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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5b
_database_code_depnum_ccdc_archive 'CCDC 1043222'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_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 
;

_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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6a
_database_code_depnum_ccdc_archive 'CCDC 1043223'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_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 
;

_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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7a
_database_code_depnum_ccdc_archive 'CCDC 1043224'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_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 
;

_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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7b
_database_code_depnum_ccdc_archive 'CCDC 1043225'
_audit_update_record             
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;

_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 
;


_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 ========================================================
