# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

#################################################################
#
#TITLE: Reactions of Phenylacetylene with Nickel POCOP-Pincer
#       Hydride Complexes Resulting in Different Outcomes from
#       their Palladium Analogues
#
#AUTHORS: Gleason L. O. Wilson, Medhanei Abraha,  
#         Jeanette A. Krause & Hairong Guan
#
#################################################################


data_global
 
#========================================================  
# 1. SUBMISSION DETAILS
 

_publ_contact_author_name         'Dr. Jeanette A. Krause'       
_publ_contact_author_address
;     Department of Chemistry
      University of Cincinnati
      Cincinnati, OH 45221-0172 USA
;
_publ_contact_author_phone        '513 556 9226'
_publ_contact_author_fax          '513 556 9239'
_publ_contact_author_email        jeanette.krause@uc.edu
 
_publ_requested_journal           'Dalton Trans' 
_publ_requested_category          ? 
_publ_requested_coeditor_name     ?
 
_publ_contact_letter
;
Please deposit the following four (4) crystal structures.
These structures are part of a manuscript to be submitted
to Dalton Transactions.

Please send the deposit numbers for this contribution to
jeanette.krause@uc.edu

Thank you.
;
 
#=====================================================  
 
# 2. TITLE AND AUTHOR LIST

_publ_section_title
;
Reactions of Phenylacetylene with Nickel POCOP-Pincer Hydride
Complexes Resulting in Different Outcomes from their Palladium
Analogues
;

 
# The loop structure below should contain the names and addresses 
# of all authors, in the required order of publication. Repeat as 
# necessary.
 
loop_
 _publ_author_name
 _publ_author_address
     'Wilson, Gleason L. O.'
;     Department of Chemistry
      University of Cincinnati
      Cincinnati, OH 45221-0172 USA
;
     'Abraha, Medhanei'
;     Department of Chemistry
      University of Cincinnati
      Cincinnati, OH 45221-0172 USA
;
     'Krause, Jeanette A.'
;     Department of Chemistry
      University of Cincinnati
      Cincinnati, OH 45221-0172 USA
;
     'Guan, Hairong'
;     Department of Chemistry
      University of Cincinnati
      Cincinnati, OH 45221-0172 USA
;


#============================================================  
  
data_5b 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C34 H46 Ni O2 P2' 
_chemical_formula_sum             'C34 H46 Ni O2 P2' 
_chemical_formula_weight          607.36 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'P'  'P'   0.2955   0.4335 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'  -3.0029   0.5091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
_symmetry_space_group_name_Hall   '-P 2yn'

  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
  
_cell_length_a                    13.0470(4) 
_cell_length_b                    16.0405(5) 
_cell_length_c                    14.9995(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  99.331(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      3097.56(17) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     4662 
_cell_measurement_theta_min       4.17 
_cell_measurement_theta_max       66.48 
  
_exptl_crystal_description        plate 
_exptl_crystal_colour             'light yellow' 
_exptl_crystal_size_max           0.21 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.302 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1296 
_exptl_absorpt_coefficient_mu     2.094 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.6675 
_exptl_absorpt_correction_T_max   0.8504 
_exptl_absorpt_process_details    'SADABS v2008/1 (Sheldrick)'    
 
_exptl_special_details 
; 
loop, paratone 
; 

_publ_section_acknowledgements 
; 
Funding for the SMART6000 diffractometer through NSF-MRI grant 
CHE-0215950 is gratefully acknowledged. 
; 
  
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker SMART6000 CCD' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          . 
_diffrn_standards_interval_count  . 
_diffrn_standards_interval_time   . 
_diffrn_reflns_number             25317 
_diffrn_reflns_av_R_equivalents   0.0918 
_diffrn_reflns_av_sigmaI/netI     0.0666 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          4.06 
_diffrn_reflns_theta_max          67.53 
_reflns_number_total              5510 
_reflns_number_gt                 3598 
_reflns_threshold_expression      >2σ(I) 
  
_computing_data_collection        'Bruker SMART v5.634' 
_computing_cell_refinement        'Bruker SAINT v7.66A' 
_computing_data_reduction         'Bruker SAINT v7.66A' 
_computing_structure_solution     'Bruker SHELXTL v6.14' 
_computing_structure_refinement   'Bruker SHELXTL v6.14'
_computing_molecular_graphics     'Bruker SHELXTL v6.14' 
_computing_publication_material   'Bruker SHELXTL v6.14' 



_refine_special_details 
; 
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. 

Two-component disorder model for 2 cyclopentyl rings.
; 
  
_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)+(0.0847P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          5510 
_refine_ls_number_parameters      379 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0971 
_refine_ls_R_factor_gt            0.0561 
_refine_ls_wR_factor_ref          0.1544 
_refine_ls_wR_factor_gt           0.1337 
_refine_ls_goodness_of_fit_ref    0.996 
_refine_ls_restrained_S_all       0.996 
_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 0.61153(5) 0.24308(4) 0.41070(4) 0.03260(19) Uani 1 1 d . . . 
P1 P 0.53181(8) 0.20979(6) 0.51942(7) 0.0343(2) Uani 1 1 d . . . 
P2 P 0.68992(8) 0.31067(6) 0.31836(7) 0.0355(3) Uani 1 1 d . . . 
O1 O 0.5356(2) 0.29224(16) 0.58635(18) 0.0424(7) Uani 1 1 d . . . 
O2 O 0.7164(2) 0.40461(17) 0.36242(19) 0.0478(7) Uani 1 1 d . . . 
C1 C 0.6235(3) 0.3475(2) 0.4726(3) 0.0354(9) Uani 1 1 d . . . 
C2 C 0.5850(3) 0.3597(2) 0.5526(3) 0.0383(9) Uani 1 1 d . . . 
C3 C 0.5931(3) 0.4349(3) 0.5991(3) 0.0450(10) Uani 1 1 d . . . 
H3 H 0.5661 0.4408 0.6539 0.054 Uiso 1 1 calc R . . 
C4 C 0.6416(4) 0.5011(2) 0.5635(3) 0.0465(11) Uani 1 1 d . . . 
H4 H 0.6472 0.5533 0.5939 0.056 Uiso 1 1 calc R . . 
C5 C 0.6820(4) 0.4922(2) 0.4840(3) 0.0467(11) Uani 1 1 d . . . 
H5 H 0.7151 0.5377 0.4597 0.056 Uiso 1 1 calc R . . 
C6 C 0.6732(3) 0.4156(2) 0.4407(3) 0.0397(9) Uani 1 1 d . . . 
C7 C 0.5885(3) 0.1292(2) 0.5975(3) 0.0408(10) Uani 1 1 d . B . 
H7 H 0.5836 0.0750 0.5643 0.049 Uiso 1 1 calc R . . 
C8 C 0.5390(4) 0.1178(3) 0.6837(3) 0.0442(10) Uani 1 1 d . B . 
H8A H 0.5130 0.1716 0.7034 0.053 Uiso 1 1 calc R . . 
H8B H 0.4807 0.0776 0.6730 0.053 Uiso 1 1 calc R . . 
C9 C 0.6270(4) 0.0845(3) 0.7538(3) 0.0605(13) Uani 1 1 d . . . 
H9A H 0.6444 0.0257 0.7430 0.073 Uiso 0.35 1 calc PR A 1 
H9B H 0.6141 0.0918 0.8165 0.073 Uiso 0.35 1 calc PR A 1 
H9C H 0.6189 0.0255 0.7608 0.073 Uiso 0.65 1 d PR A 2 
H9D H 0.6249 0.1106 0.8110 0.073 Uiso 0.65 1 d PR A 2 
C10A C 0.7141(14) 0.1513(11) 0.7261(10) 0.055(4) Uani 0.35 1 d P B 1 
H10A H 0.6997 0.2086 0.7453 0.066 Uiso 0.35 1 calc PR B 1 
H10B H 0.7852 0.1353 0.7545 0.066 Uiso 0.35 1 calc PR B 1 
C10B C 0.7306(8) 0.1022(5) 0.7242(6) 0.054(2) Uani 0.65 1 d P B 2 
H10C H 0.7687 0.0498 0.7177 0.065 Uiso 0.65 1 calc PR B 2 
H10D H 0.7741 0.1385 0.7686 0.065 Uiso 0.65 1 calc PR B 2 
C11 C 0.7032(4) 0.1462(4) 0.6336(4) 0.0723(17) Uani 1 1 d . . . 
H11A H 0.7468 0.1004 0.6160 0.087 Uiso 0.35 1 calc PR B 1 
H11B H 0.7253 0.1990 0.6085 0.087 Uiso 0.35 1 calc PR B 1 
H11C H 0.7148 0.2050 0.6411 0.087 Uiso 0.65 1 d PR B 2 
H11D H 0.7458 0.1256 0.5920 0.087 Uiso 0.65 1 d PR B 2 
C12 C 0.3934(3) 0.1881(2) 0.5005(3) 0.0378(9) Uani 1 1 d . . . 
H12 H 0.3706 0.1831 0.5608 0.045 Uiso 1 1 calc R . . 
C13 C 0.3618(3) 0.1073(2) 0.4469(3) 0.0438(10) Uani 1 1 d . . . 
H13A H 0.4111 0.0948 0.4051 0.053 Uiso 1 1 calc R . . 
H13B H 0.3603 0.0595 0.4884 0.053 Uiso 1 1 calc R . . 
C14 C 0.2525(4) 0.1248(3) 0.3941(4) 0.0676(15) Uani 1 1 d . . . 
H14A H 0.2525 0.1193 0.3284 0.081 Uiso 1 1 calc R . . 
H14B H 0.2018 0.0846 0.4118 0.081 Uiso 1 1 calc R . . 
C15 C 0.2236(4) 0.2137(3) 0.4171(4) 0.0746(17) Uani 1 1 d . . . 
H15A H 0.1815 0.2138 0.4663 0.090 Uiso 1 1 calc R . . 
H15B H 0.1840 0.2418 0.3636 0.090 Uiso 1 1 calc R . . 
C16 C 0.3283(3) 0.2567(3) 0.4471(3) 0.0510(11) Uani 1 1 d . . . 
H16A H 0.3208 0.3056 0.4857 0.061 Uiso 1 1 calc R . . 
H16B H 0.3596 0.2748 0.3944 0.061 Uiso 1 1 calc R . . 
C17 C 0.8166(3) 0.2812(3) 0.2927(3) 0.0466(11) Uani 1 1 d . D . 
H17 H 0.8469 0.3298 0.2644 0.056 Uiso 1 1 calc R . . 
C18 C 0.8941(4) 0.2536(5) 0.3783(4) 0.081(2) Uani 1 1 d . . . 
H18A H 0.9573 0.2886 0.3833 0.098 Uiso 0.50 1 calc PR C 1 
H18B H 0.8618 0.2640 0.4326 0.098 Uiso 0.50 1 calc PR C 1 
H18C H 0.8592 0.2330 0.4255 0.098 Uiso 0.50 1 d PR C 2 
H18D H 0.9415 0.2973 0.4013 0.098 Uiso 0.50 1 d PR C 2 
C19A C 0.9214(10) 0.1751(8) 0.3776(8) 0.064(3) Uani 0.50 1 d P D 1 
H19A H 0.8717 0.1387 0.4026 0.077 Uiso 0.50 1 calc PR D 1 
H19B H 0.9922 0.1661 0.4116 0.077 Uiso 0.50 1 calc PR D 1 
C20A C 0.9177(14) 0.1606(10) 0.2775(16) 0.066(6) Uani 0.50 1 d P D 1 
H20A H 0.9160 0.1002 0.2639 0.079 Uiso 0.50 1 calc PR D 1 
H20B H 0.9792 0.1854 0.2568 0.079 Uiso 0.50 1 calc PR D 1 
C19B C 0.9527(13) 0.1769(10) 0.3280(11) 0.063(4) Uani 0.50 1 d P D 2 
H19C H 1.0091 0.2008 0.2991 0.076 Uiso 0.50 1 calc PR D 2 
H19D H 0.9838 0.1360 0.3739 0.076 Uiso 0.50 1 calc PR D 2 
C20B C 0.8759(14) 0.1343(12) 0.2587(15) 0.065(5) Uani 0.50 1 d P D 2 
H20C H 0.9090 0.1101 0.2097 0.078 Uiso 0.50 1 calc PR D 2 
H20D H 0.8370 0.0904 0.2855 0.078 Uiso 0.50 1 calc PR D 2 
C21 C 0.8098(4) 0.2064(3) 0.2273(3) 0.0546(12) Uani 1 1 d . . . 
H21A H 0.8136 0.2234 0.1645 0.065 Uiso 0.50 1 calc PR D 1 
H21B H 0.7472 0.1718 0.2288 0.065 Uiso 0.50 1 calc PR D 1 
H21C H 0.8280 0.2254 0.1713 0.065 Uiso 0.50 1 d PR D 2 
H21D H 0.7389 0.1880 0.2152 0.065 Uiso 0.50 1 d PR D 2 
C22 C 0.6136(3) 0.3365(2) 0.2091(3) 0.0383(9) Uani 1 1 d . . . 
H22A H 0.5971 0.2837 0.1742 0.046 Uiso 1 1 calc R . . 
C23 C 0.5110(4) 0.3811(3) 0.2169(3) 0.0531(12) Uani 1 1 d . . . 
H23A H 0.4568 0.3403 0.2264 0.064 Uiso 1 1 calc R . . 
H23B H 0.5208 0.4211 0.2678 0.064 Uiso 1 1 calc R . . 
C24 C 0.4816(4) 0.4257(4) 0.1283(4) 0.0692(16) Uani 1 1 d . . . 
H24A H 0.4291 0.3930 0.0877 0.083 Uiso 1 1 calc R . . 
H24B H 0.4517 0.4809 0.1382 0.083 Uiso 1 1 calc R . . 
C25 C 0.5778(4) 0.4359(3) 0.0864(3) 0.0553(12) Uani 1 1 d . . . 
H25A H 0.5914 0.4957 0.0771 0.066 Uiso 1 1 calc R . . 
H25B H 0.5693 0.4073 0.0272 0.066 Uiso 1 1 calc R . . 
C26 C 0.6672(3) 0.3974(3) 0.1509(3) 0.0458(10) Uani 1 1 d . . . 
H26A H 0.7067 0.4407 0.1890 0.055 Uiso 1 1 calc R . . 
H26B H 0.7150 0.3672 0.1173 0.055 Uiso 1 1 calc R . . 
C27 C 0.6082(3) 0.1295(2) 0.3515(2) 0.0324(8) Uani 1 1 d . . . 
C28 C 0.6645(3) 0.0723(3) 0.3920(3) 0.0449(11) Uani 1 1 d . . . 
H28A H 0.6687 0.0197 0.3636 0.054 Uiso 1 1 calc R . . 
H28B H 0.7025 0.0819 0.4506 0.054 Uiso 1 1 calc R . . 
C29 C 0.5479(3) 0.1194(2) 0.2619(3) 0.0418(10) Uani 1 1 d . . . 
C30 C 0.4524(4) 0.1589(3) 0.2336(3) 0.0470(11) Uani 1 1 d . . . 
H30 H 0.4261 0.1957 0.2741 0.056 Uiso 1 1 calc R . . 
C31 C 0.3945(4) 0.1461(3) 0.1480(4) 0.0610(13) Uani 1 1 d . . . 
H31 H 0.3288 0.1722 0.1316 0.073 Uiso 1 1 calc R . . 
C32 C 0.4336(5) 0.0954(4) 0.0876(4) 0.0744(16) Uani 1 1 d . . . 
H32 H 0.3948 0.0866 0.0290 0.089 Uiso 1 1 calc R . . 
C33 C 0.5282(5) 0.0574(4) 0.1116(4) 0.0745(17) Uani 1 1 d . . . 
H33 H 0.5555 0.0234 0.0691 0.089 Uiso 1 1 calc R . . 
C34 C 0.5846(4) 0.0683(3) 0.1979(3) 0.0580(13) Uani 1 1 d . . . 
H34 H 0.6493 0.0406 0.2139 0.070 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 1.909(4) . ? 
Ni C27 2.023(4) . ? 
Ni P1 2.1393(11) . ? 
Ni P2 2.1446(11) . ? 
P1 O1 1.656(3) . ? 
P1 C12 1.815(4) . ? 
P1 C7 1.818(4) . ? 
P2 O2 1.659(3) . ? 
P2 C17 1.819(4) . ? 
P2 C22 1.823(4) . ? 
O1 C2 1.396(5) . ? 
O2 C6 1.394(5) . ? 
C1 C2 1.388(6) . ? 
C1 C6 1.394(5) . ? 
C2 C3 1.389(5) . ? 
C3 C4 1.388(6) . ? 
C4 C5 1.388(6) . ? 
C5 C6 1.385(6) . ? 
C7 C11 1.530(6) . ? 
C7 C8 1.547(5) . ? 
C8 C9 1.522(6) . ? 
C9 C10B 1.516(11) . ? 
C9 C10A 1.662(18) . ? 
C10A C11 1.373(16) . ? 
C10B C11 1.521(10) . ? 
C12 C16 1.534(5) . ? 
C12 C13 1.546(5) . ? 
C13 C14 1.540(6) . ? 
C14 C15 1.529(7) . ? 
C15 C16 1.531(7) . ? 
C17 C21 1.543(6) . ? 
C17 C18 1.564(7) . ? 
C18 C19A 1.309(13) . ? 
C18 C19B 1.690(17) . ? 
C19A C20A 1.51(2) . ? 
C20A C21 1.66(2) . ? 
C19B C20B 1.49(2) . ? 
C20B C21 1.47(2) . ? 
C22 C23 1.539(6) . ? 
C22 C26 1.550(5) . ? 
C23 C24 1.504(6) . ? 
C24 C25 1.500(7) . ? 
C25 C26 1.520(6) . ? 
C27 C28 1.267(6) . ? 
C27 C29 1.453(6) . ? 
C29 C30 1.401(6) . ? 
C29 C34 1.404(6) . ? 
C30 C31 1.395(6) . ? 
C31 C32 1.376(8) . ? 
C32 C33 1.372(8) . ? 
C33 C34 1.392(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 Ni C27 175.77(16) . . ? 
C1 Ni P1 81.95(12) . . ? 
C27 Ni P1 97.52(10) . . ? 
C1 Ni P2 81.98(12) . . ? 
C27 Ni P2 98.66(10) . . ? 
P1 Ni P2 163.80(5) . . ? 
O1 P1 C12 100.29(17) . . ? 
O1 P1 C7 102.01(18) . . ? 
C12 P1 C7 104.80(19) . . ? 
O1 P1 Ni 106.99(10) . . ? 
C12 P1 Ni 121.52(14) . . ? 
C7 P1 Ni 118.08(14) . . ? 
O2 P2 C17 100.52(19) . . ? 
O2 P2 C22 101.53(17) . . ? 
C17 P2 C22 104.58(19) . . ? 
O2 P2 Ni 106.99(11) . . ? 
C17 P2 Ni 123.35(14) . . ? 
C22 P2 Ni 116.60(13) . . ? 
C2 O1 P1 111.7(2) . . ? 
C6 O2 P2 111.3(2) . . ? 
C2 C1 C6 116.1(4) . . ? 
C2 C1 Ni 122.1(3) . . ? 
C6 C1 Ni 121.8(3) . . ? 
C1 C2 C3 123.2(4) . . ? 
C1 C2 O1 117.3(3) . . ? 
C3 C2 O1 119.5(4) . . ? 
C4 C3 C2 118.3(4) . . ? 
C5 C4 C3 120.8(4) . . ? 
C6 C5 C4 118.7(4) . . ? 
C5 C6 C1 122.9(4) . . ? 
C5 C6 O2 119.5(4) . . ? 
C1 C6 O2 117.6(3) . . ? 
C11 C7 C8 104.0(4) . . ? 
C11 C7 P1 112.0(3) . . ? 
C8 C7 P1 116.2(3) . . ? 
C9 C8 C7 104.4(4) . . ? 
C10B C9 C8 109.9(5) . . ? 
C8 C9 C10A 94.0(7) . . ? 
C11 C10A C9 104.5(10) . . ? 
C9 C10B C11 104.9(6) . . ? 
C10A C11 C7 107.7(8) . . ? 
C10B C11 C7 108.0(5) . . ? 
C16 C12 C13 104.6(4) . . ? 
C16 C12 P1 113.4(3) . . ? 
C13 C12 P1 114.6(3) . . ? 
C14 C13 C12 105.2(3) . . ? 
C15 C14 C13 107.2(4) . . ? 
C14 C15 C16 104.3(4) . . ? 
C15 C16 C12 102.9(4) . . ? 
C21 C17 C18 105.3(4) . . ? 
C21 C17 P2 112.1(3) . . ? 
C18 C17 P2 112.9(3) . . ? 
C19A C18 C17 114.0(7) . . ? 
C17 C18 C19B 96.8(6) . . ? 
C18 C19A C20A 101.0(10) . . ? 
C19A C20A C21 105.7(11) . . ? 
C20B C19B C18 110.2(14) . . ? 
C21 C20B C19B 99.0(14) . . ? 
C20B C21 C17 115.9(9) . . ? 
C17 C21 C20A 95.7(7) . . ? 
C23 C22 C26 103.2(3) . . ? 
C23 C22 P2 113.1(3) . . ? 
C26 C22 P2 114.8(3) . . ? 
C24 C23 C22 104.7(4) . . ? 
C25 C24 C23 108.2(4) . . ? 
C24 C25 C26 107.3(4) . . ? 
C25 C26 C22 104.1(3) . . ? 
C28 C27 C29 123.2(4) . . ? 
C28 C27 Ni 118.2(3) . . ? 
C29 C27 Ni 118.4(3) . . ? 
C30 C29 C34 116.2(4) . . ? 
C30 C29 C27 123.5(4) . . ? 
C34 C29 C27 120.3(4) . . ? 
C31 C30 C29 122.3(4) . . ? 
C32 C31 C30 119.3(5) . . ? 
C33 C32 C31 120.2(5) . . ? 
C32 C33 C34 120.3(5) . . ? 
C33 C34 C29 121.5(5) . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C1 Ni P1 O1 -1.88(16) . . . . ? 
C27 Ni P1 O1 173.88(16) . . . . ? 
P2 Ni P1 O1 -9.4(2) . . . . ? 
C1 Ni P1 C12 112.11(19) . . . . ? 
C27 Ni P1 C12 -72.12(18) . . . . ? 
P2 Ni P1 C12 104.6(2) . . . . ? 
C1 Ni P1 C7 -116.1(2) . . . . ? 
C27 Ni P1 C7 59.7(2) . . . . ? 
P2 Ni P1 C7 -123.5(2) . . . . ? 
C1 Ni P2 O2 3.66(17) . . . . ? 
C27 Ni P2 O2 -172.12(16) . . . . ? 
P1 Ni P2 O2 11.1(2) . . . . ? 
C1 Ni P2 C17 119.1(2) . . . . ? 
C27 Ni P2 C17 -56.7(2) . . . . ? 
P1 Ni P2 C17 126.6(2) . . . . ? 
C1 Ni P2 C22 -109.09(19) . . . . ? 
C27 Ni P2 C22 75.13(18) . . . . ? 
P1 Ni P2 C22 -101.6(2) . . . . ? 
C12 P1 O1 C2 -125.5(3) . . . . ? 
C7 P1 O1 C2 126.8(3) . . . . ? 
Ni P1 O1 C2 2.1(3) . . . . ? 
C17 P2 O2 C6 -135.2(3) . . . . ? 
C22 P2 O2 C6 117.4(3) . . . . ? 
Ni P2 O2 C6 -5.3(3) . . . . ? 
C27 Ni C1 C2 -82(2) . . . . ? 
P1 Ni C1 C2 1.6(3) . . . . ? 
P2 Ni C1 C2 179.5(3) . . . . ? 
C27 Ni C1 C6 97(2) . . . . ? 
P1 Ni C1 C6 -179.6(3) . . . . ? 
P2 Ni C1 C6 -1.7(3) . . . . ? 
C6 C1 C2 C3 0.8(6) . . . . ? 
Ni C1 C2 C3 179.7(3) . . . . ? 
C6 C1 C2 O1 -179.5(3) . . . . ? 
Ni C1 C2 O1 -0.6(5) . . . . ? 
P1 O1 C2 C1 -1.2(5) . . . . ? 
P1 O1 C2 C3 178.5(3) . . . . ? 
C1 C2 C3 C4 0.4(7) . . . . ? 
O1 C2 C3 C4 -179.3(4) . . . . ? 
C2 C3 C4 C5 -0.7(7) . . . . ? 
C3 C4 C5 C6 -0.1(7) . . . . ? 
C4 C5 C6 C1 1.4(7) . . . . ? 
C4 C5 C6 O2 -177.9(4) . . . . ? 
C2 C1 C6 C5 -1.7(6) . . . . ? 
Ni C1 C6 C5 179.4(3) . . . . ? 
C2 C1 C6 O2 177.5(4) . . . . ? 
Ni C1 C6 O2 -1.3(5) . . . . ? 
P2 O2 C6 C5 -176.2(3) . . . . ? 
P2 O2 C6 C1 4.5(5) . . . . ? 
O1 P1 C7 C11 -66.2(4) . . . . ? 
C12 P1 C7 C11 -170.4(4) . . . . ? 
Ni P1 C7 C11 50.7(4) . . . . ? 
O1 P1 C7 C8 53.0(4) . . . . ? 
C12 P1 C7 C8 -51.2(4) . . . . ? 
Ni P1 C7 C8 169.9(3) . . . . ? 
C11 C7 C8 C9 -28.4(5) . . . . ? 
P1 C7 C8 C9 -151.9(3) . . . . ? 
C7 C8 C9 C10B 18.5(6) . . . . ? 
C7 C8 C9 C10A 43.8(7) . . . . ? 
C10B C9 C10A C11 76.1(16) . . . . ? 
C8 C9 C10A C11 -48.7(11) . . . . ? 
C8 C9 C10B C11 -0.8(8) . . . . ? 
C10A C9 C10B C11 -61.4(13) . . . . ? 
C9 C10A C11 C10B -62.5(15) . . . . ? 
C9 C10A C11 C7 33.4(13) . . . . ? 
C9 C10B C11 C10A 77.0(18) . . . . ? 
C9 C10B C11 C7 -17.7(8) . . . . ? 
C8 C7 C11 C10A -4.9(10) . . . . ? 
P1 C7 C11 C10A 121.3(9) . . . . ? 
C8 C7 C11 C10B 29.1(6) . . . . ? 
P1 C7 C11 C10B 155.2(5) . . . . ? 
O1 P1 C12 C16 66.0(3) . . . . ? 
C7 P1 C12 C16 171.5(3) . . . . ? 
Ni P1 C12 C16 -51.4(3) . . . . ? 
O1 P1 C12 C13 -174.0(3) . . . . ? 
C7 P1 C12 C13 -68.6(3) . . . . ? 
Ni P1 C12 C13 68.6(3) . . . . ? 
C16 C12 C13 C14 -24.0(4) . . . . ? 
P1 C12 C13 C14 -148.8(3) . . . . ? 
C12 C13 C14 C15 0.3(5) . . . . ? 
C13 C14 C15 C16 23.5(6) . . . . ? 
C14 C15 C16 C12 -38.3(5) . . . . ? 
C13 C12 C16 C15 38.6(5) . . . . ? 
P1 C12 C16 C15 164.2(3) . . . . ? 
O2 P2 C17 C21 -164.4(3) . . . . ? 
C22 P2 C17 C21 -59.4(3) . . . . ? 
Ni P2 C17 C21 77.0(3) . . . . ? 
O2 P2 C17 C18 76.8(4) . . . . ? 
C22 P2 C17 C18 -178.2(4) . . . . ? 
Ni P2 C17 C18 -41.7(5) . . . . ? 
C21 C17 C18 C19A -7.9(9) . . . . ? 
P2 C17 C18 C19A 114.7(8) . . . . ? 
C21 C17 C18 C19B 20.3(8) . . . . ? 
P2 C17 C18 C19B 142.9(7) . . . . ? 
C17 C18 C19A C20A 31.9(13) . . . . ? 
C19B C18 C19A C20A -30.4(13) . . . . ? 
C18 C19A C20A C21 -43.4(13) . . . . ? 
C19A C18 C19B C20B 90(2) . . . . ? 
C17 C18 C19B C20B -35.7(14) . . . . ? 
C18 C19B C20B C21 34.2(16) . . . . ? 
C19B C20B C21 C17 -20.5(16) . . . . ? 
C19B C20B C21 C20A 19(3) . . . . ? 
C18 C17 C21 C20B -1.8(10) . . . . ? 
P2 C17 C21 C20B -125.0(9) . . . . ? 
C18 C17 C21 C20A -17.8(8) . . . . ? 
P2 C17 C21 C20A -141.0(7) . . . . ? 
C19A C20A C21 C20B -108(4) . . . . ? 
C19A C20A C21 C17 36.8(11) . . . . ? 
O2 P2 C22 C23 -63.5(3) . . . . ? 
C17 P2 C22 C23 -167.7(3) . . . . ? 
Ni P2 C22 C23 52.4(3) . . . . ? 
O2 P2 C22 C26 54.6(3) . . . . ? 
C17 P2 C22 C26 -49.7(3) . . . . ? 
Ni P2 C22 C26 170.4(2) . . . . ? 
C26 C22 C23 C24 33.9(5) . . . . ? 
P2 C22 C23 C24 158.5(4) . . . . ? 
C22 C23 C24 C25 -21.1(6) . . . . ? 
C23 C24 C25 C26 -0.4(6) . . . . ? 
C24 C25 C26 C22 21.6(5) . . . . ? 
C23 C22 C26 C25 -34.0(5) . . . . ? 
P2 C22 C26 C25 -157.5(3) . . . . ? 
C1 Ni C27 C28 12(2) . . . . ? 
P1 Ni C27 C28 -70.5(3) . . . . ? 
P2 Ni C27 C28 110.4(3) . . . . ? 
C1 Ni C27 C29 -163(2) . . . . ? 
P1 Ni C27 C29 114.3(3) . . . . ? 
P2 Ni C27 C29 -64.8(3) . . . . ? 
C28 C27 C29 C30 147.5(4) . . . . ? 
Ni C27 C29 C30 -37.5(5) . . . . ? 
C28 C27 C29 C34 -32.9(6) . . . . ? 
Ni C27 C29 C34 142.2(4) . . . . ? 
C34 C29 C30 C31 2.4(6) . . . . ? 
C27 C29 C30 C31 -178.0(4) . . . . ? 
C29 C30 C31 C32 -2.4(7) . . . . ? 
C30 C31 C32 C33 0.4(9) . . . . ? 
C31 C32 C33 C34 1.4(9) . . . . ? 
C32 C33 C34 C29 -1.4(9) . . . . ? 
C30 C29 C34 C33 -0.5(7) . . . . ? 
C27 C29 C34 C33 179.8(5) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              67.53 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    0.500 
_refine_diff_density_min   -0.366 
_refine_diff_density_rms    0.069 


#eof data_5b =========================================================

 
data_6a 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C26 H38 Ni O2 P2' 
_chemical_formula_sum             'C26 H38 Ni O2 P2' 
_chemical_formula_weight          503.21 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'P'  'P'   0.2955   0.4335 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'  -3.0029   0.5091 
 '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)/m 
_symmetry_space_group_name_Hall   '-P 2yb'

  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z' 
 '-x, -y, -z' 
 'x, -y-1/2, z' 
  
_cell_length_a                    7.8641(3) 
_cell_length_b                    14.1716(5) 
_cell_length_c                    11.9392(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  101.328(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      1304.67(8) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     2422 
_cell_measurement_theta_min       3.78 
_cell_measurement_theta_max       66.97 
  
_exptl_crystal_description        blade 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.38 
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.01 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.281 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              536 
_exptl_absorpt_coefficient_mu     2.375 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.4656 
_exptl_absorpt_correction_T_max   0.9766 
_exptl_absorpt_process_details    'SADABS v2008/1 (Sheldrick)'    
 
_exptl_special_details 
; 
loop, paratone 
; 

_publ_section_acknowledgements 
; 
Funding for the SMART6000 diffractometer through NSF-MRI grant 
CHE-0215950 is gratefully acknowledged. 
; 
  
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker SMART6000 CCD' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          . 
_diffrn_standards_interval_count  . 
_diffrn_standards_interval_time   . 
_diffrn_reflns_number             11066 
_diffrn_reflns_av_R_equivalents   0.0703 
_diffrn_reflns_av_sigmaI/netI     0.0485 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          3.78 
_diffrn_reflns_theta_max          67.67 
_reflns_number_total              2434 
_reflns_number_gt                 1830 
_reflns_threshold_expression      >2σ(I) 
  
_computing_data_collection        'Bruker SMART v5.634' 
_computing_cell_refinement        'Bruker SAINT v7.66A' 
_computing_data_reduction         'Bruker SAINT v7.66A' 
_computing_structure_solution     'Bruker SHELXTL v6.14' 
_computing_structure_refinement   'Bruker SHELXTL v6.14'
_computing_molecular_graphics     'Bruker SHELXTL v6.14' 
_computing_publication_material   'Bruker SHELXTL v6.14' 



_refine_special_details 
; 
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. 

Data was collected out to 0.83Å and found that high angle data 
is weak - symptomatic of a number of crystals attempted.
;  
  
_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)+(0.0666P)²+0.0216P] 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          2434 
_refine_ls_number_parameters      161 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0685 
_refine_ls_R_factor_gt            0.0463 
_refine_ls_wR_factor_ref          0.1211 
_refine_ls_wR_factor_gt           0.1095 
_refine_ls_goodness_of_fit_ref    1.029 
_refine_ls_restrained_S_all       1.029 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ni Ni 0.25817(9) 0.7500 0.74979(6) 0.0267(2) Uani 1 2 d S . . 
P1 P 0.28221(10) 0.89870(5) 0.73437(6) 0.0284(2) Uani 1 1 d . . . 
O1 O 0.3701(3) 0.91797(14) 0.62044(17) 0.0369(5) Uani 1 1 d . . . 
C1 C 0.3685(5) 0.7500 0.6215(3) 0.0283(9) Uani 1 2 d S . . 
C2 C 0.4176(4) 0.8333(2) 0.5744(2) 0.0337(7) Uani 1 1 d . . . 
C3 C 0.5082(4) 0.8359(3) 0.4859(3) 0.0392(8) Uani 1 1 d . . . 
H3 H 0.5391 0.8941 0.4558 0.047 Uiso 1 1 calc R . . 
C4 C 0.5522(6) 0.7500 0.4429(4) 0.0461(13) Uani 1 2 d S . . 
H4 H 0.6143 0.7500 0.3822 0.055 Uiso 1 2 calc SR . . 
C7 C 0.0898(4) 0.9738(2) 0.7030(3) 0.0390(8) Uani 1 1 d . . . 
H7 H 0.1225 1.0343 0.6696 0.047 Uiso 1 1 calc R . . 
C8 C -0.0481(5) 0.9251(3) 0.6140(3) 0.0575(11) Uani 1 1 d . . . 
H8A H -0.1437 0.9690 0.5874 0.086 Uiso 1 1 calc R . . 
H8B H -0.0921 0.8696 0.6482 0.086 Uiso 1 1 calc R . . 
H8C H 0.0030 0.9053 0.5492 0.086 Uiso 1 1 calc R . . 
C9 C 0.0223(4) 0.9969(2) 0.8115(3) 0.0473(9) Uani 1 1 d . . . 
H9A H -0.0902 1.0286 0.7910 0.071 Uiso 1 1 calc R . . 
H9B H 0.1049 1.0385 0.8604 0.071 Uiso 1 1 calc R . . 
H9C H 0.0090 0.9384 0.8527 0.071 Uiso 1 1 calc R . . 
C10 C 0.4386(4) 0.9567(2) 0.8471(3) 0.0306(7) Uani 1 1 d . . . 
H10 H 0.3845 0.9616 0.9160 0.037 Uiso 1 1 calc R . . 
C11 C 0.5988(4) 0.8947(2) 0.8784(3) 0.0389(8) Uani 1 1 d . . . 
H11A H 0.6847 0.9262 0.9370 0.058 Uiso 1 1 calc R . . 
H11B H 0.6484 0.8837 0.8103 0.058 Uiso 1 1 calc R . . 
H11C H 0.5665 0.8341 0.9079 0.058 Uiso 1 1 calc R . . 
C12 C 0.4858(4) 1.0569(2) 0.8151(3) 0.0402(8) Uani 1 1 d . . . 
H12A H 0.5679 1.0847 0.8790 0.060 Uiso 1 1 calc R . . 
H12B H 0.3807 1.0956 0.7984 0.060 Uiso 1 1 calc R . . 
H12C H 0.5391 1.0542 0.7475 0.060 Uiso 1 1 calc R . . 
C27 C 0.1484(6) 0.7500 0.8803(4) 0.0302(9) Uani 1 2 d S . . 
H27 H 0.0253 0.7500 0.8602 0.036 Uiso 1 2 calc SR . . 
C28 C 0.2055(6) 0.7500 0.9880(4) 0.0301(10) Uani 1 2 d S . . 
H28 H 0.3283 0.7500 1.0099 0.036 Uiso 1 2 calc SR . . 
C29 C 0.1119(5) 0.7500 1.0855(4) 0.0282(9) Uani 1 2 d S . . 
C30 C -0.0696(5) 0.7500 1.0673(4) 0.0327(10) Uani 1 2 d S . . 
H30 H -0.1352 0.7500 0.9914 0.039 Uiso 1 2 calc SR . . 
C31 C -0.1548(6) 0.7500 1.1585(4) 0.0374(11) Uani 1 2 d S . . 
H31 H -0.2780 0.7500 1.1444 0.045 Uiso 1 2 calc SR . . 
C32 C -0.0617(6) 0.7500 1.2706(4) 0.0389(11) Uani 1 2 d S . . 
H32 H -0.1205 0.7500 1.3329 0.047 Uiso 1 2 calc SR . . 
C33 C 0.1170(6) 0.7500 1.2897(4) 0.0336(10) Uani 1 2 d S . . 
H33 H 0.1818 0.7500 1.3657 0.040 Uiso 1 2 calc SR . . 
C34 C 0.2030(5) 0.7500 1.1984(4) 0.0295(9) Uani 1 2 d S . . 
H34 H 0.3261 0.7500 1.2131 0.035 Uiso 1 2 calc SR . . 
  
  
_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 1.903(4) . ? 
Ni C27 1.924(4) . ? 
Ni P1 2.1270(8) 4_575 ? 
Ni P1 2.1270(8) . ? 
P1 O1 1.665(2) . ? 
P1 C7 1.827(3) . ? 
P1 C10 1.830(3) . ? 
O1 C2 1.401(4) . ? 
C1 C2 1.394(4) 4_575 ? 
C1 C2 1.394(4) . ? 
C2 C3 1.387(4) . ? 
C3 C4 1.391(4) . ? 
C4 C3 1.391(4) 4_575 ? 
C7 C8 1.526(5) . ? 
C7 C9 1.529(5) . ? 
C10 C11 1.522(4) . ? 
C10 C12 1.535(4) . ? 
C27 C28 1.276(6) . ? 
C28 C29 1.494(5) . ? 
C29 C34 1.397(6) . ? 
C29 C30 1.401(6) . ? 
C30 C31 1.386(6) . ? 
C31 C32 1.394(6) . ? 
C32 C33 1.379(6) . ? 
C33 C34 1.391(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 C27 179.55(18) . . ? 
C1 Ni P1 82.41(3) . 4_575 ? 
C27 Ni P1 97.57(3) . 4_575 ? 
C1 Ni P1 82.41(3) . . ? 
C27 Ni P1 97.57(3) . . ? 
P1 Ni P1 164.40(5) 4_575 . ? 
O1 P1 C7 101.35(14) . . ? 
O1 P1 C10 101.56(12) . . ? 
C7 P1 C10 107.39(15) . . ? 
O1 P1 Ni 106.95(8) . . ? 
C7 P1 Ni 120.71(11) . . ? 
C10 P1 Ni 116.08(10) . . ? 
C2 O1 P1 111.44(18) . . ? 
C2 C1 C2 115.7(4) 4_575 . ? 
C2 C1 Ni 122.06(19) 4_575 . ? 
C2 C1 Ni 122.06(19) . . ? 
C3 C2 C1 123.7(3) . . ? 
C3 C2 O1 119.5(3) . . ? 
C1 C2 O1 116.8(3) . . ? 
C2 C3 C4 117.4(3) . . ? 
C3 C4 C3 122.1(4) . 4_575 ? 
C8 C7 C9 111.7(3) . . ? 
C8 C7 P1 109.0(2) . . ? 
C9 C7 P1 111.2(2) . . ? 
C11 C10 C12 111.5(3) . . ? 
C11 C10 P1 109.0(2) . . ? 
C12 C10 P1 113.1(2) . . ? 
C28 C27 Ni 133.7(4) . . ? 
C27 C28 C29 131.0(4) . . ? 
C34 C29 C30 117.6(4) . . ? 
C34 C29 C28 121.0(4) . . ? 
C30 C29 C28 121.5(4) . . ? 
C31 C30 C29 120.9(4) . . ? 
C30 C31 C32 120.7(4) . . ? 
C33 C32 C31 119.0(4) . . ? 
C32 C33 C34 120.5(4) . . ? 
C33 C34 C29 121.4(4) . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C1 Ni P1 O1 2.56(15) . . . . ? 
C27 Ni P1 O1 -177.89(16) . . . . ? 
P1 Ni P1 O1 16.1(2) 4_575 . . . ? 
C1 Ni P1 C7 117.42(18) . . . . ? 
C27 Ni P1 C7 -63.03(19) . . . . ? 
P1 Ni P1 C7 130.9(2) 4_575 . . . ? 
C1 Ni P1 C10 -109.92(16) . . . . ? 
C27 Ni P1 C10 69.63(17) . . . . ? 
P1 Ni P1 C10 -96.4(2) 4_575 . . . ? 
C7 P1 O1 C2 -132.8(2) . . . . ? 
C10 P1 O1 C2 116.6(2) . . . . ? 
Ni P1 O1 C2 -5.5(2) . . . . ? 
C27 Ni C1 C2 87.4(4) . . . 4_575 ? 
P1 Ni C1 C2 -0.8(3) 4_575 . . 4_575 ? 
P1 Ni C1 C2 175.6(3) . . . 4_575 ? 
C27 Ni C1 C2 -87.4(4) . . . . ? 
P1 Ni C1 C2 -175.6(3) 4_575 . . . ? 
P1 Ni C1 C2 0.8(3) . . . . ? 
C2 C1 C2 C3 0.5(6) 4_575 . . . ? 
Ni C1 C2 C3 175.6(3) . . . . ? 
C2 C1 C2 O1 -179.9(2) 4_575 . . . ? 
Ni C1 C2 O1 -4.7(4) . . . . ? 
P1 O1 C2 C3 -173.7(2) . . . . ? 
P1 O1 C2 C1 6.6(4) . . . . ? 
C1 C2 C3 C4 -0.2(5) . . . . ? 
O1 C2 C3 C4 -179.9(3) . . . . ? 
C2 C3 C4 C3 0.0(6) . . . 4_575 ? 
O1 P1 C7 C8 77.1(3) . . . . ? 
C10 P1 C7 C8 -176.8(2) . . . . ? 
Ni P1 C7 C8 -40.6(3) . . . . ? 
O1 P1 C7 C9 -159.3(2) . . . . ? 
C10 P1 C7 C9 -53.2(3) . . . . ? 
Ni P1 C7 C9 83.0(2) . . . . ? 
O1 P1 C10 C11 -75.8(2) . . . . ? 
C7 P1 C10 C11 178.2(2) . . . . ? 
Ni P1 C10 C11 39.7(2) . . . . ? 
O1 P1 C10 C12 48.8(2) . . . . ? 
C7 P1 C10 C12 -57.2(3) . . . . ? 
Ni P1 C10 C12 164.33(19) . . . . ? 
C1 Ni C27 C28 0.00(14) . . . . ? 
P1 Ni C27 C28 88.12(4) 4_575 . . . ? 
P1 Ni C27 C28 -88.12(4) . . . . ? 
Ni C27 C28 C29 180.000(2) . . . . ? 
C27 C28 C29 C34 180.000(3) . . . . ? 
C27 C28 C29 C30 0.000(4) . . . . ? 
C34 C29 C30 C31 0.000(3) . . . . ? 
C28 C29 C30 C31 180.000(3) . . . . ? 
C29 C30 C31 C32 0.000(3) . . . . ? 
C30 C31 C32 C33 0.000(3) . . . . ? 
C31 C32 C33 C34 0.000(3) . . . . ? 
C32 C33 C34 C29 0.000(3) . . . . ? 
C30 C29 C34 C33 0.000(3) . . . . ? 
C28 C29 C34 C33 180.000(3) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.985 
_diffrn_reflns_theta_full              67.67 
_diffrn_measured_fraction_theta_full   0.985 
_refine_diff_density_max    0.575 
_refine_diff_density_min   -0.272 
_refine_diff_density_rms    0.069 


#eof data_6a =========================================================

 
data_7a 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C26 H36 Ni O2 P2' 
_chemical_formula_sum             'C26 H36 Ni O2 P2' 
_chemical_formula_weight          501.20 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'P'  'P'   0.2955   0.4335 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'  -3.0029   0.5091 
 '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'

  
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                    18.9605(12) 
_cell_length_b                    14.8022(9) 
_cell_length_c                    9.4584(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.672(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2641.6(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     3105 
_cell_measurement_theta_min       2.34 
_cell_measurement_theta_max       66.09 
  
_exptl_crystal_description        plate 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.29 
_exptl_crystal_size_mid           0.21 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.260 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1064 
_exptl_absorpt_coefficient_mu     2.345 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.5495 
_exptl_absorpt_correction_T_max   0.8917 
_exptl_absorpt_process_details    'SADABS v2008/1 (Sheldrick)'    
 
_exptl_special_details 
; 
loop, paratone 
; 

_publ_section_acknowledgements 
; 
Funding for the SMART6000 diffractometer through NSF-MRI grant 
CHE-0215950 is gratefully acknowledged. 
; 
  
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker SMART6000 CCD' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          . 
_diffrn_standards_interval_count  . 
_diffrn_standards_interval_time   . 
_diffrn_reflns_number             15015 
_diffrn_reflns_av_R_equivalents   0.0949 
_diffrn_reflns_av_sigmaI/netI     0.0713 
_diffrn_reflns_limit_h_min        -21 
_diffrn_reflns_limit_h_max        21 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        10 
_diffrn_reflns_theta_min          2.34 
_diffrn_reflns_theta_max          61.16 
_reflns_number_total              4036 
_reflns_number_gt                 2743 
_reflns_threshold_expression      >2σ(I) 
  
_computing_data_collection        'Bruker SMART v5.634' 
_computing_cell_refinement        'Bruker SAINT v7.66A' 
_computing_data_reduction         'Bruker SAINT v7.66A' 
_computing_structure_solution     'Bruker SHELXTL v6.14' 
_computing_structure_refinement   'Bruker SHELXTL v6.14'
_computing_molecular_graphics     'Bruker SHELXTL v6.14' 
_computing_publication_material   'Bruker SHELXTL v6.14' 



_refine_special_details 
; 
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. 

Data truncated at a resolution of 0.88Å for the refinement.
Data was collected out to 0.83Å and found that high angle data 
is very weak - symptomatic of a number of crystals attempted.
;  
  
_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)+(0.0954P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4036 
_refine_ls_number_parameters      288 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0924 
_refine_ls_R_factor_gt            0.0599 
_refine_ls_wR_factor_ref          0.1634 
_refine_ls_wR_factor_gt           0.1453 
_refine_ls_goodness_of_fit_ref    0.982 
_refine_ls_restrained_S_all       0.982 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
  
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ni Ni 0.23123(4) 0.48103(5) 0.27766(8) 0.0359(3) Uani 1 1 d . . . 
P1 P 0.14612(7) 0.50373(8) 0.11842(13) 0.0364(3) Uani 1 1 d . . . 
P2 P 0.29592(6) 0.43846(8) 0.46273(13) 0.0379(3) Uani 1 1 d . . . 
O1 O 0.08206(16) 0.4320(2) 0.1499(3) 0.0407(8) Uani 1 1 d . . . 
O2 O 0.24442(17) 0.3762(2) 0.5580(3) 0.0425(8) Uani 1 1 d . . . 
C1 C 0.1636(2) 0.4062(3) 0.3549(5) 0.0348(10) Uani 1 1 d . . . 
C2 C 0.0971(2) 0.3908(3) 0.2823(5) 0.0376(11) Uani 1 1 d . . . 
C3 C 0.0459(3) 0.3374(3) 0.3376(5) 0.0445(12) Uani 1 1 d . . . 
H3 H 0.0007 0.3286 0.2865 0.053 Uiso 1 1 calc R . . 
C4 C 0.0627(3) 0.2977(3) 0.4690(6) 0.0464(13) Uani 1 1 d . . . 
H4 H 0.0284 0.2610 0.5081 0.056 Uiso 1 1 calc R . . 
C5 C 0.1281(3) 0.3099(3) 0.5449(5) 0.0423(12) Uani 1 1 d . . . 
H5 H 0.1391 0.2823 0.6350 0.051 Uiso 1 1 calc R . . 
C6 C 0.1776(2) 0.3641(3) 0.4852(5) 0.0385(11) Uani 1 1 d . . . 
C7 C 0.0997(3) 0.6124(3) 0.1237(6) 0.0483(13) Uani 1 1 d . . . 
H7 H 0.0540 0.6081 0.0614 0.058 Uiso 1 1 calc R . . 
C8 C 0.0829(3) 0.6291(3) 0.2775(6) 0.0565(15) Uani 1 1 d . . . 
H8A H 0.0527 0.6826 0.2806 0.085 Uiso 1 1 calc R . . 
H8B H 0.1271 0.6387 0.3384 0.085 Uiso 1 1 calc R . . 
H8C H 0.0581 0.5764 0.3115 0.085 Uiso 1 1 calc R . . 
C9 C 0.1437(3) 0.6896(3) 0.0692(7) 0.0689(18) Uani 1 1 d . . . 
H9A H 0.1214 0.7476 0.0881 0.103 Uiso 1 1 calc R . . 
H9B H 0.1460 0.6827 -0.0332 0.103 Uiso 1 1 calc R . . 
H9C H 0.1917 0.6879 0.1181 0.103 Uiso 1 1 calc R . . 
C10 C 0.1608(3) 0.4828(3) -0.0673(5) 0.0412(11) Uani 1 1 d . . . 
H10 H 0.1891 0.5348 -0.0986 0.049 Uiso 1 1 calc R . . 
C11 C 0.2061(3) 0.3982(3) -0.0773(5) 0.0486(13) Uani 1 1 d . . . 
H11A H 0.2161 0.3892 -0.1761 0.073 Uiso 1 1 calc R . . 
H11B H 0.1806 0.3456 -0.0454 0.073 Uiso 1 1 calc R . . 
H11C H 0.2508 0.4055 -0.0170 0.073 Uiso 1 1 calc R . . 
C12 C 0.0931(3) 0.4786(4) -0.1679(6) 0.0658(17) Uani 1 1 d . . . 
H12A H 0.1051 0.4680 -0.2649 0.099 Uiso 1 1 calc R . . 
H12B H 0.0675 0.5360 -0.1642 0.099 Uiso 1 1 calc R . . 
H12C H 0.0632 0.4292 -0.1393 0.099 Uiso 1 1 calc R . . 
C13 C 0.3311(3) 0.5242(3) 0.5896(5) 0.0460(12) Uani 1 1 d . . . 
H13 H 0.3652 0.5618 0.5409 0.055 Uiso 1 1 calc R . . 
C14 C 0.3713(3) 0.4868(4) 0.7248(6) 0.0612(15) Uani 1 1 d . . . 
H14A H 0.3891 0.5370 0.7858 0.092 Uiso 1 1 calc R . . 
H14B H 0.4112 0.4501 0.6998 0.092 Uiso 1 1 calc R . . 
H14C H 0.3394 0.4494 0.7755 0.092 Uiso 1 1 calc R . . 
C15 C 0.2702(3) 0.5862(4) 0.6220(6) 0.0590(15) Uani 1 1 d . . . 
H15A H 0.2888 0.6358 0.6832 0.089 Uiso 1 1 calc R . . 
H15B H 0.2356 0.5516 0.6704 0.089 Uiso 1 1 calc R . . 
H15C H 0.2471 0.6108 0.5330 0.089 Uiso 1 1 calc R . . 
C16 C 0.3676(2) 0.3595(3) 0.4380(5) 0.0436(12) Uani 1 1 d . . . 
H16 H 0.3822 0.3297 0.5313 0.052 Uiso 1 1 calc R . . 
C17 C 0.3409(3) 0.2872(3) 0.3329(6) 0.0556(14) Uani 1 1 d . . . 
H17A H 0.3779 0.2418 0.3259 0.083 Uiso 1 1 calc R . . 
H17B H 0.3286 0.3148 0.2394 0.083 Uiso 1 1 calc R . . 
H17C H 0.2988 0.2584 0.3651 0.083 Uiso 1 1 calc R . . 
C18 C 0.4320(3) 0.4094(4) 0.3901(6) 0.0527(13) Uani 1 1 d . . . 
H18A H 0.4689 0.3655 0.3725 0.079 Uiso 1 1 calc R . . 
H18B H 0.4505 0.4516 0.4646 0.079 Uiso 1 1 calc R . . 
H18C H 0.4179 0.4429 0.3026 0.079 Uiso 1 1 calc R . . 
C27 C 0.2977(3) 0.5498(3) 0.1909(5) 0.0392(11) Uani 1 1 d . . . 
C28 C 0.3396(3) 0.5895(3) 0.1272(5) 0.0397(11) Uani 1 1 d . . . 
C29 C 0.3894(2) 0.6380(3) 0.0488(5) 0.0373(11) Uani 1 1 d . . . 
C30 C 0.4593(3) 0.6091(3) 0.0483(5) 0.0445(12) Uani 1 1 d . . . 
H30 H 0.4750 0.5580 0.1034 0.053 Uiso 1 1 calc R . . 
C31 C 0.5065(3) 0.6538(4) -0.0315(6) 0.0514(13) Uani 1 1 d . . . 
H31 H 0.5539 0.6332 -0.0316 0.062 Uiso 1 1 calc R . . 
C32 C 0.4836(3) 0.7281(4) -0.1099(6) 0.0531(14) Uani 1 1 d . . . 
H32 H 0.5155 0.7584 -0.1651 0.064 Uiso 1 1 calc R . . 
C33 C 0.4154(3) 0.7592(3) -0.1100(5) 0.0512(14) Uani 1 1 d . . . 
H33 H 0.4005 0.8112 -0.1641 0.061 Uiso 1 1 calc R . . 
C34 C 0.3682(3) 0.7146(3) -0.0309(5) 0.0451(12) Uani 1 1 d . . . 
H34 H 0.3211 0.7364 -0.0309 0.054 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 C27 1.871(5) . ? 
Ni C1 1.895(4) . ? 
Ni P1 2.1226(14) . ? 
Ni P2 2.1309(14) . ? 
P1 O1 1.662(3) . ? 
P1 C10 1.832(5) . ? 
P1 C7 1.837(5) . ? 
P2 O2 1.670(3) . ? 
P2 C16 1.825(5) . ? 
P2 C13 1.827(5) . ? 
O1 C2 1.397(5) . ? 
O2 C6 1.393(6) . ? 
C1 C6 1.383(6) . ? 
C1 C2 1.392(6) . ? 
C2 C3 1.394(6) . ? 
C3 C4 1.383(7) . ? 
C4 C5 1.382(7) . ? 
C5 C6 1.394(6) . ? 
C7 C9 1.533(7) . ? 
C7 C8 1.540(7) . ? 
C10 C12 1.521(7) . ? 
C10 C11 1.527(6) . ? 
C13 C14 1.526(7) . ? 
C13 C15 1.529(7) . ? 
C16 C17 1.513(7) . ? 
C16 C18 1.535(6) . ? 
C27 C28 1.198(6) . ? 
C28 C29 1.447(6) . ? 
C29 C30 1.391(6) . ? 
C29 C34 1.399(6) . ? 
C30 C31 1.394(7) . ? 
C31 C32 1.372(7) . ? 
C32 C33 1.373(7) . ? 
C33 C34 1.388(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 
C27 Ni C1 176.2(2) . . ? 
C27 Ni P1 95.76(15) . . ? 
C1 Ni P1 82.52(15) . . ? 
C27 Ni P2 99.39(15) . . ? 
C1 Ni P2 82.37(15) . . ? 
P1 Ni P2 164.85(6) . . ? 
O1 P1 C10 104.25(19) . . ? 
O1 P1 C7 101.2(2) . . ? 
C10 P1 C7 107.0(2) . . ? 
O1 P1 Ni 106.84(13) . . ? 
C10 P1 Ni 118.47(16) . . ? 
C7 P1 Ni 116.89(19) . . ? 
O2 P2 C16 101.40(19) . . ? 
O2 P2 C13 102.9(2) . . ? 
C16 P2 C13 107.6(2) . . ? 
O2 P2 Ni 106.65(13) . . ? 
C16 P2 Ni 117.37(17) . . ? 
C13 P2 Ni 118.50(17) . . ? 
C2 O1 P1 110.5(3) . . ? 
C6 O2 P2 110.9(3) . . ? 
C6 C1 C2 116.7(4) . . ? 
C6 C1 Ni 122.0(4) . . ? 
C2 C1 Ni 121.3(3) . . ? 
C1 C2 C3 122.6(5) . . ? 
C1 C2 O1 117.7(4) . . ? 
C3 C2 O1 119.7(4) . . ? 
C4 C3 C2 118.0(5) . . ? 
C5 C4 C3 121.8(4) . . ? 
C4 C5 C6 118.0(5) . . ? 
C1 C6 O2 117.9(4) . . ? 
C1 C6 C5 122.9(5) . . ? 
O2 C6 C5 119.3(4) . . ? 
C9 C7 C8 111.6(5) . . ? 
C9 C7 P1 111.4(3) . . ? 
C8 C7 P1 108.1(3) . . ? 
C12 C10 C11 111.9(4) . . ? 
C12 C10 P1 114.1(4) . . ? 
C11 C10 P1 109.8(3) . . ? 
C14 C13 C15 112.0(4) . . ? 
C14 C13 P2 114.7(4) . . ? 
C15 C13 P2 108.4(4) . . ? 
C17 C16 C18 111.8(4) . . ? 
C17 C16 P2 109.4(3) . . ? 
C18 C16 P2 110.7(3) . . ? 
C28 C27 Ni 175.3(4) . . ? 
C27 C28 C29 179.2(5) . . ? 
C30 C29 C34 118.0(4) . . ? 
C30 C29 C28 121.3(4) . . ? 
C34 C29 C28 120.7(4) . . ? 
C29 C30 C31 121.2(5) . . ? 
C32 C31 C30 119.2(5) . . ? 
C31 C32 C33 121.1(5) . . ? 
C32 C33 C34 119.8(5) . . ? 
C33 C34 C29 120.7(5) . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C27 Ni P1 O1 168.28(19) . . . . ? 
C1 Ni P1 O1 -8.27(17) . . . . ? 
P2 Ni P1 O1 -12.8(3) . . . . ? 
C27 Ni P1 C10 51.1(2) . . . . ? 
C1 Ni P1 C10 -125.4(2) . . . . ? 
P2 Ni P1 C10 -130.0(3) . . . . ? 
C27 Ni P1 C7 -79.3(2) . . . . ? 
C1 Ni P1 C7 104.1(2) . . . . ? 
P2 Ni P1 C7 99.5(3) . . . . ? 
C27 Ni P2 O2 178.99(19) . . . . ? 
C1 Ni P2 O2 -4.45(17) . . . . ? 
P1 Ni P2 O2 0.1(3) . . . . ? 
C27 Ni P2 C16 -68.2(2) . . . . ? 
C1 Ni P2 C16 108.3(2) . . . . ? 
P1 Ni P2 C16 112.9(3) . . . . ? 
C27 Ni P2 C13 63.6(2) . . . . ? 
C1 Ni P2 C13 -119.8(2) . . . . ? 
P1 Ni P2 C13 -115.2(3) . . . . ? 
C10 P1 O1 C2 136.9(3) . . . . ? 
C7 P1 O1 C2 -112.1(3) . . . . ? 
Ni P1 O1 C2 10.7(3) . . . . ? 
C16 P2 O2 C6 -118.5(3) . . . . ? 
C13 P2 O2 C6 130.3(3) . . . . ? 
Ni P2 O2 C6 4.9(3) . . . . ? 
C27 Ni C1 C6 122(3) . . . . ? 
P1 Ni C1 C6 -174.9(4) . . . . ? 
P2 Ni C1 C6 3.9(3) . . . . ? 
C27 Ni C1 C2 -58(3) . . . . ? 
P1 Ni C1 C2 5.3(3) . . . . ? 
P2 Ni C1 C2 -175.9(4) . . . . ? 
C6 C1 C2 C3 1.4(6) . . . . ? 
Ni C1 C2 C3 -178.8(3) . . . . ? 
C6 C1 C2 O1 -179.4(4) . . . . ? 
Ni C1 C2 O1 0.4(6) . . . . ? 
P1 O1 C2 C1 -7.8(5) . . . . ? 
P1 O1 C2 C3 171.4(3) . . . . ? 
C1 C2 C3 C4 -0.9(7) . . . . ? 
O1 C2 C3 C4 180.0(4) . . . . ? 
C2 C3 C4 C5 0.1(7) . . . . ? 
C3 C4 C5 C6 0.0(7) . . . . ? 
C2 C1 C6 O2 178.1(4) . . . . ? 
Ni C1 C6 O2 -1.7(5) . . . . ? 
C2 C1 C6 C5 -1.3(6) . . . . ? 
Ni C1 C6 C5 178.9(3) . . . . ? 
P2 O2 C6 C1 -2.5(5) . . . . ? 
P2 O2 C6 C5 176.9(3) . . . . ? 
C4 C5 C6 C1 0.6(7) . . . . ? 
C4 C5 C6 O2 -178.8(4) . . . . ? 
O1 P1 C7 C9 -169.1(4) . . . . ? 
C10 P1 C7 C9 -60.2(5) . . . . ? 
Ni P1 C7 C9 75.4(4) . . . . ? 
O1 P1 C7 C8 67.9(4) . . . . ? 
C10 P1 C7 C8 176.8(3) . . . . ? 
Ni P1 C7 C8 -47.6(4) . . . . ? 
O1 P1 C10 C12 47.3(4) . . . . ? 
C7 P1 C10 C12 -59.4(4) . . . . ? 
Ni P1 C10 C12 165.8(3) . . . . ? 
O1 P1 C10 C11 -79.3(4) . . . . ? 
C7 P1 C10 C11 174.0(3) . . . . ? 
Ni P1 C10 C11 39.3(4) . . . . ? 
O2 P2 C13 C14 57.6(4) . . . . ? 
C16 P2 C13 C14 -49.0(5) . . . . ? 
Ni P2 C13 C14 174.9(3) . . . . ? 
O2 P2 C13 C15 -68.4(4) . . . . ? 
C16 P2 C13 C15 -175.0(3) . . . . ? 
Ni P2 C13 C15 48.9(4) . . . . ? 
O2 P2 C16 C17 72.6(4) . . . . ? 
C13 P2 C16 C17 -179.8(4) . . . . ? 
Ni P2 C16 C17 -43.1(4) . . . . ? 
O2 P2 C16 C18 -163.8(3) . . . . ? 
C13 P2 C16 C18 -56.2(4) . . . . ? 
Ni P2 C16 C18 80.5(4) . . . . ? 
C1 Ni C27 C28 1(8) . . . . ? 
P1 Ni C27 C28 -62(5) . . . . ? 
P2 Ni C27 C28 118(5) . . . . ? 
Ni C27 C28 C29 70(39) . . . . ? 
C27 C28 C29 C30 -151(37) . . . . ? 
C27 C28 C29 C34 28(37) . . . . ? 
C34 C29 C30 C31 -1.4(7) . . . . ? 
C28 C29 C30 C31 177.6(4) . . . . ? 
C29 C30 C31 C32 0.6(7) . . . . ? 
C30 C31 C32 C33 0.5(8) . . . . ? 
C31 C32 C33 C34 -0.7(8) . . . . ? 
C32 C33 C34 C29 -0.2(8) . . . . ? 
C30 C29 C34 C33 1.2(7) . . . . ? 
C28 C29 C34 C33 -177.8(4) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              61.16 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.867 
_refine_diff_density_min   -0.333 
_refine_diff_density_rms    0.080 


#eof data_7a =========================================================

 
data_7b 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          'C34 H44 Ni O2 P2' 
_chemical_formula_sum             'C34 H44 Ni O2 P2' 
_chemical_formula_weight          605.34 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'P'  'P'   0.2955   0.4335 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'  -3.0029   0.5091 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Tetragonal 
_symmetry_space_group_name_H-M    P4(1)2(1)2 
_symmetry_space_group_name_Hall   'P 4abw 2nw'

  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z+1/2' 
 '-y+1/2, x+1/2, z+1/4' 
 'y+1/2, -x+1/2, z+3/4' 
 '-x+1/2, y+1/2, -z+1/4' 
 'x+1/2, -y+1/2, -z+3/4' 
 'y, x, -z' 
 '-y, -x, -z+1/2' 
  
_cell_length_a                    14.3061(2) 
_cell_length_b                    14.3061(2) 
_cell_length_c                    15.3464(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3140.86(7) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     9095 
_cell_measurement_theta_min       4.22 
_cell_measurement_theta_max       67.65 
  
_exptl_crystal_description        'irregular block' 
_exptl_crystal_colour             'pale yellow' 
_exptl_crystal_size_max           0.27 
_exptl_crystal_size_mid           0.21 
_exptl_crystal_size_min           0.18 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.280 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1288 
_exptl_absorpt_coefficient_mu     2.065 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.6056 
_exptl_absorpt_correction_T_max   0.7075 
_exptl_absorpt_process_details    'SADABS v2008/1 (Sheldrick)'    

 
_exptl_special_details 
; 
loop, paratone 
; 

_publ_section_acknowledgements 
; 
Funding for the SMART6000 diffractometer through NSF-MRI grant 
CHE-0215950 is gratefully acknowledged. 
;

   
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker SMART6000 CCD' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          . 
_diffrn_standards_interval_count  . 
_diffrn_standards_interval_time   . 
_diffrn_reflns_number             27280 
_diffrn_reflns_av_R_equivalents   0.0534 
_diffrn_reflns_av_sigmaI/netI     0.0276 
_diffrn_reflns_limit_h_min        -16 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          4.22 
_diffrn_reflns_theta_max          67.98 
_reflns_number_total              2860 
_reflns_number_gt                 2607 
_reflns_threshold_expression      >2σ(I) 

  
_computing_data_collection        'Bruker SMART v5.634' 
_computing_cell_refinement        'Bruker SAINT v7.66A' 
_computing_data_reduction         'Bruker SAINT v7.66A' 
_computing_structure_solution     'Bruker SHELXTL v6.14' 
_computing_structure_refinement   'Bruker SHELXTL v6.14'
_computing_molecular_graphics     'Bruker SHELXTL v6.14' 
_computing_publication_material   'Bruker SHELXTL v6.14' 
 
  
_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.

Typical disorder is observed for the cyclopentyl rings. 
A multi-component disorder model is applied for C9, C14 and C15.
;  
  
_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)+(0.0529P)²+0.9617P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881, 1165 Friedel pairs' 
_refine_ls_abs_structure_Flack    -0.04(3) 
_refine_ls_number_reflns          2860 
_refine_ls_number_parameters      207 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0408 
_refine_ls_R_factor_gt            0.0360 
_refine_ls_wR_factor_ref          0.0940 
_refine_ls_wR_factor_gt           0.0906 
_refine_ls_goodness_of_fit_ref    1.048 
_refine_ls_restrained_S_all       1.057 
_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 0.31656(2) 0.68344(2) 0.7500 0.02857(16) Uani 1 2 d S . . 
P1 P 0.30920(4) 0.70470(4) 0.61231(4) 0.03158(16) Uani 1 1 d . . . 
O1 O 0.23324(13) 0.79027(12) 0.59578(11) 0.0378(4) Uani 1 1 d . . . 
C1 C 0.22317(14) 0.77683(14) 0.7500 0.0272(6) Uani 1 2 d S . . 
C2 C 0.19234(16) 0.81935(16) 0.67357(14) 0.0299(5) Uani 1 1 d . . . 
C3 C 0.12388(17) 0.88792(18) 0.67161(17) 0.0374(6) Uani 1 1 d . . . 
H3 H 0.1045 0.9152 0.6182 0.045 Uiso 1 1 calc R . . 
C4 C 0.08477(16) 0.91523(16) 0.7500 0.0412(8) Uani 1 2 d S . . 
H4 H 0.0378 0.9622 0.7500 0.049 Uiso 1 2 calc SR . . 
C7 C 0.2600(2) 0.6097(2) 0.54880(17) 0.0396(7) Uani 1 1 d . B . 
H7 H 0.3075 0.5585 0.5469 0.048 Uiso 1 1 calc R . . 
C8 C 0.2341(3) 0.6339(3) 0.45426(19) 0.0670(11) Uani 1 1 d . . . 
H8A H 0.2149 0.7002 0.4498 0.080 Uiso 0.50 1 calc PR A 1 
H8B H 0.2883 0.6235 0.4153 0.080 Uiso 0.50 1 calc PR A 1 
H8C H 0.2707 0.5965 0.4120 0.080 Uiso 0.50 1 d PR A 2 
H8D H 0.2434 0.7012 0.4421 0.080 Uiso 0.50 1 d PR A 2 
C9A C 0.1556(13) 0.5716(10) 0.4295(9) 0.092(5) Uani 0.50 1 d P B 1 
H9B H 0.1804 0.5262 0.3885 0.110 Uiso 0.50 1 d P C 1 
H9A H 0.1095 0.5961 0.3922 0.110 Uiso 1 1 d . . . 
C9B C 0.1271(13) 0.6071(10) 0.4523(10) 0.098(6) Uani 0.50 1 d P B 2 
H9C H 0.0838 0.6587 0.4598 0.118 Uiso 0.50 1 d P D 2 
C10 C 0.1152(3) 0.5340(3) 0.5133(3) 0.0822(12) Uani 1 1 d . . . 
H10A H 0.0493 0.5544 0.5192 0.099 Uiso 0.50 1 calc PR B 1 
H10B H 0.1163 0.4648 0.5124 0.099 Uiso 0.50 1 calc PR B 1 
H10C H 0.1405 0.4742 0.4910 0.099 Uiso 0.50 1 d PR B 2 
H10D H 0.0485 0.5255 0.5289 0.099 Uiso 0.50 1 d PR B 2 
C11 C 0.1712(2) 0.5693(2) 0.5896(2) 0.0518(8) Uani 1 1 d . B . 
H11A H 0.1864 0.5177 0.6302 0.062 Uiso 1 1 calc R . . 
H11B H 0.1363 0.6181 0.6218 0.062 Uiso 1 1 calc R . . 
C12 C 0.4097(2) 0.7479(2) 0.55153(19) 0.0432(7) Uani 1 1 d . F . 
H12 H 0.3894 0.7633 0.4909 0.052 Uiso 1 1 calc R . . 
C13 C 0.4904(2) 0.6761(2) 0.5472(2) 0.0563(8) Uani 1 1 d D . . 
H13A H 0.4862 0.6309 0.5959 0.068 Uiso 0.50 1 calc PR E 1 
H13B H 0.4890 0.6414 0.4914 0.068 Uiso 0.50 1 calc PR E 1 
H13C H 0.5089 0.6648 0.4880 0.068 Uiso 0.50 1 d PR E 2 
H13D H 0.4729 0.6181 0.5740 0.068 Uiso 0.50 1 d PR E 2 
C14A C 0.5770(8) 0.7336(9) 0.5543(8) 0.079(4) Uani 0.50 1 d P F 1 
H14A H 0.5906 0.7677 0.4996 0.095 Uiso 0.50 1 calc PR F 1 
H14B H 0.6319 0.6954 0.5709 0.095 Uiso 0.50 1 calc PR F 1 
C15A C 0.5472(8) 0.8000(7) 0.6277(7) 0.069(2) Uani 0.50 1 d P F 1 
H15A H 0.5923 0.8519 0.6349 0.083 Uiso 0.50 1 calc PR F 1 
H15B H 0.5406 0.7664 0.6838 0.083 Uiso 0.50 1 calc PR F 1 
C14B C 0.5712(7) 0.7249(9) 0.6026(8) 0.072(3) Uani 0.50 1 d PD F 2 
H14C H 0.5659 0.7092 0.6652 0.086 Uiso 0.50 1 calc PR F 2 
H14D H 0.6338 0.7063 0.5813 0.086 Uiso 0.50 1 calc PR F 2 
C15B C 0.5527(7) 0.8294(7) 0.5865(7) 0.067(2) Uani 0.50 1 d P F 2 
H15C H 0.5843 0.8685 0.6308 0.081 Uiso 0.50 1 calc PR F 2 
H15D H 0.5742 0.8485 0.5278 0.081 Uiso 0.50 1 calc PR F 2 
C16 C 0.4506(3) 0.8363(2) 0.5940(3) 0.0618(10) Uani 1 1 d . . . 
H16A H 0.4108 0.8586 0.6426 0.074 Uiso 0.50 1 calc PR F 1 
H16B H 0.4584 0.8872 0.5509 0.074 Uiso 0.50 1 calc PR F 1 
H16C H 0.4324 0.8398 0.6541 0.074 Uiso 0.50 1 d PR F 2 
H16D H 0.4279 0.8910 0.5645 0.074 Uiso 0.50 1 d PR F 2 
C27 C 0.40918(16) 0.59082(16) 0.7500 0.0346(7) Uani 1 2 d S . . 
C28 C 0.46913(17) 0.53087(17) 0.7500 0.0384(8) Uani 1 2 d S . . 
C29 C 0.54050(17) 0.45950(17) 0.7500 0.0430(10) Uani 1 2 d S . . 
C30 C 0.5208(3) 0.3689(2) 0.7774(2) 0.0545(8) Uani 1 1 d . . . 
H30 H 0.4595 0.3536 0.7964 0.065 Uiso 1 1 calc R . . 
C31 C 0.5900(3) 0.3004(3) 0.7774(2) 0.0680(11) Uani 1 1 d . . . 
H31 H 0.5757 0.2388 0.7964 0.082 Uiso 1 1 calc R . . 
C32 C 0.6785(2) 0.3215(2) 0.7500 0.0747(18) Uani 1 2 d S . . 
H32 H 0.7255 0.2745 0.7500 0.090 Uiso 1 2 calc SR . . 
  
  
_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 C27 1.874(3) . ? 
Ni C1 1.889(3) . ? 
Ni P1 2.1374(6) . ? 
Ni P1 2.1374(6) 8_666 ? 
P1 O1 1.6564(17) . ? 
P1 C7 1.815(3) . ? 
P1 C12 1.821(3) . ? 
O1 C2 1.393(3) . ? 
C1 C2 1.393(3) 8_666 ? 
C1 C2 1.393(3) . ? 
C2 C3 1.386(3) . ? 
C3 C4 1.383(3) . ? 
C4 C3 1.383(3) 8_666 ? 
C7 C11 1.530(4) . ? 
C7 C8 1.537(4) . ? 
C8 C9A 1.483(16) . ? 
C8 C9B 1.579(19) . ? 
C9A C10 1.510(16) . ? 
C9B C10 1.414(17) . ? 
C10 C11 1.506(5) . ? 
C12 C16 1.539(4) . ? 
C12 C13 1.546(4) . ? 
C13 C14A 1.492(12) . ? 
C13 C14B 1.595(10) . ? 
C14A C15A 1.534(17) . ? 
C15A C16 1.565(12) . ? 
C14B C15B 1.538(16) . ? 
C15B C16 1.469(11) . ? 
C27 C28 1.213(5) . ? 
C28 C29 1.444(4) . ? 
C29 C30 1.392(4) 8_666 ? 
C29 C30 1.392(4) . ? 
C30 C31 1.393(4) . ? 
C31 C32 1.368(4) . ? 
C32 C31 1.368(5) 8_666 ? 
  
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 
C27 Ni C1 180.0 . . ? 
C27 Ni P1 97.79(2) . . ? 
C1 Ni P1 82.21(2) . . ? 
C27 Ni P1 97.79(2) . 8_666 ? 
C1 Ni P1 82.21(2) . 8_666 ? 
P1 Ni P1 164.42(4) . 8_666 ? 
O1 P1 C7 102.51(12) . . ? 
O1 P1 C12 100.87(12) . . ? 
C7 P1 C12 106.57(12) . . ? 
O1 P1 Ni 106.80(6) . . ? 
C7 P1 Ni 116.33(9) . . ? 
C12 P1 Ni 121.04(10) . . ? 
C2 O1 P1 111.40(14) . . ? 
C2 C1 C2 115.6(3) 8_666 . ? 
C2 C1 Ni 122.19(14) 8_666 . ? 
C2 C1 Ni 122.19(14) . . ? 
C3 C2 C1 123.4(2) . . ? 
C3 C2 O1 119.3(2) . . ? 
C1 C2 O1 117.3(2) . . ? 
C4 C3 C2 117.8(2) . . ? 
C3 C4 C3 121.9(3) 8_666 . ? 
C11 C7 C8 105.8(3) . . ? 
C11 C7 P1 112.66(19) . . ? 
C8 C7 P1 115.6(2) . . ? 
C9A C8 C7 106.8(7) . . ? 
C7 C8 C9B 101.3(6) . . ? 
C8 C9A C10 106.6(9) . . ? 
C10 C9B C8 106.5(9) . . ? 
C9B C10 C11 101.7(6) . . ? 
C11 C10 C9A 109.8(6) . . ? 
C10 C11 C7 104.5(3) . . ? 
C16 C12 C13 106.3(3) . . ? 
C16 C12 P1 111.2(2) . . ? 
C13 C12 P1 112.7(2) . . ? 
C14A C13 C12 104.6(6) . . ? 
C12 C13 C14B 103.2(5) . . ? 
C13 C14A C15A 99.4(7) . . ? 
C14A C15A C16 102.0(8) . . ? 
C15B C14B C13 102.4(8) . . ? 
C16 C15B C14B 102.9(7) . . ? 
C15B C16 C12 106.8(5) . . ? 
C12 C16 C15A 101.7(4) . . ? 
C28 C27 Ni 180.0(3) . . ? 
C27 C28 C29 180.0(3) . . ? 
C30 C29 C30 117.9(4) 8_666 . ? 
C30 C29 C28 121.03(19) 8_666 . ? 
C30 C29 C28 121.03(19) . . ? 
C29 C30 C31 120.8(4) . . ? 
C32 C31 C30 120.2(4) . . ? 
C31 C32 C31 120.2(4) 8_666 . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C27 Ni P1 O1 -177.11(7) . . . . ? 
C1 Ni P1 O1 2.89(7) . . . . ? 
P1 Ni P1 O1 2.89(7) 8_666 . . . ? 
C27 Ni P1 C7 69.20(11) . . . . ? 
C1 Ni P1 C7 -110.80(11) . . . . ? 
P1 Ni P1 C7 -110.80(11) 8_666 . . . ? 
C27 Ni P1 C12 -62.80(12) . . . . ? 
C1 Ni P1 C12 117.20(12) . . . . ? 
P1 Ni P1 C12 117.20(12) 8_666 . . . ? 
C7 P1 O1 C2 119.10(17) . . . . ? 
C12 P1 O1 C2 -131.02(17) . . . . ? 
Ni P1 O1 C2 -3.69(17) . . . . ? 
C27 Ni C1 C2 84.24(11) . . . 8_666 ? 
P1 Ni C1 C2 178.05(12) . . . 8_666 ? 
P1 Ni C1 C2 -1.95(12) 8_666 . . 8_666 ? 
C27 Ni C1 C2 -95.76(11) . . . . ? 
P1 Ni C1 C2 -1.95(12) . . . . ? 
P1 Ni C1 C2 178.05(12) 8_666 . . . ? 
C2 C1 C2 C3 -0.09(18) 8_666 . . . ? 
Ni C1 C2 C3 179.91(18) . . . . ? 
C2 C1 C2 O1 -180.0(2) 8_666 . . . ? 
Ni C1 C2 O1 0.0(2) . . . . ? 
P1 O1 C2 C3 -177.26(19) . . . . ? 
P1 O1 C2 C1 2.6(2) . . . . ? 
C1 C2 C3 C4 0.2(3) . . . . ? 
O1 C2 C3 C4 -179.96(18) . . . . ? 
C2 C3 C4 C3 -0.09(16) . . . 8_666 ? 
O1 P1 C7 C11 -71.5(2) . . . . ? 
C12 P1 C7 C11 -177.0(2) . . . . ? 
Ni P1 C7 C11 44.6(3) . . . . ? 
O1 P1 C7 C8 50.3(3) . . . . ? 
C12 P1 C7 C8 -55.2(3) . . . . ? 
Ni P1 C7 C8 166.4(2) . . . . ? 
C11 C7 C8 C9A -25.8(8) . . . . ? 
P1 C7 C8 C9A -151.2(7) . . . . ? 
C11 C7 C8 C9B 2.2(6) . . . . ? 
P1 C7 C8 C9B -123.1(6) . . . . ? 
C7 C8 C9A C10 17.5(12) . . . . ? 
C9B C8 C9A C10 -64.9(19) . . . . ? 
C9A C8 C9B C10 75(2) . . . . ? 
C7 C8 C9B C10 -29.5(9) . . . . ? 
C8 C9B C10 C11 44.5(10) . . . . ? 
C8 C9B C10 C9A -65(2) . . . . ? 
C8 C9A C10 C9B 75.6(19) . . . . ? 
C8 C9A C10 C11 -2.6(13) . . . . ? 
C9B C10 C11 C7 -42.3(9) . . . . ? 
C9A C10 C11 C7 -13.2(8) . . . . ? 
C8 C7 C11 C10 23.5(4) . . . . ? 
P1 C7 C11 C10 150.6(3) . . . . ? 
O1 P1 C12 C16 66.7(3) . . . . ? 
C7 P1 C12 C16 173.4(2) . . . . ? 
Ni P1 C12 C16 -50.6(3) . . . . ? 
O1 P1 C12 C13 -174.0(2) . . . . ? 
C7 P1 C12 C13 -67.3(2) . . . . ? 
Ni P1 C12 C13 68.6(2) . . . . ? 
C16 C12 C13 C14A -20.5(6) . . . . ? 
P1 C12 C13 C14A -142.5(5) . . . . ? 
C16 C12 C13 C14B 8.5(5) . . . . ? 
P1 C12 C13 C14B -113.6(5) . . . . ? 
C12 C13 C14A C15A 43.6(9) . . . . ? 
C14B C13 C14A C15A -47.1(15) . . . . ? 
C13 C14A C15A C16 -50.9(9) . . . . ? 
C14A C13 C14B C15B 65.4(16) . . . . ? 
C12 C13 C14B C15B -31.0(8) . . . . ? 
C13 C14B C15B C16 42.9(10) . . . . ? 
C14B C15B C16 C12 -38.5(9) . . . . ? 
C14B C15B C16 C15A 45.3(11) . . . . ? 
C13 C12 C16 C15B 18.4(6) . . . . ? 
P1 C12 C16 C15B 141.4(5) . . . . ? 
C13 C12 C16 C15A -11.0(5) . . . . ? 
P1 C12 C16 C15A 112.0(4) . . . . ? 
C14A C15A C16 C15B -65.8(13) . . . . ? 
C14A C15A C16 C12 37.8(7) . . . . ? 
C1 Ni C27 C28 0.0 . . . . ? 
P1 Ni C27 C28 86.193(17) . . . . ? 
P1 Ni C27 C28 -93.807(17) 8_666 . . . ? 
Ni C27 C28 C29 0.0 . . . . ? 
C27 C28 C29 C30 159.32(14) . . . 8_666 ? 
C27 C28 C29 C30 -20.68(14) . . . . ? 
C30 C29 C30 C31 0.1(2) 8_666 . . . ? 
C28 C29 C30 C31 -179.9(2) . . . . ? 
C29 C30 C31 C32 -0.1(4) . . . . ? 
C30 C31 C32 C31 0.1(2) . . . 8_666 ? 
  
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              67.98 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.349 
_refine_diff_density_min   -0.193 
_refine_diff_density_rms    0.048 


#eof data_7b =========================================================

#eof all data ========================================================
