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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_oa0031-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PPMeP)Ni(CO2)
_chemical_melting_point          ?
_chemical_formula_moiety         C26H39NiO2P3
_chemical_formula_sum            'C26 H39 Ni O2 P3'
_chemical_formula_weight         535.19

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.4995(7)
_cell_length_b                   14.7887(9)
_cell_length_c                   16.1942(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.174(3)
_cell_angle_gamma                90.00
_cell_volume                     2726.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    37127
_cell_measurement_theta_min      2.04
_cell_measurement_theta_max      30.43

_exptl_crystal_description       platy
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7982
_exptl_absorpt_correction_T_max  0.9309
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37127
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         30.43
_reflns_number_total             8224
_reflns_number_gt                6622
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker APEX II'
_computing_data_reduction        'Bruker APEX II'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0427P)²+0.6238P] where P=(Fo²+2Fc²)/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_number_reflns         8224
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0831
_refine_ls_wR_factor_gt          0.0768
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.048242(15) 0.206099(12) 0.230310(11) 0.02033(5) Uani 1 1 d . . .
O1 O 1.20052(11) 0.14532(9) 0.38133(7) 0.0400(3) Uani 1 1 d . . .
O2 O 1.18924(10) 0.10522(8) 0.24429(8) 0.0354(3) Uani 1 1 d . . .
P1 P 0.94127(3) 0.25983(3) 0.12062(2) 0.02060(8) Uani 1 1 d . . .
P2 P 0.90058(3) 0.12117(3) 0.25326(2) 0.02395(9) Uani 1 1 d . . .
P3 P 1.12703(3) 0.33781(3) 0.25593(2) 0.01978(8) Uani 1 1 d . . .
C1 C 1.16289(13) 0.14537(11) 0.30710(10) 0.0274(3) Uani 1 1 d . . .
C2 C 0.76982(12) 0.16539(10) 0.18679(9) 0.0229(3) Uani 1 1 d . . .
C3 C 0.65503(13) 0.13898(11) 0.19392(10) 0.0294(3) Uani 1 1 d . . .
H3 H 0.6417 0.0962 0.2353 0.035 Uiso 1 1 calc R . .
C4 C 0.56034(14) 0.17438(12) 0.14148(11) 0.0328(4) Uani 1 1 d . . .
H4 H 0.4826 0.1567 0.1477 0.039 Uiso 1 1 calc R . .
C5 C 0.57901(14) 0.23561(12) 0.07999(11) 0.0335(4) Uani 1 1 d . . .
H5 H 0.5140 0.2593 0.0437 0.040 Uiso 1 1 calc R . .
C6 C 0.69217(14) 0.26254(11) 0.07102(10) 0.0294(3) Uani 1 1 d . . .
H6 H 0.7046 0.3038 0.0281 0.035 Uiso 1 1 calc R . .
C7 C 0.78817(12) 0.22877(10) 0.12542(9) 0.0224(3) Uani 1 1 d . . .
C8 C 1.03903(12) 0.41880(10) 0.18663(8) 0.0208(3) Uani 1 1 d . . .
C9 C 1.06056(13) 0.51165(11) 0.18902(9) 0.0258(3) Uani 1 1 d . . .
H9 H 1.1200 0.5358 0.2298 0.031 Uiso 1 1 calc R . .
C10 C 0.99567(13) 0.56891(11) 0.13217(9) 0.0273(3) Uani 1 1 d . . .
H10 H 1.0100 0.6322 0.1346 0.033 Uiso 1 1 calc R . .
C11 C 0.90984(13) 0.53382(11) 0.07171(9) 0.0266(3) Uani 1 1 d . . .
H11 H 0.8653 0.5733 0.0331 0.032 Uiso 1 1 calc R . .
C12 C 0.88886(13) 0.44171(11) 0.06731(9) 0.0247(3) Uani 1 1 d . . .
H12 H 0.8312 0.4180 0.0250 0.030 Uiso 1 1 calc R . .
C13 C 0.95247(12) 0.38325(10) 0.12515(8) 0.0211(3) Uani 1 1 d . . .
C14 C 0.94241(19) 0.00353(14) 0.12738(13) 0.0496(5) Uani 1 1 d . . .
H14A H 0.9584 -0.0583 0.1104 0.074 Uiso 1 1 calc R . .
H14B H 1.0114 0.0415 0.1239 0.074 Uiso 1 1 calc R . .
H14C H 0.8749 0.0278 0.0903 0.074 Uiso 1 1 calc R . .
C15 C 0.91528(15) 0.00306(11) 0.21695(12) 0.0361(4) Uani 1 1 d . . .
H15 H 0.9862 -0.0226 0.2520 0.043 Uiso 1 1 calc R . .
C16 C 0.81321(18) -0.06096(14) 0.22679(18) 0.0601(6) Uani 1 1 d . . .
H16A H 0.7430 -0.0419 0.1893 0.090 Uiso 1 1 calc R . .
H16B H 0.7972 -0.0592 0.2846 0.090 Uiso 1 1 calc R . .
H16C H 0.8343 -0.1227 0.2127 0.090 Uiso 1 1 calc R . .
C17 C 0.8207(2) 0.19948(14) 0.39059(12) 0.0487(5) Uani 1 1 d . . .
H17A H 0.7869 0.1911 0.4423 0.073 Uiso 1 1 calc R . .
H17B H 0.7649 0.2324 0.3501 0.073 Uiso 1 1 calc R . .
H17C H 0.8939 0.2341 0.4024 0.073 Uiso 1 1 calc R . .
C18 C 0.84628(14) 0.10754(12) 0.35492(10) 0.0333(4) Uani 1 1 d . . .
H18 H 0.7710 0.0727 0.3452 0.040 Uiso 1 1 calc R . .
C19 C 0.93307(18) 0.05469(17) 0.41655(13) 0.0555(6) Uani 1 1 d . . .
H19A H 1.0088 0.0863 0.4250 0.083 Uiso 1 1 calc R . .
H19B H 0.9436 -0.0060 0.3944 0.083 Uiso 1 1 calc R . .
H19C H 0.9027 0.0498 0.4699 0.083 Uiso 1 1 calc R . .
C20 C 1.00510(15) 0.40804(13) 0.37738(11) 0.0365(4) Uani 1 1 d . . .
H20A H 1.0000 0.4106 0.4372 0.055 Uiso 1 1 calc R . .
H20B H 0.9486 0.3636 0.3506 0.055 Uiso 1 1 calc R . .
H20C H 0.9870 0.4677 0.3525 0.055 Uiso 1 1 calc R . .
C21 C 1.12933(14) 0.38031(11) 0.36454(9) 0.0265(3) Uani 1 1 d . . .
H21 H 1.1501 0.3272 0.4019 0.032 Uiso 1 1 calc R . .
C22 C 1.21701(17) 0.45477(13) 0.39565(11) 0.0398(4) Uani 1 1 d . . .
H22A H 1.2007 0.5087 0.3608 0.060 Uiso 1 1 calc R . .
H22B H 1.2970 0.4337 0.3925 0.060 Uiso 1 1 calc R . .
H22C H 1.2095 0.4697 0.4536 0.060 Uiso 1 1 calc R . .
C23 C 1.36708(14) 0.29787(12) 0.27920(11) 0.0324(4) Uani 1 1 d . . .
H23A H 1.3499 0.2349 0.2629 0.049 Uiso 1 1 calc R . .
H23B H 1.3636 0.3050 0.3390 0.049 Uiso 1 1 calc R . .
H23C H 1.4458 0.3138 0.2675 0.049 Uiso 1 1 calc R . .
C24 C 1.27646(12) 0.36010(11) 0.22967(9) 0.0263(3) Uani 1 1 d . . .
H24 H 1.2979 0.4242 0.2445 0.032 Uiso 1 1 calc R . .
C25 C 1.27862(16) 0.34718(18) 0.13656(11) 0.0490(5) Uani 1 1 d . . .
H25A H 1.3582 0.3583 0.1239 0.073 Uiso 1 1 calc R . .
H25B H 1.2239 0.3898 0.1052 0.073 Uiso 1 1 calc R . .
H25C H 1.2551 0.2852 0.1207 0.073 Uiso 1 1 calc R . .
C26 C 0.95594(16) 0.23642(12) 0.01160(10) 0.0329(3) Uani 1 1 d . . .
H26A H 0.8964 0.2706 -0.0250 0.049 Uiso 1 1 calc R . .
H26B H 0.9449 0.1716 0.0006 0.049 Uiso 1 1 calc R . .
H26C H 1.0344 0.2545 0.0009 0.049 Uiso 1 1 calc R . .


_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 C1 1.9040(15) . ?
Ni1 P1 2.1631(4) . ?
Ni1 P3 2.1633(4) . ?
Ni1 P2 2.1860(4) . ?
Ni1 O2 2.1912(11) . ?
O1 C1 1.2184(18) . ?
O2 C1 1.2517(19) . ?
P1 C26 1.8302(16) . ?
P1 C13 1.8306(15) . ?
P1 C7 1.8319(15) . ?
P2 C2 1.8404(14) . ?
P2 C18 1.8528(17) . ?
P2 C15 1.8584(18) . ?
P3 C8 1.8426(14) . ?
P3 C24 1.8574(15) . ?
P3 C21 1.8644(15) . ?
C2 C3 1.397(2) . ?
C2 C7 1.404(2) . ?
C3 C4 1.385(2) . ?
C4 C5 1.385(2) . ?
C5 C6 1.388(2) . ?
C6 C7 1.4027(19) . ?
C8 C9 1.395(2) . ?
C8 C13 1.4060(19) . ?
C9 C10 1.388(2) . ?
C10 C11 1.388(2) . ?
C11 C12 1.383(2) . ?
C12 C13 1.4018(19) . ?
C14 C15 1.526(3) . ?
C15 C16 1.534(3) . ?
C17 C18 1.522(3) . ?
C18 C19 1.523(2) . ?
C20 C21 1.529(2) . ?
C21 C22 1.529(2) . ?
C23 C24 1.529(2) . ?
C24 C25 1.524(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni1 P1 165.89(5) . . ?
C1 Ni1 P3 93.85(5) . . ?
P1 Ni1 P3 90.030(15) . . ?
C1 Ni1 P2 95.76(5) . . ?
P1 Ni1 P2 89.191(15) . . ?
P3 Ni1 P2 143.033(17) . . ?
C1 Ni1 O2 34.70(6) . . ?
P1 Ni1 O2 131.38(3) . . ?
P3 Ni1 O2 108.04(3) . . ?
P2 Ni1 O2 99.93(4) . . ?
C1 O2 Ni1 60.00(8) . . ?
C26 P1 C13 102.22(7) . . ?
C26 P1 C7 102.39(7) . . ?
C13 P1 C7 108.11(7) . . ?
C26 P1 Ni1 127.09(6) . . ?
C13 P1 Ni1 107.75(4) . . ?
C7 P1 Ni1 108.11(5) . . ?
C2 P2 C18 101.99(7) . . ?
C2 P2 C15 104.62(7) . . ?
C18 P2 C15 103.67(8) . . ?
C2 P2 Ni1 106.63(5) . . ?
C18 P2 Ni1 125.56(6) . . ?
C15 P2 Ni1 112.23(6) . . ?
C8 P3 C24 101.02(7) . . ?
C8 P3 C21 106.76(7) . . ?
C24 P3 C21 105.46(7) . . ?
C8 P3 Ni1 106.84(5) . . ?
C24 P3 Ni1 119.46(6) . . ?
C21 P3 Ni1 115.71(5) . . ?
O1 C1 O2 135.11(15) . . ?
O1 C1 Ni1 139.51(13) . . ?
O2 C1 Ni1 85.30(9) . . ?
C3 C2 C7 118.95(13) . . ?
C3 C2 P2 123.73(12) . . ?
C7 C2 P2 117.31(10) . . ?
C4 C3 C2 120.89(15) . . ?
C3 C4 C5 119.95(15) . . ?
C4 C5 C6 120.41(14) . . ?
C5 C6 C7 119.86(15) . . ?
C6 C7 C2 119.89(13) . . ?
C6 C7 P1 124.01(12) . . ?
C2 C7 P1 116.08(10) . . ?
C9 C8 C13 119.53(13) . . ?
C9 C8 P3 122.89(11) . . ?
C13 C8 P3 117.42(11) . . ?
C10 C9 C8 120.37(14) . . ?
C9 C10 C11 120.07(15) . . ?
C12 C11 C10 120.38(14) . . ?
C11 C12 C13 120.15(14) . . ?
C12 C13 C8 119.48(13) . . ?
C12 C13 P1 124.14(11) . . ?
C8 C13 P1 116.10(10) . . ?
C14 C15 C16 111.37(17) . . ?
C14 C15 P2 109.66(13) . . ?
C16 C15 P2 116.22(14) . . ?
C17 C18 C19 110.71(17) . . ?
C17 C18 P2 110.35(12) . . ?
C19 C18 P2 111.46(13) . . ?
C20 C21 C22 110.31(14) . . ?
C20 C21 P3 109.31(11) . . ?
C22 C21 P3 118.28(12) . . ?
C25 C24 C23 109.74(14) . . ?
C25 C24 P3 110.49(11) . . ?
C23 C24 P3 110.90(11) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        30.43
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.068
_database_code_depnum_ccdc_archive 'CCDC 993623'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_0092a-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PPMeP)Ni{COOB(C6F5)3}
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H39 B F15 Ni O2 P3, 3(C7 H8)'
_chemical_formula_sum            'C65 H63 B F15 Ni O2 P3'
_chemical_formula_weight         1323.58

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'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.7796(8)
_cell_length_b                   15.3191(9)
_cell_length_c                   15.8751(9)
_cell_angle_alpha                97.002(3)
_cell_angle_beta                 95.900(3)
_cell_angle_gamma                111.372(3)
_cell_volume                     3057.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    75519
_cell_measurement_theta_min      1.31
_cell_measurement_theta_max      27.50

_exptl_crystal_description       platy
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1364
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9395
_exptl_absorpt_correction_T_max  0.9668
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            75519
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         27.50
_reflns_number_total             13947
_reflns_number_gt                9028
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1169P)²+0.0000P] where P=(Fo²+2Fc²)/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_number_reflns         13947
_refine_ls_number_parameters     787
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0621
_refine_ls_wR_factor_ref         0.1965
_refine_ls_wR_factor_gt          0.1617
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.041
_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 0.18156(3) 0.46507(3) 0.28989(3) 0.01973(13) Uani 1 1 d . . .
P1 P 0.19683(7) 0.34328(6) 0.33929(6) 0.0214(2) Uani 1 1 d . . .
P2 P 0.01574(7) 0.37495(6) 0.23928(6) 0.0201(2) Uani 1 1 d . . .
P3 P 0.35113(7) 0.51881(7) 0.28738(6) 0.0255(2) Uani 1 1 d . . .
O1 O 0.16418(19) 0.60231(17) 0.18823(15) 0.0253(5) Uani 1 1 d . . .
O2 O 0.17058(18) 0.63384(16) 0.33151(15) 0.0224(5) Uani 1 1 d . . .
B1 B 0.1435(3) 0.7222(3) 0.3299(3) 0.0240(9) Uani 1 1 d . . .
F1 F 0.03896(16) 0.72668(15) 0.15087(13) 0.0315(5) Uani 1 1 d . . .
F2 F -0.16518(18) 0.64109(18) 0.08861(14) 0.0437(6) Uani 1 1 d . . .
F3 F -0.30530(17) 0.54624(19) 0.18591(16) 0.0470(6) Uani 1 1 d . . .
F4 F -0.23503(17) 0.53573(16) 0.34983(15) 0.0389(6) Uani 1 1 d . . .
F5 F -0.02986(16) 0.61613(14) 0.41324(13) 0.0302(5) Uani 1 1 d . . .
F6 F 0.01132(16) 0.81110(15) 0.42881(13) 0.0320(5) Uani 1 1 d . . .
F7 F 0.06673(18) 0.90526(16) 0.58659(14) 0.0395(6) Uani 1 1 d . . .
F8 F 0.2557(2) 0.93103(16) 0.68276(14) 0.0426(6) Uani 1 1 d . . .
F9 F 0.38689(19) 0.85818(19) 0.61107(15) 0.0485(7) Uani 1 1 d . . .
F10 F 0.33514(17) 0.76454(17) 0.45082(14) 0.0384(6) Uani 1 1 d . . .
F11 F 0.35997(16) 0.74838(15) 0.27823(14) 0.0313(5) Uani 1 1 d . . .
F12 F 0.48325(18) 0.89629(17) 0.21865(17) 0.0454(6) Uani 1 1 d . . .
F13 F 0.4199(2) 1.04107(17) 0.19008(18) 0.0508(7) Uani 1 1 d . . .
F14 F 0.2251(2) 1.03034(16) 0.22067(16) 0.0441(6) Uani 1 1 d . . .
F15 F 0.09929(17) 0.88315(15) 0.28188(14) 0.0332(5) Uani 1 1 d . . .
C1 C 0.1709(3) 0.5791(2) 0.2590(2) 0.0207(7) Uani 1 1 d . . .
C2 C 0.1907(3) 0.3291(3) 0.4511(2) 0.0307(9) Uani 1 1 d . . .
H2A H 0.1992 0.2700 0.4599 0.046 Uiso 1 1 calc R . .
H2B H 0.1222 0.3267 0.4651 0.046 Uiso 1 1 calc R . .
H2C H 0.2473 0.3832 0.4885 0.046 Uiso 1 1 calc R . .
C3 C 0.0905(3) 0.2361(2) 0.2805(2) 0.0215(7) Uani 1 1 d . . .
C4 C 0.0860(3) 0.1444(3) 0.2804(2) 0.0284(8) Uani 1 1 d . . .
H4A H 0.1422 0.1344 0.3122 0.034 Uiso 1 1 calc R . .
C5 C 0.0006(3) 0.0669(3) 0.2345(3) 0.0302(8) Uani 1 1 d . . .
H5A H -0.0007 0.0044 0.2334 0.036 Uiso 1 1 calc R . .
C6 C -0.0831(3) 0.0811(3) 0.1903(2) 0.0293(8) Uani 1 1 d . . .
H6A H -0.1418 0.0280 0.1591 0.035 Uiso 1 1 calc R . .
C7 C -0.0815(3) 0.1722(2) 0.1914(2) 0.0273(8) Uani 1 1 d . . .
H7A H -0.1398 0.1810 0.1616 0.033 Uiso 1 1 calc R . .
C8 C 0.0054(3) 0.2516(2) 0.2362(2) 0.0227(7) Uani 1 1 d . . .
C9 C 0.3239(3) 0.3388(3) 0.3216(2) 0.0250(8) Uani 1 1 d . . .
C10 C 0.3555(3) 0.2642(3) 0.3357(3) 0.0324(9) Uani 1 1 d . . .
H10A H 0.3108 0.2121 0.3583 0.039 Uiso 1 1 calc R . .
C11 C 0.4521(3) 0.2661(3) 0.3166(3) 0.0378(10) Uani 1 1 d . . .
H11A H 0.4731 0.2149 0.3253 0.045 Uiso 1 1 calc R . .
C12 C 0.5176(3) 0.3422(3) 0.2850(3) 0.0411(10) Uani 1 1 d . . .
H12A H 0.5828 0.3425 0.2704 0.049 Uiso 1 1 calc R . .
C13 C 0.4890(3) 0.4184(3) 0.2744(3) 0.0403(10) Uani 1 1 d . . .
H13A H 0.5358 0.4714 0.2542 0.048 Uiso 1 1 calc R . .
C14 C 0.3922(3) 0.4181(3) 0.2929(2) 0.0298(8) Uani 1 1 d . . .
C15 C -0.0477(3) 0.3918(3) 0.3986(2) 0.0334(9) Uani 1 1 d . . .
H15A H -0.1007 0.4001 0.4320 0.050 Uiso 1 1 calc R . .
H15B H 0.0202 0.4450 0.4187 0.050 Uiso 1 1 calc R . .
H15C H -0.0400 0.3319 0.4059 0.050 Uiso 1 1 calc R . .
C16 C -0.0829(3) 0.3893(3) 0.3036(2) 0.0258(8) Uani 1 1 d . . .
H16A H -0.0836 0.4536 0.2990 0.031 Uiso 1 1 calc R . .
C17 C -0.1964(3) 0.3183(3) 0.2734(3) 0.0361(9) Uani 1 1 d . . .
H17A H -0.2425 0.3324 0.3115 0.054 Uiso 1 1 calc R . .
H17B H -0.1997 0.2536 0.2749 0.054 Uiso 1 1 calc R . .
H17C H -0.2200 0.3236 0.2145 0.054 Uiso 1 1 calc R . .
C18 C -0.0722(3) 0.4536(3) 0.1140(3) 0.0337(9) Uani 1 1 d . . .
H18A H -0.0985 0.4475 0.0530 0.051 Uiso 1 1 calc R . .
H18B H -0.0130 0.5149 0.1333 0.051 Uiso 1 1 calc R . .
H18C H -0.1289 0.4502 0.1476 0.051 Uiso 1 1 calc R . .
C19 C -0.0352(3) 0.3731(3) 0.1268(2) 0.0267(8) Uani 1 1 d . . .
H19A H -0.0978 0.3120 0.1075 0.032 Uiso 1 1 calc R . .
C20 C 0.0478(3) 0.3715(3) 0.0706(2) 0.0355(9) Uani 1 1 d . . .
H20A H 0.0207 0.3702 0.0107 0.053 Uiso 1 1 calc R . .
H20B H 0.0637 0.3147 0.0746 0.053 Uiso 1 1 calc R . .
H20C H 0.1122 0.4285 0.0903 0.053 Uiso 1 1 calc R . .
C21 C 0.3814(4) 0.5849(3) 0.4611(3) 0.0470(12) Uani 1 1 d . . .
H21A H 0.4238 0.6323 0.5113 0.071 Uiso 1 1 calc R . .
H21B H 0.3773 0.5216 0.4704 0.071 Uiso 1 1 calc R . .
H21C H 0.3101 0.5853 0.4524 0.071 Uiso 1 1 calc R . .
C22 C 0.4328(3) 0.6088(3) 0.3813(3) 0.0335(9) Uani 1 1 d . . .
H22A H 0.4306 0.6713 0.3713 0.040 Uiso 1 1 calc R . .
C23 C 0.5496(3) 0.6228(3) 0.4000(3) 0.0525(13) Uani 1 1 d . . .
H23A H 0.5847 0.6722 0.4508 0.079 Uiso 1 1 calc R . .
H23B H 0.5837 0.6423 0.3505 0.079 Uiso 1 1 calc R . .
H23C H 0.5549 0.5629 0.4108 0.079 Uiso 1 1 calc R . .
C24 C 0.3528(4) 0.4744(3) 0.1126(3) 0.0465(11) Uani 1 1 d . . .
H24A H 0.3695 0.4969 0.0587 0.070 Uiso 1 1 calc R . .
H24B H 0.2770 0.4364 0.1062 0.070 Uiso 1 1 calc R . .
H24C H 0.3925 0.4350 0.1266 0.070 Uiso 1 1 calc R . .
C25 C 0.3833(3) 0.5607(3) 0.1857(3) 0.0341(9) Uani 1 1 d . . .
H25A H 0.3338 0.5927 0.1710 0.041 Uiso 1 1 calc R . .
C26 C 0.4931(3) 0.6342(3) 0.1851(3) 0.0443(11) Uani 1 1 d . . .
H26A H 0.4985 0.6499 0.1273 0.066 Uiso 1 1 calc R . .
H26B H 0.5462 0.6082 0.2016 0.066 Uiso 1 1 calc R . .
H26C H 0.5053 0.6919 0.2260 0.066 Uiso 1 1 calc R . .
C27 C 0.0172(3) 0.6802(2) 0.2878(2) 0.0217(7) Uani 1 1 d . . .
C28 C -0.0251(3) 0.6829(3) 0.2048(2) 0.0246(8) Uani 1 1 d . . .
C29 C -0.1310(3) 0.6404(3) 0.1707(2) 0.0308(9) Uani 1 1 d . . .
C30 C -0.2019(3) 0.5923(3) 0.2197(3) 0.0333(9) Uani 1 1 d . . .
C31 C -0.1663(3) 0.5865(3) 0.3020(2) 0.0284(8) Uani 1 1 d . . .
C32 C -0.0591(3) 0.6287(2) 0.3330(2) 0.0243(8) Uani 1 1 d . . .
C33 C 0.1673(3) 0.7774(2) 0.4303(2) 0.0248(8) Uani 1 1 d . . .
C34 C 0.1058(3) 0.8183(2) 0.4709(2) 0.0253(8) Uani 1 1 d . . .
C35 C 0.1322(3) 0.8683(3) 0.5530(2) 0.0291(8) Uani 1 1 d . . .
C36 C 0.2273(3) 0.8821(3) 0.6019(2) 0.0310(9) Uani 1 1 d . . .
C37 C 0.2926(3) 0.8445(3) 0.5653(2) 0.0326(9) Uani 1 1 d . . .
C38 C 0.2624(3) 0.7946(3) 0.4830(2) 0.0270(8) Uani 1 1 d . . .
C39 C 0.2206(3) 0.8055(2) 0.2824(2) 0.0241(8) Uani 1 1 d . . .
C40 C 0.3210(3) 0.8164(2) 0.2650(2) 0.0256(8) Uani 1 1 d . . .
C41 C 0.3879(3) 0.8931(3) 0.2351(3) 0.0310(9) Uani 1 1 d . . .
C42 C 0.3568(3) 0.9656(3) 0.2201(3) 0.0350(9) Uani 1 1 d . . .
C43 C 0.2584(3) 0.9597(3) 0.2355(3) 0.0324(9) Uani 1 1 d . . .
C44 C 0.1939(3) 0.8823(3) 0.2660(2) 0.0258(8) Uani 1 1 d . . .
C45 C 0.8002(4) 0.9080(3) 0.4853(3) 0.0440(11) Uani 1 1 d . . .
H45A H 0.8699 0.9096 0.4976 0.053 Uiso 1 1 calc R . .
C46 C 0.7563(4) 0.9405(3) 0.5486(3) 0.0509(12) Uani 1 1 d . . .
H46A H 0.7966 0.9655 0.6044 0.061 Uiso 1 1 calc R . .
C47 C 0.6554(5) 0.9384(4) 0.5342(3) 0.0576(14) Uani 1 1 d . . .
H47A H 0.6265 0.9616 0.5795 0.069 Uiso 1 1 calc R . .
C48 C 0.5966(4) 0.9020(3) 0.4531(4) 0.0568(14) Uani 1 1 d . . .
H48A H 0.5261 0.8984 0.4423 0.068 Uiso 1 1 calc R . .
C49 C 0.6414(4) 0.8709(3) 0.3878(3) 0.0505(12) Uani 1 1 d . . .
H49A H 0.6016 0.8481 0.3317 0.061 Uiso 1 1 calc R . .
C50 C 0.7434(4) 0.8720(3) 0.4020(3) 0.0444(11) Uani 1 1 d . . .
C51 C 0.7921(5) 0.8401(4) 0.3308(3) 0.0683(16) Uani 1 1 d . . .
H51A H 0.7689 0.7706 0.3219 0.102 Uiso 1 1 calc R . .
H51B H 0.8692 0.8691 0.3459 0.102 Uiso 1 1 calc R . .
H51C H 0.7702 0.8595 0.2779 0.102 Uiso 1 1 calc R . .
C52 C 0.8313(4) 0.8374(3) 0.0910(3) 0.0521(12) Uani 1 1 d . . .
H52A H 0.8678 0.8457 0.1474 0.063 Uiso 1 1 calc R . .
C53 C 0.7229(5) 0.8077(4) 0.0772(4) 0.0718(16) Uani 1 1 d . . .
H53A H 0.6852 0.7957 0.1242 0.086 Uiso 1 1 calc R . .
C54 C 0.6691(5) 0.7954(5) -0.0031(5) 0.090(2) Uani 1 1 d . . .
H54A H 0.5945 0.7756 -0.0119 0.108 Uiso 1 1 calc R . .
C55 C 0.7242(6) 0.8121(5) -0.0728(5) 0.090(2) Uani 1 1 d . . .
H55A H 0.6875 0.8035 -0.1291 0.108 Uiso 1 1 calc R . .
C56 C 0.8329(5) 0.8412(4) -0.0582(3) 0.0628(14) Uani 1 1 d . . .
H56A H 0.8707 0.8517 -0.1052 0.075 Uiso 1 1 calc R . .
C57 C 0.8871(4) 0.8552(3) 0.0234(3) 0.0466(11) Uani 1 1 d . . .
C58 C 1.0053(4) 0.8873(3) 0.0371(3) 0.0552(13) Uani 1 1 d . . .
H58A H 1.0301 0.8899 -0.0186 0.083 Uiso 1 1 calc R . .
H58B H 1.0261 0.8424 0.0659 0.083 Uiso 1 1 calc R . .
H58C H 1.0369 0.9507 0.0728 0.083 Uiso 1 1 calc R . .
C59 C 0.7246(5) 0.1430(6) -0.0090(4) 0.090(2) Uani 1 1 d . . .
H59A H 0.7566 0.0995 -0.0251 0.107 Uiso 1 1 calc R . .
C60 C 0.7474(5) 0.2245(9) -0.0421(4) 0.117(4) Uani 1 1 d . . .
H60A H 0.7964 0.2379 -0.0812 0.140 Uiso 1 1 calc R . .
C61 C 0.7013(6) 0.2881(6) -0.0204(5) 0.108(3) Uani 1 1 d . . .
H61A H 0.7164 0.3432 -0.0465 0.130 Uiso 1 1 calc R . .
C62 C 0.6328(5) 0.2723(5) 0.0395(5) 0.090(2) Uani 1 1 d . . .
H62A H 0.6026 0.3169 0.0570 0.108 Uiso 1 1 calc R . .
C63 C 0.6097(4) 0.1876(4) 0.0733(3) 0.0628(15) Uani 1 1 d . . .
H63A H 0.5625 0.1745 0.1140 0.075 Uiso 1 1 calc R . .
C64 C 0.6535(4) 0.1243(4) 0.0490(3) 0.0611(14) Uani 1 1 d . . .
C65 C 0.6304(5) 0.0357(5) 0.0822(5) 0.097(2) Uani 1 1 d . . .
H65A H 0.6464 0.0495 0.1452 0.146 Uiso 1 1 calc R . .
H65B H 0.6736 0.0026 0.0597 0.146 Uiso 1 1 calc R . .
H65C H 0.5555 -0.0047 0.0642 0.146 Uiso 1 1 calc R . .


_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 C1 1.923(3) . ?
Ni1 P1 2.1792(10) . ?
Ni1 P3 2.1827(10) . ?
Ni1 P2 2.1966(10) . ?
P1 C3 1.818(4) . ?
P1 C2 1.822(4) . ?
P1 C9 1.826(4) . ?
P2 C8 1.837(4) . ?
P2 C16 1.840(4) . ?
P2 C19 1.844(4) . ?
P3 C14 1.835(4) . ?
P3 C25 1.845(4) . ?
P3 C22 1.848(4) . ?
O1 C1 1.223(4) . ?
O2 C1 1.340(4) . ?
O2 B1 1.532(4) . ?
B1 C33 1.651(5) . ?
B1 C39 1.655(5) . ?
B1 C27 1.652(5) . ?
F1 C28 1.351(4) . ?
F2 C29 1.342(4) . ?
F3 C30 1.355(4) . ?
F4 C31 1.353(4) . ?
F5 C32 1.353(4) . ?
F6 C34 1.361(4) . ?
F7 C35 1.348(4) . ?
F8 C36 1.345(4) . ?
F9 C37 1.353(4) . ?
F10 C38 1.364(4) . ?
F11 C40 1.363(4) . ?
F12 C41 1.351(4) . ?
F13 C42 1.343(4) . ?
F14 C43 1.356(4) . ?
F15 C44 1.358(4) . ?
C3 C4 1.384(5) . ?
C3 C8 1.414(5) . ?
C4 C5 1.385(5) . ?
C5 C6 1.386(5) . ?
C6 C7 1.386(5) . ?
C7 C8 1.405(5) . ?
C9 C10 1.395(5) . ?
C9 C14 1.401(5) . ?
C10 C11 1.386(5) . ?
C11 C12 1.377(6) . ?
C12 C13 1.384(6) . ?
C13 C14 1.393(5) . ?
C15 C16 1.527(5) . ?
C16 C17 1.529(5) . ?
C18 C19 1.523(5) . ?
C19 C20 1.527(5) . ?
C21 C22 1.531(6) . ?
C22 C23 1.536(5) . ?
C24 C25 1.546(6) . ?
C25 C26 1.524(6) . ?
C27 C32 1.390(5) . ?
C27 C28 1.397(5) . ?
C28 C29 1.381(5) . ?
C29 C30 1.368(6) . ?
C30 C31 1.373(5) . ?
C31 C32 1.385(5) . ?
C33 C34 1.387(5) . ?
C33 C38 1.399(5) . ?
C34 C35 1.369(5) . ?
C35 C36 1.383(5) . ?
C36 C37 1.372(5) . ?
C37 C38 1.370(5) . ?
C39 C40 1.393(5) . ?
C39 C44 1.399(5) . ?
C40 C41 1.376(5) . ?
C41 C42 1.365(5) . ?
C42 C43 1.375(6) . ?
C43 C44 1.375(5) . ?
C45 C46 1.360(7) . ?
C45 C50 1.400(6) . ?
C46 C47 1.373(7) . ?
C47 C48 1.381(7) . ?
C48 C49 1.381(7) . ?
C49 C50 1.393(6) . ?
C50 C51 1.493(7) . ?
C52 C53 1.379(7) . ?
C52 C57 1.382(7) . ?
C53 C54 1.362(9) . ?
C54 C55 1.402(10) . ?
C55 C56 1.383(8) . ?
C56 C57 1.378(7) . ?
C57 C58 1.503(7) . ?
C59 C60 1.358(12) . ?
C59 C64 1.390(8) . ?
C60 C61 1.372(12) . ?
C61 C62 1.389(11) . ?
C62 C63 1.406(8) . ?
C63 C64 1.355(8) . ?
C64 C65 1.455(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni1 P1 173.82(10) . . ?
C1 Ni1 P3 92.10(10) . . ?
P1 Ni1 P3 87.90(4) . . ?
C1 Ni1 P2 94.63(10) . . ?
P1 Ni1 P2 87.99(4) . . ?
P3 Ni1 P2 154.43(4) . . ?
C3 P1 C2 103.15(17) . . ?
C3 P1 C9 109.68(16) . . ?
C2 P1 C9 104.08(17) . . ?
C3 P1 Ni1 108.17(11) . . ?
C2 P1 Ni1 122.47(13) . . ?
C9 P1 Ni1 108.79(12) . . ?
C8 P2 C16 106.36(16) . . ?
C8 P2 C19 101.66(16) . . ?
C16 P2 C19 106.39(16) . . ?
C8 P2 Ni1 105.99(11) . . ?
C16 P2 Ni1 116.48(12) . . ?
C19 P2 Ni1 118.32(13) . . ?
C14 P3 C25 106.86(18) . . ?
C14 P3 C22 104.39(17) . . ?
C25 P3 C22 111.27(18) . . ?
C14 P3 Ni1 106.82(12) . . ?
C25 P3 Ni1 111.92(13) . . ?
C22 P3 Ni1 114.87(14) . . ?
C1 O2 B1 121.8(3) . . ?
O2 B1 C33 107.0(3) . . ?
O2 B1 C39 115.7(3) . . ?
C33 B1 C39 102.1(3) . . ?
O2 B1 C27 104.8(3) . . ?
C33 B1 C27 113.0(3) . . ?
C39 B1 C27 114.3(3) . . ?
O1 C1 O2 122.9(3) . . ?
O1 C1 Ni1 129.7(3) . . ?
O2 C1 Ni1 107.4(2) . . ?
C4 C3 C8 120.0(3) . . ?
C4 C3 P1 125.1(3) . . ?
C8 C3 P1 114.8(2) . . ?
C5 C4 C3 120.8(3) . . ?
C6 C5 C4 119.7(3) . . ?
C5 C6 C7 120.4(3) . . ?
C6 C7 C8 120.5(3) . . ?
C7 C8 C3 118.4(3) . . ?
C7 C8 P2 123.6(3) . . ?
C3 C8 P2 118.0(3) . . ?
C10 C9 C14 120.0(3) . . ?
C10 C9 P1 124.8(3) . . ?
C14 C9 P1 115.2(3) . . ?
C11 C10 C9 120.1(4) . . ?
C12 C11 C10 120.0(4) . . ?
C11 C12 C13 120.4(4) . . ?
C12 C13 C14 120.8(4) . . ?
C13 C14 C9 118.7(3) . . ?
C13 C14 P3 123.8(3) . . ?
C9 C14 P3 117.4(3) . . ?
C15 C16 C17 111.1(3) . . ?
C15 C16 P2 110.5(2) . . ?
C17 C16 P2 115.9(3) . . ?
C18 C19 C20 111.2(3) . . ?
C18 C19 P2 114.3(3) . . ?
C20 C19 P2 109.4(2) . . ?
C21 C22 C23 109.4(4) . . ?
C21 C22 P3 108.7(3) . . ?
C23 C22 P3 116.9(3) . . ?
C26 C25 C24 111.8(3) . . ?
C26 C25 P3 118.6(3) . . ?
C24 C25 P3 109.8(3) . . ?
C32 C27 C28 112.7(3) . . ?
C32 C27 B1 120.3(3) . . ?
C28 C27 B1 126.8(3) . . ?
F1 C28 C29 115.3(3) . . ?
F1 C28 C27 120.3(3) . . ?
C29 C28 C27 124.3(3) . . ?
F2 C29 C30 119.2(3) . . ?
F2 C29 C28 121.0(4) . . ?
C30 C29 C28 119.7(3) . . ?
F3 C30 C29 120.5(4) . . ?
F3 C30 C31 120.1(4) . . ?
C29 C30 C31 119.4(3) . . ?
F4 C31 C30 119.9(3) . . ?
F4 C31 C32 121.1(3) . . ?
C30 C31 C32 119.0(3) . . ?
F5 C32 C31 115.4(3) . . ?
F5 C32 C27 119.7(3) . . ?
C31 C32 C27 124.9(3) . . ?
C34 C33 C38 111.9(3) . . ?
C34 C33 B1 127.5(3) . . ?
C38 C33 B1 120.4(3) . . ?
F6 C34 C35 114.5(3) . . ?
F6 C34 C33 120.4(3) . . ?
C35 C34 C33 125.2(3) . . ?
F7 C35 C34 120.5(3) . . ?
F7 C35 C36 119.5(3) . . ?
C34 C35 C36 120.0(3) . . ?
F8 C36 C37 120.7(4) . . ?
F8 C36 C35 121.5(3) . . ?
C37 C36 C35 117.9(3) . . ?
F9 C37 C38 120.8(3) . . ?
F9 C37 C36 119.2(3) . . ?
C38 C37 C36 120.0(3) . . ?
F10 C38 C37 115.5(3) . . ?
F10 C38 C33 119.3(3) . . ?
C37 C38 C33 125.1(3) . . ?
C40 C39 C44 112.3(3) . . ?
C40 C39 B1 126.8(3) . . ?
C44 C39 B1 120.4(3) . . ?
F11 C40 C41 115.0(3) . . ?
F11 C40 C39 120.0(3) . . ?
C41 C40 C39 124.9(3) . . ?
F12 C41 C42 119.7(3) . . ?
F12 C41 C40 120.5(3) . . ?
C42 C41 C40 119.8(3) . . ?
F13 C42 C41 121.3(4) . . ?
F13 C42 C43 120.2(3) . . ?
C41 C42 C43 118.6(3) . . ?
F14 C43 C44 120.0(3) . . ?
F14 C43 C42 119.9(3) . . ?
C44 C43 C42 120.0(3) . . ?
F15 C44 C43 116.4(3) . . ?
F15 C44 C39 119.3(3) . . ?
C43 C44 C39 124.3(3) . . ?
C46 C45 C50 120.3(5) . . ?
C45 C46 C47 121.9(5) . . ?
C46 C47 C48 119.2(5) . . ?
C47 C48 C49 119.3(5) . . ?
C48 C49 C50 121.9(5) . . ?
C49 C50 C45 117.3(5) . . ?
C49 C50 C51 121.6(4) . . ?
C45 C50 C51 121.0(4) . . ?
C53 C52 C57 120.3(5) . . ?
C54 C53 C52 120.7(6) . . ?
C53 C54 C55 119.9(6) . . ?
C56 C55 C54 118.9(6) . . ?
C57 C56 C55 121.0(6) . . ?
C56 C57 C52 119.2(5) . . ?
C56 C57 C58 119.7(5) . . ?
C52 C57 C58 121.2(4) . . ?
C60 C59 C64 118.9(8) . . ?
C59 C60 C61 121.7(7) . . ?
C60 C61 C62 120.3(7) . . ?
C61 C62 C63 117.5(8) . . ?
C64 C63 C62 121.2(6) . . ?
C63 C64 C59 120.4(6) . . ?
C63 C64 C65 122.5(6) . . ?
C59 C64 C65 117.2(7) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.104
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.149
_database_code_depnum_ccdc_archive 'CCDC 993624'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_0134a-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            {(PPMeP)Ni}2(N2)
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H78 N2 Ni2 P6'
_chemical_formula_sum            'C50 H78 N2 Ni2 P6'
_chemical_formula_weight         1010.38

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Ibca

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

_cell_length_a                   18.5080(10)
_cell_length_b                   19.9088(10)
_cell_length_c                   28.5632(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10524.7(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    60672
_cell_measurement_theta_min      1.43
_cell_measurement_theta_max      29.36

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4304
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8652
_exptl_absorpt_correction_T_max  0.9126
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            60672
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         29.36
_reflns_number_total             7168
_reflns_number_gt                5516
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0409P)²+9.6976P] where P=(Fo²+2Fc²)/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_number_reflns         7168
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0777
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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 0.261049(13) 0.116267(11) 0.083434(8) 0.01564(7) Uani 1 1 d . . .
P1 P 0.20741(3) 0.04938(2) 0.129380(16) 0.01752(11) Uani 1 1 d . . .
P2 P 0.36351(3) 0.06870(2) 0.098473(17) 0.01822(11) Uani 1 1 d . . .
P3 P 0.20566(3) 0.20127(2) 0.113277(17) 0.01930(11) Uani 1 1 d . . .
N1 N 0.25204(9) 0.11552(7) 0.01963(5) 0.0177(3) Uani 1 1 d . . .
C1 C 0.13944(12) -0.01577(10) 0.11726(8) 0.0312(5) Uani 1 1 d . . .
H1A H 0.1255 -0.0377 0.1466 0.047 Uiso 1 1 calc R . .
H1B H 0.1598 -0.0492 0.0958 0.047 Uiso 1 1 calc R . .
H1C H 0.0968 0.0049 0.1029 0.047 Uiso 1 1 calc R . .
C2 C 0.27605(10) 0.00129(9) 0.16240(6) 0.0198(4) Uani 1 1 d . . .
C3 C 0.34839(11) 0.01192(9) 0.14893(6) 0.0206(4) Uani 1 1 d . . .
C4 C 0.40294(11) -0.02319(10) 0.17248(7) 0.0264(4) Uani 1 1 d . . .
H4A H 0.4520 -0.0160 0.1641 0.032 Uiso 1 1 calc R . .
C5 C 0.38633(12) -0.06839(10) 0.20799(7) 0.0293(5) Uani 1 1 d . . .
H5A H 0.4240 -0.0917 0.2237 0.035 Uiso 1 1 calc R . .
C6 C 0.31529(12) -0.07944(10) 0.22056(7) 0.0284(5) Uani 1 1 d . . .
H6A H 0.3040 -0.1105 0.2447 0.034 Uiso 1 1 calc R . .
C7 C 0.26062(12) -0.04499(9) 0.19772(7) 0.0245(4) Uani 1 1 d . . .
H7A H 0.2118 -0.0530 0.2063 0.029 Uiso 1 1 calc R . .
C8 C 0.15769(11) 0.10001(10) 0.17306(7) 0.0219(4) Uani 1 1 d . . .
C9 C 0.15648(11) 0.16966(10) 0.16517(7) 0.0235(4) Uani 1 1 d . . .
C10 C 0.11552(12) 0.21033(11) 0.19512(7) 0.0323(5) Uani 1 1 d . . .
H10A H 0.1137 0.2574 0.1898 0.039 Uiso 1 1 calc R . .
C11 C 0.07762(12) 0.18308(12) 0.23235(8) 0.0380(6) Uani 1 1 d . . .
H11A H 0.0511 0.2115 0.2528 0.046 Uiso 1 1 calc R . .
C12 C 0.07856(12) 0.11428(12) 0.23967(8) 0.0357(5) Uani 1 1 d . . .
H12A H 0.0524 0.0954 0.2651 0.043 Uiso 1 1 calc R . .
C13 C 0.11748(11) 0.07314(11) 0.21000(7) 0.0298(5) Uani 1 1 d . . .
H13A H 0.1169 0.0259 0.2148 0.036 Uiso 1 1 calc R . .
C14 C 0.32450(13) -0.04229(10) 0.04381(8) 0.0324(5) Uani 1 1 d . . .
H14A H 0.3368 -0.0738 0.0187 0.049 Uiso 1 1 calc R . .
H14B H 0.2805 -0.0177 0.0354 0.049 Uiso 1 1 calc R . .
H14C H 0.3163 -0.0672 0.0729 0.049 Uiso 1 1 calc R . .
C15 C 0.38675(11) 0.00739(10) 0.05075(7) 0.0241(4) Uani 1 1 d . . .
H15A H 0.3903 0.0340 0.0212 0.029 Uiso 1 1 calc R . .
C16 C 0.45783(13) -0.03121(12) 0.05545(8) 0.0384(6) Uani 1 1 d . . .
H16A H 0.4638 -0.0612 0.0285 0.058 Uiso 1 1 calc R . .
H16B H 0.4571 -0.0578 0.0843 0.058 Uiso 1 1 calc R . .
H16C H 0.4982 0.0006 0.0566 0.058 Uiso 1 1 calc R . .
C17 C 0.47771(13) 0.14804(12) 0.06871(8) 0.0374(5) Uani 1 1 d . . .
H17A H 0.5248 0.1684 0.0752 0.056 Uiso 1 1 calc R . .
H17B H 0.4423 0.1834 0.0622 0.056 Uiso 1 1 calc R . .
H17C H 0.4817 0.1184 0.0415 0.056 Uiso 1 1 calc R . .
C18 C 0.45294(11) 0.10698(10) 0.11154(7) 0.0263(4) Uani 1 1 d . . .
H18A H 0.4887 0.0702 0.1173 0.032 Uiso 1 1 calc R . .
C19 C 0.44916(12) 0.15155(11) 0.15505(8) 0.0346(5) Uani 1 1 d . . .
H19A H 0.4968 0.1712 0.1611 0.052 Uiso 1 1 calc R . .
H19B H 0.4344 0.1245 0.1821 0.052 Uiso 1 1 calc R . .
H19C H 0.4139 0.1875 0.1499 0.052 Uiso 1 1 calc R . .
C20 C 0.28315(14) 0.26857(12) 0.18383(8) 0.0391(6) Uani 1 1 d . . .
H20A H 0.3062 0.3102 0.1944 0.059 Uiso 1 1 calc R . .
H20B H 0.3195 0.2329 0.1818 0.059 Uiso 1 1 calc R . .
H20C H 0.2454 0.2555 0.2061 0.059 Uiso 1 1 calc R . .
C21 C 0.24944(12) 0.27974(10) 0.13557(7) 0.0290(5) Uani 1 1 d . . .
H21A H 0.2122 0.3160 0.1379 0.035 Uiso 1 1 calc R . .
C22 C 0.30769(14) 0.30124(11) 0.10073(9) 0.0402(6) Uani 1 1 d . . .
H22A H 0.3312 0.3423 0.1120 0.060 Uiso 1 1 calc R . .
H22B H 0.2855 0.3098 0.0702 0.060 Uiso 1 1 calc R . .
H22C H 0.3437 0.2654 0.0977 0.060 Uiso 1 1 calc R . .
C23 C 0.14901(13) 0.26673(10) 0.03349(7) 0.0338(5) Uani 1 1 d . . .
H23A H 0.1061 0.2832 0.0169 0.051 Uiso 1 1 calc R . .
H23B H 0.1740 0.2335 0.0140 0.051 Uiso 1 1 calc R . .
H23C H 0.1816 0.3044 0.0399 0.051 Uiso 1 1 calc R . .
C24 C 0.12612(11) 0.23414(10) 0.07965(7) 0.0262(4) Uani 1 1 d . . .
H24A H 0.1013 0.2689 0.0992 0.031 Uiso 1 1 calc R . .
C25 C 0.07267(12) 0.17732(11) 0.06999(8) 0.0345(5) Uani 1 1 d . . .
H25A H 0.0313 0.1949 0.0525 0.052 Uiso 1 1 calc R . .
H25B H 0.0559 0.1584 0.0997 0.052 Uiso 1 1 calc R . .
H25C H 0.0965 0.1422 0.0516 0.052 Uiso 1 1 calc R . .


_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 1.8301(15) . ?
Ni1 P1 2.1168(5) . ?
Ni1 P3 2.1544(5) . ?
Ni1 P2 2.1627(5) . ?
P1 C1 1.840(2) . ?
P1 C8 1.849(2) . ?
P1 C2 1.8495(19) . ?
P2 C3 1.8528(19) . ?
P2 C18 1.860(2) . ?
P2 C15 1.8798(19) . ?
P3 C9 1.850(2) . ?
P3 C21 1.872(2) . ?
P3 C24 1.876(2) . ?
N1 N1 1.124(3) 7_544 ?
C2 C7 1.396(3) . ?
C2 C3 1.409(3) . ?
C3 C4 1.400(3) . ?
C4 C5 1.390(3) . ?
C5 C6 1.381(3) . ?
C6 C7 1.386(3) . ?
C8 C13 1.398(3) . ?
C8 C9 1.405(3) . ?
C9 C10 1.401(3) . ?
C10 C11 1.384(3) . ?
C11 C12 1.386(3) . ?
C12 C13 1.381(3) . ?
C14 C15 1.531(3) . ?
C15 C16 1.529(3) . ?
C17 C18 1.541(3) . ?
C18 C19 1.529(3) . ?
C20 C21 1.529(3) . ?
C21 C22 1.529(3) . ?
C23 C24 1.529(3) . ?
C24 C25 1.528(3) . ?

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 P1 124.72(5) . . ?
N1 Ni1 P3 110.92(5) . . ?
P1 Ni1 P3 91.47(2) . . ?
N1 Ni1 P2 105.91(5) . . ?
P1 Ni1 P2 90.72(2) . . ?
P3 Ni1 P2 133.05(2) . . ?
C1 P1 C8 99.84(10) . . ?
C1 P1 C2 101.57(9) . . ?
C8 P1 C2 106.25(8) . . ?
C1 P1 Ni1 130.35(7) . . ?
C8 P1 Ni1 107.99(6) . . ?
C2 P1 Ni1 108.65(6) . . ?
C3 P2 C18 103.20(9) . . ?
C3 P2 C15 101.68(8) . . ?
C18 P2 C15 102.00(9) . . ?
C3 P2 Ni1 106.82(6) . . ?
C18 P2 Ni1 129.84(7) . . ?
C15 P2 Ni1 109.94(6) . . ?
C9 P3 C21 102.97(9) . . ?
C9 P3 C24 98.21(9) . . ?
C21 P3 C24 102.87(9) . . ?
C9 P3 Ni1 106.50(6) . . ?
C21 P3 Ni1 125.75(7) . . ?
C24 P3 Ni1 116.42(6) . . ?
N1 N1 Ni1 178.6(2) 7_544 . ?
C7 C2 C3 119.41(17) . . ?
C7 C2 P1 124.74(16) . . ?
C3 C2 P1 115.82(13) . . ?
C4 C3 C2 118.61(18) . . ?
C4 C3 P2 124.71(16) . . ?
C2 C3 P2 116.59(13) . . ?
C5 C4 C3 120.9(2) . . ?
C6 C5 C4 120.23(19) . . ?
C5 C6 C7 119.62(19) . . ?
C6 C7 C2 121.2(2) . . ?
C13 C8 C9 119.36(18) . . ?
C13 C8 P1 124.46(16) . . ?
C9 C8 P1 115.95(14) . . ?
C10 C9 C8 118.75(18) . . ?
C10 C9 P3 123.99(16) . . ?
C8 C9 P3 117.16(14) . . ?
C11 C10 C9 121.1(2) . . ?
C10 C11 C12 119.8(2) . . ?
C13 C12 C11 120.0(2) . . ?
C12 C13 C8 120.9(2) . . ?
C16 C15 C14 109.52(17) . . ?
C16 C15 P2 117.35(14) . . ?
C14 C15 P2 109.94(14) . . ?
C19 C18 C17 110.56(18) . . ?
C19 C18 P2 111.11(15) . . ?
C17 C18 P2 108.83(14) . . ?
C22 C21 C20 109.86(19) . . ?
C22 C21 P3 108.51(14) . . ?
C20 C21 P3 111.22(15) . . ?
C25 C24 C23 109.74(18) . . ?
C25 C24 P3 110.01(13) . . ?
C23 C24 P3 111.84(15) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        29.36
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.081
_database_code_depnum_ccdc_archive 'CCDC 994135'
