# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_p9
#TrackingRef 'compound4.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            compound4
_chemical_melting_point          ?
_chemical_formula_moiety         C37H48N1Ni1O1P2
_chemical_formula_sum            'C37 H48 N Ni O P2'
_chemical_formula_weight         643.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0021 0.0012 '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 0.0048 0.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0081 0.0047 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0832 0.0741 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3388 0.8985 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.292(3)
_cell_length_b                   9.6210(19)
_cell_length_c                   28.336(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.90(3)
_cell_angle_gamma                90.00
_cell_volume                     3346.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    103433
_cell_measurement_theta_min      0.36
_cell_measurement_theta_max      33.55

_exptl_crystal_description       platy
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1372
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'HKL3000 Scalepack'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.62998
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            53693
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         33.43
_reflns_number_total             14968
_reflns_number_gt                12719
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0951P)²+2.2381P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14968
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1672
_refine_ls_wR_factor_gt          0.1610
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.004

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
Ni Ni 0.244627(16) 0.711583(19) 0.369199(7) 0.01994(6) Uani 1 1 d . . .
P1 P 0.21943(3) 0.84100(3) 0.305009(13) 0.01713(7) Uani 1 1 d . . .
P2 P 0.21516(3) 0.52894(3) 0.415413(13) 0.01646(7) Uani 1 1 d . . .
N N 0.30162(10) 0.57170(12) 0.32642(5) 0.0201(2) Uani 1 1 d . . .
C9 C 0.35054(11) 0.45397(14) 0.34730(5) 0.0196(2) Uani 1 1 d . . .
C7 C 0.29258(12) 0.47645(15) 0.24445(6) 0.0218(2) Uani 1 1 d . . .
H7A H 0.3137 0.3861 0.2548 0.026 Uiso 1 1 calc R . .
C2 C 0.28385(10) 0.58417(13) 0.27807(5) 0.0176(2) Uani 1 1 d . . .
C3 C 0.24607(11) 0.71468(13) 0.26031(5) 0.0173(2) Uani 1 1 d . . .
C4 C 0.22534(12) 0.73559(16) 0.21192(5) 0.0215(2) Uani 1 1 d . . .
H4A H 0.2016 0.8245 0.2011 0.026 Uiso 1 1 calc R . .
C13 C 0.36741(12) 0.30467(15) 0.41728(6) 0.0229(3) Uani 1 1 d . . .
H13A H 0.3433 0.2806 0.4475 0.028 Uiso 1 1 calc R . .
C10 C 0.43586(12) 0.37681(16) 0.32858(6) 0.0235(3) Uani 1 1 d . . .
H10A H 0.4606 0.3998 0.2983 0.028 Uiso 1 1 calc R . .
C12 C 0.45132(12) 0.22818(16) 0.39831(7) 0.0258(3) Uani 1 1 d . . .
C14 C 0.31813(11) 0.41578(14) 0.39274(5) 0.0188(2) Uani 1 1 d . . .
C23 C 0.08531(11) 0.43226(15) 0.40604(6) 0.0213(2) Uani 1 1 d . . .
H23A H 0.0268 0.4889 0.4200 0.026 Uiso 1 1 calc R . .
C6 C 0.27089(12) 0.50039(17) 0.19651(6) 0.0241(3) Uani 1 1 d . . .
H6A H 0.2785 0.4258 0.1750 0.029 Uiso 1 1 calc R . .
C5 C 0.23842(11) 0.63004(18) 0.17897(5) 0.0234(3) Uani 1 1 d . . .
C17 C 0.32709(14) 0.97436(16) 0.30202(6) 0.0261(3) Uani 1 1 d . . .
H17A H 0.3182 1.0405 0.3288 0.031 Uiso 1 1 calc R . .
C22 C 0.05785(13) 0.42073(17) 0.35285(6) 0.0273(3) Uani 1 1 d . . .
H22A H -0.0107 0.3698 0.3475 0.041 Uiso 1 1 calc R . .
H22B H 0.1164 0.3710 0.3378 0.041 Uiso 1 1 calc R . .
H22C H 0.0503 0.5141 0.3392 0.041 Uiso 1 1 calc R . .
C36 C 0.19108(17) 0.2780(2) 0.59066(8) 0.0337(4) Uani 1 1 d . . .
C26 C 0.24302(13) 0.53452(17) 0.47996(5) 0.0237(3) Uani 1 1 d . . .
H26A H 0.2439 0.4370 0.4922 0.028 Uiso 1 1 calc R . .
C11 C 0.48423(12) 0.26738(17) 0.35391(7) 0.0262(3) Uani 1 1 d . . .
H11A H 0.5418 0.2176 0.3405 0.031 Uiso 1 1 calc R . .
C31 C 0.27234(16) 0.21620(19) 0.56394(7) 0.0314(3) Uani 1 1 d . . .
C20 C 0.09076(13) 0.92684(17) 0.28539(6) 0.0265(3) Uani 1 1 d . . .
H20A H 0.1001 0.9693 0.2536 0.032 Uiso 1 1 calc R . .
C24 C 0.08619(14) 0.28968(16) 0.43013(7) 0.0290(3) Uani 1 1 d . . .
H24A H 0.0156 0.2442 0.4239 0.043 Uiso 1 1 calc R . .
H24B H 0.0996 0.3015 0.4643 0.043 Uiso 1 1 calc R . .
H24C H 0.1439 0.2322 0.4177 0.043 Uiso 1 1 calc R . .
C16 C 0.43763(14) 0.9032(2) 0.31010(8) 0.0352(4) Uani 1 1 d . . .
H16A H 0.4958 0.9725 0.3086 0.053 Uiso 1 1 calc R . .
H16B H 0.4464 0.8326 0.2856 0.053 Uiso 1 1 calc R . .
H16C H 0.4416 0.8588 0.3413 0.053 Uiso 1 1 calc R . .
C27 C 0.15304(15) 0.6144(2) 0.50373(6) 0.0303(3) Uani 1 1 d . . .
H27A H 0.1690 0.6166 0.5380 0.046 Uiso 1 1 calc R . .
H27B H 0.0830 0.5681 0.4970 0.046 Uiso 1 1 calc R . .
H27C H 0.1496 0.7097 0.4915 0.046 Uiso 1 1 calc R . .
C21 C 0.06515(18) 1.0424(2) 0.32009(8) 0.0365(4) Uani 1 1 d . . .
H21A H -0.0032 1.0880 0.3097 0.055 Uiso 1 1 calc R . .
H21B H 0.1244 1.1107 0.3213 0.055 Uiso 1 1 calc R . .
H21C H 0.0578 1.0025 0.3516 0.055 Uiso 1 1 calc R . .
C15 C 0.50447(16) 0.10938(19) 0.42560(8) 0.0352(4) Uani 1 1 d . . .
H15A H 0.5613 0.0680 0.4070 0.053 Uiso 1 1 calc R . .
H15B H 0.4495 0.0389 0.4319 0.053 Uiso 1 1 calc R . .
H15C H 0.5371 0.1441 0.4556 0.053 Uiso 1 1 calc R . .
C1 C 0.25918(16) 0.85151(18) 0.40993(7) 0.0305(3) Uani 1 1 d . . .
C25 C 0.35433(15) 0.5995(2) 0.49187(7) 0.0352(4) Uani 1 1 d . . .
H25A H 0.3678 0.6017 0.5262 0.053 Uiso 1 1 calc R . .
H25B H 0.3557 0.6944 0.4794 0.053 Uiso 1 1 calc R . .
H25C H 0.4109 0.5440 0.4776 0.053 Uiso 1 1 calc R . .
C19 C -0.00186(14) 0.8201(2) 0.28098(8) 0.0361(4) Uani 1 1 d . . .
H19A H -0.0697 0.8669 0.2706 0.054 Uiso 1 1 calc R . .
H19B H -0.0109 0.7761 0.3117 0.054 Uiso 1 1 calc R . .
H19C H 0.0158 0.7490 0.2578 0.054 Uiso 1 1 calc R . .
C18 C 0.3242(2) 1.0593(2) 0.25643(8) 0.0409(5) Uani 1 1 d . . .
H18A H 0.3839 1.1269 0.2579 0.061 Uiso 1 1 calc R . .
H18B H 0.2544 1.1084 0.2527 0.061 Uiso 1 1 calc R . .
H18C H 0.3323 0.9970 0.2295 0.061 Uiso 1 1 calc R . .
C8 C 0.21387(15) 0.6547(2) 0.12722(6) 0.0341(4) Uani 1 1 d . . .
H8A H 0.2280 0.5695 0.1096 0.051 Uiso 1 1 calc R . .
H8B H 0.2604 0.7296 0.1163 0.051 Uiso 1 1 calc R . .
H8C H 0.1372 0.6812 0.1220 0.051 Uiso 1 1 calc R . .
O O 0.25176(18) 0.94514(19) 0.43473(7) 0.0523(5) Uani 1 1 d . . .
C32 C 0.24418(19) 0.1051(2) 0.53320(8) 0.0371(4) Uani 1 1 d . . .
H32A H 0.2978 0.0644 0.5145 0.044 Uiso 1 1 calc R . .
C30 C 0.38109(17) 0.2681(2) 0.56856(8) 0.0362(4) Uani 1 1 d . . .
H30A H 0.4365 0.2275 0.5509 0.043 Uiso 1 1 calc R . .
C35 C 0.08353(19) 0.2248(2) 0.58668(9) 0.0403(4) Uani 1 1 d . . .
H35A H 0.0286 0.2655 0.6046 0.048 Uiso 1 1 calc R . .
C37 C 0.2194(2) 0.3905(3) 0.62098(9) 0.0427(4) Uani 1 1 d . . .
H37A H 0.1653 0.4327 0.6390 0.051 Uiso 1 1 calc R . .
C34 C 0.05832(19) 0.1170(3) 0.55770(9) 0.0431(5) Uani 1 1 d . . .
H34A H -0.0140 0.0818 0.5557 0.052 Uiso 1 1 calc R . .
C33 C 0.1389(2) 0.0556(2) 0.53025(9) 0.0443(5) Uani 1 1 d . . .
H33A H 0.1202 -0.0198 0.5098 0.053 Uiso 1 1 calc R . .
C28 C 0.3234(2) 0.4386(3) 0.62442(9) 0.0464(5) Uani 1 1 d . . .
H28A H 0.3411 0.5151 0.6445 0.056 Uiso 1 1 calc R . .
C29 C 0.4054(2) 0.3762(3) 0.59847(9) 0.0437(5) Uani 1 1 d . . .
H29A H 0.4780 0.4097 0.6018 0.052 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni C1 1.7763(18) . ?
Ni N 1.9640(12) . ?
Ni P1 2.2131(5) . ?
Ni P2 2.2320(5) . ?
P1 C3 1.7973(14) . ?
P1 C20 1.8449(16) . ?
P1 C17 1.8483(16) . ?
P2 C14 1.8117(14) . ?
P2 C26 1.8446(16) . ?
P2 C23 1.8548(15) . ?
N C2 1.3817(19) . ?
N C9 1.3995(18) . ?
C9 C10 1.410(2) . ?
C9 C14 1.415(2) . ?
C7 C6 1.390(2) . ?
C7 C2 1.4154(19) . ?
C2 C3 1.4219(19) . ?
C3 C4 1.397(2) . ?
C4 C5 1.394(2) . ?
C13 C12 1.397(2) . ?
C13 C14 1.3968(19) . ?
C10 C11 1.391(2) . ?
C12 C11 1.393(3) . ?
C12 C15 1.510(2) . ?
C23 C22 1.532(2) . ?
C23 C24 1.532(2) . ?
C6 C5 1.394(2) . ?
C5 C8 1.501(2) . ?
C17 C18 1.528(3) . ?
C17 C16 1.529(3) . ?
C36 C37 1.414(3) . ?
C36 C31 1.415(3) . ?
C36 C35 1.417(3) . ?
C26 C25 1.526(2) . ?
C26 C27 1.531(2) . ?
C31 C32 1.411(3) . ?
C31 C30 1.427(3) . ?
C20 C21 1.527(2) . ?
C20 C19 1.534(3) . ?
C1 O 1.149(2) . ?
C32 C33 1.377(3) . ?
C30 C29 1.365(3) . ?
C35 C34 1.349(4) . ?
C37 C28 1.359(4) . ?
C34 C33 1.419(4) . ?
C28 C29 1.411(4) . ?

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 Ni N 153.25(8) . . ?
C1 Ni P1 96.48(6) . . ?
N Ni P1 85.28(4) . . ?
C1 Ni P2 103.27(6) . . ?
N Ni P2 84.04(4) . . ?
P1 Ni P2 154.825(17) . . ?
C3 P1 C20 105.92(7) . . ?
C3 P1 C17 106.31(7) . . ?
C20 P1 C17 106.28(8) . . ?
C3 P1 Ni 100.12(5) . . ?
C20 P1 Ni 125.57(6) . . ?
C17 P1 Ni 110.94(6) . . ?
C14 P2 C26 105.73(7) . . ?
C14 P2 C23 105.03(7) . . ?
C26 P2 C23 105.78(8) . . ?
C14 P2 Ni 97.35(5) . . ?
C26 P2 Ni 122.09(5) . . ?
C23 P2 Ni 118.35(5) . . ?
C2 N C9 122.17(12) . . ?
C2 N Ni 120.61(9) . . ?
C9 N Ni 116.92(10) . . ?
N C9 C10 125.38(14) . . ?
N C9 C14 117.38(12) . . ?
C10 C9 C14 117.02(13) . . ?
C6 C7 C2 121.26(14) . . ?
N C2 C7 126.18(13) . . ?
N C2 C3 117.38(11) . . ?
C7 C2 C3 116.30(13) . . ?
C4 C3 C2 120.98(12) . . ?
C4 C3 P1 124.32(11) . . ?
C2 C3 P1 114.57(10) . . ?
C5 C4 C3 122.08(14) . . ?
C12 C13 C14 121.45(15) . . ?
C11 C10 C9 120.74(15) . . ?
C11 C12 C13 117.31(14) . . ?
C11 C12 C15 121.98(15) . . ?
C13 C12 C15 120.70(17) . . ?
C13 C14 C9 121.11(13) . . ?
C13 C14 P2 125.20(12) . . ?
C9 C14 P2 113.61(10) . . ?
C22 C23 C24 111.71(14) . . ?
C22 C23 P2 108.81(11) . . ?
C24 C23 P2 113.49(11) . . ?
C7 C6 C5 122.29(13) . . ?
C6 C5 C4 116.98(14) . . ?
C6 C5 C8 122.00(15) . . ?
C4 C5 C8 120.97(16) . . ?
C18 C17 C16 110.44(17) . . ?
C18 C17 P1 115.07(14) . . ?
C16 C17 P1 108.38(11) . . ?
C37 C36 C31 119.2(2) . . ?
C37 C36 C35 121.6(2) . . ?
C31 C36 C35 119.1(2) . . ?
C25 C26 C27 110.90(15) . . ?
C25 C26 P2 110.52(12) . . ?
C27 C26 P2 110.42(11) . . ?
C10 C11 C12 122.35(14) . . ?
C32 C31 C36 119.41(19) . . ?
C32 C31 C30 121.4(2) . . ?
C36 C31 C30 119.17(19) . . ?
C21 C20 C19 111.32(16) . . ?
C21 C20 P1 109.47(13) . . ?
C19 C20 P1 110.26(12) . . ?
O C1 Ni 169.4(2) . . ?
C33 C32 C31 120.0(2) . . ?
C29 C30 C31 119.9(2) . . ?
C34 C35 C36 120.7(2) . . ?
C28 C37 C36 120.4(2) . . ?
C35 C34 C33 120.5(2) . . ?
C32 C33 C34 120.2(2) . . ?
C37 C28 C29 120.8(2) . . ?
C30 C29 C28 120.5(2) . . ?

_diffrn_measured_fraction_theta_max 0.798
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         2.774
_refine_diff_density_min         -2.284
_refine_diff_density_rms         0.095


_database_code_depnum_ccdc_archive 'CCDC 918046'
#######################################################################
#
#                 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_cdoxams
#TrackingRef '16624_web_deposit_cif_file_1_R.Selvakumar_1357376739.cdoxams.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H9 Cd N6 O9'
_chemical_formula_weight         397.57

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'
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.6999(5)
_cell_length_b                   9.4421(4)
_cell_length_c                   11.2283(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.9350(10)
_cell_angle_gamma                90.00
_cell_volume                     1073.00(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8558
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      32.59

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7864
_exptl_absorpt_correction_T_max  0.7864
_exptl_absorpt_process_details   'Bruker Sadabs'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13540
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         32.59
_reflns_number_total             3776
_reflns_number_gt                3605
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0780P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3776
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0204
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0735
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_restrained_S_all      0.831
_refine_ls_shift/su_max          0.007
_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
Cd Cd 0.224201(9) 0.153852(9) -0.322449(8) 0.01147(6) Uani 1 1 d . . .
C1 C 0.08056(14) -0.03696(14) -0.22638(13) 0.0136(2) Uani 1 1 d . . .
N1 N 0.01918(15) -0.15005(11) -0.06087(14) 0.0143(3) Uani 1 1 d . . .
H1 H 0.095(3) -0.119(3) -0.008(3) 0.031(6) Uiso 1 1 d . . .
O1 O 0.17379(10) 0.02069(11) -0.14244(10) 0.01603(19) Uani 1 1 d . . .
C2 C -0.01491(14) -0.13149(14) -0.18476(13) 0.0121(2) Uani 1 1 d . . .
O2 O 0.05550(12) -0.02083(12) -0.34253(10) 0.0193(2) Uani 1 1 d . . .
N2 N -0.06230(12) -0.23187(13) -0.01093(11) 0.0146(2) Uani 1 1 d . . .
H2A H -0.087(3) -0.182(2) 0.040(2) 0.030(6) Uiso 1 1 d . . .
H2B H -0.015(2) -0.295(3) 0.044(2) 0.027(5) Uiso 1 1 d . . .
O3 O -0.11570(11) -0.18173(12) -0.26260(10) 0.01581(19) Uani 1 1 d . . .
C3 C 0.45031(17) 0.33203(15) -0.20794(17) 0.0142(3) Uani 1 1 d . . .
N3 N 0.62681(12) 0.44749(13) -0.04564(12) 0.0154(2) Uani 1 1 d . . .
H3 H 0.592(3) 0.406(3) 0.016(3) 0.049(7) Uiso 1 1 d . . .
C4 C 0.57268(13) 0.42814(14) -0.16853(12) 0.0132(2) Uani 1 1 d . . .
O4 O 0.38241(12) 0.33264(11) -0.32204(11) 0.0184(2) Uani 1 1 d . . .
N4 N 0.73446(13) 0.54113(14) -0.00168(12) 0.0172(2) Uani 1 1 d . . .
H4A H 0.717(2) 0.608(2) 0.046(2) 0.019(5) Uiso 1 1 d . . .
H4B H 0.805(3) 0.479(3) 0.041(3) 0.043(7) Uiso 1 1 d . . .
O5 O 0.42396(11) 0.26148(11) -0.12405(11) 0.0180(2) Uani 1 1 d . . .
N5 N 0.44093(12) -0.01927(14) 0.01315(11) 0.0166(2) Uani 1 1 d . . .
H5A H 0.3747(19) -0.0204(19) -0.0567(19) 0.012(4) Uiso 1 1 d . . .
H5B H 0.466(2) -0.113(3) 0.050(2) 0.026(5) Uiso 1 1 d . . .
H5C H 0.430(2) 0.050(2) 0.077(2) 0.029(6) Uiso 1 1 d . . .
N6 N 0.27260(15) 0.65170(12) -0.26861(14) 0.0184(3) Uani 1 1 d . . .
O6 O 0.61219(10) 0.48453(12) -0.24889(10) 0.01648(19) Uani 1 1 d . . .
O11 O 0.38275(15) 0.65039(13) -0.18369(14) 0.0294(3) Uani 1 1 d . . .
O12 O 0.16761(17) 0.65294(13) -0.24308(18) 0.0291(3) Uani 1 1 d . . .
O13 O 0.27017(16) 0.65231(14) -0.38109(15) 0.0288(4) 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
Cd O6 2.3135(10) 2_644 ?
Cd O3 2.3215(11) 2_554 ?
Cd N2 2.3584(12) 2_554 ?
Cd O4 2.3897(12) . ?
Cd O2 2.4012(11) . ?
Cd N4 2.4072(13) 2_644 ?
Cd O1 2.5816(11) . ?
C1 O2 1.2526(17) . ?
C1 O1 1.2528(17) . ?
C1 C2 1.539(2) . ?
N1 C2 1.330(2) . ?
N1 N2 1.4102(18) . ?
N1 H1 0.89(3) . ?
C2 O3 1.2411(17) . ?
N2 Cd 2.3584(12) 2_544 ?
N2 H2A 0.85(3) . ?
N2 H2B 0.89(3) . ?
O3 Cd 2.3215(11) 2_544 ?
C3 O4 1.251(2) . ?
C3 O5 1.2582(19) . ?
C3 C4 1.535(2) . ?
N3 C4 1.3245(17) . ?
N3 N4 1.4083(17) . ?
N3 H3 0.97(3) . ?
C4 O6 1.2344(16) . ?
N4 Cd 2.4072(13) 2_654 ?
N4 H4A 0.89(2) . ?
N4 H4B 0.95(3) . ?
N5 N5 1.435(2) 3_655 ?
N5 H5A 0.870(19) . ?
N5 H5B 0.97(2) . ?
N5 H5C 1.00(2) . ?
N6 O12 1.246(2) . ?
N6 O11 1.253(2) . ?
N6 O13 1.255(2) . ?
O6 Cd 2.3135(10) 2_654 ?

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
O6 Cd O3 137.98(4) 2_644 2_554 ?
O6 Cd N2 150.38(4) 2_644 2_554 ?
O3 Cd N2 71.56(4) 2_554 2_554 ?
O6 Cd O4 91.81(4) 2_644 . ?
O3 Cd O4 88.58(4) 2_554 . ?
N2 Cd O4 90.91(4) 2_554 . ?
O6 Cd O2 91.10(4) 2_644 . ?
O3 Cd O2 92.12(4) 2_554 . ?
N2 Cd O2 84.46(4) 2_554 . ?
O4 Cd O2 174.83(4) . . ?
O6 Cd N4 70.04(4) 2_644 2_644 ?
O3 Cd N4 151.97(4) 2_554 2_644 ?
N2 Cd N4 80.49(4) 2_554 2_644 ?
O4 Cd N4 89.73(4) . 2_644 ?
O2 Cd N4 87.24(4) . 2_644 ?
O6 Cd O1 73.70(4) 2_644 . ?
O3 Cd O1 75.18(4) 2_554 . ?
N2 Cd O1 123.89(4) 2_554 . ?
O4 Cd O1 132.10(4) . . ?
O2 Cd O1 52.93(4) . . ?
N4 Cd O1 124.58(4) 2_644 . ?
O2 C1 O1 125.43(13) . . ?
O2 C1 C2 116.59(12) . . ?
O1 C1 C2 117.93(12) . . ?
C2 N1 N2 119.52(13) . . ?
C2 N1 H1 122.6(17) . . ?
N2 N1 H1 117.7(17) . . ?
C1 O1 Cd 86.57(8) . . ?
O3 C2 N1 124.53(14) . . ?
O3 C2 C1 121.24(12) . . ?
N1 C2 C1 114.21(12) . . ?
C1 O2 Cd 94.89(9) . . ?
N1 N2 Cd 108.97(9) . 2_544 ?
N1 N2 H2A 109.4(16) . . ?
Cd N2 H2A 118.5(17) 2_544 . ?
N1 N2 H2B 110.7(16) . . ?
Cd N2 H2B 110.7(16) 2_544 . ?
H2A N2 H2B 98(2) . . ?
C2 O3 Cd 113.72(9) . 2_544 ?
O4 C3 O5 124.92(15) . . ?
O4 C3 C4 116.74(14) . . ?
O5 C3 C4 118.32(14) . . ?
C4 N3 N4 118.89(12) . . ?
C4 N3 H3 123.4(17) . . ?
N4 N3 H3 117.5(17) . . ?
O6 C4 N3 124.35(13) . . ?
O6 C4 C3 120.43(12) . . ?
N3 C4 C3 115.18(12) . . ?
C3 O4 Cd 100.04(10) . . ?
N3 N4 Cd 109.71(9) . 2_654 ?
N3 N4 H4A 110.5(14) . . ?
Cd N4 H4A 108.2(14) 2_654 . ?
N3 N4 H4B 102.3(15) . . ?
Cd N4 H4B 111.1(17) 2_654 . ?
H4A N4 H4B 115(2) . . ?
N5 N5 H5A 109.4(13) 3_655 . ?
N5 N5 H5B 99.9(13) 3_655 . ?
H5A N5 H5B 113.7(19) . . ?
N5 N5 H5C 107.2(13) 3_655 . ?
H5A N5 H5C 113.7(18) . . ?
H5B N5 H5C 111.8(19) . . ?
O12 N6 O11 121.38(17) . . ?
O12 N6 O13 120.37(16) . . ?
O11 N6 O13 118.25(16) . . ?
C4 O6 Cd 116.43(9) . 2_654 ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        32.59
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         1.364
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.111
_database_code_depnum_ccdc_archive 'CCDC 918074'
#######################################################################
#
#                 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_0080a-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PNP)NiCOMe
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H49 N Ni O P2'
_chemical_formula_sum            'C34 H49 N Ni O P2'
_chemical_formula_weight         608.39

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   P21/c

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

_cell_length_a                   12.4045(4)
_cell_length_b                   9.6520(3)
_cell_length_c                   27.5625(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.7220(18)
_cell_angle_gamma                90.00
_cell_volume                     3296.29(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    79681
_cell_measurement_theta_min      1.48
_cell_measurement_theta_max      35.25

_exptl_crystal_description       platy
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_T_max  0.9008
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            79681
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.48
_diffrn_reflns_theta_max         35.25
_reflns_number_total             12412
_reflns_number_gt                9067
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0627P)²+0.5704P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12412
_refine_ls_number_parameters     407
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1196
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.003
_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 0.774502(15) 0.299818(18) 0.132609(6) 0.01633(6) Uani 1 1 d . . .
P1 P 0.77905(3) 0.16219(4) 0.195296(13) 0.01773(8) Uani 1 1 d . . .
P2 P 0.77904(3) 0.47044(4) 0.081692(12) 0.01641(8) Uani 1 1 d . . .
N1 N 0.70391(10) 0.43227(12) 0.17452(4) 0.0178(2) Uani 1 1 d . . .
C11 C 0.67909(12) 0.58462(14) 0.10605(5) 0.0180(3) Uani 1 1 d . . .
C4 C 0.75651(12) 0.28842(14) 0.24245(5) 0.0184(3) Uani 1 1 d . . .
C15 C 0.56564(12) 0.62111(15) 0.17325(5) 0.0213(3) Uani 1 1 d . . .
H15A H 0.5422 0.5969 0.2045 0.026 Uiso 1 1 calc R . .
C10 C 0.65106(12) 0.54639(14) 0.15344(5) 0.0178(3) Uani 1 1 d . . .
C3 C 0.71966(12) 0.41831(14) 0.22460(5) 0.0174(3) Uani 1 1 d . . .
C12 C 0.62838(13) 0.69471(14) 0.08140(5) 0.0213(3) Uani 1 1 d . . .
H12A H 0.6504 0.7188 0.0500 0.026 Uiso 1 1 calc R . .
C1 C 0.84302(15) 0.17733(16) 0.09177(5) 0.0254(3) Uani 1 1 d . . .
C5 C 0.77946(13) 0.26706(16) 0.29199(5) 0.0217(3) Uani 1 1 d . . .
H5A H 0.8034 0.1783 0.3028 0.026 Uiso 1 1 calc R . .
C14 C 0.51536(13) 0.72946(16) 0.14780(6) 0.0238(3) Uani 1 1 d . . .
H14A H 0.4581 0.7775 0.1621 0.029 Uiso 1 1 calc R . .
C7 C 0.73368(13) 0.50089(17) 0.30832(5) 0.0235(3) Uani 1 1 d . . .
H7A H 0.7261 0.5749 0.3306 0.028 Uiso 1 1 calc R . .
C26 C 0.74745(13) 0.46426(15) 0.01577(5) 0.0214(3) Uani 1 1 d . . .
H26A H 0.7417 0.5619 0.0038 0.026 Uiso 1 1 calc R . .
C8 C 0.70982(13) 0.52508(15) 0.25933(5) 0.0215(3) Uani 1 1 d . . .
H8A H 0.6866 0.6145 0.2490 0.026 Uiso 1 1 calc R . .
O1 O 0.94001(12) 0.17950(15) 0.08537(5) 0.0415(3) Uani 1 1 d . . .
C13 C 0.54633(13) 0.76993(15) 0.10181(6) 0.0232(3) Uani 1 1 d . . .
C23 C 0.91100(12) 0.55876(15) 0.08889(5) 0.0212(3) Uani 1 1 d . . .
H23A H 0.9653 0.4990 0.0733 0.025 Uiso 1 1 calc R . .
C6 C 0.76815(13) 0.37271(17) 0.32597(5) 0.0236(3) Uani 1 1 d . . .
C17 C 0.66766(14) 0.03594(16) 0.19739(5) 0.0255(3) Uani 1 1 d . . .
H17A H 0.6775 -0.0336 0.1711 0.031 Uiso 1 1 calc R . .
C24 C 0.91236(15) 0.70064(16) 0.06393(7) 0.0287(3) Uani 1 1 d . . .
H24A H 0.9841 0.7423 0.0689 0.043 Uiso 1 1 calc R . .
H24B H 0.8584 0.7611 0.0779 0.043 Uiso 1 1 calc R . .
H24C H 0.8955 0.6892 0.0291 0.043 Uiso 1 1 calc R . .
C27 C 0.63795(15) 0.39478(18) 0.00542(6) 0.0301(4) Uani 1 1 d . . .
H27A H 0.6218 0.3923 -0.0297 0.045 Uiso 1 1 calc R . .
H27B H 0.5818 0.4475 0.0212 0.045 Uiso 1 1 calc R . .
H27C H 0.6401 0.3000 0.0182 0.045 Uiso 1 1 calc R . .
C18 C 0.56141(15) 0.1111(2) 0.18595(7) 0.0345(4) Uani 1 1 d . . .
H18A H 0.5016 0.0451 0.1869 0.052 Uiso 1 1 calc R . .
H18B H 0.5626 0.1526 0.1535 0.052 Uiso 1 1 calc R . .
H18C H 0.5518 0.1841 0.2101 0.052 Uiso 1 1 calc R . .
C2 C 0.77285(19) 0.07035(18) 0.06568(7) 0.0402(5) Uani 1 1 d . . .
H2A H 0.8175 0.0123 0.0454 0.060 Uiso 1 1 calc R . .
H2B H 0.7174 0.1171 0.0451 0.060 Uiso 1 1 calc R . .
H2C H 0.7381 0.0122 0.0896 0.060 Uiso 1 1 calc R . .
C25 C 0.94493(15) 0.56977(18) 0.14299(6) 0.0305(4) Uani 1 1 d . . .
H25A H 1.0150 0.6165 0.1467 0.046 Uiso 1 1 calc R . .
H25B H 0.9507 0.4767 0.1571 0.046 Uiso 1 1 calc R . .
H25C H 0.8908 0.6231 0.1598 0.046 Uiso 1 1 calc R . .
C20 C 0.90407(15) 0.07075(18) 0.21484(6) 0.0302(4) Uani 1 1 d . . .
H20A H 0.8972 0.0399 0.2492 0.036 Uiso 1 1 calc R . .
C28 C 0.83680(15) 0.39325(18) -0.01141(5) 0.0303(4) Uani 1 1 d . . .
H28A H 0.8172 0.3921 -0.0463 0.045 Uiso 1 1 calc R . .
H28B H 0.8459 0.2980 0.0004 0.045 Uiso 1 1 calc R . .
H28C H 0.9046 0.4442 -0.0057 0.045 Uiso 1 1 calc R . .
C16 C 0.49171(15) 0.88886(17) 0.07462(7) 0.0316(4) Uani 1 1 d . . .
H16A H 0.5246 0.9012 0.0433 0.047 Uiso 1 1 calc R . .
H16B H 0.5005 0.9740 0.0938 0.047 Uiso 1 1 calc R . .
H16C H 0.4147 0.8684 0.0692 0.047 Uiso 1 1 calc R . .
C21 C 0.92204(18) -0.05872(19) 0.18345(7) 0.0404(5) Uani 1 1 d . . .
H21A H 0.9889 -0.1051 0.1948 0.061 Uiso 1 1 calc R . .
H21B H 0.9276 -0.0310 0.1495 0.061 Uiso 1 1 calc R . .
H21C H 0.8611 -0.1224 0.1861 0.061 Uiso 1 1 calc R . .
C9 C 0.79686(17) 0.3490(2) 0.37905(6) 0.0369(4) Uani 1 1 d . . .
H9A H 0.7837 0.4340 0.3973 0.055 Uiso 1 1 calc R . .
H9B H 0.8732 0.3236 0.3832 0.055 Uiso 1 1 calc R . .
H9C H 0.7523 0.2740 0.3912 0.055 Uiso 1 1 calc R . .
C19 C 0.66415(18) -0.04319(19) 0.24557(6) 0.0379(4) Uani 1 1 d . . .
H19A H 0.6034 -0.1082 0.2440 0.057 Uiso 1 1 calc R . .
H19B H 0.6551 0.0226 0.2721 0.057 Uiso 1 1 calc R . .
H19C H 0.7317 -0.0945 0.2514 0.057 Uiso 1 1 calc R . .
C22 C 0.99946(16) 0.1705(2) 0.21351(8) 0.0423(5) Uani 1 1 d . . .
H22A H 1.0660 0.1219 0.2239 0.064 Uiso 1 1 calc R . .
H22B H 0.9879 0.2486 0.2354 0.064 Uiso 1 1 calc R . .
H22C H 1.0058 0.2051 0.1803 0.064 Uiso 1 1 calc R . .
C29A C 0.303(2) 0.178(2) 0.0519(8) 0.0289(18) Uani 0.49(3) 1 d P A 1
H29A H 0.3116 0.1041 0.0297 0.035 Uiso 0.49(3) 1 calc PR A 1
C30A C 0.3927(11) 0.2565(19) 0.0697(7) 0.040(4) Uani 0.49(3) 1 d P A 1
H30A H 0.4626 0.2397 0.0583 0.048 Uiso 0.49(3) 1 calc PR A 1
C31A C 0.3773(16) 0.3525(18) 0.1022(7) 0.080(5) Uani 0.49(3) 1 d P A 1
H31A H 0.4385 0.3986 0.1166 0.096 Uiso 0.49(3) 1 calc PR A 1
C32A C 0.2734(17) 0.3904(15) 0.1168(4) 0.058(4) Uani 0.49(3) 1 d P A 1
H32A H 0.2650 0.4679 0.1376 0.069 Uiso 0.49(3) 1 calc PR A 1
C33A C 0.1850(15) 0.3152(18) 0.1009(6) 0.048(3) Uani 0.49(3) 1 d P A 1
H33A H 0.1154 0.3334 0.1124 0.057 Uiso 0.49(3) 1 calc PR A 1
C34A C 0.2016(15) 0.2111(15) 0.0673(5) 0.038(2) Uani 0.49(3) 1 d P A 1
H34A H 0.1410 0.1606 0.0545 0.046 Uiso 0.49(3) 1 calc PR A 1
C29B C 0.285(2) 0.194(2) 0.0569(9) 0.041(4) Uani 0.51(3) 1 d P A 2
H29B H 0.2743 0.1206 0.0344 0.049 Uiso 0.51(3) 1 calc PR A 2
C30B C 0.3847(12) 0.2444(18) 0.0645(7) 0.043(3) Uani 0.51(3) 1 d P A 2
H30B H 0.4440 0.2033 0.0493 0.051 Uiso 0.51(3) 1 calc PR A 2
C31B C 0.4010(9) 0.3651(10) 0.0971(3) 0.0321(16) Uani 0.51(3) 1 d P A 2
H31B H 0.4695 0.4082 0.1020 0.039 Uiso 0.51(3) 1 calc PR A 2
C32B C 0.3136(13) 0.4108(15) 0.1196(4) 0.046(2) Uani 0.51(3) 1 d P A 2
H32B H 0.3207 0.4843 0.1425 0.055 Uiso 0.51(3) 1 calc PR A 2
C33B C 0.2140(11) 0.3512(19) 0.1096(6) 0.052(4) Uani 0.51(3) 1 d P A 2
H33B H 0.1530 0.3883 0.1246 0.063 Uiso 0.51(3) 1 calc PR A 2
C34B C 0.1999(11) 0.2424(17) 0.0793(6) 0.046(3) Uani 0.51(3) 1 d P A 2
H34B H 0.1308 0.2011 0.0741 0.055 Uiso 0.51(3) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.8649(15) . ?
Ni1 N1 1.9575(11) . ?
Ni1 P2 2.1662(4) . ?
Ni1 P1 2.1780(4) . ?
P1 C4 1.8129(14) . ?
P1 C20 1.8425(17) . ?
P1 C17 1.8453(16) . ?
P2 C11 1.8115(14) . ?
P2 C26 1.8415(14) . ?
P2 C23 1.8479(16) . ?
N1 C3 1.3913(17) . ?
N1 C10 1.3945(18) . ?
C11 C12 1.395(2) . ?
C11 C10 1.4164(19) . ?
C4 C5 1.3968(19) . ?
C4 C3 1.4148(19) . ?
C15 C14 1.390(2) . ?
C15 C10 1.413(2) . ?
C3 C8 1.4158(19) . ?
C12 C13 1.391(2) . ?
C1 O1 1.225(2) . ?
C1 C2 1.510(2) . ?
C5 C6 1.396(2) . ?
C14 C13 1.397(2) . ?
C7 C8 1.388(2) . ?
C7 C6 1.389(2) . ?
C26 C28 1.529(2) . ?
C26 C27 1.529(2) . ?
C13 C16 1.513(2) . ?
C23 C24 1.533(2) . ?
C23 C25 1.534(2) . ?
C6 C9 1.507(2) . ?
C17 C18 1.524(3) . ?
C17 C19 1.534(2) . ?
C20 C22 1.527(3) . ?
C20 C21 1.542(2) . ?
C29A C34A 1.38(2) . ?
C29A C30A 1.42(3) . ?
C30A C31A 1.31(2) . ?
C31A C32A 1.42(2) . ?
C32A C33A 1.370(12) . ?
C33A C34A 1.389(16) . ?
C29B C34B 1.332(18) . ?
C29B C30B 1.33(3) . ?
C30B C31B 1.48(2) . ?
C31B C32B 1.348(17) . ?
C32B C33B 1.379(11) . ?
C33B C34B 1.347(15) . ?

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 N1 178.57(6) . . ?
C1 Ni1 P2 93.69(5) . . ?
N1 Ni1 P2 84.95(4) . . ?
C1 Ni1 P1 95.55(5) . . ?
N1 Ni1 P1 85.73(4) . . ?
P2 Ni1 P1 167.724(16) . . ?
C4 P1 C20 105.59(7) . . ?
C4 P1 C17 106.27(7) . . ?
C20 P1 C17 107.19(8) . . ?
C4 P1 Ni1 99.20(5) . . ?
C20 P1 Ni1 120.92(6) . . ?
C17 P1 Ni1 115.87(5) . . ?
C11 P2 C26 105.55(7) . . ?
C11 P2 C23 107.33(7) . . ?
C26 P2 C23 105.47(7) . . ?
C11 P2 Ni1 100.55(5) . . ?
C26 P2 Ni1 127.14(5) . . ?
C23 P2 Ni1 109.35(5) . . ?
C3 N1 C10 122.07(11) . . ?
C3 N1 Ni1 118.46(9) . . ?
C10 N1 Ni1 118.98(9) . . ?
C12 C11 C10 121.51(13) . . ?
C12 C11 P2 125.72(11) . . ?
C10 C11 P2 112.68(10) . . ?
C5 C4 C3 121.22(13) . . ?
C5 C4 P1 124.78(11) . . ?
C3 C4 P1 113.86(10) . . ?
C14 C15 C10 121.03(14) . . ?
N1 C10 C15 126.04(13) . . ?
N1 C10 C11 117.32(12) . . ?
C15 C10 C11 116.42(13) . . ?
N1 C3 C4 117.30(12) . . ?
N1 C3 C8 126.00(13) . . ?
C4 C3 C8 116.53(12) . . ?
C13 C12 C11 121.51(14) . . ?
O1 C1 C2 119.40(16) . . ?
O1 C1 Ni1 123.73(14) . . ?
C2 C1 Ni1 116.87(14) . . ?
C6 C5 C4 121.71(14) . . ?
C15 C14 C13 122.13(14) . . ?
C8 C7 C6 122.56(14) . . ?
C28 C26 C27 111.72(13) . . ?
C28 C26 P2 111.87(11) . . ?
C27 C26 P2 110.10(10) . . ?
C7 C8 C3 120.93(14) . . ?
C12 C13 C14 117.32(14) . . ?
C12 C13 C16 120.98(15) . . ?
C14 C13 C16 121.69(15) . . ?
C24 C23 C25 111.47(13) . . ?
C24 C23 P2 113.11(11) . . ?
C25 C23 P2 109.71(11) . . ?
C7 C6 C5 117.05(13) . . ?
C7 C6 C9 121.99(14) . . ?
C5 C6 C9 120.91(15) . . ?
C18 C17 C19 110.86(14) . . ?
C18 C17 P1 108.69(11) . . ?
C19 C17 P1 114.07(12) . . ?
C22 C20 C21 111.38(16) . . ?
C22 C20 P1 109.47(12) . . ?
C21 C20 P1 111.48(13) . . ?
C34A C29A C30A 118.8(17) . . ?
C31A C30A C29A 118.5(13) . . ?
C30A C31A C32A 122.8(12) . . ?
C33A C32A C31A 119.8(12) . . ?
C32A C33A C34A 117.1(15) . . ?
C29A C34A C33A 122.6(18) . . ?
C34B C29B C30B 123(2) . . ?
C29B C30B C31B 118.6(13) . . ?
C32B C31B C30B 116.5(10) . . ?
C31B C32B C33B 120.3(12) . . ?
C34B C33B C32B 122.6(14) . . ?
C29B C34B C33B 118.4(17) . . ?

_diffrn_measured_fraction_theta_max 0.839
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.111
_database_code_depnum_ccdc_archive 'CCDC 996897'
#######################################################################
#
#                 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_n0077a-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PNP)NiMe
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H43 N Ni P2, C4 H8 O'
_chemical_formula_sum            'C31 H51 N Ni O P2'
_chemical_formula_weight         574.38

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   19.2355(9)
_cell_length_b                   11.6533(5)
_cell_length_c                   14.8149(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.899(2)
_cell_angle_gamma                90.00
_cell_volume                     3102.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    57586
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      26.37

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6959
_exptl_absorpt_correction_T_max  0.8521
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            57586
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0119
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.77
_diffrn_reflns_theta_max         26.37
_reflns_number_total             6343
_reflns_number_gt                5814
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0595P)²+2.5723P] 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         6343
_refine_ls_number_parameters     382
_refine_ls_number_restraints     111
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1158
_refine_ls_wR_factor_gt          0.1003
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_restrained_S_all      1.171
_refine_ls_shift/su_max          0.049
_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 0.828033(13) 0.55741(2) 0.797878(19) 0.02157(10) Uani 1 1 d U . .
P1 P 0.89185(3) 0.40391(4) 0.79423(4) 0.01908(12) Uani 1 1 d U . .
P2 P 0.75028(3) 0.68973(4) 0.80171(4) 0.01952(12) Uani 1 1 d U . .
N1 N 0.74755(9) 0.45028(14) 0.78594(13) 0.0224(3) Uani 1 1 d U . .
C1 C 0.90746(12) 0.67134(18) 0.80340(19) 0.0307(5) Uani 1 1 d U . .
H1A H 0.9360 0.6433 0.7648 0.046 Uiso 1 1 calc R . .
H1B H 0.9408 0.6814 0.8706 0.046 Uiso 1 1 calc R . .
H1C H 0.8844 0.7451 0.7775 0.046 Uiso 1 1 calc R . .
C2 C 0.81603(10) 0.30586(16) 0.73807(14) 0.0207(4) Uani 1 1 d U . .
C3 C 0.82072(10) 0.20464(16) 0.69052(14) 0.0217(4) Uani 1 1 d U . .
H3A H 0.8679 0.1803 0.6905 0.026 Uiso 1 1 calc R . .
C4 C 0.75825(11) 0.13821(17) 0.64306(14) 0.0233(4) Uani 1 1 d U . .
C5 C 0.69078(11) 0.17705(19) 0.64603(17) 0.0295(5) Uani 1 1 d U . .
H5A H 0.6472 0.1333 0.6143 0.035 Uiso 1 1 calc R . .
C6 C 0.68440(11) 0.27684(19) 0.69334(17) 0.0300(5) Uani 1 1 d U . .
H6A H 0.6370 0.2996 0.6933 0.036 Uiso 1 1 calc R . .
C7 C 0.74725(10) 0.34504(17) 0.74158(15) 0.0223(4) Uani 1 1 d U . .
C8 C 0.76380(12) 0.03166(18) 0.58853(16) 0.0280(4) Uani 1 1 d U . .
H8A H 0.7172 -0.0117 0.5711 0.042 Uiso 1 1 calc R . .
H8B H 0.8050 -0.0160 0.6293 0.042 Uiso 1 1 calc R . .
H8C H 0.7728 0.0533 0.5297 0.042 Uiso 1 1 calc R . .
C9 C 0.67938(10) 0.60451(17) 0.82356(14) 0.0208(4) Uani 1 1 d U . .
C10 C 0.62231(11) 0.64617(18) 0.85161(15) 0.0247(4) Uani 1 1 d U . .
H10A H 0.6170 0.7267 0.8566 0.030 Uiso 1 1 calc R . .
C11 C 0.57304(11) 0.57325(19) 0.87251(15) 0.0266(4) Uani 1 1 d U . .
C12 C 0.58432(11) 0.45559(18) 0.86724(16) 0.0263(4) Uani 1 1 d U . .
H12A H 0.5526 0.4038 0.8837 0.032 Uiso 1 1 calc R . .
C13 C 0.64033(11) 0.41173(19) 0.83867(16) 0.0267(4) Uani 1 1 d U . .
H13A H 0.6462 0.3310 0.8361 0.032 Uiso 1 1 calc R . .
C14 C 0.68856(10) 0.48549(17) 0.81350(14) 0.0210(4) Uani 1 1 d U . .
C15 C 0.50885(13) 0.6188(2) 0.8983(2) 0.0380(5) Uani 1 1 d U . .
H15A H 0.5206 0.6963 0.9249 0.057 Uiso 1 1 calc R . .
H15B H 0.5005 0.5684 0.9464 0.057 Uiso 1 1 calc R . .
H15C H 0.4638 0.6211 0.8402 0.057 Uiso 1 1 calc R . .
C16 C 0.89877(14) 0.3491(2) 0.97865(17) 0.0385(5) Uani 1 1 d U . .
H16A H 0.8528 0.3048 0.9499 0.058 Uiso 1 1 calc R . .
H16B H 0.8864 0.4296 0.9850 0.058 Uiso 1 1 calc R . .
H16C H 0.9273 0.3180 1.0426 0.058 Uiso 1 1 calc R . .
C17 C 0.94524(11) 0.34126(18) 0.91377(14) 0.0254(4) Uani 1 1 d U . .
H17A H 0.9907 0.3894 0.9437 0.031 Uiso 1 1 calc R . .
C18 C 0.97081(13) 0.2179(2) 0.90864(17) 0.0337(5) Uani 1 1 d U . .
H18A H 1.0003 0.1911 0.9738 0.051 Uiso 1 1 calc R . .
H18B H 1.0013 0.2153 0.8680 0.051 Uiso 1 1 calc R . .
H18C H 0.9272 0.1683 0.8808 0.051 Uiso 1 1 calc R . .
C19 C 0.91488(14) 0.4428(2) 0.62341(17) 0.0338(5) Uani 1 1 d U . .
H19A H 0.9062 0.5247 0.6299 0.051 Uiso 1 1 calc R . .
H19B H 0.8671 0.4041 0.5914 0.051 Uiso 1 1 calc R . .
H19C H 0.9465 0.4329 0.5847 0.051 Uiso 1 1 calc R . .
C20 C 0.95331(11) 0.39087(17) 0.72308(14) 0.0230(4) Uani 1 1 d U . .
H20A H 0.9609 0.3073 0.7144 0.028 Uiso 1 1 calc R . .
C21 C 1.03009(12) 0.4449(2) 0.77472(19) 0.0327(5) Uani 1 1 d U . .
H21A H 1.0596 0.4401 0.7329 0.049 Uiso 1 1 calc R . .
H21B H 1.0556 0.4036 0.8351 0.049 Uiso 1 1 calc R . .
H21C H 1.0240 0.5256 0.7891 0.049 Uiso 1 1 calc R . .
C22 C 0.68153(15) 0.6715(2) 0.60482(17) 0.0401(6) Uani 1 1 d U . .
H22A H 0.6430 0.6224 0.6134 0.060 Uiso 1 1 calc R . .
H22B H 0.7246 0.6246 0.6080 0.060 Uiso 1 1 calc R . .
H22C H 0.6617 0.7096 0.5418 0.060 Uiso 1 1 calc R . .
C23 C 0.70523(12) 0.76185(19) 0.68460(15) 0.0271(4) Uani 1 1 d U . .
H23A H 0.7439 0.8109 0.6729 0.033 Uiso 1 1 calc R . .
C24 C 0.64045(14) 0.8405(2) 0.68015(18) 0.0381(5) Uani 1 1 d U . .
H24A H 0.6228 0.8809 0.6181 0.057 Uiso 1 1 calc R . .
H24B H 0.6572 0.8964 0.7329 0.057 Uiso 1 1 calc R . .
H24C H 0.5998 0.7944 0.6866 0.057 Uiso 1 1 calc R . .
C25 C 0.81639(13) 0.7459(2) 0.99301(16) 0.0339(5) Uani 1 1 d U . .
H25A H 0.8637 0.7157 0.9923 0.051 Uiso 1 1 calc R . .
H25B H 0.7868 0.6831 1.0048 0.051 Uiso 1 1 calc R . .
H25C H 0.8261 0.8033 1.0444 0.051 Uiso 1 1 calc R . .
C26 C 0.77335(11) 0.80183(17) 0.89534(15) 0.0246(4) Uani 1 1 d U . .
H26A H 0.7255 0.8316 0.8983 0.030 Uiso 1 1 calc R . .
C27 C 0.81581(14) 0.9041(2) 0.87511(18) 0.0351(5) Uani 1 1 d U . .
H27A H 0.8232 0.9624 0.9254 0.053 Uiso 1 1 calc R . .
H27B H 0.7871 0.9371 0.8119 0.053 Uiso 1 1 calc R . .
H27C H 0.8643 0.8782 0.8751 0.053 Uiso 1 1 calc R . .
C28A C 0.6628(5) 0.4134(10) 0.4519(9) 0.081(3) Uani 0.534(10) 1 d PU A 1
H28A H 0.6829 0.3607 0.4149 0.097 Uiso 0.534(10) 1 calc PR A 1
H28B H 0.7020 0.4279 0.5156 0.097 Uiso 0.534(10) 1 calc PR A 1
C29A C 0.5995(6) 0.3653(7) 0.4636(7) 0.074(3) Uani 0.534(10) 1 d PU A 1
H29A H 0.5928 0.3954 0.5225 0.088 Uiso 0.534(10) 1 calc PR A 1
H29B H 0.6034 0.2806 0.4682 0.088 Uiso 0.534(10) 1 calc PR A 1
C30A C 0.5363(4) 0.4015(7) 0.3743(5) 0.070(3) Uani 0.534(10) 1 d PU A 1
H30A H 0.4888 0.4058 0.3860 0.084 Uiso 0.534(10) 1 calc PR A 1
H30B H 0.5304 0.3489 0.3195 0.084 Uiso 0.534(10) 1 calc PR A 1
C31A C 0.5624(6) 0.5187(9) 0.3570(8) 0.075(3) Uani 0.534(10) 1 d PU A 1
H31A H 0.5471 0.5334 0.2868 0.090 Uiso 0.534(10) 1 calc PR A 1
H31B H 0.5401 0.5786 0.3856 0.090 Uiso 0.534(10) 1 calc PR A 1
O1A O 0.6385(5) 0.5218(10) 0.3990(6) 0.073(2) Uani 0.534(10) 1 d PU A 1
C28B C 0.6422(7) 0.4395(9) 0.3991(10) 0.066(3) Uani 0.466(10) 1 d PU A 2
H28C H 0.6853 0.4469 0.4603 0.079 Uiso 0.466(10) 1 calc PR A 2
H28D H 0.6599 0.4147 0.3471 0.079 Uiso 0.466(10) 1 calc PR A 2
C29B C 0.5831(5) 0.3558(6) 0.4099(8) 0.054(2) Uani 0.466(10) 1 d PU A 2
H29C H 0.5512 0.3245 0.3465 0.064 Uiso 0.466(10) 1 calc PR A 2
H29D H 0.6067 0.2914 0.4537 0.064 Uiso 0.466(10) 1 calc PR A 2
C30B C 0.5405(6) 0.4286(7) 0.4512(8) 0.075(3) Uani 0.466(10) 1 d PU A 2
H30C H 0.5669 0.4401 0.5213 0.090 Uiso 0.466(10) 1 calc PR A 2
H30D H 0.4906 0.3961 0.4401 0.090 Uiso 0.466(10) 1 calc PR A 2
C31B C 0.5357(5) 0.5352(8) 0.3977(7) 0.065(2) Uani 0.466(10) 1 d PU A 2
H31C H 0.4911 0.5346 0.3378 0.078 Uiso 0.466(10) 1 calc PR A 2
H31D H 0.5321 0.6017 0.4375 0.078 Uiso 0.466(10) 1 calc PR A 2
O1B O 0.6015(7) 0.5430(7) 0.3749(8) 0.067(3) Uani 0.466(10) 1 d PU A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.9471(16) . ?
Ni1 C1 2.004(2) . ?
Ni1 P2 2.1630(5) . ?
Ni1 P1 2.1810(5) . ?
P1 C2 1.8053(19) . ?
P1 C20 1.8496(19) . ?
P1 C17 1.851(2) . ?
P2 C9 1.807(2) . ?
P2 C26 1.841(2) . ?
P2 C23 1.842(2) . ?
N1 C7 1.390(2) . ?
N1 C14 1.398(2) . ?
C2 C3 1.393(3) . ?
C2 C7 1.418(3) . ?
C3 C4 1.391(3) . ?
C4 C5 1.390(3) . ?
C4 C8 1.506(3) . ?
C5 C6 1.386(3) . ?
C6 C7 1.410(3) . ?
C9 C10 1.393(3) . ?
C9 C14 1.413(3) . ?
C10 C11 1.388(3) . ?
C11 C12 1.395(3) . ?
C11 C15 1.513(3) . ?
C12 C13 1.388(3) . ?
C13 C14 1.409(3) . ?
C16 C17 1.531(3) . ?
C17 C18 1.530(3) . ?
C19 C20 1.521(3) . ?
C20 C21 1.535(3) . ?
C22 C23 1.526(3) . ?
C23 C24 1.529(3) . ?
C25 C26 1.533(3) . ?
C26 C27 1.534(3) . ?
C28A C29A 1.406(14) . ?
C28A O1A 1.473(12) . ?
C29A C30A 1.504(12) . ?
C30A C31A 1.510(11) . ?
C31A O1A 1.371(10) . ?
C28B O1B 1.413(13) . ?
C28B C29B 1.550(12) . ?
C29B C30B 1.456(13) . ?
C30B C31B 1.459(13) . ?
C31B O1B 1.426(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 C1 176.94(9) . . ?
N1 Ni1 P2 85.68(5) . . ?
C1 Ni1 P2 92.92(6) . . ?
N1 Ni1 P1 84.73(5) . . ?
C1 Ni1 P1 96.71(6) . . ?
P2 Ni1 P1 170.37(2) . . ?
C2 P1 C20 105.12(9) . . ?
C2 P1 C17 105.82(9) . . ?
C20 P1 C17 105.29(9) . . ?
C2 P1 Ni1 99.28(6) . . ?
C20 P1 Ni1 124.14(7) . . ?
C17 P1 Ni1 115.14(7) . . ?
C9 P2 C26 104.45(9) . . ?
C9 P2 C23 106.73(9) . . ?
C26 P2 C23 106.97(10) . . ?
C9 P2 Ni1 100.72(6) . . ?
C26 P2 Ni1 122.86(7) . . ?
C23 P2 Ni1 113.44(7) . . ?
C7 N1 C14 122.01(16) . . ?
C7 N1 Ni1 118.53(13) . . ?
C14 N1 Ni1 119.17(13) . . ?
C3 C2 C7 121.37(17) . . ?
C3 C2 P1 125.56(14) . . ?
C7 C2 P1 112.97(14) . . ?
C4 C3 C2 121.78(18) . . ?
C5 C4 C3 116.80(18) . . ?
C5 C4 C8 122.08(18) . . ?
C3 C4 C8 121.08(18) . . ?
C6 C5 C4 122.78(19) . . ?
C5 C6 C7 120.99(19) . . ?
N1 C7 C6 126.52(18) . . ?
N1 C7 C2 117.04(17) . . ?
C6 C7 C2 116.27(18) . . ?
C10 C9 C14 121.02(18) . . ?
C10 C9 P2 125.98(16) . . ?
C14 C9 P2 112.95(14) . . ?
C11 C10 C9 121.80(19) . . ?
C10 C11 C12 117.21(19) . . ?
C10 C11 C15 121.7(2) . . ?
C12 C11 C15 121.1(2) . . ?
C13 C12 C11 122.16(19) . . ?
C12 C13 C14 120.80(19) . . ?
N1 C14 C13 125.31(18) . . ?
N1 C14 C9 117.65(17) . . ?
C13 C14 C9 116.88(17) . . ?
C18 C17 C16 110.94(19) . . ?
C18 C17 P1 113.67(15) . . ?
C16 C17 P1 109.16(15) . . ?
C19 C20 C21 111.63(18) . . ?
C19 C20 P1 109.42(14) . . ?
C21 C20 P1 112.28(14) . . ?
C22 C23 C24 111.49(19) . . ?
C22 C23 P2 108.96(16) . . ?
C24 C23 P2 114.59(15) . . ?
C25 C26 C27 111.65(18) . . ?
C25 C26 P2 108.28(14) . . ?
C27 C26 P2 113.98(14) . . ?
C29A C28A O1A 106.4(7) . . ?
C28A C29A C30A 104.1(7) . . ?
C29A C30A C31A 100.9(6) . . ?
O1A C31A C30A 108.3(8) . . ?
C31A O1A C28A 107.7(7) . . ?
O1B C28B C29B 101.7(8) . . ?
C30B C29B C28B 102.7(6) . . ?
C29B C30B C31B 101.9(8) . . ?
O1B C31B C30B 107.0(7) . . ?
C28B O1B C31B 110.1(7) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.124
_database_code_depnum_ccdc_archive 'CCDC 996898'
#######################################################################
#
#                 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_0096a-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PNP)NiEt
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H45 N Ni P2'
_chemical_formula_sum            'C28 H45 N Ni P2'
_chemical_formula_weight         516.30

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.5204(8)
_cell_length_b                   11.0371(8)
_cell_length_c                   12.5590(10)
_cell_angle_alpha                79.346(4)
_cell_angle_beta                 84.731(4)
_cell_angle_gamma                71.343(4)
_cell_volume                     1357.00(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    43658
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      25.00

_exptl_crystal_description       platy
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8158
_exptl_absorpt_correction_T_max  0.9750
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43658
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4783
_reflns_number_gt                4286
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0927P)²+7.1686P] 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         4783
_refine_ls_number_parameters     291
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1913
_refine_ls_wR_factor_gt          0.1866
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_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 0.17392(5) 0.84558(5) 0.26574(5) 0.0135(2) Uani 1 1 d . . .
N1 N 0.3697(4) 0.7846(4) 0.2617(3) 0.0146(8) Uani 1 1 d . . .
P1 P 0.20024(11) 1.03775(10) 0.23389(9) 0.0109(3) Uani 1 1 d . . .
P2 P 0.19189(11) 0.64156(10) 0.28295(9) 0.0117(3) Uani 1 1 d . . .
C1 C -0.0224(5) 0.9054(5) 0.2840(4) 0.0207(10) Uani 1 1 d . . .
H1A H -0.0523 0.8316 0.3218 0.025 Uiso 1 1 calc R . .
H1B H -0.0479 0.9726 0.3313 0.025 Uiso 1 1 calc R . .
C2 C -0.0966(5) 0.9605(5) 0.1803(5) 0.0289(12) Uani 1 1 d . . .
H2A H -0.1935 0.9879 0.1970 0.043 Uiso 1 1 calc R . .
H2B H -0.0747 0.8941 0.1336 0.043 Uiso 1 1 calc R . .
H2C H -0.0701 1.0352 0.1430 0.043 Uiso 1 1 calc R . .
C3 C 0.4382(5) 0.8618(5) 0.2903(4) 0.0164(9) Uani 1 1 d . . .
C4 C 0.3680(4) 0.9971(4) 0.2827(4) 0.0129(9) Uani 1 1 d . . .
C5 C 0.4263(5) 1.0810(4) 0.3155(4) 0.0157(9) Uani 1 1 d . . .
H5A H 0.3770 1.1705 0.3096 0.019 Uiso 1 1 calc R . .
C6 C 0.5547(5) 1.0371(4) 0.3567(4) 0.0154(9) Uani 1 1 d . . .
C7 C 0.6226(5) 0.9049(5) 0.3644(4) 0.0173(10) Uani 1 1 d . . .
H7A H 0.7102 0.8723 0.3923 0.021 Uiso 1 1 calc R . .
C8 C 0.5674(4) 0.8188(4) 0.3328(4) 0.0171(10) Uani 1 1 d . . .
H8A H 0.6176 0.7295 0.3400 0.021 Uiso 1 1 calc R . .
C9 C 0.6157(5) 1.1282(5) 0.3940(4) 0.0213(10) Uani 1 1 d . . .
H9A H 0.5684 1.2177 0.3621 0.032 Uiso 1 1 calc R . .
H9B H 0.7108 1.1068 0.3710 0.032 Uiso 1 1 calc R . .
H9C H 0.6076 1.1191 0.4733 0.032 Uiso 1 1 calc R . .
C10 C 0.4375(5) 0.6654(4) 0.2293(4) 0.0150(9) Uani 1 1 d . . .
C11 C 0.3635(4) 0.5773(4) 0.2336(4) 0.0134(9) Uani 1 1 d . . .
C12 C 0.4201(5) 0.4595(4) 0.1948(4) 0.0174(10) Uani 1 1 d . . .
H12A H 0.3682 0.4024 0.1987 0.021 Uiso 1 1 calc R . .
C13 C 0.5500(5) 0.4245(4) 0.1511(4) 0.0182(10) Uani 1 1 d . . .
C14 C 0.6228(5) 0.5111(5) 0.1478(4) 0.0189(10) Uani 1 1 d . . .
H14A H 0.7123 0.4890 0.1186 0.023 Uiso 1 1 calc R . .
C15 C 0.5692(5) 0.6282(5) 0.1856(4) 0.0182(10) Uani 1 1 d . . .
H15A H 0.6225 0.6841 0.1818 0.022 Uiso 1 1 calc R . .
C16 C 0.6079(5) 0.3003(5) 0.1041(4) 0.0224(11) Uani 1 1 d . . .
H16A H 0.5725 0.2332 0.1459 0.034 Uiso 1 1 calc R . .
H16B H 0.7059 0.2714 0.1076 0.034 Uiso 1 1 calc R . .
H16C H 0.5827 0.3160 0.0284 0.034 Uiso 1 1 calc R . .
C17 C 0.3108(6) 0.9951(6) 0.0306(4) 0.0313(13) Uani 1 1 d . . .
H17A H 0.3181 1.0279 -0.0470 0.047 Uiso 1 1 calc R . .
H17B H 0.2777 0.9201 0.0406 0.047 Uiso 1 1 calc R . .
H17C H 0.3992 0.9691 0.0622 0.047 Uiso 1 1 calc R . .
C18 C 0.2126(5) 1.1021(5) 0.0869(4) 0.0204(10) Uani 1 1 d . . .
H18A H 0.1221 1.1223 0.0566 0.024 Uiso 1 1 calc R . .
C19 C 0.2523(6) 1.2263(6) 0.0628(4) 0.0327(13) Uani 1 1 d . . .
H19A H 0.2567 1.2545 -0.0157 0.049 Uiso 1 1 calc R . .
H19B H 0.3404 1.2098 0.0925 0.049 Uiso 1 1 calc R . .
H19C H 0.1854 1.2943 0.0963 0.049 Uiso 1 1 calc R . .
C20 C 0.0874(5) 1.1390(5) 0.4188(4) 0.0235(11) Uani 1 1 d . . .
H20A H 0.0342 1.2147 0.4511 0.035 Uiso 1 1 calc R . .
H20B H 0.1770 1.1052 0.4490 0.035 Uiso 1 1 calc R . .
H20C H 0.0430 1.0717 0.4350 0.035 Uiso 1 1 calc R . .
C21 C 0.0999(5) 1.1781(4) 0.2970(4) 0.0159(9) Uani 1 1 d . . .
H21A H 0.1503 1.2427 0.2835 0.019 Uiso 1 1 calc R . .
C22 C -0.0385(5) 1.2455(5) 0.2465(4) 0.0246(11) Uani 1 1 d . . .
H22A H -0.0874 1.3195 0.2824 0.037 Uiso 1 1 calc R . .
H22B H -0.0897 1.1839 0.2558 0.037 Uiso 1 1 calc R . .
H22C H -0.0262 1.2761 0.1690 0.037 Uiso 1 1 calc R . .
C23 C 0.2736(6) 0.6024(6) 0.4936(4) 0.0293(12) Uani 1 1 d . . .
H23A H 0.2696 0.5607 0.5693 0.044 Uiso 1 1 calc R . .
H23B H 0.2415 0.6968 0.4895 0.044 Uiso 1 1 calc R . .
H23C H 0.3665 0.5758 0.4651 0.044 Uiso 1 1 calc R . .
C24 C 0.1848(5) 0.5618(5) 0.4262(4) 0.0190(10) Uani 1 1 d . . .
H24A H 0.0902 0.5953 0.4543 0.023 Uiso 1 1 calc R . .
C25 C 0.2215(6) 0.4151(5) 0.4411(4) 0.0281(12) Uani 1 1 d . . .
H25A H 0.2150 0.3802 0.5184 0.042 Uiso 1 1 calc R . .
H25B H 0.3135 0.3791 0.4133 0.042 Uiso 1 1 calc R . .
H25C H 0.1595 0.3913 0.4014 0.042 Uiso 1 1 calc R . .
C26 C 0.1027(5) 0.6233(5) 0.0867(4) 0.0259(11) Uani 1 1 d . . .
H26A H 0.0512 0.5864 0.0479 0.039 Uiso 1 1 calc R . .
H26B H 0.1967 0.5978 0.0607 0.039 Uiso 1 1 calc R . .
H26C H 0.0654 0.7180 0.0737 0.039 Uiso 1 1 calc R . .
C27 C 0.0945(5) 0.5725(5) 0.2089(4) 0.0189(10) Uani 1 1 d . . .
H27A H 0.1374 0.4763 0.2201 0.023 Uiso 1 1 calc R . .
C28 C -0.0522(5) 0.5997(5) 0.2502(5) 0.0264(11) Uani 1 1 d . . .
H28A H -0.0989 0.5613 0.2083 0.040 Uiso 1 1 calc R . .
H28B H -0.0962 0.6935 0.2417 0.040 Uiso 1 1 calc R . .
H28C H -0.0551 0.5615 0.3270 0.040 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.950(4) . ?
Ni1 C1 1.963(5) . ?
Ni1 P2 2.1698(12) . ?
Ni1 P1 2.1857(12) . ?
N1 C3 1.389(6) . ?
N1 C10 1.396(6) . ?
P1 C4 1.812(4) . ?
P1 C21 1.843(5) . ?
P1 C18 1.859(5) . ?
P2 C11 1.813(4) . ?
P2 C27 1.853(5) . ?
P2 C24 1.857(5) . ?
C1 C2 1.504(8) . ?
C3 C8 1.408(6) . ?
C3 C4 1.428(6) . ?
C4 C5 1.397(6) . ?
C5 C6 1.395(7) . ?
C6 C7 1.394(7) . ?
C6 C9 1.511(6) . ?
C7 C8 1.390(7) . ?
C10 C15 1.403(7) . ?
C10 C11 1.419(6) . ?
C11 C12 1.402(6) . ?
C12 C13 1.386(7) . ?
C13 C14 1.395(7) . ?
C13 C16 1.516(6) . ?
C14 C15 1.388(7) . ?
C17 C18 1.535(7) . ?
C18 C19 1.528(7) . ?
C20 C21 1.516(7) . ?
C21 C22 1.542(6) . ?
C23 C24 1.532(7) . ?
C24 C25 1.519(7) . ?
C26 C27 1.538(7) . ?
C27 C28 1.535(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 C1 174.86(19) . . ?
N1 Ni1 P2 84.53(11) . . ?
C1 Ni1 P2 95.48(15) . . ?
N1 Ni1 P1 83.88(11) . . ?
C1 Ni1 P1 96.47(15) . . ?
P2 Ni1 P1 167.58(5) . . ?
C3 N1 C10 121.6(4) . . ?
C3 N1 Ni1 119.0(3) . . ?
C10 N1 Ni1 119.4(3) . . ?
C4 P1 C21 105.1(2) . . ?
C4 P1 C18 105.4(2) . . ?
C21 P1 C18 105.4(2) . . ?
C4 P1 Ni1 99.81(15) . . ?
C21 P1 Ni1 125.72(16) . . ?
C18 P1 Ni1 113.25(16) . . ?
C11 P2 C27 104.3(2) . . ?
C11 P2 C24 106.4(2) . . ?
C27 P2 C24 104.9(2) . . ?
C11 P2 Ni1 100.48(15) . . ?
C27 P2 Ni1 125.49(16) . . ?
C24 P2 Ni1 113.45(15) . . ?
C2 C1 Ni1 115.0(4) . . ?
N1 C3 C8 126.4(4) . . ?
N1 C3 C4 117.1(4) . . ?
C8 C3 C4 116.4(4) . . ?
C5 C4 C3 121.0(4) . . ?
C5 C4 P1 127.1(3) . . ?
C3 C4 P1 111.8(3) . . ?
C6 C5 C4 121.9(4) . . ?
C7 C6 C5 116.9(4) . . ?
C7 C6 C9 121.6(4) . . ?
C5 C6 C9 121.5(4) . . ?
C8 C7 C6 122.7(4) . . ?
C7 C8 C3 121.1(4) . . ?
N1 C10 C15 126.0(4) . . ?
N1 C10 C11 117.0(4) . . ?
C15 C10 C11 116.8(4) . . ?
C12 C11 C10 121.0(4) . . ?
C12 C11 P2 126.5(3) . . ?
C10 C11 P2 112.3(3) . . ?
C13 C12 C11 121.5(4) . . ?
C12 C13 C14 117.2(4) . . ?
C12 C13 C16 121.2(4) . . ?
C14 C13 C16 121.5(4) . . ?
C15 C14 C13 122.4(4) . . ?
C14 C15 C10 121.0(4) . . ?
C19 C18 C17 111.2(4) . . ?
C19 C18 P1 114.0(3) . . ?
C17 C18 P1 108.7(3) . . ?
C20 C21 C22 111.8(4) . . ?
C20 C21 P1 110.5(3) . . ?
C22 C21 P1 112.7(3) . . ?
C25 C24 C23 110.8(4) . . ?
C25 C24 P2 114.2(3) . . ?
C23 C24 P2 109.4(3) . . ?
C28 C27 C26 110.8(4) . . ?
C28 C27 P2 112.9(3) . . ?
C26 C27 P2 109.8(3) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.698
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.137
_database_code_depnum_ccdc_archive 'CCDC 996901'
#######################################################################
#
#                 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_n0074a-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PNP)NiCOnPr
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H47 N Ni O P2'
_chemical_formula_sum            'C30 H47 N Ni O P2'
_chemical_formula_weight         558.34

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   Cc

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

_cell_length_a                   16.6022(4)
_cell_length_b                   12.4707(4)
_cell_length_c                   16.0966(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.600(2)
_cell_angle_gamma                90.00
_cell_volume                     3053.92(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    38311
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      28.66

_exptl_crystal_description       platy
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7926
_exptl_absorpt_correction_T_max  0.9416
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38311
_diffrn_reflns_av_R_equivalents  0.1338
_diffrn_reflns_av_sigmaI/netI    0.1034
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         28.66
_reflns_number_total             7771
_reflns_number_gt                5736
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1007P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(15)
_refine_ls_number_reflns         7771
_refine_ls_number_parameters     316
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1452
_refine_ls_wR_factor_gt          0.1116
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_restrained_S_all      0.890
_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 0.21215(3) 0.57023(4) 0.14824(3) 0.01470(13) Uani 1 1 d . . .
P1 P 0.15684(6) 0.41125(8) 0.10912(7) 0.0153(2) Uani 1 1 d . . .
P2 P 0.24613(7) 0.73505(8) 0.19170(7) 0.0162(2) Uani 1 1 d . . .
C6 C 0.0409(3) 0.4434(3) 0.0605(3) 0.0157(9) Uani 1 1 d . . .
N1 N 0.0943(2) 0.6078(3) 0.1400(2) 0.0179(7) Uani 1 1 d . . .
C1 C 0.3253(3) 0.5323(4) 0.1606(3) 0.0223(10) Uani 1 1 d . . .
C10 C -0.0650(3) 0.5830(4) 0.0434(3) 0.0203(9) Uani 1 1 d . . .
H10A H -0.0797 0.6508 0.0569 0.024 Uiso 1 1 calc R . .
C21 C 0.0843(3) 0.8688(3) 0.3033(3) 0.0197(9) Uani 1 1 d . . .
C5 C 0.0232(3) 0.5473(3) 0.0840(3) 0.0164(8) Uani 1 1 d . . .
C25 C 0.3473(3) 0.7736(4) 0.2895(3) 0.0245(10) Uani 1 1 d . . .
H25A H 0.3381 0.8454 0.3089 0.029 Uiso 1 1 calc R . .
O1 O 0.3749(2) 0.4842(3) 0.2270(2) 0.0328(8) Uani 1 1 d . . .
C9 C -0.1291(3) 0.5173(4) -0.0160(3) 0.0250(10) Uani 1 1 d . . .
H9A H -0.1865 0.5429 -0.0422 0.030 Uiso 1 1 calc R . .
C18 C 0.0855(3) 0.6928(3) 0.1913(3) 0.0159(8) Uani 1 1 d . . .
C22 C 0.0168(3) 0.7947(4) 0.2730(3) 0.0209(9) Uani 1 1 d . . .
H22A H -0.0302 0.8028 0.2901 0.025 Uiso 1 1 calc R . .
C23 C 0.0165(3) 0.7091(3) 0.2185(3) 0.0195(9) Uani 1 1 d . . .
H23A H -0.0306 0.6615 0.1996 0.023 Uiso 1 1 calc R . .
C2 C 0.3553(3) 0.5654(4) 0.0865(3) 0.0254(10) Uani 1 1 d . . .
H2A H 0.3070 0.5539 0.0282 0.030 Uiso 1 1 calc R . .
H2B H 0.3679 0.6416 0.0923 0.030 Uiso 1 1 calc R . .
C12 C 0.1714(3) 0.3222(4) 0.0252(3) 0.0243(10) Uani 1 1 d . . .
H12A H 0.1254 0.2672 0.0081 0.029 Uiso 1 1 calc R . .
C7 C -0.0258(3) 0.3802(4) 0.0009(3) 0.0219(9) Uani 1 1 d . . .
H7A H -0.0121 0.3120 -0.0129 0.026 Uiso 1 1 calc R . .
C19 C 0.1564(3) 0.7663(3) 0.2237(3) 0.0189(8) Uani 1 1 d . . .
C8 C -0.1119(3) 0.4148(4) -0.0386(3) 0.0245(10) Uani 1 1 d . . .
C20 C 0.1542(3) 0.8526(3) 0.2778(3) 0.0187(9) Uani 1 1 d . . .
H20A H 0.2009 0.9008 0.2974 0.022 Uiso 1 1 calc R . .
C15 C 0.1760(3) 0.3273(4) 0.2097(3) 0.0230(10) Uani 1 1 d . . .
H15A H 0.2376 0.3042 0.2337 0.028 Uiso 1 1 calc R . .
C3 C 0.4348(4) 0.5074(5) 0.0868(5) 0.0496(16) Uani 1 1 d . . .
H3A H 0.4231 0.4310 0.0816 0.059 Uiso 1 1 calc R . .
H3B H 0.4839 0.5201 0.1442 0.059 Uiso 1 1 calc R . .
C28 C 0.2355(3) 0.8284(4) 0.0992(3) 0.0267(10) Uani 1 1 d . . .
H28A H 0.2851 0.8153 0.0822 0.032 Uiso 1 1 calc R . .
C24 C 0.0834(3) 0.9620(4) 0.3623(4) 0.0328(12) Uani 1 1 d . . .
H24A H 0.0303 0.9604 0.3724 0.049 Uiso 1 1 calc R . .
H24B H 0.0864 1.0279 0.3328 0.049 Uiso 1 1 calc R . .
H24C H 0.1332 0.9571 0.4194 0.049 Uiso 1 1 calc R . .
C4 C 0.4599(4) 0.5424(5) 0.0108(5) 0.0518(17) Uani 1 1 d . . .
H4A H 0.5101 0.5022 0.0133 0.078 Uiso 1 1 calc R . .
H4B H 0.4739 0.6174 0.0169 0.078 Uiso 1 1 calc R . .
H4C H 0.4116 0.5297 -0.0463 0.078 Uiso 1 1 calc R . .
C11 C -0.1828(3) 0.3457(5) -0.1055(4) 0.0395(13) Uani 1 1 d . . .
H11A H -0.1582 0.2780 -0.1116 0.059 Uiso 1 1 calc R . .
H11B H -0.2068 0.3810 -0.1633 0.059 Uiso 1 1 calc R . .
H11C H -0.2285 0.3341 -0.0842 0.059 Uiso 1 1 calc R . .
C27 C 0.3618(3) 0.6973(4) 0.3673(3) 0.0331(11) Uani 1 1 d . . .
H27A H 0.4142 0.7173 0.4183 0.050 Uiso 1 1 calc R . .
H27B H 0.3680 0.6255 0.3490 0.050 Uiso 1 1 calc R . .
H27C H 0.3124 0.7005 0.3839 0.050 Uiso 1 1 calc R . .
C30 C 0.1508(4) 0.8000(4) 0.0168(3) 0.0351(12) Uani 1 1 d . . .
H30A H 0.1440 0.8476 -0.0324 0.053 Uiso 1 1 calc R . .
H30B H 0.1012 0.8071 0.0328 0.053 Uiso 1 1 calc R . .
H30C H 0.1544 0.7274 -0.0014 0.053 Uiso 1 1 calc R . .
C16 C 0.1638(4) 0.3955(5) 0.2834(3) 0.0354(12) Uani 1 1 d . . .
H16A H 0.1737 0.3519 0.3357 0.053 Uiso 1 1 calc R . .
H16B H 0.1051 0.4236 0.2605 0.053 Uiso 1 1 calc R . .
H16C H 0.2051 0.4538 0.2999 0.053 Uiso 1 1 calc R . .
C17 C 0.1196(3) 0.2271(4) 0.1891(4) 0.0354(12) Uani 1 1 d . . .
H17A H 0.1326 0.1872 0.2440 0.053 Uiso 1 1 calc R . .
H17B H 0.1319 0.1835 0.1463 0.053 Uiso 1 1 calc R . .
H17C H 0.0586 0.2470 0.1638 0.053 Uiso 1 1 calc R . .
C14 C 0.2609(3) 0.2657(4) 0.0634(4) 0.0323(12) Uani 1 1 d . . .
H14A H 0.2659 0.2197 0.0179 0.049 Uiso 1 1 calc R . .
H14B H 0.2660 0.2238 0.1154 0.049 Uiso 1 1 calc R . .
H14C H 0.3069 0.3184 0.0810 0.049 Uiso 1 1 calc R . .
C13 C 0.1590(4) 0.3876(4) -0.0596(3) 0.0354(12) Uani 1 1 d . . .
H13A H 0.1661 0.3416 -0.1041 0.053 Uiso 1 1 calc R . .
H13B H 0.2021 0.4438 -0.0439 0.053 Uiso 1 1 calc R . .
H13C H 0.1012 0.4183 -0.0842 0.053 Uiso 1 1 calc R . .
C26 C 0.4278(3) 0.7781(5) 0.2668(4) 0.0374(13) Uani 1 1 d . . .
H26A H 0.4781 0.7990 0.3198 0.056 Uiso 1 1 calc R . .
H26B H 0.4182 0.8296 0.2194 0.056 Uiso 1 1 calc R . .
H26C H 0.4379 0.7088 0.2470 0.056 Uiso 1 1 calc R . .
C29 C 0.2375(4) 0.9462(4) 0.1237(4) 0.0353(12) Uani 1 1 d . . .
H29A H 0.2318 0.9893 0.0722 0.053 Uiso 1 1 calc R . .
H29B H 0.2922 0.9623 0.1733 0.053 Uiso 1 1 calc R . .
H29C H 0.1897 0.9615 0.1410 0.053 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.869(4) . ?
Ni1 N1 1.964(3) . ?
Ni1 P1 2.1697(12) . ?
Ni1 P2 2.1717(12) . ?
P1 C6 1.809(4) . ?
P1 C12 1.838(5) . ?
P1 C15 1.846(5) . ?
P2 C19 1.803(4) . ?
P2 C28 1.842(5) . ?
P2 C25 1.847(4) . ?
C6 C7 1.385(6) . ?
C6 C5 1.413(6) . ?
N1 C5 1.387(5) . ?
N1 C18 1.387(5) . ?
C1 O1 1.215(6) . ?
C1 C2 1.522(7) . ?
C10 C9 1.380(6) . ?
C10 C5 1.415(6) . ?
C21 C22 1.382(6) . ?
C21 C20 1.393(6) . ?
C21 C24 1.504(6) . ?
C25 C26 1.521(7) . ?
C25 C27 1.513(7) . ?
C9 C8 1.390(7) . ?
C18 C23 1.396(6) . ?
C18 C19 1.416(6) . ?
C22 C23 1.380(6) . ?
C2 C3 1.504(7) . ?
C12 C13 1.532(7) . ?
C12 C14 1.534(6) . ?
C7 C8 1.381(6) . ?
C19 C20 1.394(6) . ?
C8 C11 1.507(6) . ?
C15 C17 1.518(7) . ?
C15 C16 1.537(7) . ?
C3 C4 1.505(8) . ?
C28 C29 1.518(7) . ?
C28 C30 1.540(7) . ?

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 N1 177.7(2) . . ?
C1 Ni1 P1 95.18(14) . . ?
N1 Ni1 P1 84.50(11) . . ?
C1 Ni1 P2 94.86(14) . . ?
N1 Ni1 P2 85.36(11) . . ?
P1 Ni1 P2 169.58(4) . . ?
C6 P1 C12 104.2(2) . . ?
C6 P1 C15 106.6(2) . . ?
C12 P1 C15 106.0(2) . . ?
C6 P1 Ni1 100.15(14) . . ?
C12 P1 Ni1 126.92(16) . . ?
C15 P1 Ni1 111.04(15) . . ?
C19 P2 C28 105.8(2) . . ?
C19 P2 C25 105.9(2) . . ?
C28 P2 C25 106.5(2) . . ?
C19 P2 Ni1 99.13(14) . . ?
C28 P2 Ni1 114.17(16) . . ?
C25 P2 Ni1 123.43(16) . . ?
C7 C6 C5 120.9(4) . . ?
C7 C6 P1 126.2(3) . . ?
C5 C6 P1 112.8(3) . . ?
C5 N1 C18 122.5(3) . . ?
C5 N1 Ni1 118.6(3) . . ?
C18 N1 Ni1 118.8(3) . . ?
O1 C1 C2 120.3(4) . . ?
O1 C1 Ni1 121.1(4) . . ?
C2 C1 Ni1 118.5(3) . . ?
C9 C10 C5 120.1(4) . . ?
C22 C21 C20 116.9(4) . . ?
C22 C21 C24 121.9(4) . . ?
C20 C21 C24 121.2(4) . . ?
N1 C5 C10 125.7(4) . . ?
N1 C5 C6 117.3(4) . . ?
C10 C5 C6 116.9(4) . . ?
C26 C25 C27 111.0(4) . . ?
C26 C25 P2 113.1(3) . . ?
C27 C25 P2 109.3(3) . . ?
C10 C9 C8 123.1(4) . . ?
C23 C18 N1 126.4(4) . . ?
C23 C18 C19 117.1(4) . . ?
N1 C18 C19 116.3(4) . . ?
C21 C22 C23 122.6(4) . . ?
C18 C23 C22 121.1(4) . . ?
C3 C2 C1 115.5(4) . . ?
C13 C12 C14 111.4(4) . . ?
C13 C12 P1 108.9(3) . . ?
C14 C12 P1 111.9(3) . . ?
C8 C7 C6 122.3(4) . . ?
C20 C19 C18 120.3(4) . . ?
C20 C19 P2 125.2(3) . . ?
C18 C19 P2 114.5(3) . . ?
C7 C8 C9 116.7(4) . . ?
C7 C8 C11 121.3(4) . . ?
C9 C8 C11 122.0(4) . . ?
C19 C20 C21 122.0(4) . . ?
C17 C15 C16 111.4(4) . . ?
C17 C15 P1 113.6(3) . . ?
C16 C15 P1 109.5(3) . . ?
C2 C3 C4 112.7(5) . . ?
C29 C28 C30 111.3(4) . . ?
C29 C28 P2 114.6(4) . . ?
C30 C28 P2 108.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.66
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.194
_database_code_depnum_ccdc_archive 'CCDC 996902'
#######################################################################
#
#                 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_0098a-2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PNP)NinPr
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H47 N Ni P2'
_chemical_formula_sum            'C29 H47 N Ni P2'
_chemical_formula_weight         530.33

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   15.7352(6)
_cell_length_b                   9.8832(4)
_cell_length_c                   18.2622(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.249(2)
_cell_angle_gamma                90.00
_cell_volume                     2832.22(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    139779
_cell_measurement_theta_min      1.30
_cell_measurement_theta_max      33.06

_exptl_crystal_description       platy
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8875
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            139779
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         33.06
_reflns_number_total             10648
_reflns_number_gt                7572
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0724P)²+0.0563P] 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         10648
_refine_ls_number_parameters     332
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1326
_refine_ls_wR_factor_gt          0.1179
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_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 0.244893(14) 0.18760(2) 0.182484(11) 0.02046(7) Uani 1 1 d . . .
P1 P 0.31664(3) 0.04886(4) 0.25537(2) 0.01872(9) Uani 1 1 d . A .
P2 P 0.20161(3) 0.36734(4) 0.12008(2) 0.01968(9) Uani 1 1 d . A .
N1 N 0.24441(9) 0.30897(13) 0.26683(7) 0.0193(3) Uani 1 1 d . A .
C4 C 0.30209(10) 0.28766(15) 0.32680(8) 0.0185(3) Uani 1 1 d . . .
C5 C 0.34408(11) 0.16053(15) 0.33298(9) 0.0189(3) Uani 1 1 d . A .
C6 C 0.40459(11) 0.13376(16) 0.39101(9) 0.0213(3) Uani 1 1 d . . .
H6A H 0.4310 0.0473 0.3939 0.026 Uiso 1 1 calc R A .
C7 C 0.42739(11) 0.22940(17) 0.44467(9) 0.0225(3) Uani 1 1 d . A .
C8 C 0.38811(11) 0.35585(17) 0.43751(9) 0.0239(3) Uani 1 1 d . . .
H8A H 0.4033 0.4239 0.4728 0.029 Uiso 1 1 calc R A .
C9 C 0.32784(11) 0.38532(16) 0.38078(9) 0.0225(3) Uani 1 1 d . A .
H9A H 0.3031 0.4730 0.3779 0.027 Uiso 1 1 calc R . .
C10 C 0.49482(12) 0.20140(19) 0.50618(10) 0.0286(4) Uani 1 1 d . . .
H10A H 0.4676 0.1890 0.5523 0.043 Uiso 1 1 calc R A .
H10B H 0.5344 0.2779 0.5111 0.043 Uiso 1 1 calc R . .
H10C H 0.5262 0.1191 0.4950 0.043 Uiso 1 1 calc R . .
C11 C 0.18886(10) 0.41938(15) 0.26334(9) 0.0192(3) Uani 1 1 d . . .
C12 C 0.16092(10) 0.46750(16) 0.19289(9) 0.0204(3) Uani 1 1 d . A .
C13 C 0.10163(11) 0.57270(16) 0.18385(9) 0.0231(3) Uani 1 1 d . . .
H13A H 0.0854 0.6044 0.1357 0.028 Uiso 1 1 calc R A .
C14 C 0.06591(11) 0.63204(16) 0.24328(10) 0.0248(3) Uani 1 1 d . A .
C15 C 0.09297(11) 0.58324(17) 0.31295(10) 0.0243(3) Uani 1 1 d . . .
H15A H 0.0693 0.6214 0.3546 0.029 Uiso 1 1 calc R A .
C16 C 0.15320(11) 0.48105(16) 0.32347(9) 0.0225(3) Uani 1 1 d . A .
H16A H 0.1706 0.4523 0.3719 0.027 Uiso 1 1 calc R . .
C17 C -0.00199(13) 0.74031(19) 0.23216(11) 0.0327(4) Uani 1 1 d . . .
H17A H -0.0146 0.7561 0.1795 0.049 Uiso 1 1 calc R A .
H17B H 0.0186 0.8244 0.2558 0.049 Uiso 1 1 calc R . .
H17C H -0.0539 0.7105 0.2540 0.049 Uiso 1 1 calc R . .
C18 C 0.17824(13) -0.0538(2) 0.32019(13) 0.0392(5) Uani 1 1 d . A .
H18A H 0.1466 -0.1326 0.3361 0.059 Uiso 1 1 calc R . .
H18B H 0.1439 -0.0058 0.2815 0.059 Uiso 1 1 calc R . .
H18C H 0.1907 0.0070 0.3620 0.059 Uiso 1 1 calc R . .
C19 C 0.26122(11) -0.10020(16) 0.29068(10) 0.0245(3) Uani 1 1 d . . .
H19A H 0.2462 -0.1613 0.2480 0.029 Uiso 1 1 calc R A .
C20 C 0.31396(15) -0.1833(2) 0.34863(13) 0.0399(5) Uani 1 1 d . A .
H20A H 0.3251 -0.1289 0.3932 0.060 Uiso 1 1 calc R . .
H20B H 0.3682 -0.2092 0.3294 0.060 Uiso 1 1 calc R . .
H20C H 0.2823 -0.2649 0.3603 0.060 Uiso 1 1 calc R . .
C21 C 0.41394(14) -0.1386(2) 0.17837(12) 0.0363(4) Uani 1 1 d . A .
H21A H 0.3855 -0.1122 0.1310 0.054 Uiso 1 1 calc R . .
H21B H 0.3807 -0.2095 0.2006 0.054 Uiso 1 1 calc R . .
H21C H 0.4711 -0.1728 0.1710 0.054 Uiso 1 1 calc R . .
C22 C 0.42094(11) -0.01524(17) 0.22942(10) 0.0245(3) Uani 1 1 d . . .
H22A H 0.4546 -0.0432 0.2756 0.029 Uiso 1 1 calc R A .
C23 C 0.46949(13) 0.0991(2) 0.19489(12) 0.0383(5) Uani 1 1 d . A .
H23A H 0.5270 0.0681 0.1862 0.057 Uiso 1 1 calc R . .
H23B H 0.4731 0.1770 0.2282 0.057 Uiso 1 1 calc R . .
H23C H 0.4395 0.1255 0.1481 0.057 Uiso 1 1 calc R . .
C24 C 0.03336(13) 0.3297(2) 0.06190(12) 0.0376(5) Uani 1 1 d . A .
H24A H -0.0086 0.3433 0.0202 0.056 Uiso 1 1 calc R . .
H24B H 0.0152 0.3788 0.1047 0.056 Uiso 1 1 calc R . .
H24C H 0.0379 0.2330 0.0734 0.056 Uiso 1 1 calc R . .
C25 C 0.12000(11) 0.38284(17) 0.04242(9) 0.0247(3) Uani 1 1 d . . .
H25A H 0.1131 0.4814 0.0310 0.030 Uiso 1 1 calc R A .
C26 C 0.14662(16) 0.3126(2) -0.02741(11) 0.0400(5) Uani 1 1 d . A .
H26A H 0.1416 0.2143 -0.0219 0.060 Uiso 1 1 calc R . .
H26B H 0.2058 0.3360 -0.0352 0.060 Uiso 1 1 calc R . .
H26C H 0.1094 0.3426 -0.0697 0.060 Uiso 1 1 calc R . .
C27 C 0.36234(12) 0.4762(2) 0.15302(11) 0.0336(4) Uani 1 1 d . A .
H27A H 0.4106 0.5287 0.1373 0.050 Uiso 1 1 calc R . .
H27B H 0.3818 0.3854 0.1678 0.050 Uiso 1 1 calc R . .
H27C H 0.3386 0.5215 0.1947 0.050 Uiso 1 1 calc R . .
C28 C 0.29364(11) 0.46527(19) 0.08927(10) 0.0274(4) Uani 1 1 d . . .
H28A H 0.3181 0.4136 0.0487 0.033 Uiso 1 1 calc R A .
C29 C 0.26898(13) 0.6067(2) 0.06016(12) 0.0366(4) Uani 1 1 d . A .
H29A H 0.2441 0.6588 0.0989 0.055 Uiso 1 1 calc R . .
H29B H 0.2272 0.5982 0.0178 0.055 Uiso 1 1 calc R . .
H29C H 0.3199 0.6532 0.0452 0.055 Uiso 1 1 calc R . .
C1A C 0.2251(5) 0.0484(7) 0.1051(4) 0.0316(12) Uani 0.710(8) 1 d P A 1
H1AA H 0.2278 0.0898 0.0560 0.038 Uiso 0.710(8) 1 calc PR A 1
H1AB H 0.2693 -0.0229 0.1110 0.038 Uiso 0.710(8) 1 calc PR A 1
C2A C 0.1382(3) -0.0116(5) 0.1127(3) 0.0427(10) Uani 0.710(8) 1 d P A 1
H2AA H 0.0983 0.0622 0.1232 0.051 Uiso 0.710(8) 1 calc PR A 1
H2AB H 0.1415 -0.0738 0.1553 0.051 Uiso 0.710(8) 1 calc PR A 1
C3A C 0.1015(4) -0.0894(4) 0.0447(3) 0.0600(15) Uani 0.710(8) 1 d P A 1
H3AA H 0.0917 -0.0266 0.0034 0.090 Uiso 0.710(8) 1 calc PR A 1
H3AB H 0.0475 -0.1318 0.0553 0.090 Uiso 0.710(8) 1 calc PR A 1
H3AC H 0.1420 -0.1594 0.0320 0.090 Uiso 0.710(8) 1 calc PR A 1
C1B C 0.2412(14) 0.0752(17) 0.0934(9) 0.032(3) Uani 0.290(8) 1 d P A 2
H1BA H 0.2289 0.1323 0.0494 0.038 Uiso 0.290(8) 1 calc PR A 2
H1BB H 0.2969 0.0304 0.0894 0.038 Uiso 0.290(8) 1 calc PR A 2
C2B C 0.1742(9) -0.0265(11) 0.0984(6) 0.045(3) Uani 0.290(8) 1 d P A 2
H2BA H 0.1227 0.0178 0.1152 0.054 Uiso 0.290(8) 1 calc PR A 2
H2BB H 0.1935 -0.0948 0.1357 0.054 Uiso 0.290(8) 1 calc PR A 2
C3B C 0.1506(10) -0.0990(10) 0.0242(7) 0.0600(15) Uani 0.290(8) 1 d P A 2
H3BA H 0.1221 -0.0350 -0.0104 0.090 Uiso 0.290(8) 1 calc PR A 2
H3BB H 0.1122 -0.1749 0.0322 0.090 Uiso 0.290(8) 1 calc PR A 2
H3BC H 0.2025 -0.1330 0.0040 0.090 Uiso 0.290(8) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.9528(13) . ?
Ni1 C1B 1.967(19) . ?
Ni1 C1A 1.980(8) . ?
Ni1 P1 2.1688(5) . ?
Ni1 P2 2.1917(5) . ?
P1 C5 1.8228(16) . ?
P1 C19 1.8520(17) . ?
P1 C22 1.8532(17) . ?
P2 C12 1.8121(16) . ?
P2 C25 1.8477(17) . ?
P2 C28 1.8631(18) . ?
N1 C4 1.386(2) . ?
N1 C11 1.397(2) . ?
C4 C9 1.417(2) . ?
C4 C5 1.420(2) . ?
C5 C6 1.397(2) . ?
C6 C7 1.389(2) . ?
C7 C8 1.396(2) . ?
C7 C10 1.512(2) . ?
C8 C9 1.383(2) . ?
C11 C16 1.408(2) . ?
C11 C12 1.411(2) . ?
C12 C13 1.398(2) . ?
C13 C14 1.389(2) . ?
C14 C15 1.397(2) . ?
C14 C17 1.515(2) . ?
C15 C16 1.389(2) . ?
C18 C19 1.520(3) . ?
C19 C20 1.534(3) . ?
C21 C22 1.534(3) . ?
C22 C23 1.526(3) . ?
C24 C25 1.527(3) . ?
C25 C26 1.537(3) . ?
C27 C28 1.533(3) . ?
C28 C29 1.535(3) . ?
C1A C2A 1.507(8) . ?
C2A C3A 1.535(6) . ?
C1B C2B 1.465(19) . ?
C2B C3B 1.554(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 C1B 176.0(5) . . ?
N1 Ni1 C1A 168.55(19) . . ?
C1B Ni1 C1A 12.6(4) . . ?
N1 Ni1 P1 86.36(4) . . ?
C1B Ni1 P1 97.6(5) . . ?
C1A Ni1 P1 92.6(2) . . ?
N1 Ni1 P2 83.86(4) . . ?
C1B Ni1 P2 92.2(5) . . ?
C1A Ni1 P2 99.55(19) . . ?
P1 Ni1 P2 163.57(2) . . ?
C5 P1 C19 107.54(8) . . ?
C5 P1 C22 104.03(8) . . ?
C19 P1 C22 105.42(8) . . ?
C5 P1 Ni1 100.19(5) . . ?
C19 P1 Ni1 118.65(6) . . ?
C22 P1 Ni1 119.33(6) . . ?
C12 P2 C25 104.76(8) . . ?
C12 P2 C28 105.22(8) . . ?
C25 P2 C28 103.69(8) . . ?
C12 P2 Ni1 100.04(5) . . ?
C25 P2 Ni1 129.63(6) . . ?
C28 P2 Ni1 111.07(6) . . ?
C4 N1 C11 121.73(13) . . ?
C4 N1 Ni1 119.31(10) . . ?
C11 N1 Ni1 118.88(11) . . ?
N1 C4 C9 125.66(14) . . ?
N1 C4 C5 118.09(14) . . ?
C9 C4 C5 116.10(15) . . ?
C6 C5 C4 120.99(14) . . ?
C6 C5 P1 125.75(12) . . ?
C4 C5 P1 113.07(12) . . ?
C7 C6 C5 122.16(15) . . ?
C6 C7 C8 116.97(15) . . ?
C6 C7 C10 121.98(16) . . ?
C8 C7 C10 120.98(15) . . ?
C9 C8 C7 122.21(15) . . ?
C8 C9 C4 121.51(15) . . ?
N1 C11 C16 125.93(15) . . ?
N1 C11 C12 117.17(14) . . ?
C16 C11 C12 116.73(14) . . ?
C13 C12 C11 121.21(15) . . ?
C13 C12 P2 126.04(13) . . ?
C11 C12 P2 112.45(11) . . ?
C14 C13 C12 121.80(15) . . ?
C13 C14 C15 116.88(15) . . ?
C13 C14 C17 121.05(16) . . ?
C15 C14 C17 122.01(16) . . ?
C16 C15 C14 122.40(15) . . ?
C15 C16 C11 120.95(15) . . ?
C18 C19 C20 110.61(17) . . ?
C18 C19 P1 108.80(12) . . ?
C20 C19 P1 114.93(13) . . ?
C23 C22 C21 110.65(16) . . ?
C23 C22 P1 109.43(13) . . ?
C21 C22 P1 113.71(13) . . ?
C24 C25 C26 109.93(16) . . ?
C24 C25 P2 111.98(12) . . ?
C26 C25 P2 112.50(14) . . ?
C27 C28 C29 110.18(16) . . ?
C27 C28 P2 109.12(12) . . ?
C29 C28 P2 113.29(13) . . ?
C2A C1A Ni1 107.7(4) . . ?
C1A C2A C3A 114.4(5) . . ?
C2B C1B Ni1 108.3(10) . . ?
C1B C2B C3B 112.9(11) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        33.06
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 996903'
#######################################################################
#
#                 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_n0028a-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PNP)NiCOiPr
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H47 N Ni O P2'
_chemical_formula_sum            'C30 H47 N Ni O P2'
_chemical_formula_weight         558.34

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   P2(1)/c

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

_cell_length_a                   15.5099(5)
_cell_length_b                   9.9868(3)
_cell_length_c                   18.6693(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.5520(10)
_cell_angle_gamma                90.00
_cell_volume                     2878.20(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    41902
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.18

_exptl_crystal_description       platy
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8815
_exptl_absorpt_correction_T_max  0.9531
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41902
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.18
_reflns_number_total             6363
_reflns_number_gt                5356
_reflns_threshold_expression     >2sigma(I)

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


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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0530P)²+3.1033P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6363
_refine_ls_number_parameters     320
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.1080
_refine_ls_wR_factor_gt          0.0956
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_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 0.258643(18) 0.83058(3) 0.318840(14) 0.01428(9) Uani 1 1 d . . .
P1 P 0.30445(4) 0.65524(5) 0.38073(3) 0.01469(13) Uani 1 1 d . . .
P2 P 0.18705(4) 0.96827(5) 0.24392(3) 0.01361(12) Uani 1 1 d . . .
N1 N 0.26028(12) 0.70990(18) 0.23697(9) 0.0153(4) Uani 1 1 d . . .
C6 C 0.34422(14) 0.5522(2) 0.31120(11) 0.0154(4) Uani 1 1 d . . .
O1 O 0.18934(13) 0.91522(19) 0.43756(9) 0.0299(4) Uani 1 1 d . . .
C5 C 0.31409(14) 0.5981(2) 0.24168(11) 0.0148(4) Uani 1 1 d . . .
C23 C 0.20806(15) 0.5695(2) 0.40970(12) 0.0213(5) Uani 1 1 d . . .
H23A H 0.1838 0.6274 0.4466 0.026 Uiso 1 1 calc R . .
C9 C 0.40569(15) 0.4307(2) 0.19357(12) 0.0181(4) Uani 1 1 d . . .
H9A H 0.4266 0.3897 0.1527 0.022 Uiso 1 1 calc R . .
C14 C 0.09465(15) 0.8770(2) 0.11276(11) 0.0181(4) Uani 1 1 d . . .
H14A H 0.0689 0.9632 0.1075 0.022 Uiso 1 1 calc R . .
C20 C 0.38552(15) 0.6404(2) 0.45926(12) 0.0200(5) Uani 1 1 d . . .
H20A H 0.3896 0.5435 0.4727 0.024 Uiso 1 1 calc R . .
C27 C 0.09461(17) 1.1558(2) 0.31987(13) 0.0249(5) Uani 1 1 d . . .
H27A H 0.0376 1.1886 0.3302 0.037 Uiso 1 1 calc R . .
H27B H 0.1263 1.2279 0.2983 0.037 Uiso 1 1 calc R . .
H27C H 0.1272 1.1263 0.3647 0.037 Uiso 1 1 calc R . .
C7 C 0.40273(15) 0.4460(2) 0.32047(12) 0.0185(4) Uani 1 1 d . . .
H7A H 0.4208 0.4155 0.3677 0.022 Uiso 1 1 calc R . .
C16 C 0.10637(15) 0.6519(2) 0.07389(12) 0.0198(5) Uani 1 1 d . . .
H16A H 0.0883 0.5814 0.0417 0.024 Uiso 1 1 calc R . .
C1 C 0.24711(16) 0.9386(2) 0.39934(12) 0.0205(5) Uani 1 1 d . . .
C26 C 0.08329(15) 1.0378(2) 0.26733(12) 0.0188(4) Uani 1 1 d . . .
H26A H 0.0510 1.0714 0.2219 0.023 Uiso 1 1 calc R . .
C17 C 0.16888(15) 0.6260(2) 0.12990(12) 0.0184(4) Uani 1 1 d . . .
H17A H 0.1924 0.5384 0.1357 0.022 Uiso 1 1 calc R . .
C29 C 0.24617(15) 1.1097(2) 0.20697(12) 0.0181(4) Uani 1 1 d . . .
H29A H 0.2670 1.1691 0.2482 0.022 Uiso 1 1 calc R . .
C19 C 0.47559(16) 0.6855(3) 0.44240(14) 0.0282(5) Uani 1 1 d . . .
H19A H 0.5165 0.6755 0.4855 0.042 Uiso 1 1 calc R . .
H19B H 0.4734 0.7795 0.4274 0.042 Uiso 1 1 calc R . .
H19C H 0.4946 0.6302 0.4035 0.042 Uiso 1 1 calc R . .
C8 C 0.43529(15) 0.3836(2) 0.26197(13) 0.0194(4) Uani 1 1 d . . .
C21 C 0.35638(19) 0.7168(3) 0.52416(12) 0.0287(6) Uani 1 1 d . . .
H21A H 0.4003 0.7072 0.5652 0.043 Uiso 1 1 calc R . .
H21B H 0.3012 0.6802 0.5367 0.043 Uiso 1 1 calc R . .
H21C H 0.3491 0.8118 0.5119 0.043 Uiso 1 1 calc R . .
C13 C 0.15751(14) 0.8532(2) 0.17026(11) 0.0155(4) Uani 1 1 d . . .
C11 C 0.50192(16) 0.2745(2) 0.27091(14) 0.0257(5) Uani 1 1 d . . .
H11A H 0.5158 0.2441 0.2234 0.039 Uiso 1 1 calc R . .
H11B H 0.4790 0.1993 0.2970 0.039 Uiso 1 1 calc R . .
H11C H 0.5545 0.3088 0.2982 0.039 Uiso 1 1 calc R . .
C12 C 0.19846(14) 0.7275(2) 0.17865(11) 0.0147(4) Uani 1 1 d . . .
C10 C 0.34743(15) 0.5341(2) 0.18311(12) 0.0168(4) Uani 1 1 d . . .
H10A H 0.3293 0.5628 0.1355 0.020 Uiso 1 1 calc R . .
C18 C 0.00109(17) 0.8008(3) 0.00095(13) 0.0279(5) Uani 1 1 d . . .
H18A H -0.0181 0.8943 0.0012 0.042 Uiso 1 1 calc R . .
H18B H -0.0485 0.7417 0.0057 0.042 Uiso 1 1 calc R . .
H18C H 0.0256 0.7817 -0.0444 0.042 Uiso 1 1 calc R . .
C15 C 0.06901(15) 0.7775(2) 0.06303(11) 0.0190(5) Uani 1 1 d . . .
C2 C 0.30506(17) 1.0583(3) 0.41456(12) 0.0254(5) Uani 1 1 d D . .
C22 C 0.22858(19) 0.4331(3) 0.44417(15) 0.0318(6) Uani 1 1 d . . .
H22A H 0.1752 0.3928 0.4584 0.048 Uiso 1 1 calc R . .
H22B H 0.2701 0.4444 0.4868 0.048 Uiso 1 1 calc R . .
H22C H 0.2536 0.3746 0.4095 0.048 Uiso 1 1 calc R . .
C28 C 0.32579(17) 1.0550(3) 0.17482(14) 0.0256(5) Uani 1 1 d . . .
H28A H 0.3574 1.1291 0.1549 0.038 Uiso 1 1 calc R . .
H28B H 0.3076 0.9911 0.1365 0.038 Uiso 1 1 calc R . .
H28C H 0.3636 1.0098 0.2124 0.038 Uiso 1 1 calc R . .
C25 C 0.02861(17) 0.9274(3) 0.29725(14) 0.0278(5) Uani 1 1 d . . .
H25A H -0.0265 0.9651 0.3093 0.042 Uiso 1 1 calc R . .
H25B H 0.0600 0.8893 0.3406 0.042 Uiso 1 1 calc R . .
H25C H 0.0173 0.8570 0.2610 0.042 Uiso 1 1 calc R . .
C30 C 0.19206(18) 1.1955(3) 0.15186(14) 0.0279(5) Uani 1 1 d . . .
H30A H 0.2280 1.2676 0.1353 0.042 Uiso 1 1 calc R . .
H30B H 0.1431 1.2341 0.1741 0.042 Uiso 1 1 calc R . .
H30C H 0.1703 1.1397 0.1108 0.042 Uiso 1 1 calc R . .
C3 C 0.3968(2) 1.0437(3) 0.39775(18) 0.0407(7) Uani 1 1 d . . .
H3A H 0.3978 1.0098 0.3486 0.061 Uiso 1 1 calc R . .
H3B H 0.4270 0.9807 0.4317 0.061 Uiso 1 1 calc R . .
H3C H 0.4256 1.1311 0.4019 0.061 Uiso 1 1 calc R . .
C4 C 0.3003(2) 1.1139(3) 0.49209(14) 0.0405(7) Uani 1 1 d . . .
H4A H 0.3385 1.1918 0.4996 0.061 Uiso 1 1 calc R . .
H4B H 0.3188 1.0443 0.5273 0.061 Uiso 1 1 calc R . .
H4C H 0.2406 1.1405 0.4981 0.061 Uiso 1 1 calc R . .
C24 C 0.13873(17) 0.5553(3) 0.34631(14) 0.0287(5) Uani 1 1 d . . .
H24A H 0.0879 0.5100 0.3623 0.043 Uiso 1 1 calc R . .
H24B H 0.1618 0.5025 0.3082 0.043 Uiso 1 1 calc R . .
H24C H 0.1220 0.6443 0.3277 0.043 Uiso 1 1 calc R . .
H2A H 0.2759(17) 1.122(2) 0.3844(13) 0.027(7) Uiso 1 1 d 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 1.873(2) . ?
Ni1 N1 1.9486(18) . ?
Ni1 P1 2.1788(6) . ?
Ni1 P2 2.1862(6) . ?
P1 C6 1.811(2) . ?
P1 C20 1.843(2) . ?
P1 C23 1.849(2) . ?
P2 C13 1.817(2) . ?
P2 C26 1.844(2) . ?
P2 C29 1.853(2) . ?
N1 C12 1.391(3) . ?
N1 C5 1.391(3) . ?
C6 C7 1.396(3) . ?
C6 C5 1.413(3) . ?
O1 C1 1.221(3) . ?
C5 C10 1.408(3) . ?
C23 C24 1.527(3) . ?
C23 C22 1.527(3) . ?
C9 C10 1.374(3) . ?
C9 C8 1.396(3) . ?
C14 C15 1.391(3) . ?
C14 C13 1.399(3) . ?
C20 C19 1.529(3) . ?
C20 C21 1.537(3) . ?
C27 C26 1.532(3) . ?
C7 C8 1.394(3) . ?
C16 C17 1.380(3) . ?
C16 C15 1.389(3) . ?
C1 C2 1.506(4) . ?
C26 C25 1.529(3) . ?
C17 C12 1.409(3) . ?
C29 C28 1.525(3) . ?
C29 C30 1.526(3) . ?
C8 C11 1.500(3) . ?
C13 C12 1.409(3) . ?
C18 C15 1.507(3) . ?
C2 C3 1.493(4) . ?
C2 C4 1.559(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 N1 174.49(10) . . ?
C1 Ni1 P1 95.11(7) . . ?
N1 Ni1 P1 83.72(6) . . ?
C1 Ni1 P2 93.96(7) . . ?
N1 Ni1 P2 86.07(6) . . ?
P1 Ni1 P2 164.61(3) . . ?
C6 P1 C20 105.73(10) . . ?
C6 P1 C23 106.73(10) . . ?
C20 P1 C23 103.81(11) . . ?
C6 P1 Ni1 101.11(7) . . ?
C20 P1 Ni1 130.47(8) . . ?
C23 P1 Ni1 107.21(8) . . ?
C13 P2 C26 104.82(10) . . ?
C13 P2 C29 107.34(10) . . ?
C26 P2 C29 106.02(10) . . ?
C13 P2 Ni1 99.31(7) . . ?
C26 P2 Ni1 119.09(7) . . ?
C29 P2 Ni1 118.59(8) . . ?
C12 N1 C5 121.00(17) . . ?
C12 N1 Ni1 118.39(14) . . ?
C5 N1 Ni1 119.99(14) . . ?
C7 C6 C5 120.92(19) . . ?
C7 C6 P1 127.26(17) . . ?
C5 C6 P1 111.64(16) . . ?
N1 C5 C10 125.35(19) . . ?
N1 C5 C6 117.49(18) . . ?
C10 C5 C6 116.9(2) . . ?
C24 C23 C22 110.3(2) . . ?
C24 C23 P1 110.19(16) . . ?
C22 C23 P1 113.26(17) . . ?
C10 C9 C8 122.5(2) . . ?
C15 C14 C13 121.6(2) . . ?
C19 C20 C21 111.1(2) . . ?
C19 C20 P1 112.27(16) . . ?
C21 C20 P1 110.93(17) . . ?
C8 C7 C6 121.5(2) . . ?
C17 C16 C15 122.2(2) . . ?
O1 C1 C2 120.0(2) . . ?
O1 C1 Ni1 119.44(19) . . ?
C2 C1 Ni1 120.47(17) . . ?
C25 C26 C27 110.73(19) . . ?
C25 C26 P2 110.03(16) . . ?
C27 C26 P2 113.13(17) . . ?
C16 C17 C12 121.0(2) . . ?
C28 C29 C30 110.41(19) . . ?
C28 C29 P2 108.82(15) . . ?
C30 C29 P2 114.78(17) . . ?
C7 C8 C9 117.0(2) . . ?
C7 C8 C11 122.4(2) . . ?
C9 C8 C11 120.6(2) . . ?
C14 C13 C12 120.7(2) . . ?
C14 C13 P2 125.41(17) . . ?
C12 C13 P2 113.67(16) . . ?
N1 C12 C13 117.98(19) . . ?
N1 C12 C17 124.84(19) . . ?
C13 C12 C17 117.0(2) . . ?
C9 C10 C5 121.1(2) . . ?
C16 C15 C14 117.4(2) . . ?
C16 C15 C18 120.2(2) . . ?
C14 C15 C18 122.4(2) . . ?
C3 C2 C1 116.5(2) . . ?
C3 C2 C4 111.2(2) . . ?
C1 C2 C4 112.1(2) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.18
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.089
_database_code_depnum_ccdc_archive 'CCDC 996904'
#######################################################################
#
#                 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_p201-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PNP)NiCOtBu
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H49 N Ni O P2'
_chemical_formula_weight         572.36

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 0.0063 0.0031 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0112 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1018 0.0938 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3576 1.0944 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.110(2)
_cell_length_b                   13.584(3)
_cell_length_c                   19.335(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.49(3)
_cell_angle_gamma                90.00
_cell_volume                     3049.9(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17062
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      29.55

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9572
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_process_details   'HKL3000 Scalepack'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.70000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17062
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         29.55
_reflns_number_total             8805
_reflns_number_gt                8016
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0611P)²+0.9644P] 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         8805
_refine_ls_number_parameters     327
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0321
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_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
C1 C 0.27563(9) 0.35141(9) 0.07272(6) 0.01050(19) Uani 1 1 d . . .
C2 C 0.27156(10) 0.24514(9) 0.04049(6) 0.0137(2) Uani 1 1 d . . .
C3 C 0.31211(11) 0.16636(10) 0.09865(7) 0.0195(2) Uani 1 1 d . . .
H3A H 0.3078 0.1015 0.0758 0.029 Uiso 1 1 calc R . .
H3B H 0.2626 0.1672 0.1309 0.029 Uiso 1 1 calc R . .
H3C H 0.3918 0.1799 0.1265 0.029 Uiso 1 1 calc R . .
C4 C 0.14723(11) 0.22366(11) -0.00324(7) 0.0213(3) Uani 1 1 d . . .
H4A H 0.1426 0.1574 -0.0239 0.032 Uiso 1 1 calc R . .
H4B H 0.1226 0.2720 -0.0422 0.032 Uiso 1 1 calc R . .
H4C H 0.0969 0.2278 0.0284 0.032 Uiso 1 1 calc R . .
C5 C 0.34673(11) 0.24481(11) -0.01161(7) 0.0202(3) Uani 1 1 d . . .
H5A H 0.3457 0.1790 -0.0326 0.030 Uiso 1 1 calc R . .
H5B H 0.4260 0.2624 0.0147 0.030 Uiso 1 1 calc R . .
H5C H 0.3164 0.2928 -0.0502 0.030 Uiso 1 1 calc R . .
C6 C 0.58491(9) 0.39308(9) 0.26653(6) 0.01040(19) Uani 1 1 d . . .
C7 C 0.70306(10) 0.37660(9) 0.29471(6) 0.0138(2) Uani 1 1 d . . .
H7 H 0.7522 0.3860 0.2647 0.017 Uiso 1 1 calc R . .
C8 C 0.75039(10) 0.34669(10) 0.36595(6) 0.0150(2) Uani 1 1 d . . .
C9 C 0.67593(10) 0.33571(9) 0.40871(6) 0.0141(2) Uani 1 1 d . . .
H9 H 0.7064 0.3148 0.4573 0.017 Uiso 1 1 calc R . .
C10 C 0.55866(10) 0.35428(9) 0.38263(6) 0.0122(2) Uani 1 1 d . . .
H10 H 0.5109 0.3475 0.4137 0.015 Uiso 1 1 calc R . .
C11 C 0.51004(9) 0.38314(8) 0.31038(6) 0.00905(19) Uani 1 1 d . . .
C12 C 0.87677(11) 0.32342(12) 0.39516(7) 0.0228(3) Uani 1 1 d . . .
H12A H 0.9193 0.3838 0.4136 0.034 Uiso 1 1 calc R . .
H12B H 0.9052 0.2960 0.3565 0.034 Uiso 1 1 calc R . .
H12C H 0.8880 0.2753 0.4343 0.034 Uiso 1 1 calc R . .
C13 C 0.20075(10) 0.42560(9) 0.28267(6) 0.01119(19) Uani 1 1 d . . .
C14 C 0.12264(10) 0.46435(9) 0.31668(6) 0.0145(2) Uani 1 1 d . . .
H14 H 0.0424 0.4573 0.2942 0.017 Uiso 1 1 calc R . .
C15 C 0.15925(11) 0.51289(9) 0.38260(7) 0.0162(2) Uani 1 1 d . . .
C16 C 0.27807(11) 0.52363(9) 0.41296(6) 0.0164(2) Uani 1 1 d . . .
H16 H 0.3053 0.5578 0.4574 0.020 Uiso 1 1 calc R . .
C17 C 0.35755(10) 0.48624(9) 0.38056(6) 0.0133(2) Uani 1 1 d . . .
H17 H 0.4375 0.4961 0.4027 0.016 Uiso 1 1 calc R . .
C18 C 0.32093(9) 0.43349(8) 0.31475(6) 0.01010(19) Uani 1 1 d . . .
C19 C 0.07536(13) 0.55526(11) 0.41950(8) 0.0240(3) Uani 1 1 d . . .
H19A H -0.0036 0.5447 0.3891 0.036 Uiso 1 1 calc R . .
H19B H 0.0895 0.6260 0.4272 0.036 Uiso 1 1 calc R . .
H19C H 0.0858 0.5226 0.4661 0.036 Uiso 1 1 calc R . .
C20 C 0.45204(13) 0.60621(10) 0.21564(7) 0.0201(2) Uani 1 1 d . . .
H20A H 0.4542 0.6776 0.2090 0.030 Uiso 1 1 calc R . .
H20B H 0.4941 0.5895 0.2655 0.030 Uiso 1 1 calc R . .
H20C H 0.3718 0.5846 0.2057 0.030 Uiso 1 1 calc R . .
C21 C 0.50817(10) 0.55455(9) 0.16377(6) 0.0130(2) Uani 1 1 d . . .
H21 H 0.5902 0.5765 0.1755 0.016 Uiso 1 1 calc R . .
C22 C 0.44786(12) 0.58330(10) 0.08537(7) 0.0183(2) Uani 1 1 d . . .
H22A H 0.4489 0.6551 0.0805 0.027 Uiso 1 1 calc R . .
H22B H 0.3680 0.5601 0.0722 0.027 Uiso 1 1 calc R . .
H22C H 0.4882 0.5531 0.0534 0.027 Uiso 1 1 calc R . .
C23 C 0.69668(11) 0.43680(11) 0.11195(7) 0.0205(3) Uani 1 1 d . . .
H23A H 0.7355 0.4062 0.0793 0.031 Uiso 1 1 calc R . .
H23B H 0.7506 0.4416 0.1604 0.031 Uiso 1 1 calc R . .
H23C H 0.6703 0.5028 0.0944 0.031 Uiso 1 1 calc R . .
C24 C 0.59272(10) 0.37366(9) 0.11476(6) 0.0126(2) Uani 1 1 d . . .
H24 H 0.5395 0.3741 0.0647 0.015 Uiso 1 1 calc R . .
C25 C 0.62871(11) 0.26602(10) 0.13090(7) 0.0180(2) Uani 1 1 d . . .
H25A H 0.6738 0.2445 0.0988 0.027 Uiso 1 1 calc R . .
H25B H 0.5598 0.2248 0.1230 0.027 Uiso 1 1 calc R . .
H25C H 0.6755 0.2599 0.1812 0.027 Uiso 1 1 calc R . .
C26 C 0.08820(12) 0.54980(10) 0.13328(7) 0.0211(3) Uani 1 1 d . . .
H26A H 0.0247 0.5910 0.1053 0.032 Uiso 1 1 calc R . .
H26B H 0.1480 0.5458 0.1083 0.032 Uiso 1 1 calc R . .
H26C H 0.1207 0.5788 0.1811 0.032 Uiso 1 1 calc R . .
C27 C 0.04302(10) 0.44621(9) 0.14128(6) 0.0142(2) Uani 1 1 d . . .
H27 H -0.0143 0.4521 0.1695 0.017 Uiso 1 1 calc R . .
C28 C -0.01911(10) 0.40222(11) 0.06763(7) 0.0184(2) Uani 1 1 d . . .
H28A H -0.0820 0.4460 0.0424 0.028 Uiso 1 1 calc R . .
H28B H -0.0505 0.3376 0.0743 0.028 Uiso 1 1 calc R . .
H28C H 0.0354 0.3950 0.0390 0.028 Uiso 1 1 calc R . .
C29 C 0.18989(13) 0.18714(11) 0.26009(8) 0.0243(3) Uani 1 1 d . . .
H29A H 0.1573 0.1226 0.2656 0.036 Uiso 1 1 calc R . .
H29B H 0.2105 0.2216 0.3065 0.036 Uiso 1 1 calc R . .
H29C H 0.2589 0.1784 0.2438 0.036 Uiso 1 1 calc R . .
C30 C 0.10076(10) 0.24787(9) 0.20428(6) 0.0144(2) Uani 1 1 d . . .
H30 H 0.0861 0.2131 0.1570 0.017 Uiso 1 1 calc R . .
C31 C -0.01338(12) 0.25134(11) 0.22327(8) 0.0238(3) Uani 1 1 d . . .
H31A H -0.0399 0.1841 0.2277 0.036 Uiso 1 1 calc R . .
H31B H -0.0710 0.2860 0.1851 0.036 Uiso 1 1 calc R . .
H31C H -0.0025 0.2861 0.2691 0.036 Uiso 1 1 calc R . .
N1 N 0.39282(8) 0.39499(8) 0.27716(5) 0.00950(17) Uani 1 1 d . . .
Ni1 Ni 0.332348(11) 0.372849(10) 0.172946(7) 0.00730(5) Uani 1 1 d . . .
O1 O 0.24100(8) 0.41864(7) 0.03054(4) 0.01563(17) Uani 1 1 d . . .
P1 P 0.16335(2) 0.36951(2) 0.194086(15) 0.00888(7) Uani 1 1 d . . .
P2 P 0.50651(2) 0.41922(2) 0.173592(14) 0.00781(7) 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
C1 O1 1.2169(15) . ?
C1 C2 1.5676(17) . ?
C1 Ni1 1.8858(12) . ?
C2 C3 1.5289(18) . ?
C2 C4 1.5311(17) . ?
C2 C5 1.5375(17) . ?
C6 C7 1.3970(16) . ?
C6 C11 1.4125(15) . ?
C6 P2 1.8134(13) . ?
C7 C8 1.3940(17) . ?
C8 C9 1.3936(17) . ?
C8 C12 1.5068(17) . ?
C9 C10 1.3886(16) . ?
C10 C11 1.4090(15) . ?
C11 N1 1.3914(14) . ?
C13 C14 1.3991(15) . ?
C13 C18 1.4149(16) . ?
C13 P1 1.8109(12) . ?
C14 C15 1.3909(17) . ?
C15 C16 1.3989(19) . ?
C15 C19 1.5113(17) . ?
C16 C17 1.3853(16) . ?
C17 C18 1.4173(15) . ?
C18 N1 1.3853(14) . ?
C20 C21 1.5321(17) . ?
C21 C22 1.5347(17) . ?
C21 P2 1.8489(13) . ?
C23 C24 1.5371(17) . ?
C24 C25 1.5323(18) . ?
C24 P2 1.8549(12) . ?
C26 C27 1.5334(19) . ?
C27 C28 1.5307(18) . ?
C27 P1 1.8458(12) . ?
C29 C30 1.5326(18) . ?
C30 C31 1.5283(18) . ?
C30 P1 1.8516(13) . ?
N1 Ni1 1.9620(10) . ?
Ni1 P2 2.1978(5) . ?
Ni1 P1 2.1983(5) . ?

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 C1 C2 117.30(10) . . ?
O1 C1 Ni1 121.90(9) . . ?
C2 C1 Ni1 120.79(8) . . ?
C3 C2 C4 109.46(11) . . ?
C3 C2 C5 110.71(11) . . ?
C4 C2 C5 108.05(10) . . ?
C3 C2 C1 112.63(10) . . ?
C4 C2 C1 108.06(10) . . ?
C5 C2 C1 107.79(10) . . ?
C7 C6 C11 120.76(10) . . ?
C7 C6 P2 127.45(9) . . ?
C11 C6 P2 111.64(8) . . ?
C8 C7 C6 121.36(11) . . ?
C9 C8 C7 117.62(11) . . ?
C9 C8 C12 120.97(11) . . ?
C7 C8 C12 121.37(11) . . ?
C10 C9 C8 122.17(11) . . ?
C9 C10 C11 120.48(11) . . ?
N1 C11 C10 125.06(10) . . ?
N1 C11 C6 117.16(10) . . ?
C10 C11 C6 117.57(10) . . ?
C14 C13 C18 120.93(10) . . ?
C14 C13 P1 125.58(9) . . ?
C18 C13 P1 113.37(8) . . ?
C15 C14 C13 121.79(11) . . ?
C14 C15 C16 117.16(11) . . ?
C14 C15 C19 122.06(12) . . ?
C16 C15 C19 120.75(12) . . ?
C17 C16 C15 122.40(11) . . ?
C16 C17 C18 120.71(11) . . ?
N1 C18 C13 117.57(10) . . ?
N1 C18 C17 125.36(10) . . ?
C13 C18 C17 116.92(10) . . ?
C20 C21 C22 110.78(11) . . ?
C20 C21 P2 111.61(8) . . ?
C22 C21 P2 109.78(8) . . ?
C25 C24 C23 110.56(10) . . ?
C25 C24 P2 111.75(8) . . ?
C23 C24 P2 116.40(9) . . ?
C28 C27 C26 111.08(10) . . ?
C28 C27 P1 113.37(9) . . ?
C26 C27 P1 109.00(8) . . ?
C31 C30 C29 110.59(11) . . ?
C31 C30 P1 115.06(9) . . ?
C29 C30 P1 109.12(9) . . ?
C18 N1 C11 120.82(9) . . ?
C18 N1 Ni1 119.32(7) . . ?
C11 N1 Ni1 119.40(8) . . ?
C1 Ni1 N1 179.47(4) . . ?
C1 Ni1 P2 96.85(4) . . ?
N1 Ni1 P2 82.66(4) . . ?
C1 Ni1 P1 95.80(4) . . ?
N1 Ni1 P1 84.73(4) . . ?
P2 Ni1 P1 161.339(13) . . ?
C13 P1 C27 103.41(6) . . ?
C13 P1 C30 105.95(5) . . ?
C27 P1 C30 106.26(6) . . ?
C13 P1 Ni1 99.85(5) . . ?
C27 P1 Ni1 121.06(4) . . ?
C30 P1 Ni1 117.97(4) . . ?
C6 P2 C21 106.18(5) . . ?
C6 P2 C24 108.35(6) . . ?
C21 P2 C24 104.14(5) . . ?
C6 P2 Ni1 100.44(5) . . ?
C21 P2 Ni1 108.83(4) . . ?
C24 P2 Ni1 127.38(4) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        29.55
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.075
_database_code_depnum_ccdc_archive 'CCDC 996905'
