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

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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_wh044z_sq_d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H59 N5 Ni O4 P4, 2(B F4), 1.6(C4 H10 O)'
_chemical_formula_sum            'C64.40 H75 B2 F8 N5 Ni O5.60 P4'
_chemical_formula_weight         1364.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   C222

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

_cell_length_a                   15.1339(14)
_cell_length_b                   23.3855(14)
_cell_length_c                   20.0338(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7090.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    5565
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      24.46

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2845
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9195
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_process_details   'Bruker APEX2'

_exptl_special_details           
; 
 
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6038
_diffrn_reflns_av_R_equivalents  0.0130
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.02
_diffrn_reflns_theta_max         24.84
_reflns_number_total             5920
_reflns_number_gt                4871
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
The discerepancy in the given and calculated molecular weight is due to 
the removal of 1.6 exogeneous diethyl ether molecules from the model by 
using Platon SQUEEZE. However, the contribution of these solvent 
molecules was left in for completeness. 

In the C222 cell setting, the SHELX output suggested the use of a TWIN 
command. However, since Friedel opposites were merged before refinement; 
inclusion of a Flack parameter would be meaningless.

ADDSYM calculations were performed on a separate structure solution 
obtainedin monoclinic C2 and the output indicated missed additional 
orthorhombic symmetry, so the C222 solution was kept.

Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.1879P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_number_reflns         5920
_refine_ls_number_parameters     366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1428
_refine_ls_wR_factor_gt          0.1354
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.2500 0.2500 0.23439(4) 0.0461(2) Uani 1 2 d S . .
P2 P 0.33328(8) 0.17297(4) 0.23643(6) 0.0493(3) Uani 1 1 d . . .
P1 P 0.14939(7) 0.18998(4) 0.27288(6) 0.0478(3) Uani 1 1 d . . .
O1 O 0.3208(2) 0.09954(13) 0.63441(15) 0.0684(9) Uani 1 1 d . . .
H1 H 0.3620 0.0773 0.6400 0.082 Uiso 1 1 calc R . .
O2 O 0.1423(3) -0.13488(12) 0.1445(2) 0.0928(12) Uani 1 1 d . . .
H2 H 0.1036 -0.1380 0.1161 0.111 Uiso 1 1 calc R . .
N1 N 0.2027(3) 0.09295(14) 0.21383(19) 0.0619(10) Uani 1 1 d . . .
N2 N 0.2784(2) 0.16250(12) 0.36643(16) 0.0435(8) Uani 1 1 d . . .
N3 N 0.2500 0.2500 0.1319(2) 0.0614(14) Uani 1 2 d S . .
C21 C 0.5488(4) 0.2122(2) 0.1221(3) 0.0877(18) Uani 1 1 d . . .
H21 H 0.5608 0.2359 0.0859 0.105 Uiso 1 1 calc R . .
C12 C 0.2430(3) 0.16952(15) 0.48447(18) 0.0485(9) Uani 1 1 d . . .
H12 H 0.2016 0.1974 0.4735 0.058 Uiso 1 1 calc R . .
C11 C 0.2944(3) 0.14542(14) 0.4345(2) 0.0435(9) Uani 1 1 d . . .
C20 C 0.6149(4) 0.1777(3) 0.1479(3) 0.106(2) Uani 1 1 d . . .
H20 H 0.6717 0.1784 0.1301 0.127 Uiso 1 1 calc R . .
C19 C 0.5950(5) 0.1429(3) 0.1998(4) 0.142(4) Uani 1 1 d . . .
H19 H 0.6382 0.1186 0.2167 0.170 Uiso 1 1 calc R . .
C14 C 0.3160(3) 0.11441(18) 0.5687(2) 0.0540(10) Uani 1 1 d . . .
C10 C 0.0366(3) 0.24603(17) 0.3598(2) 0.0563(10) Uani 1 1 d . . .
H10 H 0.0880 0.2527 0.3840 0.068 Uiso 1 1 calc R . .
C17 C 0.4454(4) 0.17675(16) 0.2026(2) 0.0596(12) Uani 1 1 d . . .
C16 C 0.3603(3) 0.10632(17) 0.4533(2) 0.0501(10) Uani 1 1 d . . .
H16 H 0.3972 0.0903 0.4213 0.060 Uiso 1 1 calc R . .
C18 C 0.5123(4) 0.1428(2) 0.2279(3) 0.098(2) Uani 1 1 d . . .
H18 H 0.5010 0.1195 0.2645 0.118 Uiso 1 1 calc R . .
C13 C 0.2521(3) 0.15289(17) 0.5502(2) 0.0549(10) Uani 1 1 d . . .
H13 H 0.2145 0.1680 0.5824 0.066 Uiso 1 1 calc R . .
C3 C 0.2839(3) 0.11582(17) 0.1847(2) 0.0604(12) Uani 1 1 d . . .
H3A H 0.2710 0.1309 0.1407 0.073 Uiso 1 1 calc R . .
H3B H 0.3263 0.0851 0.1795 0.073 Uiso 1 1 calc R . .
C22 C 0.4646(4) 0.21165(19) 0.1500(3) 0.0754(15) Uani 1 1 d . . .
H22 H 0.4209 0.2353 0.1326 0.090 Uiso 1 1 calc R . .
C23 C 0.1842(4) 0.03527(16) 0.1938(2) 0.0661(13) Uani 1 1 d . . .
C9 C -0.0431(3) 0.26786(19) 0.3829(3) 0.0688(13) Uani 1 1 d . . .
H9 H -0.0457 0.2896 0.4217 0.083 Uiso 1 1 calc R . .
C8 C -0.1188(4) 0.2562(2) 0.3462(3) 0.0921(18) Uani 1 1 d . . .
H8 H -0.1728 0.2711 0.3600 0.110 Uiso 1 1 calc R . .
C2 C 0.3426(3) 0.13907(15) 0.3182(2) 0.0492(10) Uani 1 1 d . . .
H2A H 0.3329 0.0983 0.3136 0.059 Uiso 1 1 calc R . .
H2B H 0.4020 0.1447 0.3353 0.059 Uiso 1 1 calc R . .
C5 C 0.0408(3) 0.21437(16) 0.3013(2) 0.0581(12) Uani 1 1 d . . .
C15 C 0.3699(3) 0.09176(17) 0.5200(2) 0.0565(11) Uani 1 1 d . . .
H15 H 0.4139 0.0660 0.5321 0.068 Uiso 1 1 calc R . .
C6 C -0.0356(3) 0.20280(18) 0.2654(3) 0.0747(14) Uani 1 1 d . . .
H6 H -0.0337 0.1819 0.2259 0.090 Uiso 1 1 calc R . .
C1 C 0.1872(3) 0.15009(16) 0.3473(2) 0.0527(10) Uani 1 1 d . . .
H1A H 0.1487 0.1592 0.3845 0.063 Uiso 1 1 calc R . .
H1B H 0.1817 0.1094 0.3386 0.063 Uiso 1 1 calc R . .
C28 C 0.2116(4) -0.0094(2) 0.2336(3) 0.101(2) Uani 1 1 d . . .
H28 H 0.2414 -0.0011 0.2730 0.121 Uiso 1 1 calc R . .
C7 C -0.1150(3) 0.2233(2) 0.2903(3) 0.0813(18) Uani 1 1 d . . .
H7 H -0.1671 0.2144 0.2681 0.098 Uiso 1 1 calc R . .
C4 C 0.1278(4) 0.13162(17) 0.2128(2) 0.0640(13) Uani 1 1 d . . .
H4A H 0.0743 0.1113 0.2251 0.077 Uiso 1 1 calc R . .
H4B H 0.1199 0.1472 0.1683 0.077 Uiso 1 1 calc R . .
C25 C 0.1209(7) -0.0353(2) 0.1206(3) 0.142(4) Uani 1 1 d . . .
H25 H 0.0883 -0.0438 0.0825 0.170 Uiso 1 1 calc R . .
C27 C 0.1971(5) -0.0646(2) 0.2179(4) 0.107(2) Uani 1 1 d . . .
H27 H 0.2161 -0.0935 0.2464 0.128 Uiso 1 1 calc R . .
C29 C 0.2500 0.2500 0.0750(3) 0.0719(19) Uani 1 2 d S . .
C26 C 0.1540(4) -0.07791(18) 0.1598(3) 0.0776(15) Uani 1 1 d . . .
C30 C 0.2500 0.2500 -0.0009(3) 0.106(3) Uani 1 2 d S . .
H30A H 0.2175 0.2175 -0.0169 0.159 Uiso 0.50 1 calc PR . .
H30B H 0.3097 0.2480 -0.0169 0.159 Uiso 0.50 1 calc PR . .
H30C H 0.2228 0.2845 -0.0169 0.159 Uiso 0.50 1 calc PR . .
C24 C 0.1373(7) 0.0215(2) 0.1389(3) 0.142(4) Uani 1 1 d . . .
H24 H 0.1151 0.0507 0.1123 0.170 Uiso 1 1 calc R . .
F10 F 0.5000 0.4030(4) 0.0000 0.188(3) Uiso 1 2 d S . .
B2 B 0.5000 0.3459(4) 0.0000 0.084(3) Uiso 1 2 d S . .
F1 F 0.51344(19) 0.04792(10) 0.35173(13) 0.0673(7) Uani 1 1 d . . .
F3 F 0.5725(2) -0.00926(12) 0.27442(14) 0.0795(8) Uani 1 1 d . . .
B1 B 0.5000 0.0000 0.3120(3) 0.0452(15) Uani 1 2 d S . .
F11 F 0.4413(6) 0.3038(4) 0.0226(4) 0.128(3) Uiso 0.50 1 d P . 1
F13 F 0.5893(6) 0.3362(4) 0.0256(5) 0.133(3) Uiso 0.50 1 d P . 1
F7 F 0.4910(5) 0.3434(3) 0.0667(4) 0.104(2) Uiso 0.50 1 d P . 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0581(5) 0.0299(3) 0.0502(4) 0.000 0.000 0.0140(3)
P2 0.0633(7) 0.0318(4) 0.0527(5) 0.0022(4) 0.0063(6) 0.0149(4)
P1 0.0496(6) 0.0343(4) 0.0595(6) -0.0031(5) -0.0061(5) 0.0099(4)
O1 0.076(2) 0.0721(19) 0.0575(18) 0.0024(16) 0.0014(16) 0.0115(17)
O2 0.123(3) 0.0361(16) 0.119(3) -0.0069(17) -0.018(3) -0.0075(17)
N1 0.075(3) 0.0396(18) 0.071(2) -0.0149(16) -0.005(2) 0.0138(18)
N2 0.0380(19) 0.0412(16) 0.0511(18) 0.0014(14) 0.0039(14) 0.0111(13)
N3 0.082(4) 0.049(3) 0.052(3) 0.000 0.000 0.026(3)
C21 0.098(5) 0.085(4) 0.079(3) 0.034(3) 0.040(3) 0.037(3)
C12 0.049(2) 0.0404(17) 0.056(2) -0.0025(16) -0.004(2) 0.0118(19)
C11 0.042(2) 0.0344(17) 0.054(2) 0.0066(16) 0.0023(19) 0.0045(17)
C20 0.092(4) 0.119(5) 0.107(4) 0.051(4) 0.055(4) 0.053(4)
C19 0.107(6) 0.168(7) 0.152(6) 0.108(6) 0.076(5) 0.088(5)
C14 0.050(3) 0.054(2) 0.058(3) 0.006(2) 0.003(2) 0.000(2)
C10 0.051(3) 0.044(2) 0.074(3) 0.000(2) 0.002(2) 0.007(2)
C17 0.087(3) 0.0338(19) 0.058(2) 0.0086(18) 0.020(2) 0.023(2)
C16 0.042(2) 0.051(2) 0.058(2) 0.0003(19) 0.006(2) 0.0099(19)
C18 0.089(4) 0.093(4) 0.113(4) 0.061(4) 0.049(4) 0.047(3)
C13 0.051(2) 0.052(2) 0.062(2) -0.0031(18) 0.011(2) -0.001(2)
C3 0.087(4) 0.040(2) 0.055(2) -0.0028(19) 0.005(2) 0.012(2)
C22 0.091(4) 0.063(3) 0.072(3) 0.023(2) 0.020(3) 0.034(3)
C23 0.087(4) 0.032(2) 0.080(3) 0.000(2) -0.004(3) 0.012(2)
C9 0.050(3) 0.061(3) 0.095(4) -0.006(2) 0.014(3) 0.009(2)
C8 0.051(3) 0.060(3) 0.165(6) 0.002(4) 0.005(4) 0.005(3)
C2 0.055(3) 0.0384(19) 0.054(2) 0.0081(17) 0.002(2) 0.0123(18)
C5 0.050(3) 0.038(2) 0.086(3) -0.001(2) -0.012(2) 0.0071(19)
C15 0.054(3) 0.055(2) 0.061(3) 0.015(2) -0.003(2) 0.016(2)
C6 0.061(3) 0.046(2) 0.118(4) -0.013(3) -0.025(3) 0.005(2)
C1 0.055(3) 0.0395(19) 0.064(3) 0.0051(19) 0.002(2) 0.0077(19)
C28 0.113(5) 0.054(3) 0.135(5) 0.006(3) -0.059(4) 0.004(3)
C7 0.044(3) 0.051(3) 0.149(5) -0.008(3) -0.026(3) 0.005(2)
C4 0.078(3) 0.036(2) 0.078(3) -0.0133(19) -0.015(3) 0.010(2)
C25 0.284(11) 0.053(3) 0.089(4) -0.006(3) -0.076(6) 0.008(4)
C27 0.118(5) 0.047(3) 0.155(6) 0.016(3) -0.061(5) -0.001(3)
C29 0.086(5) 0.075(4) 0.054(4) 0.000 0.000 0.027(4)
C26 0.102(4) 0.034(2) 0.097(4) -0.001(2) -0.007(4) 0.001(2)
C30 0.120(7) 0.149(8) 0.050(4) 0.000 0.000 0.031(7)
C24 0.302(12) 0.041(3) 0.082(4) -0.006(3) -0.071(6) 0.015(4)
F1 0.0775(18) 0.0481(12) 0.0763(17) -0.0198(12) -0.0174(15) 0.0093(12)
F3 0.087(2) 0.0719(16) 0.0793(17) 0.0183(15) 0.0352(17) 0.0255(15)
B1 0.060(4) 0.033(3) 0.043(3) 0.000 0.000 0.003(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N3 2.054(5) . ?
Ni1 P2 2.1989(9) . ?
Ni1 P2 2.1989(9) 6 ?
Ni1 P1 2.2098(11) 6 ?
Ni1 P1 2.2098(11) . ?
P2 C2 1.826(4) . ?
P2 C17 1.830(5) . ?
P2 C3 1.849(5) . ?
P1 C5 1.830(5) . ?
P1 C4 1.849(4) . ?
P1 C1 1.850(4) . ?
O1 C14 1.364(5) . ?
O2 C26 1.379(5) . ?
N1 C23 1.435(5) . ?
N1 C4 1.451(6) . ?
N1 C3 1.461(6) . ?
N2 C11 1.441(5) . ?
N2 C1 1.461(6) . ?
N2 C2 1.476(5) . ?
N3 C29 1.139(7) . ?
C21 C20 1.386(8) . ?
C21 C22 1.393(8) . ?
C12 C13 1.380(6) . ?
C12 C11 1.389(5) . ?
C11 C16 1.404(5) . ?
C20 C19 1.354(8) . ?
C19 C18 1.373(8) . ?
C14 C13 1.372(6) . ?
C14 C15 1.378(6) . ?
C10 C9 1.388(6) . ?
C10 C5 1.388(6) . ?
C17 C22 1.364(6) . ?
C17 C18 1.382(7) . ?
C16 C15 1.386(6) . ?
C23 C24 1.349(8) . ?
C23 C28 1.377(7) . ?
C9 C8 1.388(7) . ?
C8 C7 1.360(8) . ?
C5 C6 1.389(6) . ?
C6 C7 1.386(7) . ?
C28 C27 1.346(8) . ?
C25 C26 1.364(8) . ?
C25 C24 1.401(7) . ?
C27 C26 1.370(8) . ?
C29 C30 1.521(10) . ?
F10 B2 1.337(12) . ?
B2 F7 1.343(7) 4_655 ?
B2 F7 1.343(7) . ?
B2 F11 1.399(11) 4_655 ?
B2 F11 1.399(11) . ?
B2 F13 1.462(10) 4_655 ?
B2 F13 1.462(10) . ?
F1 B1 1.390(4) . ?
F3 B1 1.348(4) . ?
B1 F3 1.348(4) 2_655 ?
B1 F1 1.390(4) 2_655 ?
F11 F13 1.310(10) 4_655 ?
F13 F11 1.310(10) 4_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni1 P2 91.06(3) . . ?
N3 Ni1 P2 91.06(3) . 6 ?
P2 Ni1 P2 177.87(7) . 6 ?
N3 Ni1 P1 110.43(3) . 6 ?
P2 Ni1 P1 96.83(4) . 6 ?
P2 Ni1 P1 82.42(4) 6 6 ?
N3 Ni1 P1 110.43(3) . . ?
P2 Ni1 P1 82.42(4) . . ?
P2 Ni1 P1 96.83(4) 6 . ?
P1 Ni1 P1 139.15(7) 6 . ?
C2 P2 C17 106.4(2) . . ?
C2 P2 C3 102.7(2) . . ?
C17 P2 C3 101.7(2) . . ?
C2 P2 Ni1 114.62(13) . . ?
C17 P2 Ni1 119.03(12) . . ?
C3 P2 Ni1 110.47(15) . . ?
C5 P1 C4 105.9(2) . . ?
C5 P1 C1 100.6(2) . . ?
C4 P1 C1 102.0(2) . . ?
C5 P1 Ni1 121.95(14) . . ?
C4 P1 Ni1 111.31(18) . . ?
C1 P1 Ni1 112.87(15) . . ?
C23 N1 C4 115.4(4) . . ?
C23 N1 C3 113.4(4) . . ?
C4 N1 C3 115.0(4) . . ?
C11 N2 C1 110.6(3) . . ?
C11 N2 C2 113.9(3) . . ?
C1 N2 C2 112.2(3) . . ?
C29 N3 Ni1 180.0 . . ?
C20 C21 C22 120.4(5) . . ?
C13 C12 C11 121.2(4) . . ?
C12 C11 C16 118.0(4) . . ?
C12 C11 N2 118.4(3) . . ?
C16 C11 N2 123.7(4) . . ?
C19 C20 C21 118.4(6) . . ?
C20 C19 C18 121.2(6) . . ?
O1 C14 C13 117.7(4) . . ?
O1 C14 C15 123.7(4) . . ?
C13 C14 C15 118.6(4) . . ?
C9 C10 C5 121.1(5) . . ?
C22 C17 C18 118.2(5) . . ?
C22 C17 P2 120.8(4) . . ?
C18 C17 P2 121.0(3) . . ?
C15 C16 C11 119.6(4) . . ?
C19 C18 C17 121.1(5) . . ?
C14 C13 C12 120.9(4) . . ?
N1 C3 P2 112.4(3) . . ?
C17 C22 C21 120.7(5) . . ?
C24 C23 C28 116.7(4) . . ?
C24 C23 N1 123.7(4) . . ?
C28 C23 N1 119.6(5) . . ?
C8 C9 C10 118.0(5) . . ?
C7 C8 C9 120.8(5) . . ?
N2 C2 P2 112.0(2) . . ?
C6 C5 C10 120.2(4) . . ?
C6 C5 P1 121.7(4) . . ?
C10 C5 P1 118.1(3) . . ?
C14 C15 C16 121.7(4) . . ?
C7 C6 C5 117.9(5) . . ?
N2 C1 P1 113.8(3) . . ?
C27 C28 C23 122.9(6) . . ?
C8 C7 C6 122.0(5) . . ?
N1 C4 P1 108.2(3) . . ?
C26 C25 C24 118.5(6) . . ?
C28 C27 C26 119.6(5) . . ?
N3 C29 C30 180.000(1) . . ?
C25 C26 C27 119.9(5) . . ?
C25 C26 O2 122.0(5) . . ?
C27 C26 O2 118.0(5) . . ?
C23 C24 C25 122.2(5) . . ?
F10 B2 F7 92.4(6) . 4_655 ?
F10 B2 F7 92.4(6) . . ?
F7 B2 F7 175.1(11) 4_655 . ?
F10 B2 F11 134.6(5) . 4_655 ?
F7 B2 F11 65.5(5) 4_655 4_655 ?
F7 B2 F11 110.8(7) . 4_655 ?
F10 B2 F11 134.6(5) . . ?
F7 B2 F11 110.8(7) 4_655 . ?
F7 B2 F11 65.5(5) . . ?
F11 B2 F11 90.8(10) 4_655 . ?
F10 B2 F13 98.9(6) . 4_655 ?
F7 B2 F13 74.9(5) 4_655 4_655 ?
F7 B2 F13 104.4(5) . 4_655 ?
F11 B2 F13 111.4(7) 4_655 4_655 ?
F11 B2 F13 54.4(5) . 4_655 ?
F10 B2 F13 98.9(6) . . ?
F7 B2 F13 104.3(5) 4_655 . ?
F7 B2 F13 74.9(5) . . ?
F11 B2 F13 54.4(5) 4_655 . ?
F11 B2 F13 111.4(7) . . ?
F13 B2 F13 162.2(11) 4_655 . ?
F3 B1 F3 112.1(5) . 2_655 ?
F3 B1 F1 108.03(16) . 2_655 ?
F3 B1 F1 109.29(19) 2_655 2_655 ?
F3 B1 F1 109.29(19) . . ?
F3 B1 F1 108.03(16) 2_655 . ?
F1 B1 F1 110.1(5) 2_655 . ?
F13 F11 B2 65.2(6) 4_655 . ?
F11 F13 B2 60.3(6) 4_655 . ?

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
N3 Ni1 P2 C2 -168.22(17) . . . . ?
P2 Ni1 P2 C2 11.76(17) 6 . . . ?
P1 Ni1 P2 C2 81.06(17) 6 . . . ?
P1 Ni1 P2 C2 -57.76(17) . . . . ?
N3 Ni1 P2 C17 64.25(18) . . . . ?
P2 Ni1 P2 C17 -115.76(18) 6 . . . ?
P1 Ni1 P2 C17 -46.47(18) 6 . . . ?
P1 Ni1 P2 C17 174.72(18) . . . . ?
N3 Ni1 P2 C3 -52.75(16) . . . . ?
P2 Ni1 P2 C3 127.23(17) 6 . . . ?
P1 Ni1 P2 C3 -163.47(17) 6 . . . ?
P1 Ni1 P2 C3 57.71(17) . . . . ?
N3 Ni1 P1 C5 -99.15(18) . . . . ?
P2 Ni1 P1 C5 172.55(18) . . . . ?
P2 Ni1 P1 C5 -5.45(19) 6 . . . ?
P1 Ni1 P1 C5 80.86(18) 6 . . . ?
N3 Ni1 P1 C4 26.98(16) . . . . ?
P2 Ni1 P1 C4 -61.32(16) . . . . ?
P2 Ni1 P1 C4 120.68(16) 6 . . . ?
P1 Ni1 P1 C4 -153.01(16) 6 . . . ?
N3 Ni1 P1 C1 140.96(15) . . . . ?
P2 Ni1 P1 C1 52.66(15) . . . . ?
P2 Ni1 P1 C1 -125.34(15) 6 . . . ?
P1 Ni1 P1 C1 -39.03(15) 6 . . . ?
P2 Ni1 N3 C29 -100(100) . . . . ?
P2 Ni1 N3 C29 80(100) 6 . . . ?
P1 Ni1 N3 C29 -2(100) 6 . . . ?
P1 Ni1 N3 C29 178(100) . . . . ?
C13 C12 C11 C16 -4.2(6) . . . . ?
C13 C12 C11 N2 176.8(4) . . . . ?
C1 N2 C11 C12 -58.7(4) . . . . ?
C2 N2 C11 C12 173.9(3) . . . . ?
C1 N2 C11 C16 122.3(4) . . . . ?
C2 N2 C11 C16 -5.1(5) . . . . ?
C22 C21 C20 C19 1.3(11) . . . . ?
C21 C20 C19 C18 -2.1(14) . . . . ?
C2 P2 C17 C22 -164.1(4) . . . . ?
C3 P2 C17 C22 88.8(4) . . . . ?
Ni1 P2 C17 C22 -32.8(5) . . . . ?
C2 P2 C17 C18 18.4(5) . . . . ?
C3 P2 C17 C18 -88.8(5) . . . . ?
Ni1 P2 C17 C18 149.7(4) . . . . ?
C12 C11 C16 C15 2.0(6) . . . . ?
N2 C11 C16 C15 -178.9(4) . . . . ?
C20 C19 C18 C17 2.4(14) . . . . ?
C22 C17 C18 C19 -1.8(10) . . . . ?
P2 C17 C18 C19 175.8(7) . . . . ?
O1 C14 C13 C12 -179.5(4) . . . . ?
C15 C14 C13 C12 -1.2(7) . . . . ?
C11 C12 C13 C14 3.8(7) . . . . ?
C23 N1 C3 P2 -154.1(3) . . . . ?
C4 N1 C3 P2 70.0(4) . . . . ?
C2 P2 C3 N1 53.5(3) . . . . ?
C17 P2 C3 N1 163.5(3) . . . . ?
Ni1 P2 C3 N1 -69.2(3) . . . . ?
C18 C17 C22 C21 1.0(8) . . . . ?
P2 C17 C22 C21 -176.6(5) . . . . ?
C20 C21 C22 C17 -0.8(10) . . . . ?
C4 N1 C23 C24 46.9(9) . . . . ?
C3 N1 C23 C24 -88.8(8) . . . . ?
C4 N1 C23 C28 -130.0(6) . . . . ?
C3 N1 C23 C28 94.3(6) . . . . ?
C5 C10 C9 C8 1.1(7) . . . . ?
C10 C9 C8 C7 1.5(8) . . . . ?
C11 N2 C2 P2 -168.5(3) . . . . ?
C1 N2 C2 P2 65.0(4) . . . . ?
C17 P2 C2 N2 145.2(3) . . . . ?
C3 P2 C2 N2 -108.4(3) . . . . ?
Ni1 P2 C2 N2 11.5(3) . . . . ?
C9 C10 C5 C6 -1.5(7) . . . . ?
C9 C10 C5 P1 177.4(3) . . . . ?
C4 P1 C5 C6 -19.2(4) . . . . ?
C1 P1 C5 C6 -125.1(4) . . . . ?
Ni1 P1 C5 C6 109.3(4) . . . . ?
C4 P1 C5 C10 161.9(3) . . . . ?
C1 P1 C5 C10 56.1(4) . . . . ?
Ni1 P1 C5 C10 -69.6(4) . . . . ?
O1 C14 C15 C16 177.2(4) . . . . ?
C13 C14 C15 C16 -0.9(7) . . . . ?
C11 C16 C15 C14 0.4(7) . . . . ?
C10 C5 C6 C7 -0.6(7) . . . . ?
P1 C5 C6 C7 -179.5(4) . . . . ?
C11 N2 C1 P1 161.6(3) . . . . ?
C2 N2 C1 P1 -70.1(3) . . . . ?
C5 P1 C1 N2 -134.5(3) . . . . ?
C4 P1 C1 N2 116.6(3) . . . . ?
Ni1 P1 C1 N2 -2.9(3) . . . . ?
C24 C23 C28 C27 3.2(11) . . . . ?
N1 C23 C28 C27 -179.6(7) . . . . ?
C9 C8 C7 C6 -3.7(8) . . . . ?
C5 C6 C7 C8 3.2(8) . . . . ?
C23 N1 C4 P1 154.8(3) . . . . ?
C3 N1 C4 P1 -70.3(4) . . . . ?
C5 P1 C4 N1 -151.9(3) . . . . ?
C1 P1 C4 N1 -47.1(4) . . . . ?
Ni1 P1 C4 N1 73.5(3) . . . . ?
C23 C28 C27 C26 0.6(12) . . . . ?
Ni1 N3 C29 C30 0(100) . . . . ?
C24 C25 C26 C27 4.2(14) . . . . ?
C24 C25 C26 O2 -178.7(8) . . . . ?
C28 C27 C26 C25 -4.4(12) . . . . ?
C28 C27 C26 O2 178.3(7) . . . . ?
C28 C23 C24 C25 -3.5(14) . . . . ?
N1 C23 C24 C25 179.6(8) . . . . ?
C26 C25 C24 C23 -0.2(16) . . . . ?
F10 B2 F11 F13 64.0(7) . . . 4_655 ?
F7 B2 F11 F13 -52.0(8) 4_655 . . 4_655 ?
F7 B2 F11 F13 131.4(7) . . . 4_655 ?
F11 B2 F11 F13 -116.0(7) 4_655 . . 4_655 ?
F13 B2 F11 F13 -167.7(7) . . . 4_655 ?
F10 B2 F13 F11 -139.6(5) . . . 4_655 ?
F7 B2 F13 F11 -44.8(7) 4_655 . . 4_655 ?
F7 B2 F13 F11 130.3(9) . . . 4_655 ?
F11 B2 F13 F11 74.8(10) . . . 4_655 ?
F13 B2 F13 F11 40.4(5) 4_655 . . 4_655 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        24.84
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.059

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 0.000 424 60 ' '
2 0.000 0.000 0.500 453 78 ' '
3 0.500 0.000 0.000 424 60 ' '
4 0.500 0.500 0.500 453 78 ' '
_platon_squeeze_details          
;
Platon SQUEEZE was used to remove the contribution of 1.6 
heavily disordered exogeneous diethyl ether molecules that 
could not be modeled in the difference map.
A total of 304  electrons in 1754 cubic angstroms of 
accessible unit cell void volume were removed. Since Z = 4, 
this translates to an average of 69 e- per whole complex 
molecule, consistent with approximately 1.6 exogenous diethyl 
ether molecules (42 e- each). This roughly matches the 
obtained elemental analysis of a crystalline sample 
see main text).
;

_database_code_depnum_ccdc_archive 'CCDC 927349'