# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Frederick Geoffrey Nethersole Cloke'
'Jennifer C Green'
'Peter B Hitchcock'
'John Nixon'
'James L Suter'
'D James Wilson'

_publ_contact_author_name        'Frederick Geoffrey Nethersole Cloke'
_publ_contact_author_email       F.G.CLOKE@SUSSEX.AC.UK

_publ_section_title              
;
ntheses, Structural studies, Photoelectron spectra
and Density Functional Theory calculations on the
"pseudo" tetraphospha-metallocenes [M(?-P2C3But3)2],
(M= Ni, Pd, Pt).
;
_publ_requested_category         FM

# Attachment 'AUG499.CIF'

data_aug499
_database_code_depnum_ccdc_archive 'CCDC 700774'

_audit_creation_date             1999-08-10T16:24:15-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_conform_dict_location     
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C30 H54 P4 Pt'
_chemical_formula_sum            'C30 H54 P4 Pt'
_chemical_formula_weight         733.7
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.4887(4)
_cell_length_b                   15.3795(4)
_cell_length_c                   15.2504(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.988(2)
_cell_angle_gamma                90
_cell_volume                     3372.99(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11489
_cell_measurement_theta_min      4.076
_cell_measurement_theta_max      27.878
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_T_max  0.805

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_reflns_number            22145
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0542
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.14
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_full        27.87
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             7982
_reflns_number_gt                5553
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+18.5204P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7982
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0523
_refine_ls_wR_factor_ref         0.1205
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_restrained_S_all      1.06
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.182
_refine_diff_density_min         -3.376
_refine_diff_density_rms         0.123

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Pt Pt 0.39037(2) 0.230537(16) 0.186188(16) 0.05416(11) Uani 1 1 d . . .
P1 P 0.29197(15) 0.18509(11) 0.05799(12) 0.0548(5) Uani 1 1 d . . .
P2 P 0.25328(17) 0.32098(13) 0.17978(14) 0.0665(6) Uani 1 1 d . . .
P3 P 0.49121(15) 0.11112(11) 0.23828(15) 0.0580(5) Uani 1 1 d . . .
P4 P 0.51121(16) 0.29295(12) 0.29629(15) 0.0629(6) Uani 1 1 d . . .
C1 C 0.1978(4) 0.1601(4) 0.1269(4) 0.0404(14) Uani 1 1 d . . .
C2 C 0.1729(4) 0.2278(4) 0.1772(4) 0.0431(14) Uani 1 1 d . . .
C3 C 0.3020(5) 0.2981(4) 0.0817(4) 0.0489(17) Uani 1 1 d . . .
C4 C 0.1633(5) 0.0652(4) 0.1099(5) 0.0507(17) Uani 1 1 d . . .
C5 C 0.2486(6) 0.0055(5) 0.1094(7) 0.074(2) Uani 1 1 d . . .
H5A H 0.2869 0.0265 0.0669 0.111 Uiso 1 1 calc R . .
H5B H 0.2283 -0.0525 0.0942 0.111 Uiso 1 1 calc R . .
H5C H 0.2837 0.0055 0.167 0.111 Uiso 1 1 calc R . .
C6 C 0.1096(8) 0.0616(7) 0.0175(7) 0.106(4) Uani 1 1 d . . .
H6A H 0.1457 0.0883 -0.0238 0.159 Uiso 1 1 calc R . .
H6B H 0.0518 0.0923 0.0173 0.159 Uiso 1 1 calc R . .
H6C H 0.0973 0.0021 0.0011 0.159 Uiso 1 1 calc R . .
C7 C 0.1093(8) 0.0234(6) 0.1777(8) 0.111(4) Uani 1 1 d . . .
H7A H 0.054 0.0566 0.1826 0.166 Uiso 1 1 calc R . .
H7B H 0.1471 0.022 0.2339 0.166 Uiso 1 1 calc R . .
H7C H 0.0925 -0.0348 0.1596 0.166 Uiso 1 1 calc R . .
C8 C 0.0891(5) 0.2407(5) 0.2312(5) 0.0516(17) Uani 1 1 d . . .
C9 C -0.0034(6) 0.2147(7) 0.1774(7) 0.082(3) Uani 1 1 d . . .
H9A H -0.0534 0.2235 0.2124 0.123 Uiso 1 1 calc R . .
H9B H -0.0011 0.1545 0.161 0.123 Uiso 1 1 calc R . .
H9C H -0.0136 0.2498 0.1251 0.123 Uiso 1 1 calc R . .
C10 C 0.1030(6) 0.1920(8) 0.3198(5) 0.088(3) Uani 1 1 d . . .
H10A H 0.0501 0.2014 0.3509 0.132 Uiso 1 1 calc R . .
H10B H 0.158 0.2132 0.3547 0.132 Uiso 1 1 calc R . .
H10C H 0.1096 0.1309 0.3091 0.132 Uiso 1 1 calc R . .
C11 C 0.0776(7) 0.3380(7) 0.2524(8) 0.104(4) Uani 1 1 d . . .
H11A H 0.0257 0.3452 0.2854 0.156 Uiso 1 1 calc R . .
H11B H 0.0667 0.3704 0.1983 0.156 Uiso 1 1 calc R . .
H11C H 0.1331 0.3589 0.2867 0.156 Uiso 1 1 calc R . .
C12 C 0.3369(5) 0.3658(4) 0.0214(4) 0.0450(15) Uani 1 1 d . . .
C13 C 0.2538(6) 0.3930(6) -0.0440(6) 0.072(2) Uani 1 1 d . . .
H13A H 0.2731 0.4361 -0.0835 0.109 Uiso 1 1 calc R . .
H13B H 0.2062 0.4168 -0.0125 0.109 Uiso 1 1 calc R . .
H13C H 0.2299 0.3432 -0.0773 0.109 Uiso 1 1 calc R . .
C14 C 0.4125(6) 0.3290(5) -0.0288(6) 0.072(2) Uani 1 1 d . . .
H14A H 0.4333 0.3732 -0.0663 0.108 Uiso 1 1 calc R . .
H14B H 0.3882 0.2807 -0.0642 0.108 Uiso 1 1 calc R . .
H14C H 0.4639 0.3098 0.0124 0.108 Uiso 1 1 calc R . .
C15 C 0.3744(6) 0.4457(5) 0.0737(5) 0.063(2) Uani 1 1 d . . .
H15A H 0.396 0.4875 0.0341 0.094 Uiso 1 1 calc R . .
H15B H 0.425 0.4288 0.1169 0.094 Uiso 1 1 calc R . .
H15C H 0.3258 0.471 0.1029 0.094 Uiso 1 1 calc R . .
C16 C 0.5778(4) 0.1751(4) 0.1883(4) 0.0419(14) Uani 1 1 d . . .
C17 C 0.5895(4) 0.2599(4) 0.2177(4) 0.0412(14) Uani 1 1 d . . .
C18 C 0.4644(5) 0.1901(4) 0.3147(4) 0.0502(17) Uani 1 1 d . . .
C19 C 0.6254(6) 0.1214(5) 0.1198(5) 0.0555(18) Uani 1 1 d . . .
C20 C 0.5988(10) 0.0249(6) 0.1221(8) 0.122(5) Uani 1 1 d . . .
H20A H 0.6173 0.002 0.1802 0.183 Uiso 1 1 calc R . .
H20B H 0.6298 -0.0066 0.0799 0.183 Uiso 1 1 calc R . .
H20C H 0.5327 0.0189 0.1078 0.183 Uiso 1 1 calc R . .
C21 C 0.5949(8) 0.1518(7) 0.0263(6) 0.095(3) Uani 1 1 d . . .
H21A H 0.625 0.1173 -0.0143 0.143 Uiso 1 1 calc R . .
H21B H 0.6118 0.2118 0.0207 0.143 Uiso 1 1 calc R . .
H21C H 0.5287 0.1458 0.0133 0.143 Uiso 1 1 calc R . .
C22 C 0.7309(7) 0.1207(8) 0.1412(7) 0.103(4) Uani 1 1 d . . .
H22A H 0.7474 0.1009 0.2008 0.154 Uiso 1 1 calc R . .
H22B H 0.7545 0.1784 0.1352 0.154 Uiso 1 1 calc R . .
H22C H 0.7572 0.0823 0.1012 0.154 Uiso 1 1 calc R . .
C23 C 0.6614(5) 0.3318(4) 0.2024(5) 0.0509(17) Uani 1 1 d . . .
C24 C 0.6831(8) 0.3426(7) 0.1068(6) 0.095(3) Uani 1 1 d . . .
H24A H 0.6265 0.3538 0.0688 0.142 Uiso 1 1 calc R . .
H24B H 0.7111 0.2902 0.0881 0.142 Uiso 1 1 calc R . .
H24C H 0.7252 0.3903 0.1037 0.142 Uiso 1 1 calc R . .
C25 C 0.7514(6) 0.3135(7) 0.2648(7) 0.088(3) Uani 1 1 d . . .
H25A H 0.797 0.357 0.2562 0.133 Uiso 1 1 calc R . .
H25B H 0.775 0.2572 0.2519 0.133 Uiso 1 1 calc R . .
H25C H 0.7382 0.315 0.3249 0.133 Uiso 1 1 calc R . .
C26 C 0.6276(6) 0.4223(5) 0.2272(7) 0.080(3) Uani 1 1 d . . .
H26A H 0.5717 0.4368 0.1896 0.12 Uiso 1 1 calc R . .
H26B H 0.6747 0.4647 0.2198 0.12 Uiso 1 1 calc R . .
H26C H 0.6153 0.4221 0.2876 0.12 Uiso 1 1 calc R . .
C27 C 0.4141(5) 0.1690(5) 0.3939(4) 0.0496(16) Uani 1 1 d . . .
C28 C 0.3424(6) 0.0968(6) 0.3725(6) 0.072(2) Uani 1 1 d . . .
H28A H 0.312 0.0849 0.4237 0.108 Uiso 1 1 calc R . .
H28B H 0.3731 0.0452 0.3557 0.108 Uiso 1 1 calc R . .
H28C H 0.2972 0.115 0.3248 0.108 Uiso 1 1 calc R . .
C29 C 0.3671(5) 0.2490(5) 0.4274(5) 0.062(2) Uani 1 1 d . . .
H29A H 0.3358 0.2332 0.4771 0.092 Uiso 1 1 calc R . .
H29B H 0.3228 0.2717 0.3812 0.092 Uiso 1 1 calc R . .
H29C H 0.4132 0.2925 0.4451 0.092 Uiso 1 1 calc R . .
C30 C 0.4884(7) 0.1355(7) 0.4672(6) 0.084(3) Uani 1 1 d . . .
H30A H 0.4595 0.1209 0.5186 0.126 Uiso 1 1 calc R . .
H30B H 0.5342 0.18 0.4819 0.126 Uiso 1 1 calc R . .
H30C H 0.5179 0.0848 0.4466 0.126 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt 0.1025(3) 0.02907(13) 0.03293(13) 0.00155(11) 0.01638(12) 0.00610(14)
P1 0.0852(14) 0.0378(9) 0.0486(10) -0.0117(8) 0.0370(10) -0.0130(9)
P2 0.0967(17) 0.0488(10) 0.0645(12) -0.0225(9) 0.0522(12) -0.0289(11)
P3 0.0646(13) 0.0321(8) 0.0832(14) -0.0067(9) 0.0334(11) -0.0060(8)
P4 0.0798(15) 0.0356(9) 0.0833(14) -0.0124(9) 0.0509(12) -0.0110(9)
C1 0.045(4) 0.042(3) 0.034(3) 0.002(3) 0.008(3) -0.007(3)
C2 0.049(4) 0.046(3) 0.037(3) -0.001(3) 0.016(3) -0.014(3)
C3 0.073(5) 0.033(3) 0.046(3) 0.001(3) 0.029(3) -0.007(3)
C4 0.055(4) 0.042(3) 0.056(4) 0.002(3) 0.010(3) -0.019(3)
C5 0.078(6) 0.040(4) 0.106(7) -0.007(4) 0.020(5) -0.006(4)
C6 0.131(10) 0.075(6) 0.096(7) -0.016(6) -0.046(7) -0.026(6)
C7 0.131(10) 0.054(5) 0.165(11) 0.012(6) 0.087(9) -0.023(6)
C8 0.043(4) 0.060(4) 0.055(4) -0.004(3) 0.018(3) -0.005(3)
C9 0.046(5) 0.095(7) 0.105(7) -0.006(6) 0.006(5) 0.004(5)
C10 0.063(6) 0.149(9) 0.059(5) 0.021(5) 0.037(4) 0.012(6)
C11 0.088(7) 0.084(7) 0.153(10) -0.032(7) 0.065(7) -0.003(6)
C12 0.054(4) 0.040(3) 0.044(3) 0.013(3) 0.016(3) 0.003(3)
C13 0.066(6) 0.068(5) 0.081(6) 0.018(5) 0.002(4) 0.001(4)
C14 0.076(6) 0.061(5) 0.088(6) 0.017(4) 0.050(5) 0.007(4)
C15 0.066(5) 0.046(4) 0.077(5) 0.015(4) 0.014(4) -0.012(4)
C16 0.043(4) 0.037(3) 0.048(3) 0.001(3) 0.014(3) 0.008(3)
C17 0.042(4) 0.036(3) 0.047(3) 0.002(3) 0.012(3) 0.002(3)
C18 0.066(5) 0.038(3) 0.050(4) 0.002(3) 0.023(3) -0.005(3)
C19 0.073(5) 0.045(4) 0.052(4) -0.005(3) 0.024(4) 0.019(3)
C20 0.189(13) 0.046(5) 0.152(11) -0.021(6) 0.105(10) 0.008(6)
C21 0.137(9) 0.094(7) 0.057(5) -0.011(5) 0.022(6) 0.037(7)
C22 0.083(7) 0.118(9) 0.110(8) -0.021(7) 0.022(6) 0.050(6)
C23 0.050(4) 0.045(4) 0.059(4) 0.006(3) 0.013(3) -0.011(3)
C24 0.131(9) 0.085(7) 0.077(6) 0.006(5) 0.048(6) -0.041(6)
C25 0.059(6) 0.095(7) 0.107(7) 0.017(6) -0.010(5) -0.022(5)
C26 0.081(6) 0.047(4) 0.115(8) 0.001(5) 0.025(5) -0.022(4)
C27 0.050(4) 0.057(4) 0.044(3) 0.010(3) 0.015(3) 0.000(3)
C28 0.073(6) 0.072(5) 0.075(5) 0.014(4) 0.029(4) -0.026(4)
C29 0.061(5) 0.079(5) 0.049(4) 0.000(4) 0.023(3) 0.001(4)
C30 0.079(7) 0.103(7) 0.069(5) 0.013(5) 0.007(5) 0.011(5)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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
Pt C3 2.182(7) . ?
Pt C18 2.207(7) . ?
Pt P1 2.380(2) . ?
Pt P2 2.417(3) . ?
Pt P3 2.420(2) . ?
Pt P4 2.468(2) . ?
P1 C3 1.777(7) . ?
P1 C1 1.861(6) . ?
P2 C3 1.765(6) . ?
P2 C2 1.844(6) . ?
P3 C18 1.760(7) . ?
P3 C16 1.832(6) . ?
P4 C18 1.757(7) . ?
P4 C17 1.820(6) . ?
C1 C2 1.368(9) . ?
C1 C4 1.555(9) . ?
C2 C8 1.560(9) . ?
C3 C12 1.517(8) . ?
C4 C7 1.514(11) . ?
C4 C6 1.525(11) . ?
C4 C5 1.539(11) . ?
C8 C10 1.536(11) . ?
C8 C9 1.538(11) . ?
C8 C11 1.544(12) . ?
C12 C14 1.522(9) . ?
C12 C13 1.525(10) . ?
C12 C15 1.527(10) . ?
C16 C17 1.383(8) . ?
C16 C19 1.558(8) . ?
C17 C23 1.556(9) . ?
C18 C27 1.519(9) . ?
C19 C21 1.514(11) . ?
C19 C22 1.524(12) . ?
C19 C20 1.535(11) . ?
C23 C24 1.538(10) . ?
C23 C26 1.538(11) . ?
C23 C25 1.543(11) . ?
C27 C29 1.524(10) . ?
C27 C28 1.527(10) . ?
C27 C30 1.543(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 Pt C18 164.1(2) . . ?
C3 Pt P1 45.59(18) . . ?
C18 Pt P1 145.57(18) . . ?
C3 Pt P2 44.76(17) . . ?
C18 Pt P2 120.42(18) . . ?
P1 Pt P2 74.25(7) . . ?
C3 Pt P3 151.43(17) . . ?
C18 Pt P3 44.41(18) . . ?
P1 Pt P3 108.91(7) . . ?
P2 Pt P3 155.55(6) . . ?
C3 Pt P4 128.07(18) . . ?
C18 Pt P4 43.72(18) . . ?
P1 Pt P4 167.83(6) . . ?
P2 Pt P4 108.37(7) . . ?
P3 Pt P4 73.85(7) . . ?
C3 P1 C1 97.7(3) . . ?
C3 P1 Pt 61.3(2) . . ?
C1 P1 Pt 90.2(2) . . ?
C3 P2 C2 98.2(3) . . ?
C3 P2 Pt 60.5(3) . . ?
C2 P2 Pt 93.9(2) . . ?
C18 P3 C16 97.0(3) . . ?
C18 P3 Pt 61.4(2) . . ?
C16 P3 Pt 82.6(2) . . ?
C18 P4 C17 97.9(3) . . ?
C18 P4 Pt 60.2(2) . . ?
C17 P4 Pt 83.7(2) . . ?
C2 C1 C4 135.0(6) . . ?
C2 C1 P1 114.9(4) . . ?
C4 C1 P1 110.0(4) . . ?
C1 C2 C8 131.9(6) . . ?
C1 C2 P2 113.2(4) . . ?
C8 C2 P2 114.9(5) . . ?
C12 C3 P2 125.0(5) . . ?
C12 C3 P1 125.0(5) . . ?
P2 C3 P1 109.7(3) . . ?
C12 C3 Pt 124.1(5) . . ?
P2 C3 Pt 74.7(3) . . ?
P1 C3 Pt 73.1(2) . . ?
C7 C4 C6 111.6(8) . . ?
C7 C4 C5 103.4(7) . . ?
C6 C4 C5 107.1(7) . . ?
C7 C4 C1 117.8(6) . . ?
C6 C4 C1 107.8(6) . . ?
C5 C4 C1 108.6(6) . . ?
C10 C8 C9 110.8(7) . . ?
C10 C8 C11 107.1(8) . . ?
C9 C8 C11 104.7(7) . . ?
C10 C8 C2 112.0(6) . . ?
C9 C8 C2 111.6(6) . . ?
C11 C8 C2 110.2(6) . . ?
C3 C12 C14 111.3(6) . . ?
C3 C12 C13 106.9(6) . . ?
C14 C12 C13 109.4(6) . . ?
C3 C12 C15 111.1(5) . . ?
C14 C12 C15 109.2(6) . . ?
C13 C12 C15 108.9(6) . . ?
C17 C16 C19 132.2(6) . . ?
C17 C16 P3 115.8(5) . . ?
C19 C16 P3 112.1(5) . . ?
C16 C17 C23 132.8(6) . . ?
C16 C17 P4 114.5(5) . . ?
C23 C17 P4 112.5(4) . . ?
C27 C18 P4 123.5(5) . . ?
C27 C18 P3 123.0(5) . . ?
P4 C18 P3 113.2(4) . . ?
C27 C18 Pt 122.5(5) . . ?
P4 C18 Pt 76.1(3) . . ?
P3 C18 Pt 74.2(3) . . ?
C21 C19 C22 112.0(8) . . ?
C21 C19 C20 106.0(8) . . ?
C22 C19 C20 103.7(8) . . ?
C21 C19 C16 111.4(6) . . ?
C22 C19 C16 112.0(7) . . ?
C20 C19 C16 111.4(6) . . ?
C24 C23 C26 104.1(7) . . ?
C24 C23 C25 110.5(8) . . ?
C26 C23 C25 106.5(7) . . ?
C24 C23 C17 115.8(6) . . ?
C26 C23 C17 111.5(6) . . ?
C25 C23 C17 108.1(6) . . ?
C18 C27 C29 111.7(6) . . ?
C18 C27 C28 111.4(6) . . ?
C29 C27 C28 109.8(6) . . ?
C18 C27 C30 106.6(6) . . ?
C29 C27 C30 109.1(6) . . ?
C28 C27 C30 108.0(7) . . ?

#===END

# Attachment 'MAR499.CIF'

data_mar499
_database_code_depnum_ccdc_archive 'CCDC 700775'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C30 H54 P4 Pd'
_chemical_formula_sum            'C30 H54 P4 Pd'
_chemical_formula_weight         645.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_number     14

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                   11.046(3)
_cell_length_b                   28.537(9)
_cell_length_c                   16.175(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.12(2)
_cell_angle_gamma                90.00
_cell_volume                     4922(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      7
_cell_measurement_theta_max      10

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2040
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was 1
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_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       '\k-geometry diffractometer'
_diffrn_measurement_device_t     'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_standards_number         2
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7228
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_sigmaI/netI    0.1895
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         23.00
_reflns_number_total             6830
_reflns_number_gt                3571
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Enraf-Nonius CAD4'
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93

_refine_special_details          
;
There are two independent molecules; one in a general position and the other
on an inversion centre.

Uij constraints (DELU) were introduced to stop a small number of C atoms
going non-positive-definite.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6830
_refine_ls_number_parameters     475
_refine_ls_number_restraints     186
_refine_ls_R_factor_all          0.1689
_refine_ls_R_factor_gt           0.0754
_refine_ls_wR_factor_ref         0.1780
_refine_ls_wR_factor_gt          0.1398
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.976
_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
Pd1 Pd 0.48578(10) 0.33891(3) 0.48315(6) 0.0219(3) Uani 1 1 d U . .
P1 P 0.2930(3) 0.29742(11) 0.48078(19) 0.0234(8) Uani 1 1 d U . .
P2 P 0.3700(3) 0.38712(11) 0.56410(19) 0.0247(8) Uani 1 1 d U . .
P3 P 0.5908(3) 0.29303(11) 0.39690(19) 0.0242(8) Uani 1 1 d U . .
P4 P 0.6943(3) 0.37399(11) 0.5009(2) 0.0263(8) Uani 1 1 d U . .
C1 C 0.3708(10) 0.3267(4) 0.5736(7) 0.023(2) Uani 1 1 d U . .
C2 C 0.2398(11) 0.3910(4) 0.4653(7) 0.024(2) Uani 1 1 d U . .
C3 C 0.2114(10) 0.3495(4) 0.4249(7) 0.023(2) Uani 1 1 d U . .
C4 C 0.4330(11) 0.3006(4) 0.6584(7) 0.023(2) Uani 1 1 d U . .
C5 C 0.5282(11) 0.3334(4) 0.7174(7) 0.026(3) Uani 1 1 d U . .
H5A H 0.5950 0.3413 0.6900 0.039 Uiso 1 1 calc R . .
H5B H 0.5646 0.3176 0.7720 0.039 Uiso 1 1 calc R . .
H5C H 0.4857 0.3621 0.7276 0.039 Uiso 1 1 calc R . .
C6 C 0.3324(12) 0.2887(4) 0.7022(8) 0.033(3) Uani 1 1 d U . .
H6A H 0.3700 0.2724 0.7562 0.050 Uiso 1 1 calc R . .
H6B H 0.2698 0.2683 0.6650 0.050 Uiso 1 1 calc R . .
H6C H 0.2919 0.3175 0.7141 0.050 Uiso 1 1 calc R . .
C7 C 0.4990(12) 0.2554(4) 0.6436(7) 0.028(3) Uani 1 1 d U . .
H7A H 0.5651 0.2629 0.6154 0.041 Uiso 1 1 calc R . .
H7B H 0.4380 0.2342 0.6072 0.041 Uiso 1 1 calc R . .
H7C H 0.5362 0.2403 0.6987 0.041 Uiso 1 1 calc R . .
C8 C 0.1836(11) 0.4403(4) 0.4474(7) 0.026(3) Uani 1 1 d U . .
C9 C 0.0432(11) 0.4382(5) 0.4395(8) 0.038(3) Uani 1 1 d U . .
H9A H 0.0285 0.4223 0.4896 0.057 Uiso 1 1 calc R . .
H9B H 0.0014 0.4210 0.3875 0.057 Uiso 1 1 calc R . .
H9C H 0.0095 0.4702 0.4362 0.057 Uiso 1 1 calc R . .
C10 C 0.2408(15) 0.4742(5) 0.5227(8) 0.060(5) Uani 1 1 d U . .
H10A H 0.2269 0.4616 0.5758 0.091 Uiso 1 1 calc R . .
H10B H 0.2006 0.5050 0.5109 0.091 Uiso 1 1 calc R . .
H10C H 0.3311 0.4774 0.5289 0.091 Uiso 1 1 calc R . .
C11 C 0.2106(12) 0.4652(4) 0.3703(8) 0.037(3) Uani 1 1 d U . .
H11A H 0.1699 0.4959 0.3630 0.056 Uiso 1 1 calc R . .
H11B H 0.1780 0.4463 0.3187 0.056 Uiso 1 1 calc R . .
H11C H 0.3014 0.4692 0.3800 0.056 Uiso 1 1 calc R . .
C12 C 0.1101(11) 0.3338(5) 0.3408(7) 0.030(3) Uani 1 1 d U . .
C13 C -0.0048(12) 0.3166(5) 0.3667(8) 0.043(3) Uani 1 1 d U . .
H13A H 0.0204 0.2930 0.4118 0.065 Uiso 1 1 calc R . .
H13B H -0.0642 0.3027 0.3169 0.065 Uiso 1 1 calc R . .
H13C H -0.0448 0.3430 0.3879 0.065 Uiso 1 1 calc R . .
C14 C 0.0715(13) 0.3707(4) 0.2691(7) 0.038(3) Uani 1 1 d U . .
H14A H 0.1461 0.3815 0.2525 0.057 Uiso 1 1 calc R . .
H14B H 0.0317 0.3974 0.2898 0.057 Uiso 1 1 calc R . .
H14C H 0.0122 0.3567 0.2194 0.057 Uiso 1 1 calc R . .
C15 C 0.1596(12) 0.2932(4) 0.2980(7) 0.035(3) Uani 1 1 d U . .
H15A H 0.2342 0.3034 0.2807 0.052 Uiso 1 1 calc R . .
H15B H 0.0948 0.2832 0.2473 0.052 Uiso 1 1 calc R . .
H15C H 0.1816 0.2671 0.3383 0.052 Uiso 1 1 calc R . .
C16 C 0.6116(11) 0.3526(4) 0.3990(7) 0.023(2) Uani 1 1 d U . .
C17 C 0.7115(10) 0.2789(4) 0.4979(6) 0.018(2) Uani 1 1 d U . .
C18 C 0.7598(11) 0.3177(4) 0.5440(7) 0.026(3) Uani 1 1 d U . .
C19 C 0.5645(12) 0.3857(4) 0.3223(7) 0.028(3) Uani 1 1 d U . .
C20 C 0.4342(11) 0.3706(4) 0.2677(8) 0.037(3) Uani 1 1 d U . .
H20A H 0.4365 0.3375 0.2524 0.055 Uiso 1 1 calc R . .
H20B H 0.4112 0.3896 0.2155 0.055 Uiso 1 1 calc R . .
H20C H 0.3721 0.3752 0.3006 0.055 Uiso 1 1 calc R . .
C21 C 0.5599(12) 0.4366(4) 0.3480(8) 0.035(3) Uani 1 1 d U . .
H21A H 0.6427 0.4462 0.3829 0.053 Uiso 1 1 calc R . .
H21B H 0.4980 0.4403 0.3813 0.053 Uiso 1 1 calc R . .
H21C H 0.5361 0.4561 0.2965 0.053 Uiso 1 1 calc R . .
C22 C 0.6582(14) 0.3809(5) 0.2684(8) 0.052(4) Uani 1 1 d U . .
H22A H 0.6608 0.3483 0.2503 0.078 Uiso 1 1 calc R . .
H22B H 0.7416 0.3904 0.3025 0.078 Uiso 1 1 calc R . .
H22C H 0.6325 0.4011 0.2178 0.078 Uiso 1 1 calc R . .
C23 C 0.7352(11) 0.2252(4) 0.5008(7) 0.029(3) Uani 1 1 d U . .
C24 C 0.8037(13) 0.2034(5) 0.5859(8) 0.046(4) Uani 1 1 d U . .
H24A H 0.8843 0.2193 0.6082 0.069 Uiso 1 1 calc R . .
H24B H 0.8183 0.1701 0.5776 0.069 Uiso 1 1 calc R . .
H24C H 0.7527 0.2068 0.6269 0.069 Uiso 1 1 calc R . .
C25 C 0.6150(12) 0.1987(4) 0.4714(7) 0.032(3) Uani 1 1 d U . .
H25A H 0.6328 0.1650 0.4735 0.048 Uiso 1 1 calc R . .
H25B H 0.5728 0.2078 0.4126 0.048 Uiso 1 1 calc R . .
H25C H 0.5607 0.2059 0.5090 0.048 Uiso 1 1 calc R . .
C26 C 0.8159(13) 0.2160(5) 0.4371(8) 0.043(4) Uani 1 1 d U . .
H26A H 0.8953 0.2331 0.4558 0.064 Uiso 1 1 calc R . .
H26B H 0.7705 0.2267 0.3799 0.064 Uiso 1 1 calc R . .
H26C H 0.8330 0.1823 0.4354 0.064 Uiso 1 1 calc R . .
C27 C 0.8720(11) 0.3224(5) 0.6269(7) 0.029(3) Uani 1 1 d U . .
C28 C 0.8964(12) 0.3734(5) 0.6534(8) 0.042(3) Uani 1 1 d U . .
H28A H 0.8217 0.3867 0.6665 0.063 Uiso 1 1 calc R . .
H28B H 0.9157 0.3911 0.6066 0.063 Uiso 1 1 calc R . .
H28C H 0.9675 0.3753 0.7043 0.063 Uiso 1 1 calc R . .
C29 C 0.8469(13) 0.2966(5) 0.7042(7) 0.039(3) Uani 1 1 d U . .
H29A H 0.7702 0.3089 0.7159 0.059 Uiso 1 1 calc R . .
H29B H 0.9177 0.3014 0.7545 0.059 Uiso 1 1 calc R . .
H29C H 0.8367 0.2630 0.6916 0.059 Uiso 1 1 calc R . .
C30 C 0.9945(12) 0.3052(5) 0.6081(8) 0.046(4) Uani 1 1 d U . .
H30A H 1.0099 0.3231 0.5601 0.069 Uiso 1 1 calc R . .
H30B H 0.9869 0.2719 0.5933 0.069 Uiso 1 1 calc R . .
H30C H 1.0645 0.3099 0.6589 0.069 Uiso 1 1 calc R . .
Pd2 Pd 0.0000 0.5000 0.0000 0.0209(3) Uani 1 2 d SU . .
P5 P -0.0168(3) 0.49222(11) -0.15311(19) 0.0230(8) Uani 1 1 d U . .
P6 P -0.0317(3) 0.41650(11) -0.0359(2) 0.0241(8) Uani 1 1 d U . .
C31 C -0.1153(10) 0.4585(4) -0.1074(7) 0.021(2) Uani 1 1 d U . .
C32 C 0.1202(11) 0.4536(4) -0.1271(7) 0.021(2) Uani 1 1 d U . .
C33 C 0.1154(10) 0.4181(4) -0.0699(7) 0.020(2) Uani 1 1 d U . .
C34 C -0.2575(11) 0.4638(4) -0.1295(8) 0.027(3) Uani 1 1 d U . .
C35 C -0.2943(10) 0.5152(4) -0.1314(8) 0.031(3) Uani 1 1 d U . .
H35A H -0.2593 0.5291 -0.0748 0.046 Uiso 1 1 calc R . .
H35B H -0.3859 0.5179 -0.1467 0.046 Uiso 1 1 calc R . .
H35C H -0.2614 0.5318 -0.1740 0.046 Uiso 1 1 calc R . .
C36 C -0.3087(12) 0.4442(5) -0.2173(9) 0.054(4) Uani 1 1 d U . .
H36A H -0.4004 0.4468 -0.2334 0.080 Uiso 1 1 calc R . .
H36B H -0.2850 0.4111 -0.2177 0.080 Uiso 1 1 calc R . .
H36C H -0.2745 0.4616 -0.2582 0.080 Uiso 1 1 calc R . .
C37 C -0.3095(13) 0.4377(5) -0.0664(10) 0.055(4) Uani 1 1 d U . .
H37A H -0.2724 0.4499 -0.0087 0.082 Uiso 1 1 calc R . .
H37B H -0.2896 0.4043 -0.0683 0.082 Uiso 1 1 calc R . .
H37C H -0.4008 0.4418 -0.0807 0.082 Uiso 1 1 calc R . .
C38 C 0.2190(11) 0.4640(4) -0.1765(7) 0.027(3) Uani 1 1 d U . .
C39 C 0.3374(12) 0.4873(5) -0.1210(8) 0.045(4) Uani 1 1 d U . .
H39A H 0.3973 0.4925 -0.1553 0.068 Uiso 1 1 calc R . .
H39B H 0.3754 0.4669 -0.0724 0.068 Uiso 1 1 calc R . .
H39C H 0.3153 0.5174 -0.0997 0.068 Uiso 1 1 calc R . .
C40 C 0.1663(13) 0.5012(6) -0.2475(9) 0.055(4) Uani 1 1 d U . .
H40A H 0.0884 0.4896 -0.2860 0.083 Uiso 1 1 calc R . .
H40B H 0.2281 0.5070 -0.2803 0.083 Uiso 1 1 calc R . .
H40C H 0.1496 0.5305 -0.2208 0.083 Uiso 1 1 calc R . .
C41 C 0.2524(13) 0.4210(5) -0.2238(8) 0.050(4) Uani 1 1 d U . .
H41A H 0.1752 0.4064 -0.2579 0.076 Uiso 1 1 calc R . .
H41B H 0.2993 0.3984 -0.1819 0.076 Uiso 1 1 calc R . .
H41C H 0.3039 0.4310 -0.2616 0.076 Uiso 1 1 calc R . .
C42 C 0.2019(12) 0.3757(4) -0.0335(7) 0.028(3) Uani 1 1 d U . .
C43 C 0.1639(14) 0.3348(4) -0.0949(8) 0.047(4) Uani 1 1 d U . .
H43A H 0.0737 0.3291 -0.1052 0.070 Uiso 1 1 calc R . .
H43B H 0.2104 0.3067 -0.0700 0.070 Uiso 1 1 calc R . .
H43C H 0.1831 0.3422 -0.1493 0.070 Uiso 1 1 calc R . .
C44 C 0.3446(12) 0.3850(5) -0.0150(8) 0.041(3) Uani 1 1 d U . .
H44A H 0.3675 0.4114 0.0247 0.062 Uiso 1 1 calc R . .
H44B H 0.3659 0.3924 -0.0687 0.062 Uiso 1 1 calc R . .
H44C H 0.3908 0.3569 0.0106 0.062 Uiso 1 1 calc R . .
C45 C 0.1773(12) 0.3594(4) 0.0527(7) 0.033(3) Uani 1 1 d U . .
H45A H 0.0880 0.3523 0.0438 0.049 Uiso 1 1 calc R . .
H45B H 0.2013 0.3845 0.0953 0.049 Uiso 1 1 calc R . .
H45C H 0.2270 0.3313 0.0733 0.049 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0270(6) 0.0257(6) 0.0130(5) -0.0030(4) 0.0051(4) -0.0041(5)
P1 0.0215(18) 0.0277(19) 0.0164(17) -0.0028(14) -0.0032(14) -0.0015(15)
P2 0.0261(19) 0.0285(19) 0.0159(17) -0.0036(14) -0.0009(14) 0.0031(15)
P3 0.0230(19) 0.0307(19) 0.0143(17) -0.0014(14) -0.0034(14) 0.0001(15)
P4 0.0250(19) 0.0269(19) 0.0223(18) -0.0032(14) -0.0025(15) -0.0050(15)
C1 0.016(6) 0.033(5) 0.016(5) 0.000(4) 0.000(3) 0.004(5)
C2 0.018(6) 0.038(5) 0.014(6) 0.002(4) 0.001(5) 0.010(5)
C3 0.017(5) 0.042(6) 0.012(5) -0.001(4) 0.005(4) 0.008(5)
C4 0.021(7) 0.033(7) 0.014(5) 0.008(4) 0.004(4) 0.005(5)
C5 0.031(7) 0.030(7) 0.016(6) 0.005(5) 0.005(5) 0.003(5)
C6 0.033(7) 0.041(8) 0.027(7) 0.009(6) 0.010(6) 0.007(6)
C7 0.040(8) 0.030(6) 0.018(6) 0.005(5) 0.015(6) 0.006(5)
C8 0.030(6) 0.037(6) 0.006(5) 0.002(4) -0.006(5) 0.006(6)
C9 0.033(6) 0.055(9) 0.029(8) 0.012(6) 0.013(6) 0.023(6)
C10 0.085(11) 0.036(8) 0.037(7) -0.003(6) -0.026(8) 0.022(8)
C11 0.042(8) 0.034(8) 0.038(7) 0.013(6) 0.018(7) 0.010(7)
C12 0.027(7) 0.042(8) 0.014(6) 0.002(5) -0.007(4) -0.004(6)
C13 0.032(7) 0.060(10) 0.034(8) -0.006(7) 0.002(6) -0.012(7)
C14 0.057(10) 0.041(8) 0.008(6) -0.004(5) -0.006(6) 0.005(7)
C15 0.034(8) 0.036(7) 0.021(7) -0.011(5) -0.015(6) -0.007(6)
C16 0.019(6) 0.030(5) 0.018(5) 0.004(4) 0.001(4) 0.006(5)
C17 0.011(6) 0.035(5) 0.007(5) 0.006(4) 0.001(4) -0.003(4)
C18 0.022(5) 0.042(6) 0.009(5) 0.003(5) -0.004(4) -0.005(5)
C19 0.035(7) 0.037(6) 0.010(5) 0.001(5) 0.004(4) -0.005(6)
C20 0.033(7) 0.039(8) 0.027(7) 0.007(6) -0.011(5) 0.000(6)
C21 0.034(8) 0.030(6) 0.032(8) 0.011(5) -0.009(6) 0.000(6)
C22 0.052(8) 0.072(11) 0.039(9) 0.012(7) 0.025(7) 0.003(8)
C23 0.029(7) 0.038(6) 0.019(6) 0.007(5) 0.005(5) 0.010(5)
C24 0.055(9) 0.042(9) 0.036(7) 0.018(6) 0.006(6) 0.013(7)
C25 0.046(7) 0.025(7) 0.025(7) -0.005(6) 0.010(6) 0.005(6)
C26 0.049(9) 0.039(8) 0.047(8) 0.015(7) 0.023(7) 0.020(7)
C27 0.011(6) 0.060(8) 0.013(6) -0.004(5) -0.006(4) 0.000(6)
C28 0.032(8) 0.066(8) 0.019(7) -0.013(6) -0.008(6) -0.007(7)
C29 0.039(9) 0.062(9) 0.016(6) 0.002(6) 0.004(6) 0.009(7)
C30 0.025(6) 0.079(11) 0.031(8) -0.002(7) 0.003(6) 0.006(7)
Pd2 0.0228(8) 0.0211(7) 0.0167(8) 0.0024(6) 0.0017(6) -0.0005(7)
P5 0.0196(17) 0.030(2) 0.0188(17) 0.0042(14) 0.0046(14) 0.0034(15)
P6 0.0226(18) 0.0222(17) 0.0287(19) 0.0049(14) 0.0089(15) 0.0004(15)
C31 0.020(5) 0.020(6) 0.023(6) -0.006(4) 0.004(4) 0.000(4)
C32 0.019(5) 0.029(7) 0.016(6) 0.002(4) 0.004(5) 0.008(5)
C33 0.018(5) 0.019(6) 0.020(6) -0.006(4) 0.000(5) -0.003(4)
C34 0.017(5) 0.022(6) 0.041(7) -0.016(5) 0.007(5) -0.007(5)
C35 0.003(6) 0.038(6) 0.047(8) -0.006(6) -0.003(6) 0.001(5)
C36 0.015(7) 0.068(10) 0.071(8) -0.039(8) -0.002(6) -0.016(7)
C37 0.024(8) 0.053(9) 0.094(10) 0.023(8) 0.027(8) 0.006(7)
C38 0.020(6) 0.034(7) 0.030(7) -0.002(5) 0.010(5) -0.002(5)
C39 0.032(7) 0.068(11) 0.037(8) -0.004(7) 0.012(6) -0.008(7)
C40 0.045(9) 0.072(9) 0.054(9) 0.035(8) 0.022(6) -0.002(8)
C41 0.047(9) 0.075(9) 0.035(9) -0.016(7) 0.022(7) 0.009(7)
C42 0.033(6) 0.023(7) 0.026(7) 0.001(5) 0.005(6) 0.020(5)
C43 0.067(10) 0.034(7) 0.036(7) -0.015(6) 0.007(7) 0.021(7)
C44 0.036(6) 0.058(10) 0.029(8) 0.008(7) 0.005(6) 0.017(6)
C45 0.037(8) 0.029(8) 0.029(6) 0.000(5) 0.003(6) 0.009(6)

_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
Pd1 C1 2.201(11) . ?
Pd1 C16 2.219(11) . ?
Pd1 P3 2.419(3) . ?
Pd1 P1 2.428(4) . ?
Pd1 P4 2.459(4) . ?
Pd1 P2 2.473(3) . ?
P1 C1 1.738(11) . ?
P1 C3 1.848(12) . ?
P2 C1 1.731(12) . ?
P2 C2 1.853(11) . ?
P3 C16 1.715(12) . ?
P3 C17 1.864(11) . ?
P4 C16 1.770(11) . ?
P4 C18 1.823(12) . ?
C1 C4 1.553(15) . ?
C2 C3 1.349(16) . ?
C2 C8 1.535(16) . ?
C3 C12 1.584(15) . ?
C4 C6 1.506(16) . ?
C4 C7 1.531(15) . ?
C4 C5 1.539(15) . ?
C8 C9 1.523(16) . ?
C8 C11 1.530(15) . ?
C8 C10 1.555(16) . ?
C12 C13 1.519(17) . ?
C12 C15 1.523(17) . ?
C12 C14 1.542(16) . ?
C16 C19 1.537(15) . ?
C17 C18 1.364(16) . ?
C17 C23 1.552(16) . ?
C18 C27 1.576(15) . ?
C19 C21 1.515(16) . ?
C19 C22 1.523(17) . ?
C19 C20 1.540(16) . ?
C23 C25 1.494(16) . ?
C23 C24 1.521(15) . ?
C23 C26 1.551(16) . ?
C27 C28 1.521(17) . ?
C27 C29 1.538(16) . ?
C27 C30 1.542(17) . ?
Pd2 C31 2.211(11) . ?
Pd2 C31 2.211(11) 3_565 ?
Pd2 P5 2.445(3) . ?
Pd2 P5 2.445(3) 3_565 ?
Pd2 P6 2.456(3) . ?
Pd2 P6 2.456(3) 3_565 ?
P5 C31 1.753(12) . ?
P5 C32 1.831(11) . ?
P6 C31 1.752(11) . ?
P6 C33 1.847(12) . ?
C31 C34 1.525(15) . ?
C32 C33 1.383(15) . ?
C32 C38 1.539(16) . ?
C33 C42 1.559(15) . ?
C34 C36 1.493(16) . ?
C34 C37 1.495(17) . ?
C34 C35 1.519(16) . ?
C38 C39 1.532(16) . ?
C38 C41 1.540(17) . ?
C38 C40 1.562(17) . ?
C42 C43 1.519(16) . ?
C42 C44 1.549(17) . ?
C42 C45 1.560(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 C16 176.3(4) . . ?
C1 Pd1 P3 138.1(3) . . ?
C16 Pd1 P3 43.1(3) . . ?
C1 Pd1 P1 43.7(3) . . ?
C16 Pd1 P1 139.8(3) . . ?
P3 Pd1 P1 106.12(12) . . ?
C1 Pd1 P4 132.2(3) . . ?
C16 Pd1 P4 44.1(3) . . ?
P3 Pd1 P4 73.25(12) . . ?
P1 Pd1 P4 172.51(11) . . ?
C1 Pd1 P2 43.0(3) . . ?
C16 Pd1 P2 136.0(3) . . ?
P3 Pd1 P2 176.90(11) . . ?
P1 Pd1 P2 72.97(12) . . ?
P4 Pd1 P2 108.05(12) . . ?
C1 P1 C3 96.0(5) . . ?
C1 P1 Pd1 61.2(4) . . ?
C3 P1 Pd1 85.9(4) . . ?
C1 P2 C2 96.9(5) . . ?
C1 P2 Pd1 60.1(4) . . ?
C2 P2 Pd1 88.2(4) . . ?
C16 P3 C17 97.8(5) . . ?
C16 P3 Pd1 62.2(4) . . ?
C17 P3 Pd1 87.3(4) . . ?
C16 P4 C18 96.3(5) . . ?
C16 P4 Pd1 60.7(4) . . ?
C18 P4 Pd1 87.3(4) . . ?
C4 C1 P2 123.1(8) . . ?
C4 C1 P1 122.5(9) . . ?
P2 C1 P1 114.3(6) . . ?
C4 C1 Pd1 117.6(7) . . ?
P2 C1 Pd1 76.9(4) . . ?
P1 C1 Pd1 75.1(4) . . ?
C3 C2 C8 132.9(10) . . ?
C3 C2 P2 113.3(9) . . ?
C8 C2 P2 113.7(8) . . ?
C2 C3 C12 133.4(11) . . ?
C2 C3 P1 116.5(8) . . ?
C12 C3 P1 109.8(8) . . ?
C6 C4 C7 108.9(10) . . ?
C6 C4 C5 108.3(9) . . ?
C7 C4 C5 109.5(10) . . ?
C6 C4 C1 108.2(9) . . ?
C7 C4 C1 112.6(9) . . ?
C5 C4 C1 109.2(9) . . ?
C9 C8 C11 111.1(10) . . ?
C9 C8 C2 109.5(10) . . ?
C11 C8 C2 115.1(10) . . ?
C9 C8 C10 106.7(11) . . ?
C11 C8 C10 102.9(11) . . ?
C2 C8 C10 111.1(9) . . ?
C13 C12 C15 107.7(11) . . ?
C13 C12 C14 110.0(11) . . ?
C15 C12 C14 103.8(9) . . ?
C13 C12 C3 108.0(9) . . ?
C15 C12 C3 110.4(9) . . ?
C14 C12 C3 116.6(10) . . ?
C19 C16 P3 125.2(8) . . ?
C19 C16 P4 121.6(8) . . ?
P3 C16 P4 113.2(6) . . ?
C19 C16 Pd1 117.9(8) . . ?
P3 C16 Pd1 74.6(4) . . ?
P4 C16 Pd1 75.1(4) . . ?
C18 C17 C23 138.3(10) . . ?
C18 C17 P3 113.0(9) . . ?
C23 C17 P3 108.4(8) . . ?
C17 C18 C27 129.9(11) . . ?
C17 C18 P4 116.6(8) . . ?
C27 C18 P4 113.3(9) . . ?
C21 C19 C22 108.6(11) . . ?
C21 C19 C16 113.3(9) . . ?
C22 C19 C16 105.6(10) . . ?
C21 C19 C20 109.4(10) . . ?
C22 C19 C20 108.7(10) . . ?
C16 C19 C20 111.1(10) . . ?
C25 C23 C24 105.8(10) . . ?
C25 C23 C26 108.6(11) . . ?
C24 C23 C26 107.2(10) . . ?
C25 C23 C17 111.2(10) . . ?
C24 C23 C17 118.1(10) . . ?
C26 C23 C17 105.6(10) . . ?
C28 C27 C29 106.5(10) . . ?
C28 C27 C30 105.0(11) . . ?
C29 C27 C30 111.2(11) . . ?
C28 C27 C18 111.3(10) . . ?
C29 C27 C18 112.5(10) . . ?
C30 C27 C18 109.9(9) . . ?
C31 Pd2 C31 180.0(5) . 3_565 ?
C31 Pd2 P5 43.9(3) . . ?
C31 Pd2 P5 136.1(3) 3_565 . ?
C31 Pd2 P5 136.1(3) . 3_565 ?
C31 Pd2 P5 43.9(3) 3_565 3_565 ?
P5 Pd2 P5 180.0 . 3_565 ?
C31 Pd2 P6 43.7(3) . . ?
C31 Pd2 P6 136.3(3) 3_565 . ?
P5 Pd2 P6 72.77(10) . . ?
P5 Pd2 P6 107.23(10) 3_565 . ?
C31 Pd2 P6 136.3(3) . 3_565 ?
C31 Pd2 P6 43.7(3) 3_565 3_565 ?
P5 Pd2 P6 107.23(10) . 3_565 ?
P5 Pd2 P6 72.77(10) 3_565 3_565 ?
P6 Pd2 P6 180.00(3) . 3_565 ?
C31 P5 C32 98.0(5) . . ?
C31 P5 Pd2 60.9(4) . . ?
C32 P5 Pd2 89.0(4) . . ?
C31 P6 C33 98.1(5) . . ?
C31 P6 Pd2 60.7(4) . . ?
C33 P6 Pd2 88.0(4) . . ?
C34 C31 P6 123.8(9) . . ?
C34 C31 P5 124.1(9) . . ?
P6 C31 P5 112.0(6) . . ?
C34 C31 Pd2 118.6(7) . . ?
P6 C31 Pd2 75.6(4) . . ?
P5 C31 Pd2 75.2(4) . . ?
C33 C32 C38 130.1(10) . . ?
C33 C32 P5 114.9(8) . . ?
C38 C32 P5 114.9(8) . . ?
C32 C33 C42 134.0(11) . . ?
C32 C33 P6 114.0(8) . . ?
C42 C33 P6 111.6(8) . . ?
C36 C34 C37 110.1(11) . . ?
C36 C34 C35 108.1(11) . . ?
C37 C34 C35 110.3(11) . . ?
C36 C34 C31 107.3(10) . . ?
C37 C34 C31 110.3(10) . . ?
C35 C34 C31 110.8(9) . . ?
C39 C38 C32 113.1(10) . . ?
C39 C38 C41 111.0(11) . . ?
C32 C38 C41 113.5(10) . . ?
C39 C38 C40 103.4(11) . . ?
C32 C38 C40 109.5(10) . . ?
C41 C38 C40 105.5(11) . . ?
C43 C42 C44 110.6(10) . . ?
C43 C42 C33 108.2(10) . . ?
C44 C42 C33 115.6(10) . . ?
C43 C42 C45 105.9(10) . . ?
C44 C42 C45 106.5(10) . . ?
C33 C42 C45 109.6(9) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.142

#===END

# Attachment 'MAR999.CIF'

data_mar999
_database_code_depnum_ccdc_archive 'CCDC 700776'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C30 H54 Ni P4'
_chemical_formula_sum            'C30 H54 Ni P4'
_chemical_formula_weight         597.32

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_number     14

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                   17.396(4)
_cell_length_b                   9.479(2)
_cell_length_c                   20.102(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.84(3)
_cell_angle_gamma                90.00
_cell_volume                     3218.5(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      7
_cell_measurement_theta_max      10

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   none

_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       'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_standards_number         2
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  120
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5840
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         24.98
_reflns_number_total             5652
_reflns_number_gt                4140
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Enraf-Nonius CAD4'
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  SHELXL-93

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0334P)^2^+0.1681P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5652
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1056
_refine_ls_wR_factor_gt          0.0942
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
Ni Ni 0.21572(3) 0.07794(5) 0.16844(2) 0.01594(13) Uani 1 1 d . . .
P1 P 0.26001(6) -0.05009(9) 0.26703(5) 0.0192(2) Uani 1 1 d . A 2
P2 P 0.16810(5) 0.20064(10) 0.24629(5) 0.0187(2) Uani 1 1 d . A 2
P3 P 0.26537(5) 0.25648(9) 0.11169(5) 0.0187(2) Uani 1 1 d . A 2
P4 P 0.15890(6) 0.01859(10) 0.05108(5) 0.0199(2) Uani 1 1 d . A 2
C1 C 0.1626(2) 0.0146(4) 0.24206(18) 0.0178(8) Uani 1 1 d . A 2
C2 C 0.2649(2) 0.2193(4) 0.31204(17) 0.0184(8) Uani 1 1 d . A 2
C3 C 0.3044(2) 0.0964(4) 0.32610(17) 0.0176(8) Uani 1 1 d . A 2
C4 C 0.0873(2) -0.0754(4) 0.2313(2) 0.0259(9) Uani 1 1 d . A 2
C5 C 0.0719(3) -0.0949(5) 0.3026(2) 0.0450(12) Uani 1 1 d . A 2
H5A H 0.0655 -0.0024 0.3223 0.068 Uiso 1 1 calc R A 2
H5B H 0.1167 -0.1445 0.3321 0.068 Uiso 1 1 calc R A 2
H5C H 0.0235 -0.1505 0.2989 0.068 Uiso 1 1 calc R A 2
C6 C 0.0983(2) -0.2192(4) 0.2010(2) 0.0345(10) Uani 1 1 d . A 2
H6A H 0.0494 -0.2740 0.1952 0.052 Uiso 1 1 calc R A 2
H6B H 0.1418 -0.2694 0.2319 0.052 Uiso 1 1 calc R A 2
H6C H 0.1108 -0.2065 0.1564 0.052 Uiso 1 1 calc R A 2
C7 C 0.0163(2) -0.0034(4) 0.1850(2) 0.0384(11) Uani 1 1 d . A 2
H7A H 0.0083 0.0891 0.2041 0.058 Uiso 1 1 calc R A 2
H7B H -0.0310 -0.0616 0.1818 0.058 Uiso 1 1 calc R A 2
H7C H 0.0259 0.0089 0.1392 0.058 Uiso 1 1 calc R A 2
C8 C 0.2774(2) 0.3730(4) 0.33853(18) 0.0230(8) Uani 1 1 d . A 2
C9 C 0.2237(2) 0.3997(4) 0.3878(2) 0.0349(10) Uani 1 1 d . A 2
H9A H 0.1691 0.3740 0.3653 0.052 Uiso 1 1 calc R A 2
H9B H 0.2259 0.4997 0.4004 0.052 Uiso 1 1 calc R A 2
H9C H 0.2418 0.3422 0.4291 0.052 Uiso 1 1 calc R A 2
C10 C 0.2524(3) 0.4758(4) 0.2776(2) 0.0370(11) Uani 1 1 d . A 2
H10A H 0.1981 0.4545 0.2524 0.056 Uiso 1 1 calc R A 2
H10B H 0.2883 0.4654 0.2470 0.056 Uiso 1 1 calc R A 2
H10C H 0.2550 0.5729 0.2948 0.056 Uiso 1 1 calc R A 2
C11 C 0.3620(2) 0.4153(4) 0.3734(2) 0.0334(10) Uani 1 1 d . A 2
H11A H 0.3963 0.3998 0.3419 0.050 Uiso 1 1 calc R A 2
H11B H 0.3807 0.3580 0.4147 0.050 Uiso 1 1 calc R A 2
H11C H 0.3632 0.5152 0.3861 0.050 Uiso 1 1 calc R A 2
C12 C 0.3747(2) 0.0514(4) 0.38597(19) 0.0254(9) Uani 1 1 d . A 2
C13 C 0.3540(2) 0.0906(4) 0.45398(18) 0.0316(10) Uani 1 1 d . A 2
H13A H 0.3478 0.1931 0.4563 0.047 Uiso 1 1 calc R A 2
H13B H 0.3966 0.0594 0.4924 0.047 Uiso 1 1 calc R A 2
H13C H 0.3044 0.0442 0.4565 0.047 Uiso 1 1 calc R A 2
C14 C 0.3846(2) -0.1103(4) 0.3884(2) 0.0338(10) Uani 1 1 d . A 2
H14A H 0.3979 -0.1429 0.3462 0.051 Uiso 1 1 calc R A 2
H14B H 0.3350 -0.1544 0.3925 0.051 Uiso 1 1 calc R A 2
H14C H 0.4271 -0.1364 0.4279 0.051 Uiso 1 1 calc R A 2
C15 C 0.4560(2) 0.1091(5) 0.3817(2) 0.0365(11) Uani 1 1 d . A 2
H15A H 0.4670 0.0809 0.3380 0.055 Uiso 1 1 calc R A 2
H15B H 0.4970 0.0709 0.4196 0.055 Uiso 1 1 calc R A 2
H15C H 0.4557 0.2123 0.3847 0.055 Uiso 1 1 calc R A 2
C16 C 0.1695(2) 0.1972(4) 0.07116(18) 0.0197(8) Uani 1 1 d . A 2
C17 C 0.2605(2) -0.0273(4) 0.08817(17) 0.0167(7) Uani 1 1 d . A 2
C18 C 0.31138(19) 0.0866(4) 0.11785(17) 0.0162(7) Uani 1 1 d . A 2
C19 C 0.1023(2) 0.3043(4) 0.04691(19) 0.0226(8) Uani 1 1 d . A 2
C20 C 0.1107(3) 0.3557(4) -0.0236(2) 0.0363(10) Uani 1 1 d . A 2
H20A H 0.1635 0.3961 -0.0191 0.054 Uiso 1 1 calc R A 2
H20B H 0.0705 0.4278 -0.0410 0.054 Uiso 1 1 calc R A 2
H20C H 0.1033 0.2761 -0.0555 0.054 Uiso 1 1 calc R A 2
C21 C 0.0205(2) 0.2403(5) 0.0394(3) 0.0446(12) Uani 1 1 d . A 2
H21A H 0.0149 0.2074 0.0842 0.067 Uiso 1 1 calc R A 2
H21B H 0.0140 0.1605 0.0075 0.067 Uiso 1 1 calc R A 2
H21C H -0.0199 0.3117 0.0216 0.067 Uiso 1 1 calc R A 2
C22 C 0.1095(2) 0.4315(4) 0.0953(2) 0.0320(10) Uani 1 1 d . A 2
H22A H 0.1617 0.4751 0.1006 0.048 Uiso 1 1 calc R A 2
H22B H 0.1031 0.4000 0.1401 0.048 Uiso 1 1 calc R A 2
H22C H 0.0682 0.5005 0.0760 0.048 Uiso 1 1 calc R A 2
C23 C 0.2804(2) -0.1852(4) 0.07561(19) 0.0237(9) Uani 1 1 d . A 2
C24 C 0.2992(2) -0.2772(4) 0.1406(2) 0.0294(9) Uani 1 1 d . A 2
H24A H 0.2556 -0.2708 0.1636 0.044 Uiso 1 1 calc R A 2
H24B H 0.3481 -0.2437 0.1716 0.044 Uiso 1 1 calc R A 2
H24C H 0.3059 -0.3755 0.1280 0.044 Uiso 1 1 calc R A 2
C25 C 0.2099(2) -0.2582(4) 0.0267(2) 0.0342(10) Uani 1 1 d . A 2
H25A H 0.1949 -0.2047 -0.0162 0.051 Uiso 1 1 calc R A 2
H25B H 0.1649 -0.2623 0.0481 0.051 Uiso 1 1 calc R A 2
H25C H 0.2251 -0.3542 0.0169 0.051 Uiso 1 1 calc R A 2
C26 C 0.3481(2) -0.1926(4) 0.0388(2) 0.0299(9) Uani 1 1 d . A 2
H26A H 0.3352 -0.1334 -0.0024 0.045 Uiso 1 1 calc R A 2
H26B H 0.3552 -0.2905 0.0257 0.045 Uiso 1 1 calc R A 2
H26C H 0.3971 -0.1587 0.0695 0.045 Uiso 1 1 calc R A 2
C27 C 0.4029(2) 0.0960(4) 0.14924(18) 0.0191(8) Uani 1 1 d . A 2
C28 C 0.4442(2) 0.1222(4) 0.09049(19) 0.0286(9) Uani 1 1 d . A 2
H28A H 0.4203 0.2043 0.0638 0.043 Uiso 1 1 calc R A 2
H28B H 0.4378 0.0390 0.0607 0.043 Uiso 1 1 calc R A 2
H28C H 0.5007 0.1398 0.1096 0.043 Uiso 1 1 calc R A 2
C29 C 0.4397(2) -0.0314(4) 0.19191(19) 0.0258(9) Uani 1 1 d . A 2
H29A H 0.4290 -0.1169 0.1638 0.039 Uiso 1 1 calc R A 2
H29B H 0.4167 -0.0412 0.2316 0.039 Uiso 1 1 calc R A 2
H29C H 0.4971 -0.0177 0.2076 0.039 Uiso 1 1 calc R A 2
C30 C 0.4231(2) 0.2229(4) 0.19765(19) 0.0259(9) Uani 1 1 d . A 2
H30A H 0.4011 0.3090 0.1733 0.039 Uiso 1 1 calc R A 2
H30B H 0.4807 0.2320 0.2132 0.039 Uiso 1 1 calc R A 2
H30C H 0.4003 0.2089 0.2373 0.039 Uiso 1 1 calc R A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.0162(2) 0.0121(2) 0.0196(2) 0.00094(19) 0.00434(18) 0.00074(19)
P1 0.0218(5) 0.0132(5) 0.0228(5) 0.0024(4) 0.0055(4) 0.0029(4)
P2 0.0188(5) 0.0132(5) 0.0241(5) -0.0007(4) 0.0053(4) 0.0014(4)
P3 0.0181(5) 0.0122(5) 0.0253(5) 0.0022(4) 0.0044(4) 0.0002(4)
P4 0.0188(5) 0.0166(5) 0.0224(5) -0.0015(4) 0.0011(4) -0.0019(4)
C1 0.0186(19) 0.0161(18) 0.0208(19) 0.0018(15) 0.0091(15) -0.0017(15)
C2 0.0214(19) 0.0191(19) 0.0163(18) 0.0005(15) 0.0076(15) -0.0029(15)
C3 0.0193(19) 0.0191(19) 0.0168(18) 0.0018(15) 0.0092(15) 0.0019(15)
C4 0.021(2) 0.023(2) 0.036(2) 0.0016(18) 0.0111(17) -0.0042(17)
C5 0.046(3) 0.050(3) 0.048(3) -0.006(2) 0.028(2) -0.022(2)
C6 0.033(2) 0.022(2) 0.051(3) -0.007(2) 0.014(2) -0.0093(19)
C7 0.017(2) 0.035(3) 0.061(3) -0.008(2) 0.004(2) -0.0073(18)
C8 0.028(2) 0.0209(19) 0.0209(19) -0.0022(16) 0.0075(16) -0.0016(17)
C9 0.038(2) 0.028(2) 0.042(3) -0.013(2) 0.015(2) -0.0027(19)
C10 0.057(3) 0.0130(19) 0.035(2) 0.0010(18) 0.000(2) -0.003(2)
C11 0.032(2) 0.027(2) 0.040(2) -0.003(2) 0.0071(19) -0.006(2)
C12 0.023(2) 0.029(2) 0.023(2) 0.0049(17) 0.0032(16) 0.0025(17)
C13 0.038(2) 0.033(2) 0.020(2) 0.0033(18) 0.0001(17) 0.002(2)
C14 0.039(2) 0.031(2) 0.027(2) 0.0051(19) -0.0018(19) 0.011(2)
C15 0.023(2) 0.046(3) 0.038(2) 0.008(2) 0.0018(18) 0.007(2)
C16 0.0183(19) 0.0153(18) 0.025(2) 0.0032(16) 0.0043(16) 0.0007(15)
C17 0.0214(19) 0.0149(17) 0.0149(17) 0.0042(14) 0.0067(15) 0.0028(15)
C18 0.0172(18) 0.0151(17) 0.0170(17) 0.0021(15) 0.0057(14) 0.0024(15)
C19 0.0154(18) 0.0189(19) 0.031(2) 0.0068(17) 0.0009(16) 0.0058(16)
C20 0.041(3) 0.031(2) 0.034(2) 0.010(2) 0.004(2) 0.019(2)
C21 0.019(2) 0.033(2) 0.078(4) 0.011(2) 0.005(2) 0.008(2)
C22 0.032(2) 0.023(2) 0.040(2) 0.0089(19) 0.0079(19) 0.0131(19)
C23 0.029(2) 0.0172(19) 0.026(2) -0.0038(16) 0.0085(17) 0.0031(16)
C24 0.034(2) 0.0155(19) 0.041(2) -0.0025(18) 0.0133(19) 0.0049(17)
C25 0.040(3) 0.019(2) 0.042(3) -0.0087(19) 0.008(2) 0.0003(19)
C26 0.042(2) 0.019(2) 0.033(2) -0.0044(18) 0.0168(19) 0.0061(18)
C27 0.0154(18) 0.0167(18) 0.0249(19) 0.0040(16) 0.0042(15) 0.0012(15)
C28 0.023(2) 0.033(2) 0.032(2) 0.0072(19) 0.0091(17) 0.0000(18)
C29 0.020(2) 0.026(2) 0.031(2) 0.0065(18) 0.0054(17) 0.0063(17)
C30 0.017(2) 0.024(2) 0.032(2) -0.0010(17) -0.0028(17) -0.0005(16)

_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 2.014(3) . ?
Ni C18 2.149(3) . ?
Ni C17 2.193(3) . ?
Ni C16 2.235(4) . ?
Ni P2 2.2601(12) . ?
Ni P1 2.2942(12) . ?
Ni P3 2.3201(11) . ?
Ni P4 2.3967(14) . ?
P1 C1 1.758(4) . ?
P1 C3 1.869(4) . ?
P2 C1 1.767(4) . ?
P2 C2 1.884(4) . ?
P3 C16 1.764(4) . ?
P3 C18 1.789(3) . ?
P4 C16 1.740(4) . ?
P4 C17 1.800(4) . ?
C1 C4 1.536(5) . ?
C2 C3 1.348(5) . ?
C2 C8 1.548(5) . ?
C3 C12 1.556(5) . ?
C4 C7 1.518(5) . ?
C4 C6 1.523(5) . ?
C4 C5 1.531(5) . ?
C8 C11 1.524(5) . ?
C8 C9 1.537(5) . ?
C8 C10 1.544(5) . ?
C12 C15 1.537(5) . ?
C12 C13 1.540(5) . ?
C12 C14 1.542(5) . ?
C16 C19 1.537(5) . ?
C17 C18 1.433(5) . ?
C17 C23 1.570(5) . ?
C18 C27 1.568(5) . ?
C19 C21 1.520(5) . ?
C19 C22 1.535(5) . ?
C19 C20 1.538(5) . ?
C23 C26 1.535(5) . ?
C23 C24 1.539(5) . ?
C23 C25 1.540(5) . ?
C27 C29 1.531(5) . ?
C27 C30 1.534(5) . ?
C27 C28 1.542(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
C1 Ni C18 154.42(14) . . ?
C1 Ni C17 135.32(13) . . ?
C18 Ni C17 38.52(12) . . ?
C1 Ni C16 131.38(14) . . ?
C18 Ni C16 73.99(13) . . ?
C17 Ni C16 72.73(13) . . ?
C1 Ni P2 48.42(10) . . ?
C18 Ni P2 139.59(10) . . ?
C17 Ni P2 175.81(9) . . ?
C16 Ni P2 103.33(10) . . ?
C1 Ni P1 47.61(10) . . ?
C18 Ni P1 106.92(10) . . ?
C17 Ni P1 106.86(9) . . ?
C16 Ni P1 178.08(10) . . ?
P2 Ni P1 77.12(4) . . ?
C1 Ni P3 150.32(10) . . ?
C18 Ni P3 47.00(9) . . ?
C17 Ni P3 74.36(9) . . ?
C16 Ni P3 45.53(9) . . ?
P2 Ni P3 101.91(4) . . ?
P1 Ni P3 136.31(4) . . ?
C1 Ni P4 119.97(11) . . ?
C18 Ni P4 74.15(10) . . ?
C17 Ni P4 45.91(9) . . ?
C16 Ni P4 43.96(10) . . ?
P2 Ni P4 132.00(4) . . ?
P1 Ni P4 134.46(4) . . ?
P3 Ni P4 78.55(4) . . ?
C1 P1 C3 98.37(16) . . ?
C1 P1 Ni 57.82(11) . . ?
C3 P1 Ni 99.10(11) . . ?
C1 P2 C2 99.00(16) . . ?
C1 P2 Ni 58.50(11) . . ?
C2 P2 Ni 96.90(11) . . ?
C16 P3 C18 95.93(16) . . ?
C16 P3 Ni 64.70(12) . . ?
C18 P3 Ni 61.48(11) . . ?
C16 P4 C17 95.76(16) . . ?
C16 P4 Ni 63.09(12) . . ?
C17 P4 Ni 61.05(11) . . ?
C4 C1 P1 125.4(3) . . ?
C4 C1 P2 126.5(3) . . ?
P1 C1 P2 107.29(19) . . ?
C4 C1 Ni 126.0(2) . . ?
P1 C1 Ni 74.57(13) . . ?
P2 C1 Ni 73.08(13) . . ?
C3 C2 C8 135.9(3) . . ?
C3 C2 P2 113.0(3) . . ?
C8 C2 P2 111.0(2) . . ?
C2 C3 C12 131.7(3) . . ?
C2 C3 P1 113.4(3) . . ?
C12 C3 P1 114.6(2) . . ?
C7 C4 C6 108.6(3) . . ?
C7 C4 C5 109.3(3) . . ?
C6 C4 C5 109.4(3) . . ?
C7 C4 C1 112.2(3) . . ?
C6 C4 C1 111.6(3) . . ?
C5 C4 C1 105.6(3) . . ?
C11 C8 C9 109.2(3) . . ?
C11 C8 C10 104.9(3) . . ?
C9 C8 C10 107.9(3) . . ?
C11 C8 C2 116.5(3) . . ?
C9 C8 C2 108.6(3) . . ?
C10 C8 C2 109.3(3) . . ?
C15 C12 C13 112.2(3) . . ?
C15 C12 C14 105.0(3) . . ?
C13 C12 C14 105.0(3) . . ?
C15 C12 C3 115.0(3) . . ?
C13 C12 C3 108.2(3) . . ?
C14 C12 C3 110.9(3) . . ?
C19 C16 P4 122.6(3) . . ?
C19 C16 P3 120.0(3) . . ?
P4 C16 P3 116.9(2) . . ?
C19 C16 Ni 134.3(3) . . ?
P4 C16 Ni 72.95(13) . . ?
P3 C16 Ni 69.77(12) . . ?
C18 C17 C23 130.4(3) . . ?
C18 C17 P4 116.0(2) . . ?
C23 C17 P4 113.3(2) . . ?
C18 C17 Ni 69.11(19) . . ?
C23 C17 Ni 133.1(2) . . ?
P4 C17 Ni 73.04(12) . . ?
C17 C18 C27 132.6(3) . . ?
C17 C18 P3 115.3(2) . . ?
C27 C18 P3 111.8(2) . . ?
C17 C18 Ni 72.37(19) . . ?
C27 C18 Ni 129.6(2) . . ?
P3 C18 Ni 71.52(12) . . ?
C21 C19 C22 108.0(3) . . ?
C21 C19 C16 113.0(3) . . ?
C22 C19 C16 112.2(3) . . ?
C21 C19 C20 109.1(3) . . ?
C22 C19 C20 108.8(3) . . ?
C16 C19 C20 105.6(3) . . ?
C26 C23 C24 110.5(3) . . ?
C26 C23 C25 104.8(3) . . ?
C24 C23 C25 105.2(3) . . ?
C26 C23 C17 110.2(3) . . ?
C24 C23 C17 114.4(3) . . ?
C25 C23 C17 111.1(3) . . ?
C29 C27 C30 105.2(3) . . ?
C29 C27 C28 110.3(3) . . ?
C30 C27 C28 106.4(3) . . ?
C29 C27 C18 115.4(3) . . ?
C30 C27 C18 110.9(3) . . ?
C28 C27 C18 108.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.076

#===END