . . . .
B2 B 0.1244(6) 0.4506(4) 0.1341(5) 0.0218(14) Uani 0.572(3) 1 d D U P B 1
F5 F 0.2045(2) 0.4120(2) 0.1127(3) 0.0574(10) Uani 0.572(3) 1 d D U P B 1
F6 F 0.0590(3) 0.39975(19) 0.1525(2) 0.0426(8) Uani 0.572(3) 1 d D U P B 1
F7 F 0.1758(3) 0.53192(16) 0.20860(16) 0.0618(11) Uani 0.572(3) 1 d D U P B 1
F8 F 0.06133(17) 0.46256(14) 0.06381(17) 0.0331(6) Uani 0.572(3) 1 d D U P B 1
B2A B 0.1249(9) 0.4295(6) 0.1306(7) 0.025(2) Uani 0.428(3) 1 d D U P B 2
F5A F 0.1107(4) 0.3771(2) 0.0410(2) 0.0533(12) Uani 0.428(3) 1 d D U P B 2
F6A F 0.0967(3) 0.3744(3) 0.1629(3) 0.0294(8) Uani 0.428(3) 1 d D U P B 2
F7A F 0.2313(2) 0.4770(3) 0.1796(3) 0.0459(11) Uani 0.428(3) 1 d D U P B 2
F8A F 0.0546(3) 0.4822(2) 0.1310(3) 0.0449(10) Uani 0.428(3) 1 d D U P 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 N1 1.9071(13) . ?
Ni1 N2 1.9440(14) . ?
Ni1 P1 2.1682(5) . ?
Ni1 P2 2.1835(4) . ?
Ni2 N3 1.8316(14) . ?
Ni2 O1 1.8346(12) . ?
Ni2 N1 1.8788(14) . ?
Ni2 P3 2.1607(5) . ?
Cl1 C58 1.768(4) . ?
Cl2 C58 1.743(4) . ?
Cl1A C58A 1.760(8) . ?
Cl2A C58A 1.753(8) . ?
Cl3 C59 1.765(2) . ?
Cl4 C59 1.760(2) . ?
Cl5 C60 1.768(2) . ?
Cl6 C60 1.768(2) . ?
Cl7 C61 1.764(2) . ?
Cl8 C61 1.771(2) . ?
Cl9 C62 1.758(3) . ?
Cl10 C62 1.766(2) . ?
P1 C14 1.8137(17) . ?
P1 C8 1.8195(17) . ?
P1 C7 1.8288(17) . ?
P2 C33 1.8072(17) . ?
P2 C27 1.8183(17) . ?
P2 C26 1.8238(17) . ?
P3 C45 1.8062(17) . ?
P3 C52 1.8081(18) . ?
P3 C46 1.8119(18) . ?
O1 N2 1.3916(17) . ?
O2 C1 1.3779(19) . ?
O2 N3 1.4284(17) . ?
N1 C1 1.266(2) . ?
N2 C20 1.282(2) . ?
N3 C39 1.286(2) . ?
C1 C2 1.473(2) . ?
C2 C3 1.400(2) . ?
C2 C7 1.403(2) . ?
C3 C4 1.385(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.389(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.394(2) . ?
C6 H6 0.9500 . ?
C8 C9 1.396(2) . ?
C8 C13 1.397(2) . ?
C9 C10 1.388(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(2) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.398(2) . ?
C14 C15 1.403(2) . ?
C15 C16 1.389(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.386(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.392(2) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.455(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.398(2) . ?
C21 C26 1.406(2) . ?
C22 C23 1.388(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.377(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.393(2) . ?
C25 H25 0.9500 . ?
C27 C28 1.393(2) . ?
C27 C32 1.397(2) . ?
C28 C29 1.389(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.386(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.391(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.397(2) . ?
C33 C34 1.399(2) . ?
C34 C35 1.380(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.391(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.386(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.389(2) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.456(2) . ?
C39 H39 0.9500 . ?
C40 C41 1.403(2) . ?
C40 C45 1.409(2) . ?
C41 C42 1.388(3) . ?
C41 H41 0.9500 . ?
C42 C43 1.383(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.391(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.394(2) . ?
C44 H44 0.9500 . ?
C46 C51 1.392(2) . ?
C46 C47 1.392(3) . ?
C47 C48 1.387(3) . ?
C47 H47 0.9500 . ?
C48 C49 1.385(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.378(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.388(3) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C57 1.387(2) . ?
C52 C53 1.395(3) . ?
C53 C54 1.387(3) . ?
C53 H53 0.9500 . ?
C54 C55 1.379(3) . ?
C54 H54 0.9500 . ?
C55 C56 1.381(3) . ?
C55 H55 0.9500 . ?
C56 C57 1.393(3) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58A H58C 0.9900 . ?
C58A H58D 0.9900 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
B1 F1 1.381(2) . ?
B1 F4 1.389(2) . ?
B1 F2 1.390(2) . ?
B1 F3 1.391(2) . ?
B2 F5 1.373(8) . ?
B2 F8 1.375(8) . ?
B2 F6 1.384(7) . ?
B2 F7 1.394(7) . ?
B2A F7A 1.356(10) . ?
B2A F8A 1.369(10) . ?
B2A F6A 1.386(10) . ?
B2A F5A 1.405(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 86.39(6) . . ?
N1 Ni1 P1 85.25(4) . . ?
N2 Ni1 P1 156.59(4) . . ?
N1 Ni1 P2 171.53(4) . . ?
N2 Ni1 P2 86.69(4) . . ?
P1 Ni1 P2 102.984(17) . . ?
N3 Ni2 O1 176.82(6) . . ?
N3 Ni2 N1 85.40(6) . . ?
O1 Ni2 N1 91.60(5) . . ?
N3 Ni2 P3 93.46(4) . . ?
O1 Ni2 P3 89.58(4) . . ?
N1 Ni2 P3 177.73(4) . . ?
C14 P1 C8 103.61(8) . . ?
C14 P1 C7 105.09(8) . . ?
C8 P1 C7 104.39(7) . . ?
C14 P1 Ni1 124.98(5) . . ?
C8 P1 Ni1 104.50(6) . . ?
C7 P1 Ni1 112.20(5) . . ?
C33 P2 C27 106.10(7) . . ?
C33 P2 C26 102.44(8) . . ?
C27 P2 C26 104.00(8) . . ?
C33 P2 Ni1 122.03(6) . . ?
C27 P2 Ni1 113.12(5) . . ?
C26 P2 Ni1 107.25(6) . . ?
C45 P3 C52 105.57(8) . . ?
C45 P3 C46 106.32(8) . . ?
C52 P3 C46 108.22(8) . . ?
C45 P3 Ni2 111.74(6) . . ?
C52 P3 Ni2 112.98(6) . . ?
C46 P3 Ni2 111.59(6) . . ?
N2 O1 Ni2 108.19(9) . . ?
C1 O2 N3 109.89(12) . . ?
C1 N1 Ni2 111.56(11) . . ?
C1 N1 Ni1 132.74(12) . . ?
Ni2 N1 Ni1 115.34(7) . . ?
C20 N2 O1 113.47(14) . . ?
C20 N2 Ni1 135.14(12) . . ?
O1 N2 Ni1 111.36(10) . . ?
C39 N3 O2 109.65(13) . . ?
C39 N3 Ni2 138.37(12) . . ?
O2 N3 Ni2 111.94(9) . . ?
N1 C1 O2 120.32(15) . . ?
N1 C1 C2 130.04(15) . . ?
O2 C1 C2 109.61(13) . . ?
C3 C2 C7 120.29(15) . . ?
C3 C2 C1 119.94(15) . . ?
C7 C2 C1 119.71(14) . . ?
C4 C3 C2 119.82(16) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 120.11(16) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.28(16) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C7 120.48(16) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C2 118.97(15) . . ?
C6 C7 P1 122.18(12) . . ?
C2 C7 P1 118.84(12) . . ?
C9 C8 C13 119.53(15) . . ?
C9 C8 P1 120.26(13) . . ?
C13 C8 P1 120.10(13) . . ?
C10 C9 C8 120.05(17) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 C10 C9 119.94(17) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C12 C11 C10 120.46(17) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.11(18) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C8 119.86(17) . . ?
C12 C13 H13 120.1 . . ?
C8 C13 H13 120.1 . . ?
C19 C14 C15 119.40(15) . . ?
C19 C14 P1 120.39(13) . . ?
C15 C14 P1 120.20(13) . . ?
C16 C15 C14 120.00(16) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C17 C16 C15 120.09(17) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 C16 120.40(17) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 119.97(17) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C14 120.12(17) . . ?
C18 C19 H19 119.9 . . ?
C14 C19 H19 119.9 . . ?
N2 C20 C21 124.12(16) . . ?
N2 C20 H20 117.9 . . ?
C21 C20 H20 117.9 . . ?
C22 C21 C26 119.63(17) . . ?
C22 C21 C20 117.27(17) . . ?
C26 C21 C20 123.09(15) . . ?
C23 C22 C21 120.65(19) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C22 119.47(18) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 120.89(18) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 120.20(18) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C21 119.13(16) . . ?
C25 C26 P2 121.04(14) . . ?
C21 C26 P2 119.76(13) . . ?
C28 C27 C32 119.43(15) . . ?
C28 C27 P2 119.08(13) . . ?
C32 C27 P2 121.43(13) . . ?
C29 C28 C27 120.40(16) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C30 C29 C28 119.95(17) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C31 C30 C29 119.98(16) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C32 120.40(17) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 119.80(16) . . ?
C31 C32 H32 120.1 . . ?
C27 C32 H32 120.1 . . ?
C38 C33 C34 119.61(15) . . ?
C38 C33 P2 122.52(13) . . ?
C34 C33 P2 117.68(12) . . ?
C35 C34 C33 120.24(16) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 120.09(17) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 119.98(17) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C38 120.45(17) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C37 C38 C33 119.62(16) . . ?
C37 C38 H38 120.2 . . ?
C33 C38 H38 120.2 . . ?
N3 C39 C40 125.09(16) . . ?
N3 C39 H39 117.5 . . ?
C40 C39 H39 117.5 . . ?
C41 C40 C45 119.18(16) . . ?
C41 C40 C39 115.56(16) . . ?
C45 C40 C39 125.13(15) . . ?
C42 C41 C40 120.71(18) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C43 C42 C41 120.07(17) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C42 C43 C44 119.88(17) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C43 C44 C45 121.08(18) . . ?
C43 C44 H44 119.5 . . ?
C45 C44 H44 119.5 . . ?
C44 C45 C40 119.05(16) . . ?
C44 C45 P3 119.46(14) . . ?
C40 C45 P3 121.45(13) . . ?
C51 C46 C47 119.62(17) . . ?
C51 C46 P3 122.25(14) . . ?
C47 C46 P3 118.11(14) . . ?
C48 C47 C46 120.08(19) . . ?
C48 C47 H47 120.0 . . ?
C46 C47 H47 120.0 . . ?
C49 C48 C47 120.1(2) . . ?
C49 C48 H48 120.0 . . ?
C47 C48 H48 120.0 . . ?
C50 C49 C48 119.95(19) . . ?
C50 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C49 C50 C51 120.6(2) . . ?
C49 C50 H50 119.7 . . ?
C51 C50 H50 119.7 . . ?
C50 C51 C46 119.68(19) . . ?
C50 C51 H51 120.2 . . ?
C46 C51 H51 120.2 . . ?
C57 C52 C53 119.59(17) . . ?
C57 C52 P3 122.84(14) . . ?
C53 C52 P3 117.41(13) . . ?
C54 C53 C52 120.26(18) . . ?
C54 C53 H53 119.9 . . ?
C52 C53 H53 119.9 . . ?
C55 C54 C53 119.67(19) . . ?
C55 C54 H54 120.2 . . ?
C53 C54 H54 120.2 . . ?
C54 C55 C56 120.66(18) . . ?
C54 C55 H55 119.7 . . ?
C56 C55 H55 119.7 . . ?
C55 C56 C57 119.94(18) . . ?
C55 C56 H56 120.0 . . ?
C57 C56 H56 120.0 . . ?
C52 C57 C56 119.87(18) . . ?
C52 C57 H57 120.1 . . ?
C56 C57 H57 120.1 . . ?
Cl2 C58 Cl1 112.2(3) . . ?
Cl2 C58 H58A 109.2 . . ?
Cl1 C58 H58A 109.2 . . ?
Cl2 C58 H58B 109.2 . . ?
Cl1 C58 H58B 109.2 . . ?
H58A C58 H58B 107.9 . . ?
Cl2A C58A Cl1A 110.0(9) . . ?
Cl2A C58A H58C 109.7 . . ?
Cl1A C58A H58C 109.7 . . ?
Cl2A C58A H58D 109.7 . . ?
Cl1A C58A H58D 109.7 . . ?
H58C C58A H58D 108.2 . . ?
Cl4 C59 Cl3 111.22(13) . . ?
Cl4 C59 H59A 109.4 . . ?
Cl3 C59 H59A 109.4 . . ?
Cl4 C59 H59B 109.4 . . ?
Cl3 C59 H59B 109.4 . . ?
H59A C59 H59B 108.0 . . ?
Cl6 C60 Cl5 110.44(12) . . ?
Cl6 C60 H60A 109.6 . . ?
Cl5 C60 H60A 109.6 . . ?
Cl6 C60 H60B 109.6 . . ?
Cl5 C60 H60B 109.6 . . ?
H60A C60 H60B 108.1 . . ?
Cl7 C61 Cl8 110.76(12) . . ?
Cl7 C61 H61A 109.5 . . ?
Cl8 C61 H61A 109.5 . . ?
Cl7 C61 H61B 109.5 . . ?
Cl8 C61 H61B 109.5 . . ?
H61A C61 H61B 108.1 . . ?
Cl9 C62 Cl10 111.79(15) . . ?
Cl9 C62 H62A 109.3 . . ?
Cl10 C62 H62A 109.3 . . ?
Cl9 C62 H62B 109.3 . . ?
Cl10 C62 H62B 109.3 . . ?
H62A C62 H62B 107.9 . . ?
F1 B1 F4 109.43(17) . . ?
F1 B1 F2 109.89(17) . . ?
F4 B1 F2 108.78(15) . . ?
F1 B1 F3 109.81(15) . . ?
F4 B1 F3 110.04(15) . . ?
F2 B1 F3 108.88(17) . . ?
F5 B2 F8 109.4(5) . . ?
F5 B2 F6 110.0(5) . . ?
F8 B2 F6 110.5(5) . . ?
F5 B2 F7 108.7(6) . . ?
F8 B2 F7 107.8(5) . . ?
F6 B2 F7 110.4(5) . . ?
F7A B2A F8A 110.7(7) . . ?
F7A B2A F6A 110.9(7) . . ?
F8A B2A F6A 110.0(8) . . ?
F7A B2A F5A 110.1(8) . . ?
F8A B2A F5A 108.2(7) . . ?
F6A B2A F5A 106.9(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni2 O1 N2 -41.60(10) . . . . ?
P3 Ni2 O1 N2 140.34(9) . . . . ?
N3 Ni2 N1 C1 6.83(12) . . . . ?
O1 Ni2 N1 C1 -174.24(12) . . . . ?
N3 Ni2 N1 Ni1 -167.15(8) . . . . ?
O1 Ni2 N1 Ni1 11.78(7) . . . . ?
Ni2 O1 N2 C20 -122.30(12) . . . . ?
Ni2 O1 N2 Ni1 59.30(10) . . . . ?
C1 O2 N3 C39 -169.40(13) . . . . ?
C1 O2 N3 Ni2 8.93(14) . . . . ?
N1 Ni2 N3 C39 168.92(19) . . . . ?
P3 Ni2 N3 C39 -13.04(18) . . . . ?
N1 Ni2 N3 O2 -8.70(10) . . . . ?
P3 Ni2 N3 O2 169.33(9) . . . . ?
Ni2 N1 C1 O2 -3.31(19) . . . . ?
Ni1 N1 C1 O2 169.27(11) . . . . ?
Ni2 N1 C1 C2 174.38(14) . . . . ?
Ni1 N1 C1 C2 -13.0(3) . . . . ?
N3 O2 C1 N1 -3.6(2) . . . . ?
N3 O2 C1 C2 178.24(12) . . . . ?
N1 C1 C2 C3 163.68(17) . . . . ?
O2 C1 C2 C3 -18.4(2) . . . . ?
N1 C1 C2 C7 -19.2(3) . . . . ?
O2 C1 C2 C7 158.65(14) . . . . ?
C7 C2 C3 C4 1.3(2) . . . . ?
C1 C2 C3 C4 178.40(15) . . . . ?
C2 C3 C4 C5 -2.1(2) . . . . ?
C3 C4 C5 C6 0.6(3) . . . . ?
C4 C5 C6 C7 1.7(2) . . . . ?
C5 C6 C7 C2 -2.5(2) . . . . ?
C5 C6 C7 P1 178.96(13) . . . . ?
C3 C2 C7 C6 1.0(2) . . . . ?
C1 C2 C7 C6 -176.09(14) . . . . ?
C3 C2 C7 P1 179.56(12) . . . . ?
C1 C2 C7 P1 2.5(2) . . . . ?
C14 P1 C7 C6 -9.60(15) . . . . ?
C8 P1 C7 C6 99.12(14) . . . . ?
Ni1 P1 C7 C6 -148.30(12) . . . . ?
C14 P1 C7 C2 171.88(12) . . . . ?
C8 P1 C7 C2 -79.40(14) . . . . ?
Ni1 P1 C7 C2 33.18(14) . . . . ?
C14 P1 C8 C9 56.75(15) . . . . ?
C7 P1 C8 C9 -53.04(15) . . . . ?
Ni1 P1 C8 C9 -171.03(12) . . . . ?
C14 P1 C8 C13 -119.39(14) . . . . ?
C7 P1 C8 C13 130.81(14) . . . . ?
Ni1 P1 C8 C13 12.82(14) . . . . ?
C13 C8 C9 C10 2.3(3) . . . . ?
P1 C8 C9 C10 -173.90(14) . . . . ?
C8 C9 C10 C11 -0.7(3) . . . . ?
C9 C10 C11 C12 -1.3(3) . . . . ?
C10 C11 C12 C13 1.8(3) . . . . ?
C11 C12 C13 C8 -0.2(3) . . . . ?
C9 C8 C13 C12 -1.8(3) . . . . ?
P1 C8 C13 C12 174.36(14) . . . . ?
C8 P1 C14 C19 19.78(15) . . . . ?
C7 P1 C14 C19 129.06(14) . . . . ?
Ni1 P1 C14 C19 -99.16(13) . . . . ?
C8 P1 C14 C15 -161.03(13) . . . . ?
C7 P1 C14 C15 -51.76(15) . . . . ?
Ni1 P1 C14 C15 80.02(14) . . . . ?
C19 C14 C15 C16 -1.3(2) . . . . ?
P1 C14 C15 C16 179.49(13) . . . . ?
C14 C15 C16 C17 0.3(3) . . . . ?
C15 C16 C17 C18 0.7(3) . . . . ?
C16 C17 C18 C19 -0.5(3) . . . . ?
C17 C18 C19 C14 -0.5(3) . . . . ?
C15 C14 C19 C18 1.4(2) . . . . ?
P1 C14 C19 C18 -179.37(13) . . . . ?
O1 N2 C20 C21 -176.31(14) . . . . ?
Ni1 N2 C20 C21 1.6(3) . . . . ?
N2 C20 C21 C22 -157.50(17) . . . . ?
N2 C20 C21 C26 22.8(3) . . . . ?
C26 C21 C22 C23 -2.4(3) . . . . ?
C20 C21 C22 C23 177.88(17) . . . . ?
C21 C22 C23 C24 1.7(3) . . . . ?
C22 C23 C24 C25 0.0(3) . . . . ?
C23 C24 C25 C26 -1.0(3) . . . . ?
C24 C25 C26 C21 0.2(3) . . . . ?
C24 C25 C26 P2 177.13(15) . . . . ?
C22 C21 C26 C25 1.5(3) . . . . ?
C20 C21 C26 C25 -178.86(16) . . . . ?
C22 C21 C26 P2 -175.51(13) . . . . ?
C20 C21 C26 P2 4.2(2) . . . . ?
C33 P2 C26 C25 11.26(16) . . . . ?
C27 P2 C26 C25 -99.08(15) . . . . ?
Ni1 P2 C26 C25 140.84(13) . . . . ?
C33 P2 C26 C21 -171.83(13) . . . . ?
C27 P2 C26 C21 77.83(14) . . . . ?
Ni1 P2 C26 C21 -42.25(14) . . . . ?
C33 P2 C27 C28 88.93(14) . . . . ?
C26 P2 C27 C28 -163.43(13) . . . . ?
Ni1 P2 C27 C28 -47.40(14) . . . . ?
C33 P2 C27 C32 -88.31(15) . . . . ?
C26 P2 C27 C32 19.33(16) . . . . ?
Ni1 P2 C27 C32 135.35(13) . . . . ?
C32 C27 C28 C29 0.9(3) . . . . ?
P2 C27 C28 C29 -176.35(13) . . . . ?
C27 C28 C29 C30 0.9(3) . . . . ?
C28 C29 C30 C31 -1.9(3) . . . . ?
C29 C30 C31 C32 1.0(3) . . . . ?
C30 C31 C32 C27 0.9(3) . . . . ?
C28 C27 C32 C31 -1.8(2) . . . . ?
P2 C27 C32 C31 175.41(13) . . . . ?
C27 P2 C33 C38 1.87(16) . . . . ?
C26 P2 C33 C38 -106.88(15) . . . . ?
Ni1 P2 C33 C38 133.37(13) . . . . ?
C27 P2 C33 C34 176.99(13) . . . . ?
C26 P2 C33 C34 68.23(14) . . . . ?
Ni1 P2 C33 C34 -51.51(15) . . . . ?
C38 C33 C34 C35 -0.3(3) . . . . ?
P2 C33 C34 C35 -175.54(13) . . . . ?
C33 C34 C35 C36 0.2(3) . . . . ?
C34 C35 C36 C37 -0.1(3) . . . . ?
C35 C36 C37 C38 0.1(3) . . . . ?
C36 C37 C38 C33 -0.2(3) . . . . ?
C34 C33 C38 C37 0.3(3) . . . . ?
P2 C33 C38 C37 175.29(14) . . . . ?
O2 N3 C39 C40 176.52(14) . . . . ?
Ni2 N3 C39 C40 -1.1(3) . . . . ?
N3 C39 C40 C41 -169.30(16) . . . . ?
N3 C39 C40 C45 6.5(3) . . . . ?
C45 C40 C41 C42 -1.9(3) . . . . ?
C39 C40 C41 C42 174.16(16) . . . . ?
C40 C41 C42 C43 0.5(3) . . . . ?
C41 C42 C43 C44 1.0(3) . . . . ?
C42 C43 C44 C45 -0.9(3) . . . . ?
C43 C44 C45 C40 -0.5(3) . . . . ?
C43 C44 C45 P3 177.30(14) . . . . ?
C41 C40 C45 C44 1.9(2) . . . . ?
C39 C40 C45 C44 -173.76(16) . . . . ?
C41 C40 C45 P3 -175.84(13) . . . . ?
C39 C40 C45 P3 8.5(2) . . . . ?
C52 P3 C45 C44 36.15(16) . . . . ?
C46 P3 C45 C44 -78.67(15) . . . . ?
Ni2 P3 C45 C44 159.35(12) . . . . ?
C52 P3 C45 C40 -146.07(14) . . . . ?
C46 P3 C45 C40 99.11(15) . . . . ?
Ni2 P3 C45 C40 -22.88(15) . . . . ?
C45 P3 C46 C51 8.61(18) . . . . ?
C52 P3 C46 C51 -104.39(17) . . . . ?
Ni2 P3 C46 C51 130.69(15) . . . . ?
C45 P3 C46 C47 -169.54(16) . . . . ?
C52 P3 C46 C47 77.45(17) . . . . ?
Ni2 P3 C46 C47 -47.47(17) . . . . ?
C51 C46 C47 C48 1.6(3) . . . . ?
P3 C46 C47 C48 179.84(19) . . . . ?
C46 C47 C48 C49 -1.9(4) . . . . ?
C47 C48 C49 C50 1.2(4) . . . . ?
C48 C49 C50 C51 -0.1(4) . . . . ?
C49 C50 C51 C46 -0.2(3) . . . . ?
C47 C46 C51 C50 -0.6(3) . . . . ?
P3 C46 C51 C50 -178.70(17) . . . . ?
C45 P3 C52 C57 -126.18(15) . . . . ?
C46 P3 C52 C57 -12.67(17) . . . . ?
Ni2 P3 C52 C57 111.42(14) . . . . ?
C45 P3 C52 C53 58.52(16) . . . . ?
C46 P3 C52 C53 172.02(14) . . . . ?
Ni2 P3 C52 C53 -63.89(15) . . . . ?
C57 C52 C53 C54 0.8(3) . . . . ?
P3 C52 C53 C54 176.30(16) . . . . ?
C52 C53 C54 C55 -0.6(3) . . . . ?
C53 C54 C55 C56 0.0(3) . . . . ?
C54 C55 C56 C57 0.4(3) . . . . ?
C53 C52 C57 C56 -0.5(3) . . . . ?
P3 C52 C57 C56 -175.67(15) . . . . ?
C55 C56 C57 C52 -0.1(3) . . . . ?

_refine_diff_density_max         0.427
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.075


__cell_measurement_temperature   100(2)

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2.00 1.00 0.00 0.1760
-5.00 -4.00 1.00 0.1170
0.00 3.00 -1.00 0.1600
4.00 -4.00 -1.00 0.1930
-4.00 3.00 -2.00 0.2190
5.00 3.00 2.00 0.1450
-1.00 2.00 0.00 0.1510
1.00 1.00 5.00 0.1370
-1.00 -2.00 6.00 0.1540
-2.00 -1.00 6.00 0.1640
1.00 2.00 -5.00 0.2530
-1.00 4.00 -5.00 0.2540
-1.00 1.00 0.00 0.1590
4.00 -1.00 -5.00 0.2670
1.00 3.00 -1.00 0.1500
-1.00 -6.00 2.00 0.0760
-1.00 -5.00 0.00 0.0520
1.00 -4.00 1.00 0.1340
0.00 0.00 -1.00 0.2000
