# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_FO5231
_publcif_datablock.id            {cdaa60af-ed14-4996-a03e-657269297004}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H26 N2 Ni O2'
_chemical_formula_sum            'C16 H26 N2 Ni O2'
_chemical_formula_weight         337.10

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'
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   'I m a 2'
_symmetry_space_group_name_Hall  'I 2 -2a'

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

_cell_length_a                   28.090(2)
_cell_length_b                   13.7216(9)
_cell_length_c                   10.9264(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4211.4(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    15012
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      27.74

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.052
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440.0
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      133(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  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4286
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         27.74
_reflns_number_total             4286
_reflns_number_gt                3643
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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. The crystal contain large voids, filled with
disordered solvent molecules. The size of the voids are 615 Å³/unit cell.
Their contribution to the structure factors was secured by back-Fourier
transformation using the SQUEEZE routine of the program PLATON
resulting in 97 electrons/unit cell.
;

_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)+(0.1050P)²+34.6077P] 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_abs_structure_details 
;
 Flack x determined using 1522 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.097(15)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         4844
_refine_ls_number_parameters     192
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.2185
_refine_ls_wR_factor_gt          0.2090
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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 -0.40399(3) -0.97823(5) -1.00287(9) 0.0249(2) Uani 1 1 d . . .
O1 O -0.41861(15) -0.8496(4) -0.9416(4) 0.0240(10) Uani 1 1 d . . .
O2 O -0.42208(16) -0.6926(3) -0.9892(5) 0.0307(10) Uani 1 1 d . . .
N1 N -0.42957(19) -1.0558(4) -0.8704(4) 0.0201(10) Uani 1 1 d . . .
N2 N -0.44922(19) -1.0856(4) -0.6634(5) 0.0217(11) Uani 1 1 d . . .
C1 C -0.41183(18) -0.7785(5) -1.0139(8) 0.0233(13) Uani 1 1 d . . .
C2 C -0.3887(2) -0.8035(5) -1.1371(6) 0.0282(15) Uani 1 1 d . . .
H2A H -0.3540 -0.7909 -1.1334 0.034 Uiso 1 1 calc R . .
H2B H -0.4025 -0.7623 -1.2026 0.034 Uiso 1 1 calc R . .
C3 C -0.3979(2) -0.9129(6) -1.1655(6) 0.0302(15) Uani 1 1 d . . .
C4 C -0.3634(3) -0.9859(6) -1.1493(7) 0.0377(18) Uani 1 1 d . . .
C5 C -0.3814(2) -1.0801(6) -1.1209(6) 0.0314(16) Uani 1 1 d . . .
H5A H -0.3583 -1.1286 -1.0895 0.038 Uiso 1 1 calc R . .
H5B H -0.4054 -1.1077 -1.1775 0.038 Uiso 1 1 calc R . .
C6 C -0.4451(2) -0.9294(6) -1.2293(6) 0.0305(16) Uani 1 1 d . . .
H6A H -0.4444 -0.8989 -1.3104 0.046 Uiso 1 1 calc R . .
H6B H -0.4708 -0.9004 -1.1807 0.046 Uiso 1 1 calc R . .
H6C H -0.4507 -0.9995 -1.2382 0.046 Uiso 1 1 calc R . .
C7 C -0.3104(3) -0.9664(9) -1.1304(10) 0.066(3) Uani 1 1 d . . .
H7A H -0.2982 -0.9279 -1.1991 0.099 Uiso 1 1 calc R . .
H7B H -0.2932 -1.0285 -1.1260 0.099 Uiso 1 1 calc R . .
H7C H -0.3058 -0.9302 -1.0540 0.099 Uiso 1 1 calc R . .
C8 C -0.4655(3) -1.1253(5) -0.9068(6) 0.0314(15) Uani 1 1 d . . .
H8A H -0.4562 -1.1536 -0.9867 0.038 Uiso 1 1 calc R . .
H8B H -0.4959 -1.0903 -0.9186 0.038 Uiso 1 1 calc R . .
C9 C -0.4732(2) -1.2063(5) -0.8179(7) 0.0296(15) Uani 1 1 d . . .
H9A H -0.4443 -1.2473 -0.8126 0.035 Uiso 1 1 calc R . .
H9B H -0.5000 -1.2477 -0.8452 0.035 Uiso 1 1 calc R . .
C10 C -0.4844(2) -1.1618(5) -0.6920(7) 0.0291(14) Uani 1 1 d . . .
H10A H -0.5168 -1.1334 -0.6926 0.035 Uiso 1 1 calc R . .
H10B H -0.4834 -1.2133 -0.6285 0.035 Uiso 1 1 calc R . .
C11 C -0.4424(3) -1.0654(5) -0.5318(5) 0.0319(16) Uani 1 1 d . . .
H11A H -0.4696 -1.0932 -0.4861 0.038 Uiso 1 1 calc R . .
H11B H -0.4429 -0.9940 -0.5194 0.038 Uiso 1 1 calc R . .
C12 C -0.3973(3) -1.1049(7) -0.4787(7) 0.052(3) Uani 1 1 d . . .
H12A H -0.3917 -1.1711 -0.5120 0.062 Uiso 1 1 calc R . .
H12B H -0.4011 -1.1110 -0.3889 0.062 Uiso 1 1 calc R . .
C13 C -0.3531(3) -1.0410(6) -0.5055(12) 0.057(3) Uani 1 1 d . . .
H13A H -0.3573 -0.9770 -0.4651 0.069 Uiso 1 1 calc R . .
H13B H -0.3247 -1.0725 -0.4692 0.069 Uiso 1 1 calc R . .
C14 C -0.3441(3) -1.0244(6) -0.6416(8) 0.0406(19) Uani 1 1 d . . .
H14A H -0.3383 -1.0884 -0.6808 0.049 Uiso 1 1 calc R . .
H14B H -0.3148 -0.9852 -0.6506 0.049 Uiso 1 1 calc R . .
C15 C -0.3848(2) -0.9726(5) -0.7114(6) 0.0276(15) Uani 1 1 d . . .
H15A H -0.3991 -0.9225 -0.6577 0.033 Uiso 1 1 calc R . .
H15B H -0.3713 -0.9391 -0.7838 0.033 Uiso 1 1 calc R . .
C16 C -0.4225(2) -1.0412(5) -0.7521(5) 0.0208(12) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.932(5) . ?
Ni1 N1 1.935(5) . ?
Ni1 C4 1.968(7) . ?
Ni1 C3 1.998(7) . ?
Ni1 C5 2.005(7) . ?
O1 C1 1.270(9) . ?
O2 C1 1.244(8) . ?
N1 C16 1.323(8) . ?
N1 C8 1.444(8) . ?
N2 C16 1.369(8) . ?
N2 C10 1.473(8) . ?
N2 C11 1.476(8) . ?
C1 C2 1.534(10) . ?
C2 C3 1.554(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.407(10) . ?
C3 C6 1.515(9) . ?
C4 C5 1.422(12) . ?
C4 C7 1.526(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.492(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.537(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.495(12) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.548(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.525(15) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.546(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.486(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 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
O1 Ni1 N1 99.4(2) . . ?
O1 Ni1 C4 117.0(3) . . ?
N1 Ni1 C4 142.5(3) . . ?
O1 Ni1 C3 85.2(3) . . ?
N1 Ni1 C3 160.7(3) . . ?
C4 Ni1 C3 41.5(3) . . ?
O1 Ni1 C5 158.0(3) . . ?
N1 Ni1 C5 102.4(3) . . ?
C4 Ni1 C5 41.9(3) . . ?
C3 Ni1 C5 73.4(3) . . ?
C1 O1 Ni1 117.0(4) . . ?
C16 N1 C8 118.3(5) . . ?
C16 N1 Ni1 126.3(4) . . ?
C8 N1 Ni1 114.6(4) . . ?
C16 N2 C10 122.2(5) . . ?
C16 N2 C11 122.3(6) . . ?
C10 N2 C11 115.3(5) . . ?
O2 C1 O1 123.9(7) . . ?
O2 C1 C2 120.1(7) . . ?
O1 C1 C2 116.0(5) . . ?
C1 C2 C3 108.7(5) . . ?
C1 C2 H2A 110.0 . . ?
C3 C2 H2A 110.0 . . ?
C1 C2 H2B 110.0 . . ?
C3 C2 H2B 110.0 . . ?
H2A C2 H2B 108.3 . . ?
C4 C3 C6 123.7(7) . . ?
C4 C3 C2 123.2(6) . . ?
C6 C3 C2 112.5(6) . . ?
C4 C3 Ni1 68.1(4) . . ?
C6 C3 Ni1 105.5(5) . . ?
C2 C3 Ni1 105.7(4) . . ?
C3 C4 C5 115.4(6) . . ?
C3 C4 C7 124.4(8) . . ?
C5 C4 C7 118.5(8) . . ?
C3 C4 Ni1 70.3(4) . . ?
C5 C4 Ni1 70.4(4) . . ?
C7 C4 Ni1 116.5(6) . . ?
C4 C5 Ni1 67.7(4) . . ?
C4 C5 H5A 116.9 . . ?
Ni1 C5 H5A 116.9 . . ?
C4 C5 H5B 116.9 . . ?
Ni1 C5 H5B 116.9 . . ?
H5A C5 H5B 113.9 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C9 114.4(5) . . ?
N1 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C8 C9 C10 108.5(6) . . ?
C8 C9 H9A 110.0 . . ?
C10 C9 H9A 110.0 . . ?
C8 C9 H9B 110.0 . . ?
C10 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 C9 109.5(5) . . ?
N2 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
N2 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
N2 C11 C12 114.9(6) . . ?
N2 C11 H11A 108.5 . . ?
C12 C11 H11A 108.5 . . ?
N2 C11 H11B 108.5 . . ?
C12 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 C13 113.5(7) . . ?
C11 C12 H12A 108.9 . . ?
C13 C12 H12A 108.9 . . ?
C11 C12 H12B 108.9 . . ?
C13 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C14 C13 C12 113.7(7) . . ?
C14 C13 H13A 108.8 . . ?
C12 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
C12 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 C15 115.3(7) . . ?
C13 C14 H14A 108.4 . . ?
C15 C14 H14A 108.4 . . ?
C13 C14 H14B 108.4 . . ?
C15 C14 H14B 108.4 . . ?
H14A C14 H14B 107.5 . . ?
C16 C15 C14 112.5(6) . . ?
C16 C15 H15A 109.1 . . ?
C14 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C14 C15 H15B 109.1 . . ?
H15A C15 H15B 107.8 . . ?
N1 C16 N2 122.9(6) . . ?
N1 C16 C15 119.7(6) . . ?
N2 C16 C15 117.4(5) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.74
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.104
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.126
# SQUEEZE RESULTS
# 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 0.250 0.609 -0.055 615 97 ' '
2 0.750 0.385 -0.054 615 97 ' '
_platon_squeeze_details          ?
_database_code_depnum_ccdc_archive 'CCDC 1002896'
#######################################################################
#
#                 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_FO5287
_publcif_datablock.id            {7436809c-f5f4-456f-aee0-88e9a4b7f37b}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H35 N2 Ni O2 P'
_chemical_formula_sum            'C28 H35 N2 Ni O2 P'
_chemical_formula_weight         521.26

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  '-P 2yn'

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                   13.8132(5)
_cell_length_b                   12.2553(4)
_cell_length_c                   14.9680(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.186(2)
_cell_angle_gamma                90.00
_cell_volume                     2513.95(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    6389
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.029
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      133(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  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24526
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         27.58
_reflns_number_total             5761
_reflns_number_gt                4441
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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)+(0.0356P)²+4.8523P] 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         5761
_refine_ls_number_parameters     319
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1194
_refine_ls_wR_factor_gt          0.1081
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.39376(3) 0.26569(10) 0.09648(4) 0.0219(2) Uani 1 1 d P A 1
P1 P 0.48386(5) 0.30914(6) 0.21377(5) 0.02188(17) Uani 1 1 d . . .
O1 O 0.24063(14) 0.27839(18) 0.08420(13) 0.0302(5) Uani 1 1 d . . .
N1 N 0.39298(18) 0.1194(2) 0.15434(16) 0.0275(5) Uani 1 1 d . . .
N2 N 0.4255(2) 0.0076(2) 0.28409(18) 0.0330(6) Uani 1 1 d . . .
C1 C 0.1986(2) 0.2858(2) 0.00426(19) 0.0266(6) Uani 1 1 d . A .
O2 O 0.10939(15) 0.29852(18) -0.01788(14) 0.0323(5) Uani 1 1 d . . .
C2 C 0.2624(2) 0.2805(3) -0.0723(2) 0.0394(8) Uani 1 1 d . . .
H2A H 0.2285 0.2338 -0.1203 0.047 Uiso 1 1 calc R A .
H2B H 0.2655 0.3549 -0.0976 0.047 Uiso 1 1 calc R . .
C3 C 0.3667(2) 0.2386(3) -0.0511(2) 0.0370(8) Uani 1 1 d . A .
C4 C 0.4423(2) 0.3084(3) -0.0212(2) 0.0350(7) Uani 1 1 d . . .
C5 C 0.4189(3) 0.4009(3) 0.0307(2) 0.0378(8) Uani 1 1 d . A .
H5A H 0.3610 0.4439 0.0062 0.045 Uiso 1 1 calc R B 1
H5B H 0.4744 0.4463 0.0573 0.045 Uiso 1 1 calc R B 1
C6 C 0.3850(3) 0.1310(3) -0.0969(2) 0.0479(9) Uani 1 1 d . . .
H6A H 0.3931 0.1444 -0.1600 0.072 Uiso 1 1 calc R A .
H6B H 0.3293 0.0821 -0.0938 0.072 Uiso 1 1 calc R . .
H6C H 0.4442 0.0970 -0.0662 0.072 Uiso 1 1 calc R . .
C7 C 0.5471(3) 0.2838(3) -0.0328(2) 0.0438(9) Uani 1 1 d . A .
H7A H 0.5570 0.2952 -0.0958 0.066 Uiso 1 1 calc R . .
H7B H 0.5619 0.2077 -0.0160 0.066 Uiso 1 1 calc R . .
H7C H 0.5904 0.3323 0.0059 0.066 Uiso 1 1 calc R . .
C8 C 0.4558(2) 0.2034(2) 0.29496(17) 0.0217(6) Uani 1 1 d . A .
H8A H 0.5151 0.1865 0.3382 0.026 Uiso 1 1 calc R . .
C9 C 0.3708(2) 0.2401(2) 0.34662(19) 0.0262(6) Uani 1 1 d . . .
H9A H 0.3787 0.3187 0.3610 0.031 Uiso 1 1 calc R A .
H9B H 0.3086 0.2312 0.3066 0.031 Uiso 1 1 calc R . .
C10 C 0.3640(2) 0.1778(3) 0.4335(2) 0.0337(7) Uani 1 1 d . A .
H10A H 0.4220 0.1960 0.4766 0.040 Uiso 1 1 calc R . .
H10B H 0.3059 0.2043 0.4596 0.040 Uiso 1 1 calc R . .
C11 C 0.3572(2) 0.0544(3) 0.4256(2) 0.0337(7) Uani 1 1 d . . .
H11A H 0.2948 0.0351 0.3892 0.040 Uiso 1 1 calc R A .
H11B H 0.3564 0.0231 0.4864 0.040 Uiso 1 1 calc R . .
C12 C 0.4408(2) 0.0024(3) 0.3827(2) 0.0363(7) Uani 1 1 d . A .
H12A H 0.5025 0.0403 0.4048 0.044 Uiso 1 1 calc R . .
H12B H 0.4475 -0.0749 0.4017 0.044 Uiso 1 1 calc R . .
C13 C 0.3827(3) -0.0905(3) 0.2371(3) 0.0453(9) Uani 1 1 d . A .
H13A H 0.3487 -0.1347 0.2790 0.054 Uiso 1 1 calc R . .
H13B H 0.4352 -0.1358 0.2169 0.054 Uiso 1 1 calc R . .
C14 C 0.3110(3) -0.0578(3) 0.1563(2) 0.0458(9) Uani 1 1 d . . .
H14A H 0.2939 -0.1230 0.1185 0.055 Uiso 1 1 calc R A .
H14B H 0.2504 -0.0305 0.1776 0.055 Uiso 1 1 calc R . .
C15 C 0.3502(3) 0.0274(3) 0.1008(2) 0.0379(8) Uani 1 1 d . A .
H15A H 0.4007 -0.0053 0.0676 0.046 Uiso 1 1 calc R C 2
H15B H 0.2970 0.0547 0.0559 0.046 Uiso 1 1 calc R C 2
C16 C 0.4235(2) 0.1038(2) 0.23991(19) 0.0250(6) Uani 1 1 d . A .
C18 C 0.6534(2) 0.1889(3) 0.19616(19) 0.0315(7) Uani 1 1 d . . .
H18A H 0.6156 0.1260 0.2051 0.038 Uiso 1 1 calc R A .
C19 C 0.7490(2) 0.1774(3) 0.1778(2) 0.0402(8) Uani 1 1 d . A .
H19A H 0.7764 0.1066 0.1748 0.048 Uiso 1 1 calc R . .
C20 C 0.8047(2) 0.2683(3) 0.1639(2) 0.0401(8) Uani 1 1 d . . .
H20A H 0.8700 0.2598 0.1514 0.048 Uiso 1 1 calc R A .
C21 C 0.6127(2) 0.2926(2) 0.20145(18) 0.0250(6) Uani 1 1 d . A .
C21A C 0.7651(2) 0.3714(3) 0.1684(2) 0.0380(8) Uani 1 1 d . A .
H21A H 0.8031 0.4339 0.1586 0.046 Uiso 1 1 calc R . .
C22 C 0.6696(2) 0.3839(3) 0.18703(19) 0.0308(7) Uani 1 1 d . . .
H22A H 0.6427 0.4549 0.1900 0.037 Uiso 1 1 calc R A .
C23 C 0.4811(2) 0.4374(2) 0.27427(19) 0.0254(6) Uani 1 1 d . A .
C24 C 0.5414(2) 0.4555(3) 0.35497(19) 0.0306(7) Uani 1 1 d . . .
H24A H 0.5890 0.4026 0.3767 0.037 Uiso 1 1 calc R A .
C25 C 0.5320(3) 0.5506(3) 0.4035(2) 0.0387(8) Uani 1 1 d . A .
H25A H 0.5735 0.5627 0.4582 0.046 Uiso 1 1 calc R . .
C26 C 0.4630(3) 0.6277(3) 0.3731(3) 0.0417(8) Uani 1 1 d . . .
H26A H 0.4564 0.6922 0.4070 0.050 Uiso 1 1 calc R A .
C27 C 0.4042(3) 0.6108(3) 0.2941(3) 0.0415(8) Uani 1 1 d . A .
H27A H 0.3567 0.6639 0.2732 0.050 Uiso 1 1 calc R . .
C28 C 0.4132(2) 0.5159(3) 0.2436(2) 0.0343(7) Uani 1 1 d . . .
H28A H 0.3725 0.5055 0.1882 0.041 Uiso 1 1 calc R A .


_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 C5 1.980(3) . ?
Ni1 N1 1.992(3) . ?
Ni1 C4 2.030(3) . ?
Ni1 P1 2.0900(11) . ?
Ni1 O1 2.106(2) . ?
Ni1 C3 2.219(3) . ?
P1 C23 1.816(3) . ?
P1 C21 1.824(3) . ?
P1 C8 1.851(3) . ?
O1 C1 1.266(3) . ?
N1 C16 1.311(4) . ?
N1 C15 1.464(4) . ?
N2 C16 1.351(4) . ?
N2 C12 1.466(4) . ?
N2 C13 1.479(4) . ?
C1 O2 1.245(3) . ?
C1 C2 1.531(4) . ?
C2 C3 1.525(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.381(5) . ?
C3 C6 1.522(5) . ?
C4 C5 1.433(5) . ?
C4 C7 1.510(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C16 1.508(4) . ?
C8 C9 1.551(4) . ?
C8 H8A 1.0000 . ?
C9 C10 1.521(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.518(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.528(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.518(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.479(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C18 C19 1.390(4) . ?
C18 C21 1.396(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.384(5) . ?
C19 H19A 0.9500 . ?
C20 C21A 1.383(5) . ?
C20 H20A 0.9500 . ?
C21 C22 1.399(4) . ?
C21A C22 1.390(4) . ?
C21A H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C28 1.382(4) . ?
C23 C24 1.397(4) . ?
C24 C25 1.389(4) . ?
C24 H24A 0.9500 . ?
C25 C26 1.378(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.364(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.402(5) . ?
C27 H27A 0.9500 . ?
C28 H28A 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
C5 Ni1 N1 168.60(13) . . ?
C5 Ni1 C4 41.86(14) . . ?
N1 Ni1 C4 129.05(13) . . ?
C5 Ni1 P1 94.66(11) . . ?
N1 Ni1 P1 84.21(7) . . ?
C4 Ni1 P1 115.88(10) . . ?
C5 Ni1 O1 97.56(12) . . ?
N1 Ni1 O1 92.55(10) . . ?
C4 Ni1 O1 110.01(11) . . ?
P1 Ni1 O1 122.72(7) . . ?
C5 Ni1 C3 69.41(13) . . ?
N1 Ni1 C3 106.81(13) . . ?
C4 Ni1 C3 37.59(13) . . ?
P1 Ni1 C3 151.99(9) . . ?
O1 Ni1 C3 83.21(10) . . ?
C23 P1 C21 103.18(13) . . ?
C23 P1 C8 105.03(12) . . ?
C21 P1 C8 106.01(13) . . ?
C23 P1 Ni1 126.30(11) . . ?
C21 P1 Ni1 111.90(9) . . ?
C8 P1 Ni1 102.79(9) . . ?
C1 O1 Ni1 115.11(19) . . ?
C16 N1 C15 118.8(3) . . ?
C16 N1 Ni1 122.5(2) . . ?
C15 N1 Ni1 118.6(2) . . ?
C16 N2 C12 121.5(3) . . ?
C16 N2 C13 119.7(3) . . ?
C12 N2 C13 116.3(3) . . ?
O2 C1 O1 125.6(3) . . ?
O2 C1 C2 116.7(3) . . ?
O1 C1 C2 117.7(3) . . ?
C3 C2 C1 118.4(2) . . ?
C3 C2 H2A 107.7 . . ?
C1 C2 H2A 107.7 . . ?
C3 C2 H2B 107.7 . . ?
C1 C2 H2B 107.7 . . ?
H2A C2 H2B 107.1 . . ?
C4 C3 C6 121.5(3) . . ?
C4 C3 C2 121.0(3) . . ?
C6 C3 C2 113.8(3) . . ?
C4 C3 Ni1 63.75(17) . . ?
C6 C3 Ni1 124.1(2) . . ?
C2 C3 Ni1 101.2(2) . . ?
C3 C4 C5 117.0(3) . . ?
C3 C4 C7 122.4(3) . . ?
C5 C4 C7 120.3(3) . . ?
C3 C4 Ni1 78.67(19) . . ?
C5 C4 Ni1 67.20(17) . . ?
C7 C4 Ni1 118.2(2) . . ?
C4 C5 Ni1 70.94(19) . . ?
C4 C5 H5A 116.5 . . ?
Ni1 C5 H5A 116.5 . . ?
C4 C5 H5B 116.5 . . ?
Ni1 C5 H5B 116.5 . . ?
H5A C5 H5B 113.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C16 C8 C9 108.5(2) . . ?
C16 C8 P1 106.24(18) . . ?
C9 C8 P1 111.00(19) . . ?
C16 C8 H8A 110.3 . . ?
C9 C8 H8A 110.3 . . ?
P1 C8 H8A 110.3 . . ?
C10 C9 C8 114.4(2) . . ?
C10 C9 H9A 108.7 . . ?
C8 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
C8 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C11 C10 C9 116.3(3) . . ?
C11 C10 H10A 108.2 . . ?
C9 C10 H10A 108.2 . . ?
C11 C10 H10B 108.2 . . ?
C9 C10 H10B 108.2 . . ?
H10A C10 H10B 107.4 . . ?
C10 C11 C12 114.0(3) . . ?
C10 C11 H11A 108.8 . . ?
C12 C11 H11A 108.8 . . ?
C10 C11 H11B 108.8 . . ?
C12 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
N2 C12 C11 112.5(3) . . ?
N2 C12 H12A 109.1 . . ?
C11 C12 H12A 109.1 . . ?
N2 C12 H12B 109.1 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
N2 C13 C14 110.2(3) . . ?
N2 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
N2 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C15 C14 C13 112.7(3) . . ?
C15 C14 H14A 109.1 . . ?
C13 C14 H14A 109.1 . . ?
C15 C14 H14B 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
N1 C15 C14 112.8(3) . . ?
N1 C15 H15A 109.0 . . ?
C14 C15 H15A 109.0 . . ?
N1 C15 H15B 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
N1 C16 N2 126.1(3) . . ?
N1 C16 C8 116.9(2) . . ?
N2 C16 C8 116.9(2) . . ?
C19 C18 C21 120.2(3) . . ?
C19 C18 H18A 119.9 . . ?
C21 C18 H18A 119.9 . . ?
C20 C19 C18 120.5(3) . . ?
C20 C19 H19A 119.7 . . ?
C18 C19 H19A 119.7 . . ?
C21A C20 C19 119.9(3) . . ?
C21A C20 H20A 120.1 . . ?
C19 C20 H20A 120.1 . . ?
C18 C21 C22 118.8(3) . . ?
C18 C21 P1 120.8(2) . . ?
C22 C21 P1 120.0(2) . . ?
C20 C21A C22 120.1(3) . . ?
C20 C21A H21A 120.0 . . ?
C22 C21A H21A 120.0 . . ?
C21A C22 C21 120.6(3) . . ?
C21A C22 H22A 119.7 . . ?
C21 C22 H22A 119.7 . . ?
C28 C23 C24 118.9(3) . . ?
C28 C23 P1 119.5(2) . . ?
C24 C23 P1 121.4(2) . . ?
C25 C24 C23 120.1(3) . . ?
C25 C24 H24A 120.0 . . ?
C23 C24 H24A 120.0 . . ?
C26 C25 C24 120.6(3) . . ?
C26 C25 H25A 119.7 . . ?
C24 C25 H25A 119.7 . . ?
C27 C26 C25 119.6(3) . . ?
C27 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C26 C27 C28 120.7(3) . . ?
C26 C27 H27A 119.6 . . ?
C28 C27 H27A 119.6 . . ?
C23 C28 C27 120.0(3) . . ?
C23 C28 H28A 120.0 . . ?
C27 C28 H28A 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.58
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.074
_database_code_depnum_ccdc_archive 'CCDC 1002897'
#######################################################################
#
#                 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_FO5374
_publcif_datablock.id            {32115b92-9250-4555-bbbc-1e83c1c6824d}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H42 Ni2 O4 P2, C4 H10 O'
_chemical_formula_sum            'C43 H52 Ni2 O5 P2'
_chemical_formula_weight         828.21

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.9306(3)
_cell_length_b                   11.3308(3)
_cell_length_c                   18.4592(5)
_cell_angle_alpha                72.221(1)
_cell_angle_beta                 76.133(1)
_cell_angle_gamma                67.433(1)
_cell_volume                     1990.74(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    6728
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      25.35

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.038
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.032
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      133(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  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7238
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.35
_reflns_number_total             7238
_reflns_number_gt                6342
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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)+(0.0000P)²+23.4291P] 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         7238
_refine_ls_number_parameters     476
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0971
_refine_ls_wR_factor_ref         0.2196
_refine_ls_wR_factor_gt          0.2132
_refine_ls_goodness_of_fit_ref   1.231
_refine_ls_restrained_S_all      1.231
_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 0.19243(10) 0.08542(11) 0.26681(6) 0.0164(3) Uani 1 1 d . . .
Ni2 Ni 0.30457(10) 0.35486(10) 0.23708(6) 0.0141(3) Uani 1 1 d . . .
P1 P 0.3459(2) 0.0485(2) 0.16599(12) 0.0131(4) Uani 1 1 d . . .
P2 P 0.4896(2) 0.2160(2) 0.19021(12) 0.0126(4) Uani 1 1 d . . .
O1 O 0.2476(6) 0.1725(6) 0.3210(3) 0.0204(13) Uani 1 1 d . . .
O2 O 0.2384(7) 0.1955(7) 0.4386(4) 0.0322(16) Uani 1 1 d . . .
O3 O 0.1900(5) 0.3631(5) 0.1696(3) 0.0175(12) Uani 1 1 d . . .
O4 O 0.0109(6) 0.4929(6) 0.1115(4) 0.0226(13) Uani 1 1 d . . .
C1 C 0.1991(9) 0.1600(9) 0.3945(5) 0.0214(18) Uani 1 1 d . . .
C2 C 0.0893(10) 0.0985(11) 0.4209(5) 0.030(2) Uani 1 1 d . . .
H2A H 0.1251 0.0071 0.4512 0.036 Uiso 1 1 calc R . .
H2B H 0.0153 0.1490 0.4542 0.036 Uiso 1 1 calc R . .
C3 C 0.0368(8) 0.0989(10) 0.3515(5) 0.025(2) Uani 1 1 d . . .
C4 C 0.0696(9) -0.0141(10) 0.3232(5) 0.025(2) Uani 1 1 d . . .
C5 C 0.0728(9) 0.0091(10) 0.2439(5) 0.028(2) Uani 1 1 d . . .
H5A H -0.0091 0.0722 0.2221 0.034 Uiso 1 1 calc R . .
H5B H 0.1169 -0.0682 0.2211 0.034 Uiso 1 1 calc R . .
C6 C -0.0706(10) 0.2262(11) 0.3218(7) 0.041(3) Uani 1 1 d . . .
H6A H -0.1493 0.2402 0.3612 0.062 Uiso 1 1 calc R . .
H6B H -0.0955 0.2216 0.2754 0.062 Uiso 1 1 calc R . .
H6C H -0.0366 0.2995 0.3095 0.062 Uiso 1 1 calc R . .
C7 C 0.1243(11) -0.1531(10) 0.3713(6) 0.039(3) Uani 1 1 d . . .
H7A H 0.0501 -0.1855 0.3978 0.058 Uiso 1 1 calc R . .
H7B H 0.1734 -0.1530 0.4092 0.058 Uiso 1 1 calc R . .
H7C H 0.1847 -0.2105 0.3378 0.058 Uiso 1 1 calc R . .
C8 C 0.0909(8) 0.4729(8) 0.1545(5) 0.0160(16) Uani 1 1 d . . .
C9 C 0.0801(9) 0.5799(9) 0.1917(5) 0.0243(19) Uani 1 1 d . . .
H9A H -0.0150 0.6234 0.2103 0.029 Uiso 1 1 calc R . .
H9B H 0.1136 0.6471 0.1531 0.029 Uiso 1 1 calc R . .
C10 C 0.1617(8) 0.5215(8) 0.2594(6) 0.0232(19) Uani 1 1 d . . .
C11 C 0.2942(9) 0.5226(8) 0.2512(5) 0.0214(18) Uani 1 1 d . . .
C12 C 0.3790(9) 0.4198(8) 0.3005(5) 0.0205(18) Uani 1 1 d . . .
H12A H 0.3456 0.4052 0.3562 0.025 Uiso 1 1 calc R . .
H12B H 0.4756 0.4079 0.2881 0.025 Uiso 1 1 calc R . .
C13 C 0.0790(10) 0.4949(10) 0.3366(6) 0.033(2) Uani 1 1 d . . .
H13A H 0.0208 0.5786 0.3493 0.049 Uiso 1 1 calc R . .
H13B H 0.1383 0.4438 0.3758 0.049 Uiso 1 1 calc R . .
H13C H 0.0241 0.4451 0.3349 0.049 Uiso 1 1 calc R . .
C14 C 0.3527(10) 0.6100(9) 0.1834(6) 0.029(2) Uani 1 1 d . . .
H14A H 0.3411 0.6912 0.1970 0.043 Uiso 1 1 calc R . .
H14B H 0.3065 0.6316 0.1392 0.043 Uiso 1 1 calc R . .
H14C H 0.4482 0.5636 0.1703 0.043 Uiso 1 1 calc R . .
C15 C 0.4501(8) 0.1531(8) 0.1207(4) 0.0140(16) Uani 1 1 d . . .
H15A H 0.4027 0.2285 0.0816 0.017 Uiso 1 1 calc R . .
H15B H 0.5346 0.1018 0.0939 0.017 Uiso 1 1 calc R . .
C16 C 0.2693(7) 0.0587(8) 0.0854(4) 0.0129(15) Uani 1 1 d . . .
C17 C 0.1801(8) 0.1800(8) 0.0539(5) 0.0189(17) Uani 1 1 d . . .
H17A H 0.1683 0.2551 0.0710 0.023 Uiso 1 1 calc R . .
C18 C 0.1075(8) 0.1929(9) -0.0025(5) 0.0214(18) Uani 1 1 d . . .
H18A H 0.0488 0.2768 -0.0246 0.026 Uiso 1 1 calc R . .
C19 C 0.1213(8) 0.0830(9) -0.0263(5) 0.0227(19) Uani 1 1 d . . .
H19A H 0.0710 0.0911 -0.0640 0.027 Uiso 1 1 calc R . .
C20 C 0.2081(9) -0.0381(9) 0.0051(5) 0.0217(18) Uani 1 1 d . . .
H20A H 0.2168 -0.1136 -0.0107 0.026 Uiso 1 1 calc R . .
C21 C 0.2833(8) -0.0504(8) 0.0599(5) 0.0174(17) Uani 1 1 d . . .
H21A H 0.3448 -0.1339 0.0801 0.021 Uiso 1 1 calc R . .
C22 C 0.4704(8) -0.1140(7) 0.1871(5) 0.0153(16) Uani 1 1 d . . .
C23 C 0.4635(9) -0.1883(8) 0.2637(5) 0.0234(19) Uani 1 1 d . . .
H23A H 0.3934 -0.1532 0.3011 0.028 Uiso 1 1 calc R . .
C24 C 0.5572(10) -0.3118(9) 0.2854(5) 0.027(2) Uani 1 1 d . . .
H24A H 0.5523 -0.3601 0.3375 0.032 Uiso 1 1 calc R . .
C25 C 0.6583(9) -0.3644(9) 0.2306(6) 0.028(2) Uani 1 1 d . . .
H25A H 0.7220 -0.4495 0.2450 0.034 Uiso 1 1 calc R . .
C26 C 0.6665(8) -0.2933(9) 0.1550(6) 0.0240(19) Uani 1 1 d . . .
H26A H 0.7361 -0.3296 0.1177 0.029 Uiso 1 1 calc R . .
C27 C 0.5737(8) -0.1693(8) 0.1334(5) 0.0200(18) Uani 1 1 d . . .
H27A H 0.5805 -0.1212 0.0814 0.024 Uiso 1 1 calc R . .
C28 C 0.5933(8) 0.0730(8) 0.2543(5) 0.0167(17) Uani 1 1 d . . .
C29 C 0.7079(9) -0.0176(9) 0.2254(5) 0.0238(19) Uani 1 1 d . . .
H29A H 0.7306 -0.0099 0.1715 0.029 Uiso 1 1 calc R . .
C30 C 0.7888(9) -0.1193(9) 0.2754(6) 0.028(2) Uani 1 1 d . . .
H30A H 0.8672 -0.1808 0.2556 0.033 Uiso 1 1 calc R . .
C31 C 0.7563(9) -0.1321(9) 0.3543(6) 0.029(2) Uani 1 1 d . . .
H31A H 0.8116 -0.2024 0.3883 0.035 Uiso 1 1 calc R . .
C32 C 0.6421(9) -0.0410(10) 0.3829(5) 0.028(2) Uani 1 1 d . . .
H32A H 0.6198 -0.0484 0.4367 0.033 Uiso 1 1 calc R . .
C33 C 0.5611(9) 0.0602(9) 0.3334(5) 0.0211(18) Uani 1 1 d . . .
H33A H 0.4827 0.1217 0.3534 0.025 Uiso 1 1 calc R . .
C34 C 0.6119(8) 0.2934(7) 0.1331(5) 0.0140(16) Uani 1 1 d . . .
C35 C 0.6068(8) 0.3565(8) 0.0546(5) 0.0207(18) Uani 1 1 d . . .
H35A H 0.5434 0.3530 0.0286 0.025 Uiso 1 1 calc R . .
C36 C 0.6956(9) 0.4241(8) 0.0153(5) 0.0191(17) Uani 1 1 d . . .
H36A H 0.6913 0.4674 -0.0375 0.023 Uiso 1 1 calc R . .
C37 C 0.7895(8) 0.4292(8) 0.0514(5) 0.0217(19) Uani 1 1 d . . .
H37A H 0.8497 0.4751 0.0237 0.026 Uiso 1 1 calc R . .
C38 C 0.7953(9) 0.3666(9) 0.1289(6) 0.027(2) Uani 1 1 d . . .
H38A H 0.8593 0.3698 0.1545 0.032 Uiso 1 1 calc R . .
C39 C 0.7070(9) 0.2994(9) 0.1686(5) 0.0232(19) Uani 1 1 d . . .
H39A H 0.7119 0.2565 0.2214 0.028 Uiso 1 1 calc R . .
O1E O 0.3020(8) -0.3518(7) 0.5191(4) 0.0400(18) Uani 1 1 d . . .
C1E C 0.1736(13) -0.4687(12) 0.5026(7) 0.045(3) Uani 1 1 d . . .
H1EA H 0.1563 -0.5524 0.5202 0.067 Uiso 1 1 calc R . .
H1EB H 0.2141 -0.4574 0.4486 0.067 Uiso 1 1 calc R . .
H1EC H 0.0892 -0.3962 0.5078 0.067 Uiso 1 1 calc R . .
C2E C 0.2672(11) -0.4691(11) 0.5502(6) 0.040(3) Uani 1 1 d . . .
H2EA H 0.2236 -0.4724 0.6041 0.048 Uiso 1 1 calc R . .
H2EB H 0.3489 -0.5476 0.5497 0.048 Uiso 1 1 calc R . .
C3E C 0.4005(12) -0.3493(12) 0.5563(6) 0.044(3) Uani 1 1 d . . .
H3EA H 0.4815 -0.4279 0.5537 0.053 Uiso 1 1 calc R . .
H3EB H 0.3656 -0.3496 0.6110 0.053 Uiso 1 1 calc R . .
C4E C 0.4342(14) -0.2279(13) 0.5167(7) 0.052(3) Uani 1 1 d . . .
H4EA H 0.5100 -0.2298 0.5371 0.079 Uiso 1 1 calc R . .
H4EB H 0.3567 -0.1507 0.5255 0.079 Uiso 1 1 calc R . .
H4EC H 0.4580 -0.2230 0.4615 0.079 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 O1 1.919(6) . ?
Ni1 C4 1.983(8) . ?
Ni1 C5 1.999(9) . ?
Ni1 C3 2.008(8) . ?
Ni1 P1 2.212(2) . ?
Ni2 O3 1.927(6) . ?
Ni2 C11 1.953(8) . ?
Ni2 C12 2.004(8) . ?
Ni2 C10 2.020(8) . ?
Ni2 P2 2.205(2) . ?
Ni2 O1 2.372(6) . ?
P1 C22 1.813(8) . ?
P1 C16 1.829(8) . ?
P1 C15 1.836(8) . ?
P2 C34 1.824(8) . ?
P2 C28 1.837(8) . ?
P2 C15 1.845(8) . ?
O1 C1 1.319(10) . ?
O2 C1 1.228(11) . ?
O3 C8 1.303(10) . ?
O4 C8 1.231(10) . ?
C1 C2 1.522(12) . ?
C2 C3 1.522(13) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.416(13) . ?
C3 C6 1.512(14) . ?
C4 C5 1.400(13) . ?
C4 C7 1.518(14) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.521(11) . ?
C9 C10 1.541(12) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.424(12) . ?
C10 C13 1.505(13) . ?
C11 C12 1.405(12) . ?
C11 C14 1.517(13) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.390(11) . ?
C16 C21 1.396(11) . ?
C17 C18 1.397(12) . ?
C17 H17A 0.9500 . ?
C18 C19 1.386(12) . ?
C18 H18A 0.9500 . ?
C19 C20 1.378(13) . ?
C19 H19A 0.9500 . ?
C20 C21 1.393(12) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
C22 C27 1.396(11) . ?
C22 C23 1.409(12) . ?
C23 C24 1.387(12) . ?
C23 H23A 0.9500 . ?
C24 C25 1.388(13) . ?
C24 H24A 0.9500 . ?
C25 C26 1.383(14) . ?
C25 H25A 0.9500 . ?
C26 C27 1.385(12) . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9500 . ?
C28 C33 1.392(12) . ?
C28 C29 1.391(12) . ?
C29 C30 1.386(13) . ?
C29 H29A 0.9500 . ?
C30 C31 1.389(14) . ?
C30 H30A 0.9500 . ?
C31 C32 1.389(14) . ?
C31 H31A 0.9500 . ?
C32 C33 1.380(13) . ?
C32 H32A 0.9500 . ?
C33 H33A 0.9500 . ?
C34 C39 1.388(12) . ?
C34 C35 1.410(12) . ?
C35 C36 1.396(11) . ?
C35 H35A 0.9500 . ?
C36 C37 1.378(13) . ?
C36 H36A 0.9500 . ?
C37 C38 1.394(13) . ?
C37 H37A 0.9500 . ?
C38 C39 1.390(12) . ?
C38 H38A 0.9500 . ?
C39 H39A 0.9500 . ?
O1E C3E 1.422(13) . ?
O1E C2E 1.435(13) . ?
C1E C2E 1.499(16) . ?
C1E H1EA 0.9800 . ?
C1E H1EB 0.9800 . ?
C1E H1EC 0.9800 . ?
C2E H2EA 0.9900 . ?
C2E H2EB 0.9900 . ?
C3E C4E 1.486(17) . ?
C3E H3EA 0.9900 . ?
C3E H3EB 0.9900 . ?
C4E H4EA 0.9800 . ?
C4E H4EB 0.9800 . ?
C4E H4EC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 C4 119.1(3) . . ?
O1 Ni1 C5 156.8(3) . . ?
C4 Ni1 C5 41.2(4) . . ?
O1 Ni1 C3 83.8(3) . . ?
C4 Ni1 C3 41.6(4) . . ?
C5 Ni1 C3 73.0(4) . . ?
O1 Ni1 P1 107.53(18) . . ?
C4 Ni1 P1 128.0(3) . . ?
C5 Ni1 P1 95.6(3) . . ?
C3 Ni1 P1 168.6(3) . . ?
O3 Ni2 C11 116.5(3) . . ?
O3 Ni2 C12 157.7(3) . . ?
C11 Ni2 C12 41.6(4) . . ?
O3 Ni2 C10 85.7(3) . . ?
C11 Ni2 C10 42.0(4) . . ?
C12 Ni2 C10 73.3(4) . . ?
O3 Ni2 P2 97.33(18) . . ?
C11 Ni2 P2 123.5(3) . . ?
C12 Ni2 P2 100.5(3) . . ?
C10 Ni2 P2 162.7(3) . . ?
O3 Ni2 O1 87.8(2) . . ?
C11 Ni2 O1 133.1(3) . . ?
C12 Ni2 O1 105.8(3) . . ?
C10 Ni2 O1 108.4(3) . . ?
P2 Ni2 O1 88.84(15) . . ?
C22 P1 C16 107.4(4) . . ?
C22 P1 C15 102.1(4) . . ?
C16 P1 C15 102.2(4) . . ?
C22 P1 Ni1 111.5(3) . . ?
C16 P1 Ni1 110.6(2) . . ?
C15 P1 Ni1 121.8(3) . . ?
C34 P2 C28 101.6(4) . . ?
C34 P2 C15 103.3(3) . . ?
C28 P2 C15 107.0(4) . . ?
C34 P2 Ni2 113.4(3) . . ?
C28 P2 Ni2 120.8(3) . . ?
C15 P2 Ni2 109.2(3) . . ?
C1 O1 Ni1 115.7(5) . . ?
C1 O1 Ni2 126.4(5) . . ?
Ni1 O1 Ni2 111.5(3) . . ?
C8 O3 Ni2 116.2(5) . . ?
O2 C1 O1 123.0(8) . . ?
O2 C1 C2 122.3(8) . . ?
O1 C1 C2 114.7(7) . . ?
C3 C2 C1 109.9(7) . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C2 123.9(9) . . ?
C4 C3 C6 121.6(9) . . ?
C2 C3 C6 113.9(9) . . ?
C4 C3 Ni1 68.3(5) . . ?
C2 C3 Ni1 105.4(6) . . ?
C6 C3 Ni1 105.2(7) . . ?
C5 C4 C3 115.7(9) . . ?
C5 C4 C7 120.5(9) . . ?
C3 C4 C7 122.7(9) . . ?
C5 C4 Ni1 70.0(5) . . ?
C3 C4 Ni1 70.1(5) . . ?
C7 C4 Ni1 120.0(7) . . ?
C4 C5 Ni1 68.8(5) . . ?
C4 C5 H5A 116.8 . . ?
Ni1 C5 H5A 116.8 . . ?
C4 C5 H5B 116.8 . . ?
Ni1 C5 H5B 116.8 . . ?
H5A C5 H5B 113.8 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O4 C8 O3 123.4(8) . . ?
O4 C8 C9 120.6(7) . . ?
O3 C8 C9 116.0(7) . . ?
C8 C9 C10 110.8(7) . . ?
C8 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C13 122.6(8) . . ?
C11 C10 C9 122.1(8) . . ?
C13 C10 C9 113.7(8) . . ?
C11 C10 Ni2 66.5(4) . . ?
C13 C10 Ni2 111.6(6) . . ?
C9 C10 Ni2 105.4(6) . . ?
C12 C11 C10 116.3(8) . . ?
C12 C11 C14 119.6(8) . . ?
C10 C11 C14 122.9(8) . . ?
C12 C11 Ni2 71.1(5) . . ?
C10 C11 Ni2 71.5(5) . . ?
C14 C11 Ni2 116.7(6) . . ?
C11 C12 Ni2 67.3(5) . . ?
C11 C12 H12A 117.0 . . ?
Ni2 C12 H12A 117.0 . . ?
C11 C12 H12B 117.0 . . ?
Ni2 C12 H12B 117.0 . . ?
H12A C12 H12B 114.0 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P1 C15 P2 112.8(4) . . ?
P1 C15 H15A 109.0 . . ?
P2 C15 H15A 109.0 . . ?
P1 C15 H15B 109.0 . . ?
P2 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C21 118.3(7) . . ?
C17 C16 P1 117.5(6) . . ?
C21 C16 P1 123.7(6) . . ?
C16 C17 C18 120.9(8) . . ?
C16 C17 H17A 119.5 . . ?
C18 C17 H17A 119.5 . . ?
C19 C18 C17 119.9(8) . . ?
C19 C18 H18A 120.1 . . ?
C17 C18 H18A 120.1 . . ?
C20 C19 C18 119.8(8) . . ?
C20 C19 H19A 120.1 . . ?
C18 C19 H19A 120.1 . . ?
C19 C20 C21 120.4(8) . . ?
C19 C20 H20A 119.8 . . ?
C21 C20 H20A 119.8 . . ?
C16 C21 C20 120.7(8) . . ?
C16 C21 H21A 119.7 . . ?
C20 C21 H21A 119.7 . . ?
C27 C22 C23 117.9(7) . . ?
C27 C22 P1 124.8(6) . . ?
C23 C22 P1 117.3(6) . . ?
C24 C23 C22 121.1(8) . . ?
C24 C23 H23A 119.4 . . ?
C22 C23 H23A 119.4 . . ?
C25 C24 C23 119.5(9) . . ?
C25 C24 H24A 120.2 . . ?
C23 C24 H24A 120.2 . . ?
C24 C25 C26 120.2(8) . . ?
C24 C25 H25A 119.9 . . ?
C26 C25 H25A 119.9 . . ?
C27 C26 C25 120.2(8) . . ?
C27 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
C26 C27 C22 121.0(8) . . ?
C26 C27 H27A 119.5 . . ?
C22 C27 H27A 119.5 . . ?
C33 C28 C29 119.5(8) . . ?
C33 C28 P2 119.0(6) . . ?
C29 C28 P2 121.3(7) . . ?
C30 C29 C28 119.7(8) . . ?
C30 C29 H29A 120.1 . . ?
C28 C29 H29A 120.1 . . ?
C29 C30 C31 120.7(8) . . ?
C29 C30 H30A 119.7 . . ?
C31 C30 H30A 119.7 . . ?
C32 C31 C30 119.4(9) . . ?
C32 C31 H31A 120.3 . . ?
C30 C31 H31A 120.3 . . ?
C33 C32 C31 120.2(9) . . ?
C33 C32 H32A 119.9 . . ?
C31 C32 H32A 119.9 . . ?
C32 C33 C28 120.5(8) . . ?
C32 C33 H33A 119.8 . . ?
C28 C33 H33A 119.8 . . ?
C39 C34 C35 118.5(8) . . ?
C39 C34 P2 119.4(6) . . ?
C35 C34 P2 121.9(6) . . ?
C36 C35 C34 119.5(8) . . ?
C36 C35 H35A 120.2 . . ?
C34 C35 H35A 120.2 . . ?
C37 C36 C35 121.3(8) . . ?
C37 C36 H36A 119.3 . . ?
C35 C36 H36A 119.3 . . ?
C36 C37 C38 119.4(8) . . ?
C36 C37 H37A 120.3 . . ?
C38 C37 H37A 120.3 . . ?
C39 C38 C37 119.7(8) . . ?
C39 C38 H38A 120.1 . . ?
C37 C38 H38A 120.1 . . ?
C38 C39 C34 121.5(9) . . ?
C38 C39 H39A 119.2 . . ?
C34 C39 H39A 119.2 . . ?
C3E O1E C2E 112.9(8) . . ?
C2E C1E H1EA 109.5 . . ?
C2E C1E H1EB 109.5 . . ?
H1EA C1E H1EB 109.5 . . ?
C2E C1E H1EC 109.5 . . ?
H1EA C1E H1EC 109.5 . . ?
H1EB C1E H1EC 109.5 . . ?
O1E C2E C1E 108.9(8) . . ?
O1E C2E H2EA 109.9 . . ?
C1E C2E H2EA 109.9 . . ?
O1E C2E H2EB 109.9 . . ?
C1E C2E H2EB 109.9 . . ?
H2EA C2E H2EB 108.3 . . ?
O1E C3E C4E 108.2(9) . . ?
O1E C3E H3EA 110.1 . . ?
C4E C3E H3EA 110.1 . . ?
O1E C3E H3EB 110.1 . . ?
C4E C3E H3EB 110.1 . . ?
H3EA C3E H3EB 108.4 . . ?
C3E C4E H4EA 109.5 . . ?
C3E C4E H4EB 109.5 . . ?
H4EA C4E H4EB 109.5 . . ?
C3E C4E H4EC 109.5 . . ?
H4EA C4E H4EC 109.5 . . ?
H4EB C4E H4EC 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.35
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.315
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.161
_database_code_depnum_ccdc_archive 'CCDC 1002898'
#######################################################################
#
#                 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_FO5351
_publcif_datablock.id            {e4b8375b-7b54-45cf-b8ae-3a7b8009ad7d}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H56 Ni O2 P2, C H4 O'
_chemical_formula_sum            'C33 H60 Ni O3 P2'
_chemical_formula_weight         625.46

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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   9.6594(4)
_cell_length_b                   32.5695(15)
_cell_length_c                   10.9054(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.745(1)
_cell_angle_gamma                90.00
_cell_volume                     3359.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    7820
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      26.37

_exptl_crystal_description       prism
_exptl_crystal_colour            red-brown
_exptl_crystal_size_max          0.048
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.024
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      133(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  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16775
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         26.37
_reflns_number_total             6726
_reflns_number_gt                5704
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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)+(0.0292P)²+11.4828P] 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         6726
_refine_ls_number_parameters     366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0774
_refine_ls_wR_factor_ref         0.1642
_refine_ls_wR_factor_gt          0.1565
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.009
_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(3) 0.40625(13) 0.1033(6) 0.0241(7) Uani 0.74(2) 1 d P A 1
Ni1A Ni 0.2668(7) 0.4142(3) 0.148(2) 0.025(2) Uani 0.26(2) 1 d P A 2
P1 P 0.37143(11) 0.35594(3) 0.05715(10) 0.0293(2) Uani 1 1 d . . .
P2 P 0.40458(12) 0.39124(3) 0.28836(10) 0.0311(3) Uani 1 1 d . . .
O1 O 0.0669(3) 0.37675(11) 0.1382(3) 0.0507(9) Uani 1 1 d . . .
O2 O -0.1454(4) 0.38980(11) 0.1717(4) 0.0624(11) Uani 1 1 d . . .
C1 C -0.0324(4) 0.39989(13) 0.1415(4) 0.0358(10) Uani 1 1 d . A .
C2 C -0.0137(6) 0.44457(17) 0.1149(7) 0.0650(16) Uani 1 1 d . . .
H2A H -0.0597 0.4609 0.1720 0.078 Uiso 1 1 calc R A .
H2B H -0.0650 0.4503 0.0284 0.078 Uiso 1 1 calc R . .
C3 C 0.1415(6) 0.46035(16) 0.1281(5) 0.0567(14) Uani 1 1 d . A .
C4 C 0.1977(6) 0.46092(17) 0.0235(6) 0.0644(18) Uani 1 1 d . . .
C5 C 0.1561(6) 0.42977(18) -0.0733(6) 0.0645(16) Uani 1 1 d . A .
H5A H 0.2118 0.4282 -0.1399 0.077 Uiso 1 1 calc R B 1
H5B H 0.0536 0.4249 -0.1028 0.077 Uiso 1 1 calc R B 1
C6 C 0.1940(7) 0.4873(2) 0.2335(5) 0.0679(17) Uani 1 1 d . . .
H6A H 0.1552 0.5149 0.2148 0.102 Uiso 1 1 calc R A .
H6B H 0.2974 0.4884 0.2483 0.102 Uiso 1 1 calc R . .
H6C H 0.1647 0.4767 0.3084 0.102 Uiso 1 1 calc R . .
C7 C 0.3211(5) 0.49155(15) 0.0089(5) 0.0496(13) Uani 1 1 d . A .
H7A H 0.2804 0.5170 -0.0305 0.074 Uiso 1 1 calc R . .
H7B H 0.3806 0.4788 -0.0434 0.074 Uiso 1 1 calc R . .
H7C H 0.3787 0.4977 0.0917 0.074 Uiso 1 1 calc R . .
C8 C 0.4959(4) 0.35231(12) 0.2093(4) 0.0298(9) Uani 1 1 d . A .
H8A H 0.5932 0.3606 0.2044 0.036 Uiso 1 1 calc R . .
H8B H 0.4966 0.3248 0.2478 0.036 Uiso 1 1 calc R . .
C9 C 0.2629(4) 0.30903(13) 0.0394(4) 0.0347(9) Uani 1 1 d . A .
H9A H 0.2019 0.3115 0.1030 0.042 Uiso 1 1 calc R . .
C10 C 0.1590(5) 0.30869(17) -0.0892(4) 0.0475(12) Uani 1 1 d . . .
H10A H 0.1103 0.3355 -0.1039 0.057 Uiso 1 1 calc R A .
H10B H 0.2117 0.3040 -0.1569 0.057 Uiso 1 1 calc R . .
C11 C 0.0493(5) 0.2741(2) -0.0900(5) 0.0610(16) Uani 1 1 d . A .
H11A H -0.0116 0.2811 -0.0302 0.073 Uiso 1 1 calc R . .
H11B H -0.0117 0.2723 -0.1746 0.073 Uiso 1 1 calc R . .
C12 C 0.1177(6) 0.23289(18) -0.0553(5) 0.0585(15) Uani 1 1 d . . .
H12A H 0.1656 0.2238 -0.1227 0.070 Uiso 1 1 calc R A .
H12B H 0.0434 0.2125 -0.0491 0.070 Uiso 1 1 calc R . .
C13 C 0.2243(6) 0.23385(17) 0.0673(5) 0.0579(14) Uani 1 1 d . A .
H13A H 0.2711 0.2068 0.0825 0.070 Uiso 1 1 calc R . .
H13B H 0.1752 0.2395 0.1369 0.070 Uiso 1 1 calc R . .
C14 C 0.3356(5) 0.26711(14) 0.0639(5) 0.0451(11) Uani 1 1 d . . .
H14A H 0.3877 0.2609 -0.0032 0.054 Uiso 1 1 calc R A .
H14B H 0.4042 0.2677 0.1448 0.054 Uiso 1 1 calc R . .
C15 C 0.4767(4) 0.35603(13) -0.0667(4) 0.0343(9) Uani 1 1 d . A .
H15A H 0.4094 0.3514 -0.1482 0.041 Uiso 1 1 calc R . .
C16 C 0.5883(5) 0.32196(14) -0.0528(5) 0.0424(11) Uani 1 1 d . . .
H16A H 0.5420 0.2950 -0.0499 0.051 Uiso 1 1 calc R A .
H16B H 0.6575 0.3257 0.0269 0.051 Uiso 1 1 calc R . .
C17 C 0.6657(6) 0.32267(16) -0.1625(5) 0.0484(12) Uani 1 1 d . A .
H17A H 0.7384 0.3008 -0.1505 0.058 Uiso 1 1 calc R . .
H17B H 0.5974 0.3169 -0.2415 0.058 Uiso 1 1 calc R . .
C18 C 0.7355(6) 0.36369(16) -0.1727(5) 0.0488(12) Uani 1 1 d . . .
H18A H 0.7800 0.3637 -0.2469 0.059 Uiso 1 1 calc R A .
H18B H 0.8106 0.3683 -0.0975 0.059 Uiso 1 1 calc R . .
C19 C 0.6270(6) 0.39837(17) -0.1848(5) 0.0577(15) Uani 1 1 d . A .
H19A H 0.5585 0.3956 -0.2652 0.069 Uiso 1 1 calc R . .
H19B H 0.6758 0.4251 -0.1854 0.069 Uiso 1 1 calc R . .
C20 C 0.5465(6) 0.39774(15) -0.0755(5) 0.0489(13) Uani 1 1 d . . .
H20A H 0.6134 0.4036 0.0042 0.059 Uiso 1 1 calc R A .
H20B H 0.4733 0.4195 -0.0888 0.059 Uiso 1 1 calc R . .
C21 C 0.5495(5) 0.42358(13) 0.3772(4) 0.0388(10) Uani 1 1 d . A .
H21A H 0.5075 0.4414 0.4348 0.047 Uiso 1 1 calc R . .
C22 C 0.6138(6) 0.45222(15) 0.2909(5) 0.0489(12) Uani 1 1 d . . .
H22A H 0.6559 0.4355 0.2320 0.059 Uiso 1 1 calc R A .
H22B H 0.5380 0.4693 0.2410 0.059 Uiso 1 1 calc R . .
C23 C 0.7278(7) 0.48011(19) 0.3669(6) 0.0705(19) Uani 1 1 d . A .
H23A H 0.7694 0.4974 0.3091 0.085 Uiso 1 1 calc R . .
H23B H 0.6839 0.4985 0.4204 0.085 Uiso 1 1 calc R . .
C24 C 0.8442(7) 0.4550(2) 0.4491(6) 0.074(2) Uani 1 1 d . . .
H24A H 0.9128 0.4738 0.5009 0.089 Uiso 1 1 calc R A .
H24B H 0.8953 0.4390 0.3952 0.089 Uiso 1 1 calc R . .
C25 C 0.7838(6) 0.4258(2) 0.5347(5) 0.0626(17) Uani 1 1 d . A .
H25A H 0.8608 0.4085 0.5820 0.075 Uiso 1 1 calc R . .
H25B H 0.7432 0.4419 0.5957 0.075 Uiso 1 1 calc R . .
C26 C 0.6692(5) 0.39820(16) 0.4592(4) 0.0466(12) Uani 1 1 d . . .
H26A H 0.6287 0.3808 0.5174 0.056 Uiso 1 1 calc R A .
H26B H 0.7123 0.3799 0.4048 0.056 Uiso 1 1 calc R . .
C27 C 0.3346(4) 0.36628(13) 0.4167(4) 0.0333(9) Uani 1 1 d . A .
H27A H 0.4172 0.3589 0.4844 0.040 Uiso 1 1 calc R . .
C28 C 0.2432(5) 0.39720(15) 0.4717(4) 0.0399(10) Uani 1 1 d . . .
H28A H 0.3000 0.4220 0.5002 0.048 Uiso 1 1 calc R A .
H28B H 0.1620 0.4057 0.4056 0.048 Uiso 1 1 calc R . .
C29 C 0.1881(5) 0.37867(18) 0.5825(4) 0.0508(13) Uani 1 1 d . A .
H29A H 0.2687 0.3734 0.6528 0.061 Uiso 1 1 calc R . .
H29B H 0.1240 0.3985 0.6114 0.061 Uiso 1 1 calc R . .
C30 C 0.1086(5) 0.33836(19) 0.5446(4) 0.0543(14) Uani 1 1 d . . .
H30A H 0.0814 0.3259 0.6191 0.065 Uiso 1 1 calc R A .
H30B H 0.0210 0.3442 0.4823 0.065 Uiso 1 1 calc R . .
C31 C 0.1988(5) 0.30826(17) 0.4893(5) 0.0525(14) Uani 1 1 d . A .
H31A H 0.1430 0.2832 0.4623 0.063 Uiso 1 1 calc R . .
H31B H 0.2815 0.3003 0.5545 0.063 Uiso 1 1 calc R . .
C32 C 0.2506(5) 0.32661(14) 0.3767(4) 0.0393(10) Uani 1 1 d . . .
H32A H 0.1686 0.3328 0.3086 0.047 Uiso 1 1 calc R A .
H32B H 0.3116 0.3065 0.3448 0.047 Uiso 1 1 calc R . .
O3 O -0.1617(4) 0.31604(13) 0.2814(4) 0.0600(10) Uani 1 1 d . . .
H3 H -0.1552 0.3382 0.2434 0.090 Uiso 1 1 calc R . .
C33 C -0.1123(6) 0.28347(18) 0.2169(5) 0.0558(14) Uani 1 1 d . . .
H33A H -0.0173 0.2900 0.2038 0.084 Uiso 1 1 calc R . .
H33B H -0.1763 0.2796 0.1356 0.084 Uiso 1 1 calc R . .
H33C H -0.1088 0.2582 0.2664 0.084 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 C4 2.001(5) . ?
Ni1 C3 2.096(6) . ?
Ni1 C5 2.099(8) . ?
Ni1 O1 2.114(4) . ?
Ni1 P1 2.134(4) . ?
Ni1 P2 2.305(6) . ?
Ni1A C3 1.913(7) . ?
Ni1A P2 1.959(14) . ?
Ni1A C4 2.059(9) . ?
Ni1A O1 2.268(9) . ?
Ni1A P1 2.454(15) . ?
Ni1A C5 2.49(2) . ?
P1 C9 1.841(4) . ?
P1 C8 1.844(4) . ?
P1 C15 1.849(4) . ?
P2 C8 1.854(4) . ?
P2 C21 1.859(5) . ?
P2 C27 1.860(4) . ?
O1 C1 1.226(5) . ?
O2 C1 1.248(5) . ?
C1 C2 1.502(7) . ?
C2 C3 1.564(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.360(7) . ?
C3 C6 1.453(8) . ?
C4 C5 1.460(9) . ?
C4 C7 1.588(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C14 1.533(6) . ?
C9 C10 1.549(6) . ?
C9 H9A 1.0000 . ?
C10 C11 1.545(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.510(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.513(8) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.532(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.528(6) . ?
C15 C16 1.533(6) . ?
C15 H15A 1.0000 . ?
C16 C17 1.535(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.511(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.528(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.550(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.542(6) . ?
C21 C26 1.549(7) . ?
C21 H21A 1.0000 . ?
C22 C23 1.534(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.525(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.530(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.528(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.539(6) . ?
C27 C32 1.540(6) . ?
C27 H27A 1.0000 . ?
C28 C29 1.539(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.535(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.516(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.538(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
O3 C33 1.409(6) . ?
O3 H3 0.8400 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 Ni1 C3 38.7(2) . . ?
C4 Ni1 C5 41.6(2) . . ?
C3 Ni1 C5 71.2(2) . . ?
C4 Ni1 O1 109.6(2) . . ?
C3 Ni1 O1 84.3(2) . . ?
C5 Ni1 O1 96.3(3) . . ?
C4 Ni1 P1 133.1(3) . . ?
C3 Ni1 P1 171.6(2) . . ?
C5 Ni1 P1 102.7(3) . . ?
O1 Ni1 P1 102.3(2) . . ?
C4 Ni1 P2 129.1(4) . . ?
C3 Ni1 P2 108.5(4) . . ?
C5 Ni1 P2 164.2(2) . . ?
O1 Ni1 P2 99.35(16) . . ?
P1 Ni1 P2 75.79(7) . . ?
C3 Ni1A P2 134.7(12) . . ?
C3 Ni1A C4 39.8(2) . . ?
P2 Ni1A C4 151.1(8) . . ?
C3 Ni1A O1 84.5(3) . . ?
P2 Ni1A O1 105.6(3) . . ?
C4 Ni1A O1 101.9(5) . . ?
C3 Ni1A P1 149.8(11) . . ?
P2 Ni1A P1 75.51(19) . . ?
C4 Ni1A P1 114.1(9) . . ?
O1 Ni1A P1 88.9(6) . . ?
C3 Ni1A C5 65.9(4) . . ?
P2 Ni1A C5 157.7(7) . . ?
C4 Ni1A C5 35.9(4) . . ?
O1 Ni1A C5 82.5(6) . . ?
P1 Ni1A C5 84.0(7) . . ?
C9 P1 C8 107.12(19) . . ?
C9 P1 C15 108.1(2) . . ?
C8 P1 C15 107.63(19) . . ?
C9 P1 Ni1 109.48(18) . . ?
C8 P1 Ni1 97.2(2) . . ?
C15 P1 Ni1 125.55(16) . . ?
C9 P1 Ni1A 114.3(2) . . ?
C8 P1 Ni1A 86.1(4) . . ?
C15 P1 Ni1A 128.9(2) . . ?
Ni1 P1 Ni1A 11.2(2) . . ?
C8 P2 C21 104.51(19) . . ?
C8 P2 C27 109.31(19) . . ?
C21 P2 C27 101.9(2) . . ?
C8 P2 Ni1A 102.2(6) . . ?
C21 P2 Ni1A 120.6(4) . . ?
C27 P2 Ni1A 117.4(2) . . ?
C8 P2 Ni1 91.30(18) . . ?
C21 P2 Ni1 128.38(19) . . ?
C27 P2 Ni1 118.77(15) . . ?
Ni1A P2 Ni1 11.5(4) . . ?
C1 O1 Ni1 114.4(3) . . ?
C1 O1 Ni1A 109.3(4) . . ?
Ni1 O1 Ni1A 13.8(3) . . ?
O1 C1 O2 125.3(4) . . ?
O1 C1 C2 117.7(4) . . ?
O2 C1 C2 116.9(4) . . ?
C1 C2 C3 116.8(4) . . ?
C1 C2 H2A 108.1 . . ?
C3 C2 H2A 108.1 . . ?
C1 C2 H2B 108.1 . . ?
C3 C2 H2B 108.1 . . ?
H2A C2 H2B 107.3 . . ?
C4 C3 C6 121.4(6) . . ?
C4 C3 C2 117.8(6) . . ?
C6 C3 C2 116.4(5) . . ?
C4 C3 Ni1A 75.9(6) . . ?
C6 C3 Ni1A 105.8(8) . . ?
C2 C3 Ni1A 109.0(5) . . ?
C4 C3 Ni1 66.9(3) . . ?
C6 C3 Ni1 120.5(5) . . ?
C2 C3 Ni1 102.0(4) . . ?
Ni1A C3 Ni1 14.9(5) . . ?
C3 C4 C5 119.9(6) . . ?
C3 C4 C7 121.9(6) . . ?
C5 C4 C7 117.8(5) . . ?
C3 C4 Ni1 74.4(3) . . ?
C5 C4 Ni1 72.8(4) . . ?
C7 C4 Ni1 118.3(4) . . ?
C3 C4 Ni1A 64.3(5) . . ?
C5 C4 Ni1A 88.2(7) . . ?
C7 C4 Ni1A 112.4(4) . . ?
Ni1 C4 Ni1A 15.5(4) . . ?
C4 C5 Ni1 65.6(4) . . ?
C4 C5 Ni1A 55.8(4) . . ?
Ni1 C5 Ni1A 9.78(18) . . ?
C4 C5 H5A 117.2 . . ?
Ni1 C5 H5A 117.2 . . ?
Ni1A C5 H5A 120.8 . . ?
C4 C5 H5B 117.2 . . ?
Ni1 C5 H5B 117.2 . . ?
Ni1A C5 H5B 119.2 . . ?
H5A C5 H5B 114.2 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P1 C8 P2 95.16(18) . . ?
P1 C8 H8A 112.7 . . ?
P2 C8 H8A 112.7 . . ?
P1 C8 H8B 112.7 . . ?
P2 C8 H8B 112.7 . . ?
H8A C8 H8B 110.2 . . ?
C14 C9 C10 109.9(4) . . ?
C14 C9 P1 119.3(3) . . ?
C10 C9 P1 110.6(3) . . ?
C14 C9 H9A 105.3 . . ?
C10 C9 H9A 105.3 . . ?
P1 C9 H9A 105.3 . . ?
C11 C10 C9 109.1(4) . . ?
C11 C10 H10A 109.9 . . ?
C9 C10 H10A 109.9 . . ?
C11 C10 H10B 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C12 C11 C10 112.4(4) . . ?
C12 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 C13 112.8(4) . . ?
C11 C12 H12A 109.0 . . ?
C13 C12 H12A 109.0 . . ?
C11 C12 H12B 109.0 . . ?
C13 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C12 C13 C14 110.3(4) . . ?
C12 C13 H13A 109.6 . . ?
C14 C13 H13A 109.6 . . ?
C12 C13 H13B 109.6 . . ?
C14 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 C9 109.6(4) . . ?
C13 C14 H14A 109.8 . . ?
C9 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
C9 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
C20 C15 C16 109.8(4) . . ?
C20 C15 P1 111.3(3) . . ?
C16 C15 P1 114.0(3) . . ?
C20 C15 H15A 107.1 . . ?
C16 C15 H15A 107.1 . . ?
P1 C15 H15A 107.1 . . ?
C15 C16 C17 110.9(4) . . ?
C15 C16 H16A 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C18 C17 C16 111.5(4) . . ?
C18 C17 H17A 109.3 . . ?
C16 C17 H17A 109.3 . . ?
C18 C17 H17B 109.3 . . ?
C16 C17 H17B 109.3 . . ?
H17A C17 H17B 108.0 . . ?
C17 C18 C19 110.6(4) . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C18 C19 C20 111.5(4) . . ?
C18 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
C18 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
C15 C20 C19 110.9(4) . . ?
C15 C20 H20A 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 108.0 . . ?
C22 C21 C26 109.2(4) . . ?
C22 C21 P2 112.3(3) . . ?
C26 C21 P2 113.1(3) . . ?
C22 C21 H21A 107.3 . . ?
C26 C21 H21A 107.3 . . ?
P2 C21 H21A 107.3 . . ?
C23 C22 C21 111.2(4) . . ?
C23 C22 H22A 109.4 . . ?
C21 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C24 C23 C22 111.3(5) . . ?
C24 C23 H23A 109.4 . . ?
C22 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C23 C24 C25 111.4(5) . . ?
C23 C24 H24A 109.3 . . ?
C25 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
C25 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
C26 C25 C24 111.2(4) . . ?
C26 C25 H25A 109.4 . . ?
C24 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
C24 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C25 C26 C21 111.8(5) . . ?
C25 C26 H26A 109.3 . . ?
C21 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
C21 C26 H26B 109.3 . . ?
H26A C26 H26B 107.9 . . ?
C28 C27 C32 110.4(4) . . ?
C28 C27 P2 109.4(3) . . ?
C32 C27 P2 113.9(3) . . ?
C28 C27 H27A 107.6 . . ?
C32 C27 H27A 107.6 . . ?
P2 C27 H27A 107.6 . . ?
C29 C28 C27 111.5(4) . . ?
C29 C28 H28A 109.3 . . ?
C27 C28 H28A 109.3 . . ?
C29 C28 H28B 109.3 . . ?
C27 C28 H28B 109.3 . . ?
H28A C28 H28B 108.0 . . ?
C30 C29 C28 111.0(4) . . ?
C30 C29 H29A 109.4 . . ?
C28 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
C28 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
C31 C30 C29 111.3(4) . . ?
C31 C30 H30A 109.4 . . ?
C29 C30 H30A 109.4 . . ?
C31 C30 H30B 109.4 . . ?
C29 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
C30 C31 C32 111.9(4) . . ?
C30 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
C30 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 C27 109.8(4) . . ?
C31 C32 H32A 109.7 . . ?
C27 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C27 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
C33 O3 H3 109.5 . . ?
O3 C33 H33A 109.5 . . ?
O3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.371
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.077
_database_code_depnum_ccdc_archive 'CCDC 1002899'
#######################################################################
#
#                 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_FO5218
_publcif_datablock.id            {6d24c546-0e02-45d9-bdc2-408f9948e4c4}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H96 Ni P4'
_chemical_formula_sum            'C52 H96 Ni P4'
_chemical_formula_weight         903.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   'P 2/n'
_symmetry_space_group_name_Hall  '-P 2yac'

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

_cell_length_a                   13.2538(3)
_cell_length_b                   9.9914(2)
_cell_length_c                   21.0848(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.144(1)
_cell_angle_gamma                90.00
_cell_volume                     2718.98(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    6467
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      27.49

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.064
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.054
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      133(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  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6212
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6212
_reflns_number_gt                5382
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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. The crystal contain large voids, filled with
disordered solvent molecules. The size of the voids are 161 Å³/unit cell.
Their contribution to the structure factors was secured by back-Fourier
transformation using the SQUEEZE routine of the program PLATON
resulting in 20 electrons/unit cell.
;

_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)+(0.0928P)²+4.8408P] 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         6212
_refine_ls_number_parameters     258
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0640
_refine_ls_wR_factor_ref         0.1793
_refine_ls_wR_factor_gt          0.1723
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.2500 0.11593(5) 0.2500 0.02085(15) Uani 1 2 d S . .
P1 P 0.28986(6) 0.26949(7) 0.32494(3) 0.02352(18) Uani 1 1 d . . .
P2 P 0.13465(5) -0.03721(7) 0.25695(4) 0.02580(18) Uani 1 1 d . . .
C1 C 0.2894(3) 0.4324(3) 0.28297(14) 0.0355(7) Uani 1 1 d . . .
H1A H 0.2718 0.5045 0.3108 0.043 Uiso 1 1 calc R . .
H1B H 0.3595 0.4507 0.2760 0.043 Uiso 1 1 calc R . .
C2 C 0.4198(3) 0.2771(4) 0.38364(19) 0.0509(10) Uani 1 1 d . . .
H2A H 0.4660 0.2292 0.3597 0.061 Uiso 1 1 calc R . .
C3 C 0.4239(3) 0.1875(4) 0.44320(16) 0.0390(7) Uani 1 1 d . . .
H3A H 0.3753 0.2233 0.4684 0.047 Uiso 1 1 calc R . .
H3B H 0.4001 0.0967 0.4281 0.047 Uiso 1 1 calc R . .
C4 C 0.5315(4) 0.1771(7) 0.4881(3) 0.0808(17) Uani 1 1 d . . .
H4A H 0.5249 0.1355 0.5296 0.097 Uiso 1 1 calc R . .
H4B H 0.5744 0.1169 0.4678 0.097 Uiso 1 1 calc R . .
C5 C 0.5831(4) 0.3002(6) 0.5019(3) 0.0864(19) Uani 1 1 d . . .
H5A H 0.6554 0.2829 0.5257 0.104 Uiso 1 1 calc R . .
H5B H 0.5491 0.3525 0.5311 0.104 Uiso 1 1 calc R . .
C6 C 0.5849(3) 0.3843(4) 0.4418(3) 0.0618(12) Uani 1 1 d . . .
H6A H 0.6169 0.4724 0.4553 0.074 Uiso 1 1 calc R . .
H6B H 0.6269 0.3388 0.4150 0.074 Uiso 1 1 calc R . .
C7 C 0.4748(3) 0.4040(4) 0.4020(2) 0.0544(10) Uani 1 1 d . . .
H7A H 0.4357 0.4581 0.4277 0.065 Uiso 1 1 calc R . .
H7B H 0.4770 0.4547 0.3620 0.065 Uiso 1 1 calc R . .
C8 C 0.1968(2) 0.2990(3) 0.37810(14) 0.0294(6) Uani 1 1 d . . .
H8A H 0.1968 0.2143 0.4034 0.035 Uiso 1 1 calc R . .
C9 C 0.2175(3) 0.4109(4) 0.42902(16) 0.0395(7) Uani 1 1 d . . .
H9A H 0.2885 0.4017 0.4563 0.047 Uiso 1 1 calc R . .
H9B H 0.2124 0.4988 0.4068 0.047 Uiso 1 1 calc R . .
C10 C 0.1398(4) 0.4051(4) 0.47208(19) 0.0511(10) Uani 1 1 d . . .
H10A H 0.1499 0.3209 0.4975 0.061 Uiso 1 1 calc R . .
H10B H 0.1527 0.4807 0.5032 0.061 Uiso 1 1 calc R . .
C11 C 0.0296(3) 0.4117(4) 0.4330(2) 0.0484(9) Uani 1 1 d . . .
H11A H 0.0163 0.5012 0.4127 0.058 Uiso 1 1 calc R . .
H11B H -0.0182 0.3994 0.4624 0.058 Uiso 1 1 calc R . .
C12 C 0.0078(3) 0.3039(4) 0.3797(2) 0.0449(9) Uani 1 1 d . . .
H12A H 0.0117 0.2141 0.4000 0.054 Uiso 1 1 calc R . .
H12B H -0.0630 0.3159 0.3523 0.054 Uiso 1 1 calc R . .
C13 C 0.0867(2) 0.3137(3) 0.33720(16) 0.0344(7) Uani 1 1 d . . .
H13A H 0.0728 0.2425 0.3037 0.041 Uiso 1 1 calc R . .
H13B H 0.0794 0.4013 0.3147 0.041 Uiso 1 1 calc R . .
C14 C 0.1911(3) -0.1999(3) 0.23861(19) 0.0386(8) Uani 1 1 d . . .
H14A H 0.1621 -0.2732 0.2605 0.046 Uiso 1 1 calc R . .
H14B H 0.1717 -0.2165 0.1911 0.046 Uiso 1 1 calc R . .
C15 C 0.1036(2) -0.0667(3) 0.33829(15) 0.0279(6) Uani 1 1 d . . .
H15A H 0.0674 0.0163 0.3477 0.033 Uiso 1 1 calc R . .
C16 C 0.0322(3) -0.1833(3) 0.34757(17) 0.0369(7) Uani 1 1 d . . .
H16A H -0.0337 -0.1776 0.3143 0.044 Uiso 1 1 calc R . .
H16B H 0.0659 -0.2694 0.3417 0.044 Uiso 1 1 calc R . .
C17 C 0.0098(3) -0.1784(4) 0.41578(19) 0.0428(8) Uani 1 1 d . . .
H17A H -0.0307 -0.0967 0.4196 0.051 Uiso 1 1 calc R . .
H17B H -0.0330 -0.2568 0.4215 0.051 Uiso 1 1 calc R . .
C18 C 0.1082(3) -0.1783(4) 0.46956(18) 0.0445(8) Uani 1 1 d . . .
H18A H 0.1439 -0.2654 0.4699 0.053 Uiso 1 1 calc R . .
H18B H 0.0900 -0.1668 0.5122 0.053 Uiso 1 1 calc R . .
C19 C 0.1809(3) -0.0660(4) 0.45956(17) 0.0411(8) Uani 1 1 d . . .
H19A H 0.1487 0.0216 0.4648 0.049 Uiso 1 1 calc R . .
H19B H 0.2466 -0.0725 0.4930 0.049 Uiso 1 1 calc R . .
C20 C 0.2034(2) -0.0744(3) 0.39207(16) 0.0334(7) Uani 1 1 d . . .
H20A H 0.2395 -0.1597 0.3880 0.040 Uiso 1 1 calc R . .
H20B H 0.2501 -0.0002 0.3865 0.040 Uiso 1 1 calc R . .
C21 C 0.0034(3) -0.0432(3) 0.19839(18) 0.0382(7) Uani 1 1 d . . .
H21A H 0.0140 0.0027 0.1583 0.046 Uiso 1 1 calc R . .
C22 C -0.0754(2) 0.0447(4) 0.22216(18) 0.0394(7) Uani 1 1 d . . .
H22A H -0.0454 0.1347 0.2333 0.047 Uiso 1 1 calc R . .
H22B H -0.0902 0.0051 0.2621 0.047 Uiso 1 1 calc R . .
C23 C -0.1774(3) 0.0579(5) 0.1699(2) 0.0580(11) Uani 1 1 d . . .
H23A H -0.2281 0.1091 0.1882 0.070 Uiso 1 1 calc R . .
H23B H -0.1641 0.1088 0.1323 0.070 Uiso 1 1 calc R . .
C24 C -0.2228(3) -0.0760(5) 0.1468(2) 0.0624(12) Uani 1 1 d . . .
H24A H -0.2856 -0.0632 0.1115 0.075 Uiso 1 1 calc R . .
H24B H -0.2434 -0.1233 0.1831 0.075 Uiso 1 1 calc R . .
C25 C -0.1446(3) -0.1597(5) 0.1219(2) 0.0605(12) Uani 1 1 d . . .
H25A H -0.1284 -0.1155 0.0834 0.073 Uiso 1 1 calc R . .
H25B H -0.1750 -0.2485 0.1081 0.073 Uiso 1 1 calc R . .
C26 C -0.0443(3) -0.1782(4) 0.1744(2) 0.0493(9) Uani 1 1 d . . .
H26A H -0.0596 -0.2288 0.2115 0.059 Uiso 1 1 calc R . .
H26B H 0.0058 -0.2308 0.1563 0.059 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 P1 2.1795(8) . ?
Ni1 P1 2.1796(8) 2 ?
Ni1 P2 2.1913(8) . ?
Ni1 P2 2.1913(8) 2 ?
P1 C1 1.852(3) . ?
P1 C8 1.869(3) . ?
P1 C2 1.880(4) . ?
P2 C14 1.866(3) . ?
P2 C15 1.876(3) . ?
P2 C21 1.892(3) . ?
C1 C1 1.537(6) 2 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.470(6) . ?
C2 C3 1.533(5) . ?
C2 H2A 1.0000 . ?
C3 C4 1.525(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.406(8) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.525(7) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.522(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.524(5) . ?
C8 C9 1.531(4) . ?
C8 H8A 1.0000 . ?
C9 C10 1.521(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.507(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.537(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.526(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C14 1.525(7) 2 ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.537(4) . ?
C15 C16 1.541(4) . ?
C15 H15A 1.0000 . ?
C16 C17 1.534(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.522(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.524(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.521(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C26 1.526(5) . ?
C21 C22 1.533(5) . ?
C21 H21A 1.0000 . ?
C22 C23 1.543(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.502(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.516(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.535(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 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
P1 Ni1 P1 90.51(4) . 2 ?
P1 Ni1 P2 120.06(3) . . ?
P1 Ni1 P2 118.83(3) 2 . ?
P1 Ni1 P2 118.83(3) . 2 ?
P1 Ni1 P2 120.06(3) 2 2 ?
P2 Ni1 P2 91.43(4) . 2 ?
C1 P1 C8 102.54(15) . . ?
C1 P1 C2 100.49(16) . . ?
C8 P1 C2 103.26(17) . . ?
C1 P1 Ni1 107.35(10) . . ?
C8 P1 Ni1 117.49(10) . . ?
C2 P1 Ni1 122.72(16) . . ?
C14 P2 C15 103.57(15) . . ?
C14 P2 C21 100.95(16) . . ?
C15 P2 C21 103.37(14) . . ?
C14 P2 Ni1 105.99(10) . . ?
C15 P2 Ni1 118.19(10) . . ?
C21 P2 Ni1 122.04(11) . . ?
C1 C1 P1 111.09(15) 2 . ?
C1 C1 H1A 109.4 2 . ?
P1 C1 H1A 109.4 . . ?
C1 C1 H1B 109.4 2 . ?
P1 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C7 C2 C3 111.4(3) . . ?
C7 C2 P1 122.3(3) . . ?
C3 C2 P1 111.9(2) . . ?
C7 C2 H2A 102.9 . . ?
C3 C2 H2A 102.9 . . ?
P1 C2 H2A 102.9 . . ?
C4 C3 C2 113.8(3) . . ?
C4 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C5 C4 C3 114.2(5) . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C4 C5 C6 114.2(5) . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C7 C6 C5 109.6(4) . . ?
C7 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
C7 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
C2 C7 C6 112.9(4) . . ?
C2 C7 H7A 109.0 . . ?
C6 C7 H7A 109.0 . . ?
C2 C7 H7B 109.0 . . ?
C6 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C13 C8 C9 108.8(3) . . ?
C13 C8 P1 110.7(2) . . ?
C9 C8 P1 119.9(2) . . ?
C13 C8 H8A 105.4 . . ?
C9 C8 H8A 105.4 . . ?
P1 C8 H8A 105.4 . . ?
C10 C9 C8 110.7(3) . . ?
C10 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C9 112.1(3) . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 C12 111.5(3) . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C13 C12 C11 110.2(3) . . ?
C13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C8 C13 C12 111.0(3) . . ?
C8 C13 H13A 109.4 . . ?
C12 C13 H13A 109.4 . . ?
C8 C13 H13B 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C14 C14 P2 111.39(17) 2 . ?
C14 C14 H14A 109.4 2 . ?
P2 C14 H14A 109.4 . . ?
C14 C14 H14B 109.4 2 . ?
P2 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C20 C15 C16 108.6(2) . . ?
C20 C15 P2 110.56(19) . . ?
C16 C15 P2 120.2(2) . . ?
C20 C15 H15A 105.4 . . ?
C16 C15 H15A 105.4 . . ?
P2 C15 H15A 105.4 . . ?
C17 C16 C15 110.5(3) . . ?
C17 C16 H16A 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C18 C17 C16 112.5(3) . . ?
C18 C17 H17A 109.1 . . ?
C16 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 C19 111.0(3) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 110.7(3) . . ?
C20 C19 H19A 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C19 C20 C15 111.6(3) . . ?
C19 C20 H20A 109.3 . . ?
C15 C20 H20A 109.3 . . ?
C19 C20 H20B 109.3 . . ?
C15 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
C26 C21 C22 110.7(3) . . ?
C26 C21 P2 119.6(3) . . ?
C22 C21 P2 111.2(2) . . ?
C26 C21 H21A 104.6 . . ?
C22 C21 H21A 104.6 . . ?
P2 C21 H21A 104.6 . . ?
C21 C22 C23 111.5(3) . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C24 C23 C22 112.1(4) . . ?
C24 C23 H23A 109.2 . . ?
C22 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
C22 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 C25 110.4(4) . . ?
C23 C24 H24A 109.6 . . ?
C25 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
C25 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
C24 C25 C26 111.4(3) . . ?
C24 C25 H25A 109.3 . . ?
C26 C25 H25A 109.3 . . ?
C24 C25 H25B 109.3 . . ?
C26 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
C21 C26 C25 111.0(4) . . ?
C21 C26 H26A 109.4 . . ?
C25 C26 H26A 109.4 . . ?
C21 C26 H26B 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         2.156
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.098
# SQUEEZE RESULTS (APPEND TO CIF)
# 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 0.250 0.500 0.750 161 20 ' '
2 0.750 0.500 0.250 161 20 ' '
_platon_squeeze_details          ?
_database_code_depnum_ccdc_archive 'CCDC 1002900'
#######################################################################
#
#                 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_FO5266
_publcif_datablock.id            {60e0c720-2cfd-4cbd-87e9-f16964fc2f62}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H58 Ni P2), C4 H8 O'
_chemical_formula_sum            'C34 H62 Ni O0.50 P2'
_chemical_formula_weight         599.49

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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.5810(2)
_cell_length_b                   12.3040(2)
_cell_length_c                   13.7385(2)
_cell_angle_alpha                97.923(1)
_cell_angle_beta                 106.776(1)
_cell_angle_gamma                101.793(1)
_cell_volume                     1638.94(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    6733
_cell_measurement_theta_min      2.08
_cell_measurement_theta_max      27.37

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.059
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.028
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      133(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  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11318
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         27.37
_reflns_number_total             7307
_reflns_number_gt                6759
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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)+(0.1288P)²+1.9073P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7307
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1873
_refine_ls_wR_factor_gt          0.1799
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.81176(3) 0.74639(3) 0.81234(2) 0.01365(14) Uani 1 1 d . . .
P1 P 0.78176(7) 0.83344(6) 0.68612(5) 0.01413(17) Uani 1 1 d . . .
P2 P 0.81972(7) 0.59565(6) 0.71591(5) 0.01330(17) Uani 1 1 d . . .
C1 C 0.8332(4) 0.8535(3) 0.9386(2) 0.0239(6) Uani 1 1 d . . .
C2 C 0.8573(3) 0.7486(3) 0.9652(2) 0.0218(6) Uani 1 1 d . . .
C3 C 0.7495(3) 0.6680(3) 0.9870(2) 0.0253(6) Uani 1 1 d . . .
C4 C 0.7752(5) 0.5866(3) 1.0398(3) 0.0377(8) Uani 1 1 d . . .
C5 C 1.0029(3) 0.7438(3) 1.0138(2) 0.0336(7) Uani 1 1 d . . .
H5A H 1.0263 0.7587 1.0896 0.050 Uiso 1 1 calc R . .
H5B H 1.0644 0.8013 0.9943 0.050 Uiso 1 1 calc R . .
H5C H 1.0125 0.6683 0.9890 0.050 Uiso 1 1 calc R . .
C6 C 0.6060(4) 0.6810(3) 0.9512(3) 0.0342(7) Uani 1 1 d . . .
H6A H 0.5428 0.6138 0.9570 0.051 Uiso 1 1 calc R . .
H6B H 0.5816 0.6889 0.8786 0.051 Uiso 1 1 calc R . .
H6C H 0.6001 0.7487 0.9946 0.051 Uiso 1 1 calc R . .
C7 C 0.8055(3) 0.7427(2) 0.5757(2) 0.0168(5) Uani 1 1 d . . .
H7A H 0.7487 0.7550 0.5091 0.020 Uiso 1 1 calc R . .
H7B H 0.9023 0.7644 0.5791 0.020 Uiso 1 1 calc R . .
C8 C 0.7648(3) 0.6167(2) 0.5800(2) 0.0178(5) Uani 1 1 d . . .
H8A H 0.8073 0.5730 0.5383 0.021 Uiso 1 1 calc R . .
H8B H 0.6644 0.5872 0.5490 0.021 Uiso 1 1 calc R . .
C9 C 0.9897(3) 0.5661(2) 0.7352(2) 0.0162(5) Uani 1 1 d . . .
H9A H 1.0132 0.5392 0.8020 0.019 Uiso 1 1 calc R . .
C10 C 1.1018(3) 0.6739(2) 0.7507(2) 0.0209(6) Uani 1 1 d . . .
H10A H 1.0859 0.7026 0.6855 0.025 Uiso 1 1 calc R . .
H10B H 1.0990 0.7334 0.8059 0.025 Uiso 1 1 calc R . .
C11 C 1.2422(3) 0.6487(3) 0.7814(3) 0.0260(6) Uani 1 1 d . . .
H11A H 1.3136 0.7185 0.7896 0.031 Uiso 1 1 calc R . .
H11B H 1.2605 0.6248 0.8490 0.031 Uiso 1 1 calc R . .
C12 C 1.2485(3) 0.5550(3) 0.6989(3) 0.0299(7) Uani 1 1 d . . .
H12A H 1.3385 0.5378 0.7219 0.036 Uiso 1 1 calc R . .
H12B H 1.2390 0.5819 0.6331 0.036 Uiso 1 1 calc R . .
C13 C 1.1356(3) 0.4469(2) 0.6798(2) 0.0220(6) Uani 1 1 d . . .
H13A H 1.1518 0.4145 0.7430 0.026 Uiso 1 1 calc R . .
H13B H 1.1379 0.3901 0.6222 0.026 Uiso 1 1 calc R . .
C14 C 0.9946(3) 0.4717(2) 0.6521(2) 0.0193(5) Uani 1 1 d . . .
H14A H 0.9735 0.4948 0.5842 0.023 Uiso 1 1 calc R . .
H14B H 0.9243 0.4017 0.6454 0.023 Uiso 1 1 calc R . .
C15 C 0.7099(3) 0.4529(2) 0.7052(2) 0.0161(5) Uani 1 1 d . . .
H15A H 0.7063 0.4014 0.6409 0.019 Uiso 1 1 calc R . .
C16 C 0.7691(3) 0.4033(2) 0.7995(2) 0.0225(6) Uani 1 1 d . . .
H16A H 0.7863 0.4594 0.8639 0.027 Uiso 1 1 calc R . .
H16B H 0.8577 0.3894 0.7986 0.027 Uiso 1 1 calc R . .
C17 C 0.6734(3) 0.2918(3) 0.8008(3) 0.0291(7) Uani 1 1 d . . .
H17A H 0.6654 0.2326 0.7412 0.035 Uiso 1 1 calc R . .
H17B H 0.7129 0.2662 0.8655 0.035 Uiso 1 1 calc R . .
C18 C 0.5321(3) 0.3066(3) 0.7946(3) 0.0270(6) Uani 1 1 d . . .
H18A H 0.5387 0.3620 0.8566 0.032 Uiso 1 1 calc R . .
H18B H 0.4716 0.2332 0.7934 0.032 Uiso 1 1 calc R . .
C19 C 0.4723(3) 0.3489(3) 0.6964(3) 0.0244(6) Uani 1 1 d . . .
H19A H 0.3806 0.3589 0.6926 0.029 Uiso 1 1 calc R . .
H19B H 0.4621 0.2919 0.6344 0.029 Uiso 1 1 calc R . .
C20 C 0.5651(3) 0.4619(2) 0.6965(2) 0.0219(6) Uani 1 1 d . . .
H20A H 0.5692 0.5200 0.7557 0.026 Uiso 1 1 calc R . .
H20B H 0.5255 0.4870 0.6316 0.026 Uiso 1 1 calc R . .
C21 C 0.9040(3) 0.9728(2) 0.7057(2) 0.0166(5) Uani 1 1 d . . .
H21A H 0.8840 1.0269 0.7571 0.020 Uiso 1 1 calc R . .
C22 C 0.8905(3) 1.0244(3) 0.6095(2) 0.0248(6) Uani 1 1 d . . .
H22A H 0.7959 1.0313 0.5808 0.030 Uiso 1 1 calc R . .
H22B H 0.9086 0.9734 0.5557 0.030 Uiso 1 1 calc R . .
C23 C 0.9907(3) 1.1420(3) 0.6353(3) 0.0292(7) Uani 1 1 d . . .
H23A H 0.9836 1.1709 0.5706 0.035 Uiso 1 1 calc R . .
H23B H 0.9660 1.1954 0.6829 0.035 Uiso 1 1 calc R . .
C24 C 1.1371(3) 1.1370(3) 0.6858(2) 0.0248(6) Uani 1 1 d . . .
H24A H 1.1654 1.0905 0.6352 0.030 Uiso 1 1 calc R . .
H24B H 1.1985 1.2146 0.7056 0.030 Uiso 1 1 calc R . .
C25 C 1.1509(3) 1.0859(3) 0.7819(2) 0.0230(6) Uani 1 1 d . . .
H25A H 1.1320 1.1367 0.8354 0.028 Uiso 1 1 calc R . .
H25B H 1.2458 1.0798 0.8109 0.028 Uiso 1 1 calc R . .
C26 C 1.0521(3) 0.9684(2) 0.7562(2) 0.0202(5) Uani 1 1 d . . .
H26A H 1.0601 0.9391 0.8207 0.024 Uiso 1 1 calc R . .
H26B H 1.0770 0.9155 0.7082 0.024 Uiso 1 1 calc R . .
C27 C 0.6145(3) 0.8631(2) 0.6249(2) 0.0166(5) Uani 1 1 d . . .
H27A H 0.6176 0.8912 0.5605 0.020 Uiso 1 1 calc R . .
C28 C 0.4959(3) 0.7561(2) 0.5936(2) 0.0210(6) Uani 1 1 d . . .
H28A H 0.4936 0.7247 0.6559 0.025 Uiso 1 1 calc R . .
H28B H 0.5104 0.6980 0.5435 0.025 Uiso 1 1 calc R . .
C29 C 0.3590(3) 0.7826(3) 0.5443(2) 0.0241(6) Uani 1 1 d . . .
H29A H 0.3583 0.8074 0.4786 0.029 Uiso 1 1 calc R . .
H29B H 0.2841 0.7128 0.5274 0.029 Uiso 1 1 calc R . .
C30 C 0.3342(3) 0.8751(3) 0.6167(2) 0.0240(6) Uani 1 1 d . . .
H30A H 0.2480 0.8933 0.5810 0.029 Uiso 1 1 calc R . .
H30B H 0.3248 0.8472 0.6792 0.029 Uiso 1 1 calc R . .
C31 C 0.4514(3) 0.9818(3) 0.6495(2) 0.0261(6) Uani 1 1 d . . .
H31A H 0.4360 1.0385 0.7005 0.031 Uiso 1 1 calc R . .
H31B H 0.4534 1.0148 0.5881 0.031 Uiso 1 1 calc R . .
C32 C 0.5895(3) 0.9564(3) 0.6983(2) 0.0222(6) Uani 1 1 d . . .
H32A H 0.5915 0.9319 0.7643 0.027 Uiso 1 1 calc R . .
H32B H 0.6637 1.0265 0.7145 0.027 Uiso 1 1 calc R . .
O1T O 1.4823(8) 1.0515(7) 0.9075(6) 0.0611(18) Uani 0.50 1 d P . .
C1T C 1.5724(11) 1.0705(8) 0.9763(8) 0.109(3) Uani 1 1 d . . .
H1TA H 1.6202 1.1510 0.9845 0.130 Uiso 1 1 calc R . .
H1TB H 1.6327 1.0248 0.9588 0.130 Uiso 1 1 calc R . .
C2T C 1.4315(6) 0.9444(4) 0.9175(4) 0.0617(14) Uani 1 1 d . . .
H2TA H 1.4855 0.8973 0.8974 0.074 Uiso 1 1 d R . .
H2TB H 1.3408 0.9170 0.8685 0.074 Uiso 1 1 d R . .
H1B H 0.750(4) 0.872(3) 0.935(3) 0.021(9) Uiso 1 1 d . . .
H1A H 0.914(4) 0.919(4) 0.960(3) 0.032(10) Uiso 1 1 d . . .
H4A H 0.695(6) 0.531(5) 1.040(5) 0.072(17) Uiso 1 1 d . . .
H4B H 0.867(6) 0.581(5) 1.065(4) 0.061(15) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.954(3) . ?
Ni1 C2 2.009(3) . ?
Ni1 P1 2.1420(7) . ?
Ni1 P2 2.1571(7) . ?
P1 C21 1.857(3) . ?
P1 C27 1.860(3) . ?
P1 C7 1.865(3) . ?
P2 C15 1.859(3) . ?
P2 C9 1.859(3) . ?
P2 C8 1.860(3) . ?
C1 C2 1.440(4) . ?
C1 H1B 0.95(4) . ?
C1 H1A 0.99(4) . ?
C2 C3 1.481(4) . ?
C2 C5 1.508(4) . ?
C3 C4 1.341(5) . ?
C3 C6 1.504(5) . ?
C4 H4A 0.98(6) . ?
C4 H4B 0.95(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.536(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.531(4) . ?
C9 C14 1.533(4) . ?
C9 H9A 1.0000 . ?
C10 C11 1.531(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.526(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.529(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.534(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.530(4) . ?
C15 C16 1.532(4) . ?
C15 H15A 1.0000 . ?
C16 C17 1.535(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.523(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.526(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.528(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.527(4) . ?
C21 C26 1.536(4) . ?
C21 H21A 1.0000 . ?
C22 C23 1.536(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.521(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.521(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.529(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.533(4) . ?
C27 C32 1.538(4) . ?
C27 H27A 1.0000 . ?
C28 C29 1.533(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.521(4) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.520(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.537(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
O1T C1T 1.088(11) . ?
O1T C2T 1.358(9) . ?
C1T C2T 1.507(9) 2_877 ?
C1T C2T 1.815(13) . ?
C1T H1TA 0.9900 . ?
C1T H1TB 0.9900 . ?
C2T C1T 1.507(9) 2_877 ?
C2T H2TA 0.9600 . ?
C2T H2TB 0.9600 . ?

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 C2 42.60(12) . . ?
C1 Ni1 P1 108.11(9) . . ?
C2 Ni1 P1 150.30(9) . . ?
C1 Ni1 P2 158.87(10) . . ?
C2 Ni1 P2 116.52(9) . . ?
P1 Ni1 P2 92.25(3) . . ?
C21 P1 C27 102.18(12) . . ?
C21 P1 C7 104.10(12) . . ?
C27 P1 C7 102.73(12) . . ?
C21 P1 Ni1 117.38(9) . . ?
C27 P1 Ni1 121.31(9) . . ?
C7 P1 Ni1 107.04(9) . . ?
C15 P2 C9 101.85(12) . . ?
C15 P2 C8 102.53(12) . . ?
C9 P2 C8 104.45(12) . . ?
C15 P2 Ni1 122.35(9) . . ?
C9 P2 Ni1 117.38(9) . . ?
C8 P2 Ni1 106.12(9) . . ?
C2 C1 Ni1 70.75(16) . . ?
C2 C1 H1B 121(2) . . ?
Ni1 C1 H1B 110(2) . . ?
C2 C1 H1A 116(2) . . ?
Ni1 C1 H1A 115(2) . . ?
H1B C1 H1A 115(3) . . ?
C1 C2 C3 119.5(3) . . ?
C1 C2 C5 118.4(3) . . ?
C3 C2 C5 117.1(3) . . ?
C1 C2 Ni1 66.65(16) . . ?
C3 C2 Ni1 111.5(2) . . ?
C5 C2 Ni1 111.9(2) . . ?
C4 C3 C2 122.8(3) . . ?
C4 C3 C6 119.0(3) . . ?
C2 C3 C6 118.1(3) . . ?
C3 C4 H4A 116(3) . . ?
C3 C4 H4B 118(3) . . ?
H4A C4 H4B 125(5) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P1 110.58(18) . . ?
C8 C7 H7A 109.5 . . ?
P1 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
P1 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 P2 111.46(18) . . ?
C7 C8 H8A 109.3 . . ?
P2 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
P2 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C14 110.5(2) . . ?
C10 C9 P2 112.10(18) . . ?
C14 C9 P2 115.29(18) . . ?
C10 C9 H9A 106.1 . . ?
C14 C9 H9A 106.1 . . ?
P2 C9 H9A 106.1 . . ?
C11 C10 C9 110.2(2) . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 110.8(3) . . ?
C12 C11 H11A 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 111.4(3) . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
C12 C13 C14 111.1(2) . . ?
C12 C13 H13A 109.4 . . ?
C14 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C14 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C9 C14 C13 111.3(2) . . ?
C9 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
C9 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C20 C15 C16 110.5(2) . . ?
C20 C15 P2 109.48(18) . . ?
C16 C15 P2 110.47(18) . . ?
C20 C15 H15A 108.8 . . ?
C16 C15 H15A 108.8 . . ?
P2 C15 H15A 108.8 . . ?
C15 C16 C17 112.4(2) . . ?
C15 C16 H16A 109.1 . . ?
C17 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
C17 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C18 C17 C16 111.2(3) . . ?
C18 C17 H17A 109.4 . . ?
C16 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
C16 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C17 C18 C19 109.6(3) . . ?
C17 C18 H18A 109.7 . . ?
C19 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
C19 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C18 C19 C20 110.5(2) . . ?
C18 C19 H19A 109.6 . . ?
C20 C19 H19A 109.6 . . ?
C18 C19 H19B 109.6 . . ?
C20 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C19 C20 C15 112.1(2) . . ?
C19 C20 H20A 109.2 . . ?
C15 C20 H20A 109.2 . . ?
C19 C20 H20B 109.2 . . ?
C15 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C22 C21 C26 110.6(2) . . ?
C22 C21 P1 115.59(19) . . ?
C26 C21 P1 111.45(18) . . ?
C22 C21 H21A 106.2 . . ?
C26 C21 H21A 106.2 . . ?
P1 C21 H21A 106.2 . . ?
C21 C22 C23 111.4(2) . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22B 109.3 . . ?
C23 C22 H22B 109.3 . . ?
H22A C22 H22B 108.0 . . ?
C24 C23 C22 111.3(3) . . ?
C24 C23 H23A 109.4 . . ?
C22 C23 H23A 109.4 . . ?
C24 C23 H23B 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C25 C24 C23 111.1(2) . . ?
C25 C24 H24A 109.4 . . ?
C23 C24 H24A 109.4 . . ?
C25 C24 H24B 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 C26 111.3(2) . . ?
C24 C25 H25A 109.4 . . ?
C26 C25 H25A 109.4 . . ?
C24 C25 H25B 109.4 . . ?
C26 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C25 C26 C21 111.2(2) . . ?
C25 C26 H26A 109.4 . . ?
C21 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
C21 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C32 110.0(2) . . ?
C28 C27 P1 111.94(19) . . ?
C32 C27 P1 110.60(19) . . ?
C28 C27 H27A 108.1 . . ?
C32 C27 H27A 108.1 . . ?
P1 C27 H27A 108.1 . . ?
C27 C28 C29 111.1(2) . . ?
C27 C28 H28A 109.4 . . ?
C29 C28 H28A 109.4 . . ?
C27 C28 H28B 109.4 . . ?
C29 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
C30 C29 C28 111.6(2) . . ?
C30 C29 H29A 109.3 . . ?
C28 C29 H29A 109.3 . . ?
C30 C29 H29B 109.3 . . ?
C28 C29 H29B 109.3 . . ?
H29A C29 H29B 108.0 . . ?
C31 C30 C29 110.9(2) . . ?
C31 C30 H30A 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 108.0 . . ?
C30 C31 C32 111.6(2) . . ?
C30 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
C30 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
C31 C32 C27 111.5(2) . . ?
C31 C32 H32A 109.3 . . ?
C27 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
C27 C32 H32B 109.3 . . ?
H32A C32 H32B 108.0 . . ?
C1T O1T C2T 95.1(8) . . ?
O1T C1T C2T 124.1(9) . 2_877 ?
O1T C1T C2T 48.2(7) . . ?
C2T C1T C2T 89.8(5) 2_877 . ?
O1T C1T H1TA 106.3 . . ?
C2T C1T H1TA 106.3 2_877 . ?
C2T C1T H1TA 154.2 . . ?
O1T C1T H1TB 106.3 . . ?
C2T C1T H1TB 106.3 2_877 . ?
C2T C1T H1TB 87.5 . . ?
H1TA C1T H1TB 106.4 . . ?
O1T C2T C1T 117.1(6) . 2_877 ?
O1T C2T C1T 36.7(4) . . ?
C1T C2T C1T 90.2(5) 2_877 . ?
O1T C2T H2TA 108.0 . . ?
C1T C2T H2TA 107.7 2_877 . ?
C1T C2T H2TA 95.5 . . ?
O1T C2T H2TB 107.4 . . ?
C1T C2T H2TB 109.1 2_877 . ?
C1T C2T H2TB 143.2 . . ?
H2TA C2T H2TB 107.3 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.37
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.777
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.161
_database_code_depnum_ccdc_archive 'CCDC 1002901'
#######################################################################
#
#                 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_FO5250
_publcif_datablock.id            {f4f32fe4-31ef-4e2d-8229-a2401f301e96}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H58 Ni P2'
_chemical_formula_sum            'C32 H58 Ni P2'
_chemical_formula_weight         563.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.1055(3)
_cell_length_b                   11.0712(3)
_cell_length_c                   14.8446(4)
_cell_angle_alpha                104.247(2)
_cell_angle_beta                 92.999(1)
_cell_angle_gamma                103.896(2)
_cell_volume                     1551.63(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    4727
_cell_measurement_theta_min      1.97
_cell_measurement_theta_max      27.49

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.013
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             616
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      133(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  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9680
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6983
_reflns_number_gt                6124
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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)+(0.0000P)²+3.5404P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6983
_refine_ls_number_parameters     537
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1065
_refine_ls_wR_factor_gt          0.0999
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_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 0.36355(3) 0.27029(3) 0.24707(2) 0.01821(10) Uani 1 1 d . . .
P1 P 0.17745(7) 0.29373(6) 0.18735(5) 0.01665(14) Uani 1 1 d . . .
P2 P 0.25381(7) 0.10996(6) 0.29513(5) 0.01663(14) Uani 1 1 d . . .
C1 C 0.5164(3) 0.4071(3) 0.2314(2) 0.0274(6) Uani 1 1 d . . .
H1A H 0.507(4) 0.492(4) 0.259(2) 0.037(10) Uiso 1 1 d . . .
H1B H 0.536(3) 0.391(3) 0.166(2) 0.029(9) Uiso 1 1 d . . .
C2 C 0.5641(3) 0.3381(3) 0.2910(2) 0.0247(6) Uani 1 1 d . . .
C3 C 0.6355(3) 0.2379(3) 0.2542(2) 0.0276(6) Uani 1 1 d . . .
C4 C 0.7134(3) 0.1952(3) 0.3098(3) 0.0332(7) Uani 1 1 d . . .
H4A H 0.754(3) 0.120(3) 0.281(2) 0.032(9) Uiso 1 1 d . . .
H4B H 0.718(4) 0.232(4) 0.380(3) 0.054(12) Uiso 1 1 d . . .
C5 C 0.5922(3) 0.4025(3) 0.3953(2) 0.0311(7) Uani 1 1 d . . .
H5A H 0.575(3) 0.333(3) 0.432(2) 0.029(9) Uiso 1 1 d . . .
H5B H 0.536(3) 0.468(3) 0.4078(19) 0.013(7) Uiso 1 1 d . . .
H5C H 0.689(4) 0.455(4) 0.415(3) 0.043(10) Uiso 1 1 d . . .
C6 C 0.6193(4) 0.1809(4) 0.1504(2) 0.0371(8) Uani 1 1 d . . .
H6A H 0.5215 0.1462 0.1272 0.045 Uiso 1 1 calc R . .
H6B H 0.6655 0.1113 0.1361 0.045 Uiso 1 1 calc R . .
H6C H 0.6603 0.2479 0.1202 0.045 Uiso 1 1 calc R . .
C7 C 0.0680(3) 0.1042(3) 0.27775(19) 0.0194(5) Uani 1 1 d . . .
H7A H 0.014(3) 0.021(3) 0.271(2) 0.018(7) Uiso 1 1 d . . .
H7B H 0.050(3) 0.160(3) 0.334(2) 0.022(8) Uiso 1 1 d . . .
C8 C 0.0351(3) 0.1570(3) 0.1948(2) 0.0195(5) Uani 1 1 d . . .
H8A H -0.049(3) 0.179(3) 0.196(2) 0.025(8) Uiso 1 1 d . . .
H8B H 0.023(3) 0.092(3) 0.136(2) 0.030(9) Uiso 1 1 d . . .
C9 C 0.1520(3) 0.2930(3) 0.06203(18) 0.0192(5) Uani 1 1 d . . .
H9 H 0.053(4) 0.277(3) 0.043(2) 0.033(9) Uiso 1 1 d . . .
C10 C 0.2084(4) 0.1868(3) 0.0025(2) 0.0264(6) Uani 1 1 d . . .
H10A H 0.160(4) 0.108(4) 0.008(2) 0.032(9) Uiso 1 1 d . . .
H10B H 0.303(4) 0.201(3) 0.025(2) 0.030(9) Uiso 1 1 d . . .
C11 C 0.2031(4) 0.1868(3) -0.1004(2) 0.0291(7) Uani 1 1 d . . .
H11A H 0.109(4) 0.167(3) -0.126(2) 0.035(10) Uiso 1 1 d . . .
H11B H 0.240(3) 0.120(3) -0.135(2) 0.028(9) Uiso 1 1 d . . .
C12 C 0.2752(3) 0.3185(3) -0.1120(2) 0.0268(6) Uani 1 1 d . . .
H12A H 0.272(4) 0.316(3) -0.177(3) 0.035(9) Uiso 1 1 d . . .
H12B H 0.376(4) 0.338(3) -0.087(2) 0.037(10) Uiso 1 1 d . . .
C13 C 0.2131(3) 0.4212(3) -0.0561(2) 0.0253(6) Uani 1 1 d . . .
H13A H 0.114(3) 0.401(3) -0.078(2) 0.025(8) Uiso 1 1 d . . .
H13B H 0.257(3) 0.502(3) -0.063(2) 0.027(8) Uiso 1 1 d . . .
C14 C 0.2226(3) 0.4240(3) 0.0473(2) 0.0236(6) Uani 1 1 d . . .
H14A H 0.314(3) 0.446(3) 0.073(2) 0.016(7) Uiso 1 1 d . . .
H14B H 0.185(3) 0.489(3) 0.084(2) 0.019(8) Uiso 1 1 d . . .
C15 C 0.1312(3) 0.4411(3) 0.25136(18) 0.0183(5) Uani 1 1 d . . .
H15 H 0.195(3) 0.507(3) 0.238(2) 0.016(7) Uiso 1 1 d . . .
C16 C -0.0128(3) 0.4517(3) 0.2237(2) 0.0254(6) Uani 1 1 d . . .
H16A H -0.030(4) 0.440(3) 0.155(3) 0.034(9) Uiso 1 1 d . . .
H16B H -0.080(4) 0.385(3) 0.241(2) 0.030(9) Uiso 1 1 d . . .
C17 C -0.0322(3) 0.5831(3) 0.2766(2) 0.0287(6) Uani 1 1 d . . .
H17A H -0.130(4) 0.584(3) 0.258(2) 0.033(9) Uiso 1 1 d . . .
H17B H 0.028(3) 0.648(3) 0.255(2) 0.021(8) Uiso 1 1 d . . .
C18 C -0.0022(3) 0.6080(3) 0.3819(2) 0.0294(7) Uani 1 1 d . . .
H18A H -0.072(4) 0.548(4) 0.398(3) 0.040(10) Uiso 1 1 d . . .
H18B H -0.007(4) 0.698(4) 0.416(3) 0.040(10) Uiso 1 1 d . . .
C19 C 0.1386(4) 0.5940(3) 0.4094(2) 0.0303(7) Uani 1 1 d . . .
H19A H 0.211(3) 0.665(3) 0.396(2) 0.025(8) Uiso 1 1 d . . .
H19B H 0.151(4) 0.606(4) 0.472(3) 0.041(10) Uiso 1 1 d . . .
C20 C 0.1560(3) 0.4623(3) 0.3578(2) 0.0260(6) Uani 1 1 d . . .
H20A H 0.246(3) 0.452(3) 0.377(2) 0.026(8) Uiso 1 1 d . . .
H20B H 0.090(4) 0.396(3) 0.374(2) 0.031(9) Uiso 1 1 d . . .
C21 C 0.2819(3) 0.1075(3) 0.41920(18) 0.0186(5) Uani 1 1 d . . .
H21 H 0.374(3) 0.100(3) 0.429(2) 0.017(7) Uiso 1 1 d . . .
C22 C 0.2781(3) 0.2354(3) 0.48683(19) 0.0229(6) Uani 1 1 d . . .
H22A H 0.185(3) 0.242(3) 0.483(2) 0.019(8) Uiso 1 1 d . . .
H22B H 0.335(3) 0.303(3) 0.468(2) 0.022(8) Uiso 1 1 d . . .
C23 C 0.3207(3) 0.2382(3) 0.5883(2) 0.0282(6) Uani 1 1 d . . .
H23A H 0.416(3) 0.234(3) 0.595(2) 0.018(7) Uiso 1 1 d . . .
H23B H 0.316(4) 0.320(4) 0.629(3) 0.036(10) Uiso 1 1 d . . .
C24 C 0.2296(3) 0.1247(3) 0.6159(2) 0.0286(6) Uani 1 1 d . . .
H24A H 0.131(4) 0.135(3) 0.617(2) 0.028(9) Uiso 1 1 d . . .
H24B H 0.260(4) 0.123(4) 0.680(3) 0.046(11) Uiso 1 1 d . . .
C25 C 0.2260(4) -0.0039(3) 0.5472(2) 0.0292(7) Uani 1 1 d . . .
H25A H 0.318(3) -0.020(3) 0.552(2) 0.025(8) Uiso 1 1 d . . .
H25B H 0.165(4) -0.072(3) 0.564(2) 0.034(9) Uiso 1 1 d . . .
C26 C 0.1869(3) -0.0045(3) 0.4460(2) 0.0247(6) Uani 1 1 d . . .
H26A H 0.190(3) -0.083(3) 0.405(2) 0.022(8) Uiso 1 1 d . . .
H26B H 0.093(4) 0.005(3) 0.440(2) 0.030(9) Uiso 1 1 d . . .
C27 C 0.2573(3) -0.0565(3) 0.23238(19) 0.0191(5) Uani 1 1 d . . .
H27 H 0.182(3) -0.118(3) 0.250(2) 0.023(8) Uiso 1 1 d . . .
C28 C 0.3960(3) -0.0812(3) 0.2569(2) 0.0232(6) Uani 1 1 d . . .
H28A H 0.470(3) -0.015(3) 0.247(2) 0.022(8) Uiso 1 1 d . . .
H28B H 0.410(3) -0.075(3) 0.320(3) 0.031(9) Uiso 1 1 d . . .
C29 C 0.4073(3) -0.2133(3) 0.2005(2) 0.0264(6) Uani 1 1 d . . .
H29A H 0.344(4) -0.280(3) 0.219(2) 0.031(9) Uiso 1 1 d . . .
H29B H 0.498(4) -0.219(3) 0.215(2) 0.033(9) Uiso 1 1 d . . .
C30 C 0.3785(3) -0.2304(3) 0.0961(2) 0.0266(6) Uani 1 1 d . . .
H30A H 0.382(3) -0.314(3) 0.059(2) 0.030(9) Uiso 1 1 d . . .
H30B H 0.452(3) -0.168(3) 0.077(2) 0.020(8) Uiso 1 1 d . . .
C31 C 0.2374(3) -0.2129(3) 0.0727(2) 0.0256(6) Uani 1 1 d . . .
H31A H 0.175(3) -0.273(3) 0.092(2) 0.012(7) Uiso 1 1 d . . .
H31B H 0.219(3) -0.224(3) 0.008(2) 0.030(9) Uiso 1 1 d . . .
C32 C 0.2269(3) -0.0794(3) 0.12627(19) 0.0226(6) Uani 1 1 d . . .
H32A H 0.136(3) -0.073(3) 0.111(2) 0.026(8) Uiso 1 1 d . . .
H32B H 0.293(3) -0.014(3) 0.107(2) 0.022(8) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.955(3) . ?
Ni1 C2 1.997(3) . ?
Ni1 P1 2.1362(7) . ?
Ni1 P2 2.1565(7) . ?
P1 C8 1.851(3) . ?
P1 C15 1.853(3) . ?
P1 C9 1.862(3) . ?
P2 C21 1.857(3) . ?
P2 C27 1.859(3) . ?
P2 C7 1.865(3) . ?
C1 C2 1.437(4) . ?
C1 H1A 0.96(4) . ?
C1 H1B 0.99(3) . ?
C2 C3 1.475(4) . ?
C2 C5 1.515(4) . ?
C3 C4 1.352(4) . ?
C3 C6 1.498(5) . ?
C4 H4A 1.03(3) . ?
C4 H4B 1.01(4) . ?
C5 H5A 1.04(3) . ?
C5 H5B 1.01(3) . ?
C5 H5C 1.00(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.540(4) . ?
C7 H7A 0.93(3) . ?
C7 H7B 0.97(3) . ?
C8 H8A 0.94(3) . ?
C8 H8B 0.96(3) . ?
C9 C14 1.529(4) . ?
C9 C10 1.533(4) . ?
C9 H9 0.98(3) . ?
C10 C11 1.527(4) . ?
C10 H10A 0.92(4) . ?
C10 H10B 0.96(4) . ?
C11 C12 1.521(4) . ?
C11 H11A 0.96(4) . ?
C11 H11B 0.96(3) . ?
C12 C13 1.520(4) . ?
C12 H12A 0.96(4) . ?
C12 H12B 1.02(4) . ?
C13 C14 1.525(4) . ?
C13 H13A 0.99(3) . ?
C13 H13B 0.93(3) . ?
C14 H14A 0.93(3) . ?
C14 H14B 0.96(3) . ?
C15 C16 1.530(4) . ?
C15 C20 1.537(4) . ?
C15 H15 0.92(3) . ?
C16 C17 1.537(4) . ?
C16 H16A 0.99(4) . ?
C16 H16B 0.97(4) . ?
C17 C18 1.521(4) . ?
C17 H17A 1.02(4) . ?
C17 H17B 0.96(3) . ?
C18 C19 1.514(4) . ?
C18 H18A 0.94(4) . ?
C18 H18B 1.01(4) . ?
C19 C20 1.527(4) . ?
C19 H19A 1.01(3) . ?
C19 H19B 0.91(4) . ?
C20 H20A 0.98(3) . ?
C20 H20B 0.96(4) . ?
C21 C26 1.526(4) . ?
C21 C22 1.531(4) . ?
C21 H21 0.96(3) . ?
C22 C23 1.536(4) . ?
C22 H22A 0.96(3) . ?
C22 H22B 0.94(3) . ?
C23 C24 1.526(4) . ?
C23 H23A 0.98(3) . ?
C23 H23B 0.97(4) . ?
C24 C25 1.525(4) . ?
C24 H24A 1.03(3) . ?
C24 H24B 0.99(4) . ?
C25 C26 1.530(4) . ?
C25 H25A 0.99(3) . ?
C25 H25B 0.95(4) . ?
C26 H26A 0.94(3) . ?
C26 H26B 0.98(3) . ?
C27 C28 1.534(4) . ?
C27 C32 1.535(4) . ?
C27 H27 0.99(3) . ?
C28 C29 1.529(4) . ?
C28 H28A 0.96(3) . ?
C28 H28B 0.92(4) . ?
C29 C30 1.519(4) . ?
C29 H29A 0.96(4) . ?
C29 H29B 0.95(4) . ?
C30 C31 1.518(4) . ?
C30 H30A 0.96(3) . ?
C30 H30B 0.99(3) . ?
C31 C32 1.528(4) . ?
C31 H31A 0.91(3) . ?
C31 H31B 0.94(3) . ?
C32 H32A 0.95(3) . ?
C32 H32B 0.97(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
C1 Ni1 C2 42.65(12) . . ?
C1 Ni1 P1 108.47(9) . . ?
C2 Ni1 P1 150.23(9) . . ?
C1 Ni1 P2 159.35(9) . . ?
C2 Ni1 P2 116.70(9) . . ?
P1 Ni1 P2 91.92(3) . . ?
C8 P1 C15 105.47(13) . . ?
C8 P1 C9 102.57(12) . . ?
C15 P1 C9 104.18(12) . . ?
C8 P1 Ni1 108.07(9) . . ?
C15 P1 Ni1 113.74(9) . . ?
C9 P1 Ni1 121.28(9) . . ?
C21 P2 C27 101.54(12) . . ?
C21 P2 C7 103.41(12) . . ?
C27 P2 C7 102.70(12) . . ?
C21 P2 Ni1 121.07(9) . . ?
C27 P2 Ni1 119.16(9) . . ?
C7 P2 Ni1 106.56(9) . . ?
C2 C1 Ni1 70.24(16) . . ?
C2 C1 H1A 119(2) . . ?
Ni1 C1 H1A 113(2) . . ?
C2 C1 H1B 120(2) . . ?
Ni1 C1 H1B 111(2) . . ?
H1A C1 H1B 115(3) . . ?
C1 C2 C3 121.0(3) . . ?
C1 C2 C5 117.8(3) . . ?
C3 C2 C5 116.9(3) . . ?
C1 C2 Ni1 67.12(16) . . ?
C3 C2 Ni1 109.7(2) . . ?
C5 C2 Ni1 112.3(2) . . ?
C4 C3 C2 123.0(3) . . ?
C4 C3 C6 119.0(3) . . ?
C2 C3 C6 118.0(3) . . ?
C3 C4 H4A 119.5(19) . . ?
C3 C4 H4B 117(2) . . ?
H4A C4 H4B 123(3) . . ?
C2 C5 H5A 109.8(18) . . ?
C2 C5 H5B 106.2(16) . . ?
H5A C5 H5B 117(2) . . ?
C2 C5 H5C 113(2) . . ?
H5A C5 H5C 107(3) . . ?
H5B C5 H5C 104(3) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P2 111.55(19) . . ?
C8 C7 H7A 111.4(19) . . ?
P2 C7 H7A 110.7(18) . . ?
C8 C7 H7B 108.1(18) . . ?
P2 C7 H7B 106.1(18) . . ?
H7A C7 H7B 109(3) . . ?
C7 C8 P1 111.12(18) . . ?
C7 C8 H8A 113(2) . . ?
P1 C8 H8A 111.7(19) . . ?
C7 C8 H8B 111(2) . . ?
P1 C8 H8B 107(2) . . ?
H8A C8 H8B 104(3) . . ?
C14 C9 C10 110.2(2) . . ?
C14 C9 P1 111.28(19) . . ?
C10 C9 P1 109.18(18) . . ?
C14 C9 H9 107(2) . . ?
C10 C9 H9 110(2) . . ?
P1 C9 H9 109(2) . . ?
C11 C10 C9 112.7(2) . . ?
C11 C10 H10A 110(2) . . ?
C9 C10 H10A 109(2) . . ?
C11 C10 H10B 106(2) . . ?
C9 C10 H10B 109(2) . . ?
H10A C10 H10B 109(3) . . ?
C12 C11 C10 111.5(3) . . ?
C12 C11 H11A 108(2) . . ?
C10 C11 H11A 109(2) . . ?
C12 C11 H11B 112(2) . . ?
C10 C11 H11B 110(2) . . ?
H11A C11 H11B 107(3) . . ?
C13 C12 C11 110.0(3) . . ?
C13 C12 H12A 112(2) . . ?
C11 C12 H12A 110(2) . . ?
C13 C12 H12B 109(2) . . ?
C11 C12 H12B 108(2) . . ?
H12A C12 H12B 107(3) . . ?
C12 C13 C14 111.1(2) . . ?
C12 C13 H13A 109.8(19) . . ?
C14 C13 H13A 106.3(19) . . ?
C12 C13 H13B 110(2) . . ?
C14 C13 H13B 110(2) . . ?
H13A C13 H13B 109(3) . . ?
C13 C14 C9 111.8(2) . . ?
C13 C14 H14A 110.4(18) . . ?
C9 C14 H14A 107.7(18) . . ?
C13 C14 H14B 112.4(18) . . ?
C9 C14 H14B 109.3(18) . . ?
H14A C14 H14B 105(3) . . ?
C16 C15 C20 110.1(2) . . ?
C16 C15 P1 116.50(19) . . ?
C20 C15 P1 111.23(18) . . ?
C16 C15 H15 108.8(18) . . ?
C20 C15 H15 105.5(18) . . ?
P1 C15 H15 104.0(18) . . ?
C15 C16 C17 110.6(2) . . ?
C15 C16 H16A 111(2) . . ?
C17 C16 H16A 109(2) . . ?
C15 C16 H16B 109(2) . . ?
C17 C16 H16B 108(2) . . ?
H16A C16 H16B 109(3) . . ?
C18 C17 C16 111.7(3) . . ?
C18 C17 H17A 111(2) . . ?
C16 C17 H17A 108(2) . . ?
C18 C17 H17B 110.5(19) . . ?
C16 C17 H17B 107.6(19) . . ?
H17A C17 H17B 108(3) . . ?
C19 C18 C17 111.7(3) . . ?
C19 C18 H18A 112(2) . . ?
C17 C18 H18A 105(2) . . ?
C19 C18 H18B 108(2) . . ?
C17 C18 H18B 112(2) . . ?
H18A C18 H18B 108(3) . . ?
C18 C19 C20 111.3(3) . . ?
C18 C19 H19A 109.4(18) . . ?
C20 C19 H19A 110.6(18) . . ?
C18 C19 H19B 109(2) . . ?
C20 C19 H19B 111(2) . . ?
H19A C19 H19B 106(3) . . ?
C19 C20 C15 110.5(2) . . ?
C19 C20 H20A 111.4(19) . . ?
C15 C20 H20A 111.9(19) . . ?
C19 C20 H20B 109(2) . . ?
C15 C20 H20B 108(2) . . ?
H20A C20 H20B 106(3) . . ?
C26 C21 C22 109.6(2) . . ?
C26 C21 P2 115.60(19) . . ?
C22 C21 P2 111.82(18) . . ?
C26 C21 H21 107.3(18) . . ?
C22 C21 H21 106.3(18) . . ?
P2 C21 H21 105.7(18) . . ?
C21 C22 C23 111.0(2) . . ?
C21 C22 H22A 108.0(18) . . ?
C23 C22 H22A 107.3(18) . . ?
C21 C22 H22B 107.8(19) . . ?
C23 C22 H22B 112.5(19) . . ?
H22A C22 H22B 110(3) . . ?
C24 C23 C22 111.1(2) . . ?
C24 C23 H23A 109.1(18) . . ?
C22 C23 H23A 109.1(18) . . ?
C24 C23 H23B 111(2) . . ?
C22 C23 H23B 109(2) . . ?
H23A C23 H23B 108(3) . . ?
C25 C24 C23 111.7(3) . . ?
C25 C24 H24A 108.7(19) . . ?
C23 C24 H24A 109.4(19) . . ?
C25 C24 H24B 109(2) . . ?
C23 C24 H24B 111(2) . . ?
H24A C24 H24B 106(3) . . ?
C24 C25 C26 111.8(2) . . ?
C24 C25 H25A 109.1(19) . . ?
C26 C25 H25A 108.3(19) . . ?
C24 C25 H25B 109(2) . . ?
C26 C25 H25B 111(2) . . ?
H25A C25 H25B 107(3) . . ?
C21 C26 C25 111.5(2) . . ?
C21 C26 H26A 109.6(19) . . ?
C25 C26 H26A 110.1(19) . . ?
C21 C26 H26B 108(2) . . ?
C25 C26 H26B 108(2) . . ?
H26A C26 H26B 109(3) . . ?
C28 C27 C32 110.7(2) . . ?
C28 C27 P2 110.70(19) . . ?
C32 C27 P2 110.62(18) . . ?
C28 C27 H27 110.9(18) . . ?
C32 C27 H27 105.6(18) . . ?
P2 C27 H27 108.3(18) . . ?
C29 C28 C27 112.3(2) . . ?
C29 C28 H28A 109.7(19) . . ?
C27 C28 H28A 110.6(19) . . ?
C29 C28 H28B 110(2) . . ?
C27 C28 H28B 110(2) . . ?
H28A C28 H28B 104(3) . . ?
C30 C29 C28 111.3(2) . . ?
C30 C29 H29A 110(2) . . ?
C28 C29 H29A 109(2) . . ?
C30 C29 H29B 109(2) . . ?
C28 C29 H29B 108(2) . . ?
H29A C29 H29B 109(3) . . ?
C31 C30 C29 110.3(2) . . ?
C31 C30 H30A 108(2) . . ?
C29 C30 H30A 113(2) . . ?
C31 C30 H30B 112.2(18) . . ?
C29 C30 H30B 108.3(18) . . ?
H30A C30 H30B 105(3) . . ?
C30 C31 C32 110.7(2) . . ?
C30 C31 H31A 107.7(18) . . ?
C32 C31 H31A 107.6(18) . . ?
C30 C31 H31B 111(2) . . ?
C32 C31 H31B 110(2) . . ?
H31A C31 H31B 110(3) . . ?
C31 C32 C27 111.6(2) . . ?
C31 C32 H32A 108.0(19) . . ?
C27 C32 H32A 110(2) . . ?
C31 C32 H32B 109.3(18) . . ?
C27 C32 H32B 108.7(18) . . ?
H32A C32 H32B 109(3) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 1002902'
#######################################################################
#
#                 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_FO5359
_publcif_datablock.id            {a6f4d565-93b5-43ae-9e8e-7b43699d9bc8}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H60 Ni P2, C4 H8 O'
_chemical_formula_sum            'C38 H68 Ni O P2'
_chemical_formula_weight         661.57

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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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                   11.7198(2)
_cell_length_b                   20.4120(3)
_cell_length_c                   15.3870(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.370(1)
_cell_angle_gamma                90.00
_cell_volume                     3620.75(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    14025
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      27.45

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.066
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.051
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      133(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  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27930
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.45
_reflns_number_total             8240
_reflns_number_gt                7490
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_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)+(0.0337P)²+2.8035P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8240
_refine_ls_number_parameters     619
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_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 0.793445(15) 0.679944(9) 0.908925(12) 0.01247(6) Uani 1 1 d . . .
P1 P 0.63512(3) 0.695522(18) 0.96094(2) 0.01326(8) Uani 1 1 d . . .
P2 P 0.73199(3) 0.744967(18) 0.79832(2) 0.01327(8) Uani 1 1 d . . .
C1 C 0.81317(14) 0.57864(8) 0.92483(12) 0.0216(3) Uani 1 1 d . . .
H1 H 0.744(2) 0.5595(12) 0.9122(15) 0.042(6) Uiso 1 1 d . . .
C2 C 0.86504(14) 0.59755(8) 0.85458(11) 0.0204(3) Uani 1 1 d . . .
H2 H 0.8221(18) 0.5896(11) 0.7961(14) 0.032(6) Uiso 1 1 d . . .
C3 C 0.99537(15) 0.60589(9) 0.86067(12) 0.0243(3) Uani 1 1 d . . .
H3B H 1.0356(17) 0.5753(10) 0.9040(13) 0.024(5) Uiso 1 1 d . . .
H3A H 1.0160(17) 0.5935(10) 0.8048(14) 0.026(5) Uiso 1 1 d . . .
C4 C 1.03758(14) 0.67579(9) 0.88558(12) 0.0246(4) Uani 1 1 d . . .
H4B H 1.121(2) 0.6761(10) 0.9129(15) 0.033(6) Uiso 1 1 d . . .
H4A H 1.0343(19) 0.7023(11) 0.8293(14) 0.032(6) Uiso 1 1 d . . .
C5 C 0.96545(13) 0.71073(8) 0.94291(11) 0.0203(3) Uani 1 1 d . . .
H5 H 0.9643(18) 0.7570(11) 0.9366(13) 0.026(5) Uiso 1 1 d . . .
C6 C 0.93293(14) 0.68522(9) 1.01792(11) 0.0213(3) Uani 1 1 d . . .
H6 H 0.9138(18) 0.7143(11) 1.0578(14) 0.029(5) Uiso 1 1 d . . .
C7 C 0.96642(15) 0.61683(10) 1.05359(12) 0.0270(4) Uani 1 1 d . . .
H7B H 1.0407(18) 0.6055(10) 1.0392(13) 0.027(5) Uiso 1 1 d . . .
H7A H 0.9770(19) 0.6185(11) 1.1153(15) 0.035(6) Uiso 1 1 d . . .
C8 C 0.87621(16) 0.56457(9) 1.01730(12) 0.0264(4) Uani 1 1 d . . .
H8B H 0.8175(18) 0.5635(10) 1.0557(13) 0.028(5) Uiso 1 1 d . . .
H8A H 0.9121(19) 0.5201(11) 1.0201(14) 0.036(6) Uiso 1 1 d . . .
C9 C 0.55520(13) 0.76502(8) 0.89874(10) 0.0170(3) Uani 1 1 d . . .
H9B H 0.5823(17) 0.8035(10) 0.9335(13) 0.024(5) Uiso 1 1 d . . .
H9A H 0.4744(18) 0.7615(10) 0.8993(13) 0.023(5) Uiso 1 1 d . . .
C10 C 0.58103(13) 0.77075(8) 0.80446(10) 0.0172(3) Uani 1 1 d . . .
H10B H 0.5679(19) 0.8155(11) 0.7818(14) 0.030(6) Uiso 1 1 d . . .
H10A H 0.5293(16) 0.7426(9) 0.7657(12) 0.017(4) Uiso 1 1 d . . .
C11 C 0.63112(13) 0.72069(8) 1.07699(10) 0.0170(3) Uani 1 1 d . . .
H11 H 0.5515(16) 0.7304(9) 1.0799(12) 0.017(4) Uiso 1 1 d . . .
C12 C 0.70315(15) 0.78287(9) 1.10397(11) 0.0222(3) Uani 1 1 d . . .
H12B H 0.7838(17) 0.7752(9) 1.0982(12) 0.021(5) Uiso 1 1 d . . .
H12A H 0.6698(19) 0.8219(11) 1.0649(15) 0.031(6) Uiso 1 1 d . . .
C13 C 0.70322(16) 0.80115(9) 1.20076(11) 0.0258(4) Uani 1 1 d . . .
H13B H 0.6248(18) 0.8130(9) 1.2066(13) 0.021(5) Uiso 1 1 d . . .
H13A H 0.753(2) 0.8389(11) 1.2175(14) 0.034(6) Uiso 1 1 d . . .
C14 C 0.74271(16) 0.74429(10) 1.26318(11) 0.0279(4) Uani 1 1 d . . .
H14A H 0.741(2) 0.7570(12) 1.3230(16) 0.042(6) Uiso 1 1 d . . .
H14B H 0.821(2) 0.7314(11) 1.2622(15) 0.036(6) Uiso 1 1 d . . .
C15 C 0.66782(16) 0.68384(9) 1.23726(11) 0.0251(4) Uani 1 1 d . . .
H15B H 0.5885(18) 0.6935(10) 1.2436(13) 0.025(5) Uiso 1 1 d . . .
H15A H 0.6924(18) 0.6466(11) 1.2748(14) 0.029(5) Uiso 1 1 d . . .
C16 C 0.67143(15) 0.66436(9) 1.14138(10) 0.0213(3) Uani 1 1 d . . .
H16B H 0.6255(18) 0.6266(10) 1.1275(13) 0.024(5) Uiso 1 1 d . . .
H16A H 0.7505(18) 0.6534(10) 1.1366(13) 0.024(5) Uiso 1 1 d . . .
C17 C 0.52687(13) 0.62697(7) 0.94656(10) 0.0149(3) Uani 1 1 d . . .
H17 H 0.5685(17) 0.5913(10) 0.9770(13) 0.022(5) Uiso 1 1 d . . .
C18 C 0.41521(13) 0.63647(8) 0.98471(11) 0.0186(3) Uani 1 1 d . . .
H18B H 0.4347(17) 0.6467(10) 1.0472(13) 0.023(5) Uiso 1 1 d . . .
H18A H 0.3708(18) 0.6743(10) 0.9547(13) 0.025(5) Uiso 1 1 d . . .
C19 C 0.33836(14) 0.57516(8) 0.97080(11) 0.0204(3) Uani 1 1 d . . .
H19B H 0.3791(17) 0.5390(10) 1.0038(13) 0.022(5) Uiso 1 1 d . . .
H19A H 0.2669(17) 0.5844(10) 0.9960(13) 0.024(5) Uiso 1 1 d . . .
C20 C 0.30907(14) 0.55576(9) 0.87351(11) 0.0220(3) Uani 1 1 d . . .
H20B H 0.2666(19) 0.5161(11) 0.8671(14) 0.031(5) Uiso 1 1 d . . .
H20A H 0.2627(17) 0.5882(10) 0.8412(13) 0.024(5) Uiso 1 1 d . . .
C21 C 0.41969(14) 0.54633(8) 0.83520(11) 0.0214(3) Uani 1 1 d . . .
H21B H 0.3982(17) 0.5357(10) 0.7738(14) 0.024(5) Uiso 1 1 d . . .
H21A H 0.4636(16) 0.5093(10) 0.8656(12) 0.019(5) Uiso 1 1 d . . .
C22 C 0.49561(13) 0.60777(8) 0.84852(10) 0.0179(3) Uani 1 1 d . . .
H22B H 0.5662(17) 0.6012(9) 0.8240(12) 0.021(5) Uiso 1 1 d . . .
H22A H 0.4520(18) 0.6464(10) 0.8167(13) 0.027(5) Uiso 1 1 d . . .
C23 C 0.71296(13) 0.71909(8) 0.67994(10) 0.0170(3) Uani 1 1 d . . .
H23 H 0.6723(17) 0.7545(10) 0.6447(13) 0.022(5) Uiso 1 1 d . . .
C24 C 0.63730(14) 0.65747(8) 0.66175(10) 0.0201(3) Uani 1 1 d . . .
H24B H 0.6721(17) 0.6212(10) 0.6993(13) 0.021(5) Uiso 1 1 d . . .
H24A H 0.5567(19) 0.6674(10) 0.6730(14) 0.028(5) Uiso 1 1 d . . .
C25 C 0.62541(17) 0.63461(9) 0.56556(11) 0.0262(4) Uani 1 1 d . . .
H25B H 0.5811(18) 0.5960(11) 0.5583(14) 0.028(5) Uiso 1 1 d . . .
H25A H 0.5831(19) 0.6671(11) 0.5277(15) 0.031(6) Uiso 1 1 d . . .
C26 C 0.74371(19) 0.62358(10) 0.53973(12) 0.0319(4) Uani 1 1 d . . .
H26B H 0.731(2) 0.6098(13) 0.4790(18) 0.053(7) Uiso 1 1 d . . .
H26A H 0.7815(19) 0.5858(11) 0.5760(15) 0.035(6) Uiso 1 1 d . . .
C27 C 0.81818(19) 0.68491(10) 0.55609(12) 0.0307(4) Uani 1 1 d . . .
H27B H 0.782(2) 0.7192(11) 0.5199(15) 0.035(6) Uiso 1 1 d . . .
H27A H 0.898(2) 0.6769(11) 0.5423(15) 0.037(6) Uiso 1 1 d . . .
C28 C 0.83158(15) 0.70733(8) 0.65267(11) 0.0211(3) Uani 1 1 d . . .
H28B H 0.8732(18) 0.6734(10) 0.6923(14) 0.027(5) Uiso 1 1 d . . .
H28A H 0.8786(18) 0.7465(11) 0.6622(13) 0.027(5) Uiso 1 1 d . . .
C29 C 0.80993(13) 0.82474(7) 0.79645(10) 0.0155(3) Uani 1 1 d . . .
H29 H 0.8878(17) 0.8125(9) 0.7980(12) 0.019(5) Uiso 1 1 d . . .
C30 C 0.77426(15) 0.86935(8) 0.71555(11) 0.0210(3) Uani 1 1 d . . .
H30B H 0.7774(18) 0.8457(10) 0.6613(14) 0.027(5) Uiso 1 1 d . . .
H30A H 0.6944(18) 0.8827(10) 0.7133(13) 0.022(5) Uiso 1 1 d . . .
C31 C 0.85353(16) 0.92965(8) 0.72100(11) 0.0249(3) Uani 1 1 d . . .
H31A H 0.9340(18) 0.9154(10) 0.7193(13) 0.025(5) Uiso 1 1 d . . .
H31B H 0.8273(18) 0.9580(11) 0.6694(14) 0.032(6) Uiso 1 1 d . . .
C32 C 0.85375(17) 0.96835(8) 0.80598(12) 0.0263(4) Uani 1 1 d . . .
H32B H 0.7769(19) 0.9866(11) 0.8045(14) 0.031(6) Uiso 1 1 d . . .
H32A H 0.906(2) 1.0044(12) 0.8097(15) 0.037(6) Uiso 1 1 d . . .
C33 C 0.88483(17) 0.92457(8) 0.88731(11) 0.0255(4) Uani 1 1 d . . .
H33B H 0.8774(17) 0.9510(10) 0.9413(14) 0.027(5) Uiso 1 1 d . . .
H33A H 0.9637(19) 0.9091(11) 0.8917(14) 0.030(5) Uiso 1 1 d . . .
C34 C 0.80556(15) 0.86433(8) 0.88112(11) 0.0197(3) Uani 1 1 d . . .
H34B H 0.7277(17) 0.8781(9) 0.8792(12) 0.018(5) Uiso 1 1 d . . .
H34A H 0.8259(16) 0.8372(10) 0.9324(13) 0.019(5) Uiso 1 1 d . . .
O1T O 0.8041(2) 0.53648(13) 1.33981(19) 0.0924(8) Uani 1 1 d . . .
C1T C 0.8298(2) 0.48068(13) 1.3905(2) 0.0576(7) Uani 1 1 d . . .
H1TA H 0.7746 0.4453 1.3677 0.069 Uiso 1 1 calc R . .
H1TB H 0.8220 0.4899 1.4524 0.069 Uiso 1 1 calc R . .
C2T C 0.9530(2) 0.45873(12) 1.38754(19) 0.0550(6) Uani 1 1 d . . .
H2TA H 0.9533 0.4198 1.3492 0.066 Uiso 1 1 calc R . .
H2TB H 0.9958 0.4483 1.4474 0.066 Uiso 1 1 calc R . .
C3T C 1.0054(3) 0.51804(15) 1.3490(2) 0.0674(8) Uani 1 1 d . . .
H3TB H 1.0612 0.5410 1.3950 0.081 Uiso 1 1 calc R . .
H3TC H 1.0455 0.5049 1.3003 0.081 Uiso 1 1 calc R . .
C4T C 0.9031(3) 0.56017(19) 1.3159(3) 0.0930(13) Uani 1 1 d . . .
H4TA H 0.9180 0.6050 1.3397 0.112 Uiso 1 1 calc R . .
H4TB H 0.8920 0.5628 1.2506 0.112 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 C5 2.0863(15) . ?
Ni1 C1 2.0903(16) . ?
Ni1 C2 2.1177(16) . ?
Ni1 C6 2.1235(16) . ?
Ni1 P1 2.1724(4) . ?
Ni1 P2 2.1761(4) . ?
P1 C9 1.8663(16) . ?
P1 C11 1.8667(15) . ?
P1 C17 1.8750(15) . ?
P2 C10 1.8645(16) . ?
P2 C29 1.8698(15) . ?
P2 C23 1.8709(15) . ?
C1 C2 1.387(2) . ?
C1 C8 1.508(3) . ?
C1 H1 0.89(2) . ?
C2 C3 1.523(2) . ?
C2 H2 0.96(2) . ?
C3 C4 1.536(3) . ?
C3 H3B 0.97(2) . ?
C3 H3A 0.97(2) . ?
C4 C5 1.507(2) . ?
C4 H4B 0.99(2) . ?
C4 H4A 1.02(2) . ?
C5 C6 1.381(2) . ?
C5 H5 0.95(2) . ?
C6 C7 1.525(2) . ?
C6 H6 0.91(2) . ?
C7 C8 1.535(3) . ?
C7 H7B 0.96(2) . ?
C7 H7A 0.94(2) . ?
C8 H8B 0.98(2) . ?
C8 H8A 1.00(2) . ?
C9 C10 1.539(2) . ?
C9 H9B 0.97(2) . ?
C9 H9A 0.95(2) . ?
C10 H10B 0.98(2) . ?
C10 H10A 0.961(19) . ?
C11 C16 1.536(2) . ?
C11 C12 1.539(2) . ?
C11 H11 0.963(19) . ?
C12 C13 1.535(2) . ?
C12 H12B 0.98(2) . ?
C12 H12A 1.03(2) . ?
C13 C14 1.524(3) . ?
C13 H13B 0.97(2) . ?
C13 H13A 0.98(2) . ?
C14 C15 1.525(3) . ?
C14 H14A 0.96(2) . ?
C14 H14B 0.96(2) . ?
C15 C16 1.536(2) . ?
C15 H15B 0.97(2) . ?
C15 H15A 0.97(2) . ?
C16 H16B 0.94(2) . ?
C16 H16A 0.97(2) . ?
C17 C22 1.538(2) . ?
C17 C18 1.540(2) . ?
C17 H17 0.95(2) . ?
C18 C19 1.534(2) . ?
C18 H18B 0.97(2) . ?
C18 H18A 1.00(2) . ?
C19 C20 1.527(2) . ?
C19 H19B 0.97(2) . ?
C19 H19A 1.00(2) . ?
C20 C21 1.530(2) . ?
C20 H20B 0.95(2) . ?
C20 H20A 0.94(2) . ?
C21 C22 1.530(2) . ?
C21 H21B 0.96(2) . ?
C21 H21A 0.984(19) . ?
C22 H22B 0.978(19) . ?
C22 H22A 1.02(2) . ?
C23 C24 1.535(2) . ?
C23 C28 1.542(2) . ?
C23 H23 0.97(2) . ?
C24 C25 1.534(2) . ?
C24 H24B 0.98(2) . ?
C24 H24A 1.01(2) . ?
C25 C26 1.526(3) . ?
C25 H25B 0.94(2) . ?
C25 H25A 0.96(2) . ?
C26 C27 1.521(3) . ?
C26 H26B 0.96(3) . ?
C26 H26A 1.01(2) . ?
C27 C28 1.536(2) . ?
C27 H27B 0.95(2) . ?
C27 H27A 1.01(2) . ?
C28 H28B 0.99(2) . ?
C28 H28A 0.97(2) . ?
C29 C30 1.538(2) . ?
C29 C34 1.542(2) . ?
C29 H29 0.94(2) . ?
C30 C31 1.535(2) . ?
C30 H30B 0.97(2) . ?
C30 H30A 0.97(2) . ?
C31 C32 1.527(2) . ?
C31 H31A 0.99(2) . ?
C31 H31B 0.99(2) . ?
C32 C33 1.528(2) . ?
C32 H32B 0.97(2) . ?
C32 H32A 0.95(2) . ?
C33 C34 1.533(2) . ?
C33 H33B 1.01(2) . ?
C33 H33A 0.97(2) . ?
C34 H34B 0.95(2) . ?
C34 H34A 0.96(2) . ?
O1T C4T 1.367(4) . ?
O1T C1T 1.383(4) . ?
C1T C2T 1.520(4) . ?
C1T H1TA 0.9900 . ?
C1T H1TB 0.9900 . ?
C2T C3T 1.525(4) . ?
C2T H2TA 0.9900 . ?
C2T H2TB 0.9900 . ?
C3T C4T 1.489(4) . ?
C3T H3TB 0.9900 . ?
C3T H3TC 0.9900 . ?
C4T H4TA 0.9900 . ?
C4T H4TB 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
C5 Ni1 C1 100.79(6) . . ?
C5 Ni1 C2 84.52(7) . . ?
C1 Ni1 C2 38.48(6) . . ?
C5 Ni1 C6 38.29(6) . . ?
C1 Ni1 C6 84.52(7) . . ?
C2 Ni1 C6 92.80(6) . . ?
C5 Ni1 P1 135.59(5) . . ?
C1 Ni1 P1 100.69(5) . . ?
C2 Ni1 P1 133.40(5) . . ?
C6 Ni1 P1 106.78(5) . . ?
C5 Ni1 P2 100.43(5) . . ?
C1 Ni1 P2 135.16(5) . . ?
C2 Ni1 P2 105.93(5) . . ?
C6 Ni1 P2 133.32(5) . . ?
P1 Ni1 P2 90.831(15) . . ?
C9 P1 C11 100.64(7) . . ?
C9 P1 C17 103.90(7) . . ?
C11 P1 C17 100.68(7) . . ?
C9 P1 Ni1 107.78(5) . . ?
C11 P1 Ni1 124.26(5) . . ?
C17 P1 Ni1 116.87(5) . . ?
C10 P2 C29 103.04(7) . . ?
C10 P2 C23 100.44(7) . . ?
C29 P2 C23 101.76(7) . . ?
C10 P2 Ni1 108.42(5) . . ?
C29 P2 Ni1 116.70(5) . . ?
C23 P2 Ni1 123.63(5) . . ?
C2 C1 C8 125.40(15) . . ?
C2 C1 Ni1 71.83(9) . . ?
C8 C1 Ni1 108.90(12) . . ?
C2 C1 H1 117.5(15) . . ?
C8 C1 H1 113.3(15) . . ?
Ni1 C1 H1 109.4(16) . . ?
C1 C2 C3 123.96(15) . . ?
C1 C2 Ni1 69.69(9) . . ?
C3 C2 Ni1 110.56(11) . . ?
C1 C2 H2 117.0(13) . . ?
C3 C2 H2 115.2(13) . . ?
Ni1 C2 H2 109.0(13) . . ?
C2 C3 C4 113.18(14) . . ?
C2 C3 H3B 109.1(12) . . ?
C4 C3 H3B 109.4(12) . . ?
C2 C3 H3A 108.9(12) . . ?
C4 C3 H3A 110.1(12) . . ?
H3B C3 H3A 105.9(16) . . ?
C5 C4 C3 113.36(13) . . ?
C5 C4 H4B 111.2(13) . . ?
C3 C4 H4B 111.1(13) . . ?
C5 C4 H4A 107.9(12) . . ?
C3 C4 H4A 108.8(12) . . ?
H4B C4 H4A 104.0(17) . . ?
C6 C5 C4 125.39(15) . . ?
C6 C5 Ni1 72.31(9) . . ?
C4 C5 Ni1 109.22(11) . . ?
C6 C5 H5 117.3(12) . . ?
C4 C5 H5 114.2(12) . . ?
Ni1 C5 H5 106.2(13) . . ?
C5 C6 C7 123.64(15) . . ?
C5 C6 Ni1 69.40(9) . . ?
C7 C6 Ni1 110.45(11) . . ?
C5 C6 H6 117.1(14) . . ?
C7 C6 H6 115.7(13) . . ?
Ni1 C6 H6 108.5(13) . . ?
C6 C7 C8 112.93(14) . . ?
C6 C7 H7B 108.7(13) . . ?
C8 C7 H7B 110.0(13) . . ?
C6 C7 H7A 108.0(14) . . ?
C8 C7 H7A 110.6(14) . . ?
H7B C7 H7A 106.4(18) . . ?
C1 C8 C7 113.53(14) . . ?
C1 C8 H8B 107.1(12) . . ?
C7 C8 H8B 107.9(12) . . ?
C1 C8 H8A 110.2(13) . . ?
C7 C8 H8A 111.0(13) . . ?
H8B C8 H8A 106.8(17) . . ?
C10 C9 P1 112.05(10) . . ?
C10 C9 H9B 110.9(12) . . ?
P1 C9 H9B 104.4(12) . . ?
C10 C9 H9A 112.3(12) . . ?
P1 C9 H9A 110.3(12) . . ?
H9B C9 H9A 106.5(17) . . ?
C9 C10 P2 112.08(10) . . ?
C9 C10 H10B 111.2(13) . . ?
P2 C10 H10B 109.6(13) . . ?
C9 C10 H10A 109.3(11) . . ?
P2 C10 H10A 107.3(11) . . ?
H10B C10 H10A 107.2(17) . . ?
C16 C11 C12 110.69(13) . . ?
C16 C11 P1 110.69(11) . . ?
C12 C11 P1 112.20(10) . . ?
C16 C11 H11 108.2(11) . . ?
C12 C11 H11 107.9(11) . . ?
P1 C11 H11 107.0(11) . . ?
C13 C12 C11 111.50(14) . . ?
C13 C12 H12B 107.2(11) . . ?
C11 C12 H12B 109.6(11) . . ?
C13 C12 H12A 108.2(12) . . ?
C11 C12 H12A 110.4(13) . . ?
H12B C12 H12A 110.0(16) . . ?
C14 C13 C12 111.92(15) . . ?
C14 C13 H13B 108.5(12) . . ?
C12 C13 H13B 108.4(12) . . ?
C14 C13 H13A 109.6(13) . . ?
C12 C13 H13A 110.1(13) . . ?
H13B C13 H13A 108.3(17) . . ?
C13 C14 C15 110.86(14) . . ?
C13 C14 H14A 110.0(14) . . ?
C15 C14 H14A 110.9(14) . . ?
C13 C14 H14B 112.5(14) . . ?
C15 C14 H14B 106.3(14) . . ?
H14A C14 H14B 106.2(19) . . ?
C14 C15 C16 110.28(15) . . ?
C14 C15 H15B 108.9(12) . . ?
C16 C15 H15B 109.9(12) . . ?
C14 C15 H15A 112.6(13) . . ?
C16 C15 H15A 108.3(12) . . ?
H15B C15 H15A 106.7(17) . . ?
C11 C16 C15 111.55(14) . . ?
C11 C16 H16B 111.6(12) . . ?
C15 C16 H16B 108.4(12) . . ?
C11 C16 H16A 108.1(12) . . ?
C15 C16 H16A 108.9(12) . . ?
H16B C16 H16A 108.1(17) . . ?
C22 C17 C18 109.72(12) . . ?
C22 C17 P1 110.03(10) . . ?
C18 C17 P1 117.67(11) . . ?
C22 C17 H17 107.4(12) . . ?
C18 C17 H17 107.7(12) . . ?
P1 C17 H17 103.7(12) . . ?
C19 C18 C17 111.22(13) . . ?
C19 C18 H18B 109.9(12) . . ?
C17 C18 H18B 109.9(12) . . ?
C19 C18 H18A 108.8(12) . . ?
C17 C18 H18A 109.2(12) . . ?
H18B C18 H18A 107.7(16) . . ?
C20 C19 C18 111.78(13) . . ?
C20 C19 H19B 108.5(12) . . ?
C18 C19 H19B 109.0(12) . . ?
C20 C19 H19A 111.9(11) . . ?
C18 C19 H19A 107.6(12) . . ?
H19B C19 H19A 108.0(16) . . ?
C19 C20 C21 110.73(13) . . ?
C19 C20 H20B 110.2(13) . . ?
C21 C20 H20B 108.6(13) . . ?
C19 C20 H20A 110.0(12) . . ?
C21 C20 H20A 109.5(12) . . ?
H20B C20 H20A 107.7(17) . . ?
C22 C21 C20 110.98(14) . . ?
C22 C21 H21B 111.2(12) . . ?
C20 C21 H21B 108.6(12) . . ?
C22 C21 H21A 108.9(11) . . ?
C20 C21 H21A 108.7(11) . . ?
H21B C21 H21A 108.4(16) . . ?
C21 C22 C17 111.74(13) . . ?
C21 C22 H22B 110.4(11) . . ?
C17 C22 H22B 110.1(11) . . ?
C21 C22 H22A 110.0(12) . . ?
C17 C22 H22A 106.6(11) . . ?
H22B C22 H22A 107.9(16) . . ?
C24 C23 C28 110.02(13) . . ?
C24 C23 P2 111.87(10) . . ?
C28 C23 P2 110.72(11) . . ?
C24 C23 H23 107.3(12) . . ?
C28 C23 H23 109.8(12) . . ?
P2 C23 H23 107.0(11) . . ?
C25 C24 C23 111.97(14) . . ?
C25 C24 H24B 107.1(11) . . ?
C23 C24 H24B 110.2(11) . . ?
C25 C24 H24A 107.5(12) . . ?
C23 C24 H24A 109.4(12) . . ?
H24B C24 H24A 110.6(16) . . ?
C26 C25 C24 111.55(15) . . ?
C26 C25 H25B 110.7(13) . . ?
C24 C25 H25B 108.8(13) . . ?
C26 C25 H25A 109.8(13) . . ?
C24 C25 H25A 108.8(13) . . ?
H25B C25 H25A 107.0(18) . . ?
C27 C26 C25 110.89(16) . . ?
C27 C26 H26B 112.7(16) . . ?
C25 C26 H26B 107.8(16) . . ?
C27 C26 H26A 110.9(13) . . ?
C25 C26 H26A 107.4(12) . . ?
H26B C26 H26A 107(2) . . ?
C26 C27 C28 111.16(15) . . ?
C26 C27 H27B 109.2(14) . . ?
C28 C27 H27B 107.8(14) . . ?
C26 C27 H27A 111.0(13) . . ?
C28 C27 H27A 108.3(13) . . ?
H27B C27 H27A 109.3(19) . . ?
C27 C28 C23 111.70(15) . . ?
C27 C28 H28B 109.9(12) . . ?
C23 C28 H28B 108.0(12) . . ?
C27 C28 H28A 110.4(12) . . ?
C23 C28 H28A 110.3(12) . . ?
H28B C28 H28A 106.3(17) . . ?
C30 C29 C34 109.14(13) . . ?
C30 C29 P2 117.75(11) . . ?
C34 C29 P2 110.66(10) . . ?
C30 C29 H29 107.4(12) . . ?
C34 C29 H29 107.3(12) . . ?
P2 C29 H29 104.0(11) . . ?
C31 C30 C29 110.91(13) . . ?
C31 C30 H30B 109.2(12) . . ?
C29 C30 H30B 110.8(12) . . ?
C31 C30 H30A 110.3(12) . . ?
C29 C30 H30A 108.3(12) . . ?
H30B C30 H30A 107.2(17) . . ?
C32 C31 C30 111.66(14) . . ?
C32 C31 H31A 108.6(12) . . ?
C30 C31 H31A 109.4(12) . . ?
C32 C31 H31B 109.8(13) . . ?
C30 C31 H31B 109.2(13) . . ?
H31A C31 H31B 108.1(17) . . ?
C33 C32 C31 111.23(14) . . ?
C33 C32 H32B 109.1(13) . . ?
C31 C32 H32B 108.6(13) . . ?
C33 C32 H32A 110.3(14) . . ?
C31 C32 H32A 110.6(14) . . ?
H32B C32 H32A 106.8(19) . . ?
C32 C33 C34 111.46(14) . . ?
C32 C33 H33B 108.5(12) . . ?
C34 C33 H33B 109.9(12) . . ?
C32 C33 H33A 109.4(13) . . ?
C34 C33 H33A 107.7(13) . . ?
H33B C33 H33A 109.9(17) . . ?
C33 C34 C29 111.15(13) . . ?
C33 C34 H34B 109.4(11) . . ?
C29 C34 H34B 107.9(11) . . ?
C33 C34 H34A 110.7(12) . . ?
C29 C34 H34A 110.6(12) . . ?
H34B C34 H34A 106.9(16) . . ?
C4T O1T C1T 109.6(3) . . ?
O1T C1T C2T 109.7(2) . . ?
O1T C1T H1TA 109.7 . . ?
C2T C1T H1TA 109.7 . . ?
O1T C1T H1TB 109.7 . . ?
C2T C1T H1TB 109.7 . . ?
H1TA C1T H1TB 108.2 . . ?
C1T C2T C3T 103.2(2) . . ?
C1T C2T H2TA 111.1 . . ?
C3T C2T H2TA 111.1 . . ?
C1T C2T H2TB 111.1 . . ?
C3T C2T H2TB 111.1 . . ?
H2TA C2T H2TB 109.1 . . ?
C4T C3T C2T 103.6(2) . . ?
C4T C3T H3TB 111.0 . . ?
C2T C3T H3TB 111.0 . . ?
C4T C3T H3TC 111.0 . . ?
C2T C3T H3TC 111.0 . . ?
H3TB C3T H3TC 109.0 . . ?
O1T C4T C3T 111.9(3) . . ?
O1T C4T H4TA 109.2 . . ?
C3T C4T H4TA 109.2 . . ?
O1T C4T H4TB 109.2 . . ?
C3T C4T H4TB 109.2 . . ?
H4TA C4T H4TB 107.9 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.062

loop_
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
? ? ?
y y y
y y y
y y y
y y y
y y y
y y y
y y y
y y y

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?

_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{2feb1263-a85e-4854-a189-22dbd8cae466} '_publcif_info_datablock.publ_exptl'
loop_
_publcif_info_cif.paper_type
?

_database_code_depnum_ccdc_archive 'CCDC 1002903'
