# 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_ij5
_database_code_depnum_ccdc_archive 'CCDC 1052343'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '2b in manuscript'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H56 Ni P2'
_chemical_formula_weight         585.43

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   10.6643(18)
_cell_length_b                   9.5838(16)
_cell_length_c                   31.345(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.564(5)
_cell_angle_gamma                90
_cell_volume                     3175.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    3098
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      24.97

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.733
_shelx_estimated_absorpt_T_min   0.867
_shelx_estimated_absorpt_T_max   0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7686
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2008). SADABS. University of Göttingen, Germany.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17547
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.926
_diffrn_reflns_theta_max         25.090
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             5635
_reflns_number_gt                4308
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+3.9910P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5635
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.0993
_refine_ls_wR_factor_gt          0.0884
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.31955(5) 1.03361(5) 0.37814(2) 0.02872(14) Uani 1 1 d . . . . .
P1 P 0.18972(9) 0.94686(10) 0.32623(3) 0.0242(2) Uani 1 1 d . . . . .
P2 P 0.34319(10) 0.83476(10) 0.41008(3) 0.0275(2) Uani 1 1 d . . . . .
C1 C 0.4327(6) 1.1778(5) 0.4057(2) 0.0621(18) Uani 1 1 d . . . . .
H1A H 0.416(4) 1.197(4) 0.4344(14) 0.043(14) Uiso 1 1 d . . . . .
H1B H 0.518(5) 1.161(6) 0.3990(17) 0.09(2) Uiso 1 1 d . . . . .
C2 C 0.3515(4) 1.2354(4) 0.37111(16) 0.0407(11) Uani 1 1 d . . . . .
H2 H 0.384(4) 1.249(4) 0.3462(14) 0.047(15) Uiso 1 1 d . . . . .
C3 C 0.2346(4) 1.3107(4) 0.37553(13) 0.0329(10) Uani 1 1 d . . . . .
C4 C 0.1595(4) 1.3622(4) 0.33914(13) 0.0327(10) Uani 1 1 d . . . . .
H4 H 0.1867 1.3495 0.3117 0.039 Uiso 1 1 calc R U . . .
C5 C 0.0470(4) 1.4309(4) 0.34160(15) 0.0407(11) Uani 1 1 d . . . . .
H5 H -0.0021 1.4631 0.3160 0.049 Uiso 1 1 calc R U . . .
C6 C 0.0053(5) 1.4534(5) 0.38078(18) 0.0551(13) Uani 1 1 d . . . . .
H6 H -0.0720 1.5009 0.3825 0.066 Uiso 1 1 calc R U . . .
C7 C 0.0780(5) 1.4056(5) 0.41732(17) 0.0610(15) Uani 1 1 d . . . . .
H7 H 0.0512 1.4221 0.4446 0.073 Uiso 1 1 calc R U . . .
C8 C 0.1892(5) 1.3342(5) 0.41505(14) 0.0486(13) Uani 1 1 d . . . . .
H8 H 0.2361 1.3000 0.4408 0.058 Uiso 1 1 calc R U . . .
C9 C 0.1647(4) 0.7615(4) 0.33957(12) 0.0303(9) Uani 1 1 d . . . . .
H9A H 0.0854 0.7531 0.3526 0.036 Uiso 1 1 calc R U . . .
H9B H 0.1549 0.7059 0.3127 0.036 Uiso 1 1 calc R U . . .
C10 C 0.2747(4) 0.7009(4) 0.37095(12) 0.0280(9) Uani 1 1 d . . . . .
H10A H 0.3413 0.6660 0.3545 0.034 Uiso 1 1 calc R U . . .
H10B H 0.2436 0.6212 0.3867 0.034 Uiso 1 1 calc R U . . .
C11 C 0.0258(3) 1.0131(4) 0.31322(12) 0.0257(8) Uani 1 1 d . . . . .
H11 H 0.0322 1.1043 0.2982 0.031 Uiso 1 1 calc R U . . .
C12 C -0.0324(3) 1.0449(4) 0.35427(12) 0.0312(9) Uani 1 1 d . . . . .
H12A H -0.0389 0.9574 0.3706 0.037 Uiso 1 1 calc R U . . .
H12B H 0.0236 1.1095 0.3726 0.037 Uiso 1 1 calc R U . . .
C13 C -0.1637(4) 1.1102(4) 0.34406(13) 0.0376(10) Uani 1 1 d . . . . .
H13A H -0.2004 1.1246 0.3711 0.045 Uiso 1 1 calc R U . . .
H13B H -0.1561 1.2025 0.3304 0.045 Uiso 1 1 calc R U . . .
C14 C -0.2513(4) 1.0179(4) 0.31405(13) 0.0363(10) Uani 1 1 d . . . . .
H14A H -0.2655 0.9289 0.3287 0.044 Uiso 1 1 calc R U . . .
H14B H -0.3341 1.0648 0.3068 0.044 Uiso 1 1 calc R U . . .
C15 C -0.1947(3) 0.9884(5) 0.27322(12) 0.0368(10) Uani 1 1 d . . . . .
H15A H -0.1880 1.0767 0.2573 0.044 Uiso 1 1 calc R U . . .
H15B H -0.2513 0.9248 0.2547 0.044 Uiso 1 1 calc R U . . .
C16 C -0.0637(3) 0.9221(4) 0.28307(13) 0.0353(10) Uani 1 1 d . . . . .
H16A H -0.0718 0.8296 0.2965 0.042 Uiso 1 1 calc R U . . .
H16B H -0.0278 0.9079 0.2558 0.042 Uiso 1 1 calc R U . . .
C21 C 0.2468(3) 0.9359(4) 0.27276(12) 0.0252(8) Uani 1 1 d . . . . .
H21 H 0.1863 0.8766 0.2535 0.030 Uiso 1 1 calc R U . . .
C22 C 0.3775(4) 0.8672(4) 0.27682(13) 0.0345(10) Uani 1 1 d . . . . .
H22A H 0.4364 0.9198 0.2980 0.041 Uiso 1 1 calc R U . . .
H22B H 0.3713 0.7710 0.2879 0.041 Uiso 1 1 calc R U . . .
C23 C 0.4311(4) 0.8621(4) 0.23414(14) 0.0387(11) Uani 1 1 d . . . . .
H23A H 0.5173 0.8218 0.2388 0.046 Uiso 1 1 calc R U . . .
H23B H 0.3776 0.8005 0.2139 0.046 Uiso 1 1 calc R U . . .
C24 C 0.4367(4) 1.0060(4) 0.21430(14) 0.0407(11) Uani 1 1 d . . . . .
H24A H 0.4976 1.0648 0.2329 0.049 Uiso 1 1 calc R U . . .
H24B H 0.4665 0.9981 0.1858 0.049 Uiso 1 1 calc R U . . .
C25 C 0.3072(4) 1.0737(5) 0.20930(14) 0.0434(11) Uani 1 1 d . . . . .
H25A H 0.2491 1.0203 0.1881 0.052 Uiso 1 1 calc R U . . .
H25B H 0.3137 1.1696 0.1981 0.052 Uiso 1 1 calc R U . . .
C26 C 0.2526(4) 1.0796(4) 0.25199(13) 0.0353(10) Uani 1 1 d . . . . .
H26A H 0.3054 1.1423 0.2721 0.042 Uiso 1 1 calc R U . . .
H26B H 0.1663 1.1195 0.2469 0.042 Uiso 1 1 calc R U . . .
C31 C 0.2636(4) 0.8003(4) 0.45839(12) 0.0315(9) Uani 1 1 d . . . . .
H31 H 0.2852 0.7026 0.4678 0.038 Uiso 1 1 calc R U . . .
C32 C 0.3134(4) 0.8967(5) 0.49580(13) 0.0393(11) Uani 1 1 d . . . . .
H32A H 0.4064 0.8866 0.5021 0.047 Uiso 1 1 calc R U . . .
H32B H 0.2946 0.9948 0.4874 0.047 Uiso 1 1 calc R U . . .
C33 C 0.2540(4) 0.8631(5) 0.53626(13) 0.0449(12) Uani 1 1 d . . . . .
H33A H 0.2825 0.7696 0.5469 0.054 Uiso 1 1 calc R U . . .
H33B H 0.2835 0.9319 0.5589 0.054 Uiso 1 1 calc R U . . .
C34 C 0.1114(4) 0.8654(5) 0.52828(13) 0.0456(12) Uani 1 1 d . . . . .
H34A H 0.0820 0.9624 0.5224 0.055 Uiso 1 1 calc R U . . .
H34B H 0.0771 0.8327 0.5544 0.055 Uiso 1 1 calc R U . . .
C35 C 0.0618(4) 0.7732(5) 0.49049(13) 0.0459(12) Uani 1 1 d . . . . .
H35A H -0.0312 0.7833 0.4845 0.055 Uiso 1 1 calc R U . . .
H35B H 0.0808 0.6745 0.4981 0.055 Uiso 1 1 calc R U . . .
C36 C 0.1201(4) 0.8100(5) 0.45011(13) 0.0390(11) Uani 1 1 d . . . . .
H36A H 0.0877 0.7454 0.4266 0.047 Uiso 1 1 calc R U . . .
H36B H 0.0950 0.9060 0.4409 0.047 Uiso 1 1 calc R U . . .
C41 C 0.5035(4) 0.7650(4) 0.42835(13) 0.0322(9) Uani 1 1 d . . . . .
H41 H 0.5382 0.8216 0.4540 0.039 Uiso 1 1 calc R U . . .
C42 C 0.5096(4) 0.6127(5) 0.44292(16) 0.0545(14) Uani 1 1 d . . . . .
H42A H 0.4538 0.5995 0.4655 0.065 Uiso 1 1 calc R U . . .
H42B H 0.4780 0.5521 0.4182 0.065 Uiso 1 1 calc R U . . .
C43 C 0.6432(5) 0.5696(6) 0.46047(16) 0.0680(17) Uani 1 1 d . . . . .
H43A H 0.6716 0.6237 0.4869 0.082 Uiso 1 1 calc R U . . .
H43B H 0.6439 0.4695 0.4683 0.082 Uiso 1 1 calc R U . . .
C44 C 0.7334(4) 0.5935(5) 0.42814(15) 0.0530(13) Uani 1 1 d . . . . .
H44A H 0.7122 0.5296 0.4034 0.064 Uiso 1 1 calc R U . . .
H44B H 0.8206 0.5721 0.4415 0.064 Uiso 1 1 calc R U . . .
C45 C 0.7277(4) 0.7434(5) 0.41211(17) 0.0541(14) Uani 1 1 d . . . . .
H45A H 0.7820 0.7533 0.3890 0.065 Uiso 1 1 calc R U . . .
H45B H 0.7609 0.8063 0.4360 0.065 Uiso 1 1 calc R U . . .
C46 C 0.5932(4) 0.7864(5) 0.39491(14) 0.0388(11) Uani 1 1 d . . . . .
H46A H 0.5634 0.7307 0.3689 0.047 Uiso 1 1 calc R U . . .
H46B H 0.5924 0.8859 0.3864 0.047 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.959(5) . ?
Ni1 C2 1.981(4) . ?
Ni1 P2 2.1521(12) . ?
Ni1 P1 2.1592(11) . ?
P1 C9 1.853(4) . ?
P1 C11 1.854(4) . ?
P1 C21 1.860(4) . ?
P2 C41 1.855(4) . ?
P2 C10 1.857(4) . ?
P2 C31 1.860(4) . ?
C1 C2 1.409(7) . ?
C1 H1A 0.96(4) . ?
C1 H1B 0.98(5) . ?
C2 C3 1.463(6) . ?
C2 H2 0.90(4) . ?
C3 C4 1.395(5) . ?
C3 C8 1.406(6) . ?
C4 C5 1.379(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.377(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.374(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.379(7) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.541(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C16 1.526(5) . ?
C11 C12 1.531(5) . ?
C11 H11 1.0000 . ?
C12 C13 1.529(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.520(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.511(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.529(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C21 C26 1.528(5) . ?
C21 C22 1.531(5) . ?
C21 H21 1.0000 . ?
C22 C23 1.523(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.517(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.515(5) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.529(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C31 C36 1.521(5) . ?
C31 C32 1.532(5) . ?
C31 H31 1.0000 . ?
C32 C33 1.525(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.508(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.516(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.523(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C41 C46 1.523(5) . ?
C41 C42 1.528(5) . ?
C41 H41 1.0000 . ?
C42 C43 1.516(6) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.504(6) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.520(6) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.521(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni1 C2 41.91(19) . . ?
C1 Ni1 P2 113.04(16) . . ?
C2 Ni1 P2 154.81(14) . . ?
C1 Ni1 P1 154.26(18) . . ?
C2 Ni1 P1 113.25(14) . . ?
P2 Ni1 P1 91.94(4) . . ?
C9 P1 C11 102.64(18) . . ?
C9 P1 C21 102.87(17) . . ?
C11 P1 C21 103.42(17) . . ?
C9 P1 Ni1 107.23(12) . . ?
C11 P1 Ni1 121.76(12) . . ?
C21 P1 Ni1 116.57(12) . . ?
C41 P2 C10 102.79(18) . . ?
C41 P2 C31 100.70(18) . . ?
C10 P2 C31 103.49(18) . . ?
C41 P2 Ni1 120.63(14) . . ?
C10 P2 Ni1 107.01(12) . . ?
C31 P2 Ni1 119.85(13) . . ?
C2 C1 Ni1 69.9(3) . . ?
C2 C1 H1A 118(3) . . ?
Ni1 C1 H1A 112(3) . . ?
C2 C1 H1B 113(3) . . ?
Ni1 C1 H1B 109(3) . . ?
H1A C1 H1B 122(4) . . ?
C1 C2 C3 124.4(5) . . ?
C1 C2 Ni1 68.2(3) . . ?
C3 C2 Ni1 108.0(3) . . ?
C1 C2 H2 117(3) . . ?
C3 C2 H2 116(3) . . ?
Ni1 C2 H2 109(3) . . ?
C4 C3 C8 115.9(4) . . ?
C4 C3 C2 120.1(4) . . ?
C8 C3 C2 124.0(4) . . ?
C5 C4 C3 122.2(4) . . ?
C5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C6 C5 C4 120.6(4) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C7 C6 C5 118.6(5) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
C6 C7 C8 121.1(5) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C7 C8 C3 121.5(4) . . ?
C7 C8 H8 119.2 . . ?
C3 C8 H8 119.2 . . ?
C10 C9 P1 112.6(3) . . ?
C10 C9 H9A 109.1 . . ?
P1 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
P1 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 P2 111.2(2) . . ?
C9 C10 H10A 109.4 . . ?
P2 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
P2 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C16 C11 C12 110.1(3) . . ?
C16 C11 P1 115.8(3) . . ?
C12 C11 P1 111.0(2) . . ?
C16 C11 H11 106.4 . . ?
C12 C11 H11 106.4 . . ?
P1 C11 H11 106.4 . . ?
C13 C12 C11 111.5(3) . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
C14 C13 C12 111.2(3) . . ?
C14 C13 H13A 109.4 . . ?
C12 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C15 C14 C13 110.6(3) . . ?
C15 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C14 C15 C16 111.2(3) . . ?
C14 C15 H15A 109.4 . . ?
C16 C15 H15A 109.4 . . ?
C14 C15 H15B 109.4 . . ?
C16 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C11 C16 C15 111.6(3) . . ?
C11 C16 H16A 109.3 . . ?
C15 C16 H16A 109.3 . . ?
C11 C16 H16B 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C26 C21 C22 109.6(3) . . ?
C26 C21 P1 111.7(3) . . ?
C22 C21 P1 110.6(3) . . ?
C26 C21 H21 108.3 . . ?
C22 C21 H21 108.3 . . ?
P1 C21 H21 108.3 . . ?
C23 C22 C21 112.6(3) . . ?
C23 C22 H22A 109.1 . . ?
C21 C22 H22A 109.1 . . ?
C23 C22 H22B 109.1 . . ?
C21 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 C22 111.7(3) . . ?
C24 C23 H23A 109.3 . . ?
C22 C23 H23A 109.3 . . ?
C24 C23 H23B 109.3 . . ?
C22 C23 H23B 109.3 . . ?
H23A C23 H23B 107.9 . . ?
C25 C24 C23 110.3(3) . . ?
C25 C24 H24A 109.6 . . ?
C23 C24 H24A 109.6 . . ?
C25 C24 H24B 109.6 . . ?
C23 C24 H24B 109.6 . . ?
H24A C24 H24B 108.1 . . ?
C24 C25 C26 111.8(3) . . ?
C24 C25 H25A 109.2 . . ?
C26 C25 H25A 109.2 . . ?
C24 C25 H25B 109.2 . . ?
C26 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C21 C26 C25 112.4(3) . . ?
C21 C26 H26A 109.1 . . ?
C25 C26 H26A 109.1 . . ?
C21 C26 H26B 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.9 . . ?
C36 C31 C32 109.5(3) . . ?
C36 C31 P2 114.0(3) . . ?
C32 C31 P2 111.5(3) . . ?
C36 C31 H31 107.2 . . ?
C32 C31 H31 107.2 . . ?
P2 C31 H31 107.2 . . ?
C33 C32 C31 111.7(4) . . ?
C33 C32 H32A 109.3 . . ?
C31 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
C31 C32 H32B 109.3 . . ?
H32A C32 H32B 107.9 . . ?
C34 C33 C32 112.3(4) . . ?
C34 C33 H33A 109.1 . . ?
C32 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
C32 C33 H33B 109.1 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 C35 111.2(4) . . ?
C33 C34 H34A 109.4 . . ?
C35 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
C35 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C34 C35 C36 112.1(4) . . ?
C34 C35 H35A 109.2 . . ?
C36 C35 H35A 109.2 . . ?
C34 C35 H35B 109.2 . . ?
C36 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
C31 C36 C35 110.8(3) . . ?
C31 C36 H36A 109.5 . . ?
C35 C36 H36A 109.5 . . ?
C31 C36 H36B 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
C46 C41 C42 109.2(3) . . ?
C46 C41 P2 112.1(3) . . ?
C42 C41 P2 115.9(3) . . ?
C46 C41 H41 106.3 . . ?
C42 C41 H41 106.3 . . ?
P2 C41 H41 106.3 . . ?
C43 C42 C41 111.7(4) . . ?
C43 C42 H42A 109.3 . . ?
C41 C42 H42A 109.3 . . ?
C43 C42 H42B 109.3 . . ?
C41 C42 H42B 109.3 . . ?
H42A C42 H42B 107.9 . . ?
C44 C43 C42 111.6(4) . . ?
C44 C43 H43A 109.3 . . ?
C42 C43 H43A 109.3 . . ?
C44 C43 H43B 109.3 . . ?
C42 C43 H43B 109.3 . . ?
H43A C43 H43B 108.0 . . ?
C43 C44 C45 111.4(4) . . ?
C43 C44 H44A 109.3 . . ?
C45 C44 H44A 109.3 . . ?
C43 C44 H44B 109.3 . . ?
C45 C44 H44B 109.3 . . ?
H44A C44 H44B 108.0 . . ?
C44 C45 C46 111.6(4) . . ?
C44 C45 H45A 109.3 . . ?
C46 C45 H45A 109.3 . . ?
C44 C45 H45B 109.3 . . ?
C46 C45 H45B 109.3 . . ?
H45A C45 H45B 108.0 . . ?
C45 C46 C41 111.6(4) . . ?
C45 C46 H46A 109.3 . . ?
C41 C46 H46A 109.3 . . ?
C45 C46 H46B 109.3 . . ?
C41 C46 H46B 109.3 . . ?
H46A C46 H46B 108.0 . . ?

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
Ni1 C1 C2 C3 97.5(4) . . . . ?
C1 C2 C3 C4 -179.1(4) . . . . ?
Ni1 C2 C3 C4 -103.5(4) . . . . ?
C1 C2 C3 C8 -0.2(7) . . . . ?
Ni1 C2 C3 C8 75.4(4) . . . . ?
C8 C3 C4 C5 -0.5(6) . . . . ?
C2 C3 C4 C5 178.4(4) . . . . ?
C3 C4 C5 C6 1.1(7) . . . . ?
C4 C5 C6 C7 -0.1(7) . . . . ?
C5 C6 C7 C8 -1.3(8) . . . . ?
C6 C7 C8 C3 1.9(8) . . . . ?
C4 C3 C8 C7 -0.9(6) . . . . ?
C2 C3 C8 C7 -179.8(4) . . . . ?
C11 P1 C9 C10 -152.8(3) . . . . ?
C21 P1 C9 C10 100.0(3) . . . . ?
Ni1 P1 C9 C10 -23.5(3) . . . . ?
P1 C9 C10 P2 34.6(3) . . . . ?
C41 P2 C10 C9 -158.4(3) . . . . ?
C31 P2 C10 C9 97.1(3) . . . . ?
Ni1 P2 C10 C9 -30.4(3) . . . . ?
C9 P1 C11 C16 -46.8(3) . . . . ?
C21 P1 C11 C16 59.9(3) . . . . ?
Ni1 P1 C11 C16 -166.6(2) . . . . ?
C9 P1 C11 C12 79.6(3) . . . . ?
C21 P1 C11 C12 -173.6(3) . . . . ?
Ni1 P1 C11 C12 -40.1(3) . . . . ?
C16 C11 C12 C13 -54.9(4) . . . . ?
P1 C11 C12 C13 175.6(3) . . . . ?
C11 C12 C13 C14 56.0(5) . . . . ?
C12 C13 C14 C15 -56.4(5) . . . . ?
C13 C14 C15 C16 56.5(5) . . . . ?
C12 C11 C16 C15 55.0(4) . . . . ?
P1 C11 C16 C15 -178.0(3) . . . . ?
C14 C15 C16 C11 -56.6(5) . . . . ?
C9 P1 C21 C26 170.4(3) . . . . ?
C11 P1 C21 C26 63.8(3) . . . . ?
Ni1 P1 C21 C26 -72.6(3) . . . . ?
C9 P1 C21 C22 -67.2(3) . . . . ?
C11 P1 C21 C22 -173.8(3) . . . . ?
Ni1 P1 C21 C22 49.8(3) . . . . ?
C26 C21 C22 C23 -53.7(4) . . . . ?
P1 C21 C22 C23 -177.3(3) . . . . ?
C21 C22 C23 C24 55.8(5) . . . . ?
C22 C23 C24 C25 -55.5(5) . . . . ?
C23 C24 C25 C26 55.4(5) . . . . ?
C22 C21 C26 C25 53.5(4) . . . . ?
P1 C21 C26 C25 176.4(3) . . . . ?
C24 C25 C26 C21 -55.6(5) . . . . ?
C41 P2 C31 C36 -164.5(3) . . . . ?
C10 P2 C31 C36 -58.4(3) . . . . ?
Ni1 P2 C31 C36 60.5(3) . . . . ?
C41 P2 C31 C32 70.8(3) . . . . ?
C10 P2 C31 C32 176.9(3) . . . . ?
Ni1 P2 C31 C32 -64.1(3) . . . . ?
C36 C31 C32 C33 56.2(5) . . . . ?
P2 C31 C32 C33 -176.7(3) . . . . ?
C31 C32 C33 C34 -54.6(5) . . . . ?
C32 C33 C34 C35 52.6(5) . . . . ?
C33 C34 C35 C36 -54.1(5) . . . . ?
C32 C31 C36 C35 -57.2(5) . . . . ?
P2 C31 C36 C35 177.1(3) . . . . ?
C34 C35 C36 C31 57.1(5) . . . . ?
C10 P2 C41 C46 76.1(3) . . . . ?
C31 P2 C41 C46 -177.3(3) . . . . ?
Ni1 P2 C41 C46 -42.8(4) . . . . ?
C10 P2 C41 C42 -50.2(4) . . . . ?
C31 P2 C41 C42 56.5(4) . . . . ?
Ni1 P2 C41 C42 -169.1(3) . . . . ?
C46 C41 C42 C43 56.8(5) . . . . ?
P2 C41 C42 C43 -175.5(3) . . . . ?
C41 C42 C43 C44 -56.5(6) . . . . ?
C42 C43 C44 C45 54.1(6) . . . . ?
C43 C44 C45 C46 -53.8(6) . . . . ?
C44 C45 C46 C41 55.6(5) . . . . ?
C42 C41 C46 C45 -56.4(5) . . . . ?
P2 C41 C46 C45 173.8(3) . . . . ?

_refine_diff_density_max         0.451
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.074

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_ij21
_database_code_depnum_ccdc_archive 'CCDC 1052344'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '4c in manuscript'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H54 Ni O2 P2'
_chemical_formula_weight         579.39

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   31.6368(16)
_cell_length_b                   21.6435(12)
_cell_length_c                   9.1291(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6251.0(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    5292
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      21.34

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_F_000             2512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.748
_shelx_estimated_absorpt_T_min   0.909
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8798
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2008). SADABS. University of Göttingen, Germany.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'ImuS microsource'
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40500
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.287
_diffrn_reflns_theta_max         22.984
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.770
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.770
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.770
_reflns_number_total             4469
_reflns_number_gt                2880
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 In the structure are two independent (half) molecules, each on a 
 special position with m-symmetry. Unfortunately the molecules 
 do not fulfill this symmetry. For parts of the molecule (substrate 
 and ethylene bridge of the ligand) the disorder evoked by this 
 symmetry violation could be separated and modelled, but for other 
 parts (central atom and main part of the dcpe ligand) the separation 
 was not distinct enough and the structure had to be modelled as symmetric. 
 We are of course aware of the very limited quantitative significance 
 of such a model, especially in the transition region between separated 
 and non separated parts of the molecule. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0630P)²+20.3407P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4469
_refine_ls_number_parameters     409
_refine_ls_number_restraints     528
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0765
_refine_ls_wR_factor_ref         0.1969
_refine_ls_wR_factor_gt          0.1733
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.065
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1_1 Ni 0.33877(3) 0.7500 1.01220(11) 0.0573(4) Uani 1 2 d DS TU P A .
P1_1 P 0.30469(5) 0.68027(9) 0.8932(2) 0.0648(6) Uani 1 1 d D U . . .
C1_1 C 0.3869(4) 0.6804(7) 1.0629(16) 0.056(4) Uani 0.5 1 d D U P A -1
H1A_1 H 0.3885 0.6655 1.1652 0.067 Uiso 0.5 1 calc R U P A -1
H1B_1 H 0.3926 0.6484 0.9878 0.067 Uiso 0.5 1 calc R U P A -1
C2_1 C 0.4015(3) 0.7416(13) 1.0338(11) 0.050(4) Uani 0.5 1 d D U P A -1
H2_1 H 0.4205 0.7497 0.9484 0.060 Uiso 0.5 1 calc R U P A -1
C3_1 C 0.3872(4) 0.7896(7) 1.1176(14) 0.053(3) Uani 0.5 1 d D U P A -1
H3_1 H 0.3951 0.8317 1.0821 0.063 Uiso 0.5 1 calc R U P A -1
C4_1 C 0.3764(4) 0.7854(6) 1.2781(12) 0.065(3) Uani 0.5 1 d D U P A -1
H4A_1 H 0.3806 0.8268 1.3219 0.079 Uiso 0.5 1 calc R U P A -1
H4B_1 H 0.3970 0.7572 1.3250 0.079 Uiso 0.5 1 calc R U P A -1
C5_1 C 0.3323(4) 0.7635(8) 1.3178(11) 0.061(4) Uani 0.5 1 d D U P A -1
O5_1 O 0.3137(2) 0.7318(4) 1.2226(8) 0.060(3) Uani 0.5 1 d D U P A -1
O6_1 O 0.3183(3) 0.7774(5) 1.4384(9) 0.093(4) Uani 0.5 1 d D U P A -1
C10_1 C 0.2612(5) 0.7261(7) 0.7883(19) 0.054(4) Uani 0.5 1 d D U P B -1
H10A_1 H 0.2537 0.7033 0.6979 0.065 Uiso 0.5 1 calc R U P B -1
H10B_1 H 0.2355 0.7284 0.8501 0.065 Uiso 0.5 1 calc R U P B -1
C9_1 C 0.2744(5) 0.7899(8) 0.748(2) 0.060(5) Uani 0.5 1 d D U P . .
H9A_1 H 0.2492 0.8161 0.7316 0.072 Uiso 0.5 1 calc R U P B .
H9B_1 H 0.2913 0.7891 0.6571 0.072 Uiso 0.5 1 calc R U P . .
C11_1 C 0.2709(2) 0.6272(3) 1.0018(9) 0.082(2) Uani 1 1 d D U . . .
H11_1 H 0.2560 0.5987 0.9328 0.098 Uiso 1 1 calc R U . . .
C12_1 C 0.2984(2) 0.5888(4) 1.1040(9) 0.088(3) Uani 1 1 d D U . . .
H12A_1 H 0.3142 0.6166 1.1704 0.105 Uiso 1 1 calc R U . . .
H12B_1 H 0.3192 0.5651 1.0455 0.105 Uiso 1 1 calc R U . . .
C13_1 C 0.2715(3) 0.5436(4) 1.1958(12) 0.123(4) Uani 1 1 d D U . . .
H13A_1 H 0.2571 0.5137 1.1304 0.148 Uiso 1 1 calc R U . . .
H13B_1 H 0.2899 0.5201 1.2634 0.148 Uiso 1 1 calc R U . . .
C14_1 C 0.2388(3) 0.5796(4) 1.2829(12) 0.135(4) Uani 1 1 d D U . . .
H14A_1 H 0.2210 0.5506 1.3393 0.162 Uiso 1 1 calc R U . . .
H14B_1 H 0.2534 0.6072 1.3533 0.162 Uiso 1 1 calc R U . . .
C15_1 C 0.2111(2) 0.6180(4) 1.1823(12) 0.124(4) Uani 1 1 d D U . . .
H15A_1 H 0.1906 0.6419 1.2415 0.149 Uiso 1 1 calc R U . . .
H15B_1 H 0.1950 0.5903 1.1166 0.149 Uiso 1 1 calc R U . . .
C16_1 C 0.2379(2) 0.6623(3) 1.0904(11) 0.100(3) Uani 1 1 d D U . . .
H16A_1 H 0.2194 0.6858 1.0232 0.120 Uiso 1 1 calc R U . . .
H16B_1 H 0.2522 0.6922 1.1558 0.120 Uiso 1 1 calc R U . . .
C21_1 C 0.3365(2) 0.6280(4) 0.7753(10) 0.094(3) Uani 1 1 d D U . . .
H21_1 H 0.3524 0.6005 0.8438 0.112 Uiso 1 1 calc R U . . .
C22_1 C 0.3100(3) 0.5852(5) 0.6796(13) 0.135(4) Uani 1 1 d D U . . .
H22A_1 H 0.2923 0.6101 0.6124 0.163 Uiso 1 1 calc R U . . .
H22B_1 H 0.2910 0.5602 0.7422 0.163 Uiso 1 1 calc R U . . .
C23_1 C 0.3390(4) 0.5415(6) 0.5887(17) 0.193(6) Uani 1 1 d D U . . .
H23A_1 H 0.3528 0.5118 0.6559 0.232 Uiso 1 1 calc R U . . .
H23B_1 H 0.3213 0.5176 0.5195 0.232 Uiso 1 1 calc R U . . .
C24_1 C 0.3712(4) 0.5736(6) 0.5073(15) 0.197(6) Uani 1 1 d D U . . .
H24A_1 H 0.3577 0.5972 0.4271 0.236 Uiso 1 1 calc R U . . .
H24B_1 H 0.3905 0.5430 0.4624 0.236 Uiso 1 1 calc R U . . .
C25_1 C 0.3970(3) 0.6179(5) 0.6019(13) 0.149(5) Uani 1 1 d D U . . .
H25A_1 H 0.4147 0.5938 0.6709 0.179 Uiso 1 1 calc R U . . .
H25B_1 H 0.4162 0.6422 0.5383 0.179 Uiso 1 1 calc R U . . .
C26_1 C 0.3694(3) 0.6615(4) 0.6874(10) 0.113(3) Uani 1 1 d D U . . .
H26A_1 H 0.3872 0.6864 0.7542 0.135 Uiso 1 1 calc R U . . .
H26B_1 H 0.3552 0.6902 0.6187 0.135 Uiso 1 1 calc R U . . .
Ni1_2 Ni 0.45924(3) 0.2500 0.31070(13) 0.0836(6) Uani 1 2 d DS TU P C .
P1_2 P 0.42568(6) 0.32070(14) 0.4321(2) 0.0992(9) Uani 1 1 d D U . . .
C1_2 C 0.5070(5) 0.3172(9) 0.2445(18) 0.069(4) Uani 0.5 1 d D U P C -1
H1A_2 H 0.5078 0.3294 0.1400 0.083 Uiso 0.5 1 calc R U P C -1
H1B_2 H 0.5137 0.3509 0.3140 0.083 Uiso 0.5 1 calc R U P C -1
C2_2 C 0.5215(3) 0.2561(16) 0.2811(11) 0.065(4) Uani 0.5 1 d D U P C -1
H2_2 H 0.5414 0.2494 0.3646 0.077 Uiso 0.5 1 calc R U P C -1
C3_2 C 0.5050(5) 0.2068(9) 0.2053(16) 0.069(4) Uani 0.5 1 d D U P C -1
H3_2 H 0.5125 0.1654 0.2462 0.082 Uiso 0.5 1 calc R U P C -1
C4_2 C 0.4924(3) 0.2063(7) 0.0480(12) 0.071(4) Uani 0.5 1 d D U P C -1
H4A_2 H 0.4939 0.1631 0.0129 0.086 Uiso 0.5 1 calc R U P C -1
H4B_2 H 0.5138 0.2302 -0.0073 0.086 Uiso 0.5 1 calc R U P C -1
C5_2 C 0.4493(3) 0.2314(8) 0.0082(13) 0.075(5) Uani 0.5 1 d D U P C -1
O5_2 O 0.4319(2) 0.2664(6) 0.1023(8) 0.075(4) Uani 0.5 1 d D U P C -1
O6_2 O 0.4337(3) 0.2168(6) -0.1099(10) 0.113(5) Uani 0.5 1 d D U P C -1
C10_2 C 0.3819(4) 0.2695(8) 0.5318(15) 0.086(4) Uani 0.5 1 d D U P D -1
H10A_2 H 0.3719 0.2924 0.6190 0.103 Uiso 0.5 1 calc R U P D -1
H10B_2 H 0.3576 0.2651 0.4645 0.103 Uiso 0.5 1 calc R U P D -1
C9_2 C 0.3952(4) 0.2061(8) 0.5799(15) 0.073(4) Uani 0.5 1 d D U P . .
H9A_2 H 0.3704 0.1792 0.5966 0.087 Uiso 0.5 1 calc R U P D .
H9B_2 H 0.4122 0.2079 0.6709 0.087 Uiso 0.5 1 calc R U P . .
C11_2 C 0.39178(19) 0.3743(4) 0.3280(8) 0.089(2) Uani 1 1 d D U . . .
H11_2 H 0.3763 0.4007 0.4001 0.107 Uiso 1 1 calc R U . . .
C12_2 C 0.4183(2) 0.4168(4) 0.2311(8) 0.082(2) Uani 1 1 d D U . . .
H12A_2 H 0.4362 0.3914 0.1657 0.098 Uiso 1 1 calc R U . . .
H12B_2 H 0.4373 0.4418 0.2939 0.098 Uiso 1 1 calc R U . . .
C13_2 C 0.3909(2) 0.4605(4) 0.1374(9) 0.093(3) Uani 1 1 d D U . . .
H13A_2 H 0.3759 0.4900 0.2020 0.112 Uiso 1 1 calc R U . . .
H13B_2 H 0.4092 0.4845 0.0705 0.112 Uiso 1 1 calc R U . . .
C14_2 C 0.3590(2) 0.4243(4) 0.0489(10) 0.092(3) Uani 1 1 d D U . . .
H14A_2 H 0.3410 0.4533 -0.0068 0.111 Uiso 1 1 calc R U . . .
H14B_2 H 0.3741 0.3978 -0.0224 0.111 Uiso 1 1 calc R U . . .
C15_2 C 0.3315(2) 0.3844(4) 0.1454(10) 0.098(3) Uani 1 1 d D U . . .
H15A_2 H 0.3118 0.3600 0.0840 0.118 Uiso 1 1 calc R U . . .
H15B_2 H 0.3145 0.4108 0.2114 0.118 Uiso 1 1 calc R U . . .
C16_2 C 0.3591(2) 0.3406(4) 0.2364(10) 0.102(3) Uani 1 1 d D U . . .
H16A_2 H 0.3407 0.3160 0.3020 0.122 Uiso 1 1 calc R U . . .
H16B_2 H 0.3738 0.3116 0.1697 0.122 Uiso 1 1 calc R U . . .
C21_2 C 0.4575(2) 0.3731(5) 0.5517(9) 0.129(3) Uani 1 1 d D U . . .
H21_2 H 0.4732 0.4001 0.4814 0.154 Uiso 1 1 calc R U . . .
C22_2 C 0.4313(3) 0.4185(6) 0.6445(11) 0.149(4) Uani 1 1 d D U . . .
H22A_2 H 0.4128 0.3950 0.7122 0.179 Uiso 1 1 calc R U . . .
H22B_2 H 0.4130 0.4434 0.5794 0.179 Uiso 1 1 calc R U . . .
C23_2 C 0.4604(4) 0.4619(7) 0.7338(16) 0.214(6) Uani 1 1 d D U . . .
H23A_2 H 0.4741 0.4912 0.6652 0.257 Uiso 1 1 calc R U . . .
H23B_2 H 0.4426 0.4864 0.8013 0.257 Uiso 1 1 calc R U . . .
C24_2 C 0.4929(4) 0.4321(8) 0.8184(14) 0.221(7) Uani 1 1 d D U . . .
H24A_2 H 0.4799 0.4094 0.9010 0.265 Uiso 1 1 calc R U . . .
H24B_2 H 0.5122 0.4637 0.8596 0.265 Uiso 1 1 calc R U . . .
C25_2 C 0.5184(3) 0.3870(7) 0.7242(12) 0.198(6) Uani 1 1 d D U . . .
H25A_2 H 0.5361 0.4108 0.6550 0.237 Uiso 1 1 calc R U . . .
H25B_2 H 0.5375 0.3629 0.7883 0.237 Uiso 1 1 calc R U . . .
C26_2 C 0.4909(3) 0.3430(6) 0.6388(11) 0.183(5) Uani 1 1 d D U . . .
H26A_2 H 0.5091 0.3187 0.5721 0.219 Uiso 1 1 calc R U . . .
H26B_2 H 0.4775 0.3138 0.7081 0.219 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1_1 C3_1 2.001(12) . ?
Ni1_1 C2_1 2.003(8) . ?
Ni1_1 O5_1 2.115(7) . ?
Ni1_1 P1_1 2.149(2) 7_575 ?
Ni1_1 P1_1 2.149(2) . ?
Ni1_1 C1_1 2.191(13) . ?
P1_1 C9_1 1.757(16) 7_575 ?
P1_1 C11_1 1.855(6) . ?
P1_1 C21_1 1.857(8) . ?
P1_1 C10_1 1.949(13) . ?
C1_1 C2_1 1.43(3) . ?
C1_1 H1A_1 0.9900 . ?
C1_1 H1B_1 0.9900 . ?
C2_1 C3_1 1.37(2) . ?
C2_1 H2_1 1.0000 . ?
C3_1 C4_1 1.506(15) . ?
C3_1 H3_1 1.0000 . ?
C4_1 C5_1 1.520(15) . ?
C4_1 H4A_1 0.9900 . ?
C4_1 H4B_1 0.9900 . ?
C5_1 O6_1 1.224(12) . ?
C5_1 O5_1 1.254(14) . ?
C10_1 C9_1 1.487(15) . ?
C10_1 H10A_1 0.9900 . ?
C10_1 H10B_1 0.9900 . ?
C9_1 P1_1 1.757(16) 7_575 ?
C9_1 H9A_1 0.9900 . ?
C9_1 H9B_1 0.9900 . ?
C11_1 C12_1 1.522(9) . ?
C11_1 C16_1 1.524(9) . ?
C11_1 H11_1 1.0000 . ?
C12_1 C13_1 1.544(9) . ?
C12_1 H12A_1 0.9900 . ?
C12_1 H12B_1 0.9900 . ?
C13_1 C14_1 1.520(11) . ?
C13_1 H13A_1 0.9900 . ?
C13_1 H13B_1 0.9900 . ?
C14_1 C15_1 1.517(11) . ?
C14_1 H14A_1 0.9900 . ?
C14_1 H14B_1 0.9900 . ?
C15_1 C16_1 1.532(9) . ?
C15_1 H15A_1 0.9900 . ?
C15_1 H15B_1 0.9900 . ?
C16_1 H16A_1 0.9900 . ?
C16_1 H16B_1 0.9900 . ?
C21_1 C26_1 1.501(10) . ?
C21_1 C22_1 1.525(10) . ?
C21_1 H21_1 1.0000 . ?
C22_1 C23_1 1.557(12) . ?
C22_1 H22A_1 0.9900 . ?
C22_1 H22B_1 0.9900 . ?
C23_1 C24_1 1.440(13) . ?
C23_1 H23A_1 0.9900 . ?
C23_1 H23B_1 0.9900 . ?
C24_1 C25_1 1.527(12) . ?
C24_1 H24A_1 0.9900 . ?
C24_1 H24B_1 0.9900 . ?
C25_1 C26_1 1.505(11) . ?
C25_1 H25A_1 0.9900 . ?
C25_1 H25B_1 0.9900 . ?
C26_1 H26A_1 0.9900 . ?
C26_1 H26B_1 0.9900 . ?
Ni1_2 C3_2 1.973(14) . ?
Ni1_2 C2_2 1.992(8) . ?
Ni1_2 O5_2 2.120(7) . ?
Ni1_2 P1_2 2.167(3) 7_565 ?
Ni1_2 P1_2 2.167(3) . ?
Ni1_2 C1_2 2.183(15) . ?
P1_2 C9_2 1.756(15) 7_565 ?
P1_2 C11_2 1.843(7) . ?
P1_2 C21_2 1.868(9) . ?
P1_2 C10_2 1.993(13) . ?
C1_2 C2_2 1.44(3) . ?
C1_2 H1A_2 0.9900 . ?
C1_2 H1B_2 0.9900 . ?
C2_2 C3_2 1.37(2) . ?
C2_2 H2_2 1.0000 . ?
C3_2 C4_2 1.490(17) . ?
C3_2 H3_2 1.0000 . ?
C4_2 C5_2 1.513(15) . ?
C4_2 H4A_2 0.9900 . ?
C4_2 H4B_2 0.9900 . ?
C5_2 O6_2 1.227(12) . ?
C5_2 O5_2 1.270(14) . ?
C10_2 C9_2 1.502(16) . ?
C10_2 H10A_2 0.9900 . ?
C10_2 H10B_2 0.9900 . ?
C9_2 P1_2 1.756(15) 7_565 ?
C9_2 H9A_2 0.9900 . ?
C9_2 H9B_2 0.9900 . ?
C11_2 C16_2 1.515(10) . ?
C11_2 C12_2 1.528(9) . ?
C11_2 H11_2 1.0000 . ?
C12_2 C13_2 1.543(9) . ?
C12_2 H12A_2 0.9900 . ?
C12_2 H12B_2 0.9900 . ?
C13_2 C14_2 1.511(9) . ?
C13_2 H13A_2 0.9900 . ?
C13_2 H13B_2 0.9900 . ?
C14_2 C15_2 1.510(10) . ?
C14_2 H14A_2 0.9900 . ?
C14_2 H14B_2 0.9900 . ?
C15_2 C16_2 1.533(9) . ?
C15_2 H15A_2 0.9900 . ?
C15_2 H15B_2 0.9900 . ?
C16_2 H16A_2 0.9900 . ?
C16_2 H16B_2 0.9900 . ?
C21_2 C26_2 1.475(11) . ?
C21_2 C22_2 1.540(11) . ?
C21_2 H21_2 1.0000 . ?
C22_2 C23_2 1.549(13) . ?
C22_2 H22A_2 0.9900 . ?
C22_2 H22B_2 0.9900 . ?
C23_2 C24_2 1.440(14) . ?
C23_2 H23A_2 0.9900 . ?
C23_2 H23B_2 0.9900 . ?
C24_2 C25_2 1.529(12) . ?
C24_2 H24A_2 0.9900 . ?
C24_2 H24B_2 0.9900 . ?
C25_2 C26_2 1.506(13) . ?
C25_2 H25A_2 0.9900 . ?
C25_2 H25B_2 0.9900 . ?
C26_2 H26A_2 0.9900 . ?
C26_2 H26B_2 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3_1 Ni1_1 C2_1 39.9(6) . . ?
C3_1 Ni1_1 O5_1 86.0(4) . . ?
C2_1 Ni1_1 O5_1 105.4(4) . . ?
C3_1 Ni1_1 P1_1 109.0(4) . 7_575 ?
C2_1 Ni1_1 P1_1 127.6(7) . 7_575 ?
O5_1 Ni1_1 P1_1 113.7(2) . 7_575 ?
C3_1 Ni1_1 P1_1 158.0(4) . . ?
C2_1 Ni1_1 P1_1 118.9(7) . . ?
O5_1 Ni1_1 P1_1 98.0(2) . . ?
P1_1 Ni1_1 P1_1 89.20(11) 7_575 . ?
C3_1 Ni1_1 C1_1 70.2(6) . . ?
C2_1 Ni1_1 C1_1 39.5(8) . . ?
O5_1 Ni1_1 C1_1 86.6(4) . . ?
P1_1 Ni1_1 C1_1 159.7(4) 7_575 . ?
P1_1 Ni1_1 C1_1 88.4(4) . . ?
C9_1 P1_1 C11_1 108.4(7) 7_575 . ?
C9_1 P1_1 C21_1 94.8(6) 7_575 . ?
C11_1 P1_1 C21_1 104.1(4) . . ?
C9_1 P1_1 C10_1 19.5(7) 7_575 . ?
C11_1 P1_1 C10_1 99.8(6) . . ?
C21_1 P1_1 C10_1 114.1(6) . . ?
C9_1 P1_1 Ni1_1 113.3(6) 7_575 . ?
C11_1 P1_1 Ni1_1 117.0(3) . . ?
C21_1 P1_1 Ni1_1 116.7(3) . . ?
C10_1 P1_1 Ni1_1 104.2(4) . . ?
C2_1 C1_1 Ni1_1 63.2(6) . . ?
C2_1 C1_1 H1A_1 117.4 . . ?
Ni1_1 C1_1 H1A_1 117.4 . . ?
C2_1 C1_1 H1B_1 117.4 . . ?
Ni1_1 C1_1 H1B_1 117.4 . . ?
H1A_1 C1_1 H1B_1 114.5 . . ?
C3_1 C2_1 C1_1 119.5(12) . . ?
C3_1 C2_1 Ni1_1 69.9(7) . . ?
C1_1 C2_1 Ni1_1 77.3(8) . . ?
C3_1 C2_1 H2_1 120.2 . . ?
C1_1 C2_1 H2_1 120.2 . . ?
Ni1_1 C2_1 H2_1 120.2 . . ?
C2_1 C3_1 C4_1 125.0(14) . . ?
C2_1 C3_1 Ni1_1 70.1(7) . . ?
C4_1 C3_1 Ni1_1 105.7(8) . . ?
C2_1 C3_1 H3_1 115.3 . . ?
C4_1 C3_1 H3_1 115.3 . . ?
Ni1_1 C3_1 H3_1 115.3 . . ?
C3_1 C4_1 C5_1 117.2(10) . . ?
C3_1 C4_1 H4A_1 108.0 . . ?
C5_1 C4_1 H4A_1 108.0 . . ?
C3_1 C4_1 H4B_1 108.0 . . ?
C5_1 C4_1 H4B_1 108.0 . . ?
H4A_1 C4_1 H4B_1 107.2 . . ?
O6_1 C5_1 O5_1 126.1(12) . . ?
O6_1 C5_1 C4_1 118.0(12) . . ?
O5_1 C5_1 C4_1 115.9(9) . . ?
C5_1 O5_1 Ni1_1 110.6(7) . . ?
C9_1 C10_1 P1_1 113.3(13) . . ?
C9_1 C10_1 H10A_1 108.9 . . ?
P1_1 C10_1 H10A_1 108.9 . . ?
C9_1 C10_1 H10B_1 108.9 . . ?
P1_1 C10_1 H10B_1 108.9 . . ?
H10A_1 C10_1 H10B_1 107.7 . . ?
C10_1 C9_1 P1_1 108.0(13) . 7_575 ?
C10_1 C9_1 H9A_1 110.1 . . ?
P1_1 C9_1 H9A_1 110.1 7_575 . ?
C10_1 C9_1 H9B_1 110.1 . . ?
P1_1 C9_1 H9B_1 110.1 7_575 . ?
H9A_1 C9_1 H9B_1 108.4 . . ?
C12_1 C11_1 C16_1 109.7(7) . . ?
C12_1 C11_1 P1_1 109.7(4) . . ?
C16_1 C11_1 P1_1 111.7(5) . . ?
C12_1 C11_1 H11_1 108.5 . . ?
C16_1 C11_1 H11_1 108.5 . . ?
P1_1 C11_1 H11_1 108.5 . . ?
C11_1 C12_1 C13_1 111.4(6) . . ?
C11_1 C12_1 H12A_1 109.3 . . ?
C13_1 C12_1 H12A_1 109.3 . . ?
C11_1 C12_1 H12B_1 109.3 . . ?
C13_1 C12_1 H12B_1 109.3 . . ?
H12A_1 C12_1 H12B_1 108.0 . . ?
C14_1 C13_1 C12_1 109.4(7) . . ?
C14_1 C13_1 H13A_1 109.8 . . ?
C12_1 C13_1 H13A_1 109.8 . . ?
C14_1 C13_1 H13B_1 109.8 . . ?
C12_1 C13_1 H13B_1 109.8 . . ?
H13A_1 C13_1 H13B_1 108.2 . . ?
C15_1 C14_1 C13_1 110.9(8) . . ?
C15_1 C14_1 H14A_1 109.5 . . ?
C13_1 C14_1 H14A_1 109.5 . . ?
C15_1 C14_1 H14B_1 109.5 . . ?
C13_1 C14_1 H14B_1 109.5 . . ?
H14A_1 C14_1 H14B_1 108.0 . . ?
C14_1 C15_1 C16_1 110.7(7) . . ?
C14_1 C15_1 H15A_1 109.5 . . ?
C16_1 C15_1 H15A_1 109.5 . . ?
C14_1 C15_1 H15B_1 109.5 . . ?
C16_1 C15_1 H15B_1 109.5 . . ?
H15A_1 C15_1 H15B_1 108.1 . . ?
C11_1 C16_1 C15_1 111.0(6) . . ?
C11_1 C16_1 H16A_1 109.4 . . ?
C15_1 C16_1 H16A_1 109.4 . . ?
C11_1 C16_1 H16B_1 109.4 . . ?
C15_1 C16_1 H16B_1 109.4 . . ?
H16A_1 C16_1 H16B_1 108.0 . . ?
C26_1 C21_1 C22_1 111.6(7) . . ?
C26_1 C21_1 P1_1 113.0(6) . . ?
C22_1 C21_1 P1_1 113.9(6) . . ?
C26_1 C21_1 H21_1 105.9 . . ?
C22_1 C21_1 H21_1 105.9 . . ?
P1_1 C21_1 H21_1 105.9 . . ?
C21_1 C22_1 C23_1 110.5(8) . . ?
C21_1 C22_1 H22A_1 109.5 . . ?
C23_1 C22_1 H22A_1 109.5 . . ?
C21_1 C22_1 H22B_1 109.5 . . ?
C23_1 C22_1 H22B_1 109.5 . . ?
H22A_1 C22_1 H22B_1 108.1 . . ?
C24_1 C23_1 C22_1 113.5(10) . . ?
C24_1 C23_1 H23A_1 108.9 . . ?
C22_1 C23_1 H23A_1 108.9 . . ?
C24_1 C23_1 H23B_1 108.9 . . ?
C22_1 C23_1 H23B_1 108.9 . . ?
H23A_1 C23_1 H23B_1 107.7 . . ?
C23_1 C24_1 C25_1 113.0(10) . . ?
C23_1 C24_1 H24A_1 109.0 . . ?
C25_1 C24_1 H24A_1 109.0 . . ?
C23_1 C24_1 H24B_1 109.0 . . ?
C25_1 C24_1 H24B_1 109.0 . . ?
H24A_1 C24_1 H24B_1 107.8 . . ?
C26_1 C25_1 C24_1 112.0(9) . . ?
C26_1 C25_1 H25A_1 109.2 . . ?
C24_1 C25_1 H25A_1 109.2 . . ?
C26_1 C25_1 H25B_1 109.2 . . ?
C24_1 C25_1 H25B_1 109.2 . . ?
H25A_1 C25_1 H25B_1 107.9 . . ?
C21_1 C26_1 C25_1 112.2(8) . . ?
C21_1 C26_1 H26A_1 109.2 . . ?
C25_1 C26_1 H26A_1 109.2 . . ?
C21_1 C26_1 H26B_1 109.2 . . ?
C25_1 C26_1 H26B_1 109.2 . . ?
H26A_1 C26_1 H26B_1 107.9 . . ?
C3_2 Ni1_2 C2_2 40.5(7) . . ?
C3_2 Ni1_2 O5_2 86.6(5) . . ?
C2_2 Ni1_2 O5_2 105.7(4) . . ?
C3_2 Ni1_2 P1_2 105.9(6) . 7_565 ?
C2_2 Ni1_2 P1_2 126.9(9) . 7_565 ?
O5_2 Ni1_2 P1_2 112.2(3) . 7_565 ?
C3_2 Ni1_2 P1_2 160.6(6) . . ?
C2_2 Ni1_2 P1_2 120.5(9) . . ?
O5_2 Ni1_2 P1_2 98.1(3) . . ?
P1_2 Ni1_2 P1_2 89.83(15) 7_565 . ?
C3_2 Ni1_2 C1_2 70.9(6) . . ?
C2_2 Ni1_2 C1_2 40.0(8) . . ?
O5_2 Ni1_2 C1_2 85.6(5) . . ?
P1_2 Ni1_2 C1_2 162.0(5) 7_565 . ?
P1_2 Ni1_2 C1_2 90.6(5) . . ?
C9_2 P1_2 C11_2 106.5(6) 7_565 . ?
C9_2 P1_2 C21_2 92.7(5) 7_565 . ?
C11_2 P1_2 C21_2 103.5(4) . . ?
C9_2 P1_2 C10_2 23.8(6) 7_565 . ?
C11_2 P1_2 C10_2 100.4(5) . . ?
C21_2 P1_2 C10_2 116.4(5) . . ?
C9_2 P1_2 Ni1_2 115.4(6) 7_565 . ?
C11_2 P1_2 Ni1_2 117.7(3) . . ?
C21_2 P1_2 Ni1_2 117.6(3) . . ?
C10_2 P1_2 Ni1_2 100.4(5) . . ?
C2_2 C1_2 Ni1_2 62.8(7) . . ?
C2_2 C1_2 H1A_2 117.5 . . ?
Ni1_2 C1_2 H1A_2 117.5 . . ?
C2_2 C1_2 H1B_2 117.5 . . ?
Ni1_2 C1_2 H1B_2 117.5 . . ?
H1A_2 C1_2 H1B_2 114.6 . . ?
C3_2 C2_2 C1_2 118.4(12) . . ?
C3_2 C2_2 Ni1_2 69.0(8) . . ?
C1_2 C2_2 Ni1_2 77.2(9) . . ?
C3_2 C2_2 H2_2 120.7 . . ?
C1_2 C2_2 H2_2 120.7 . . ?
Ni1_2 C2_2 H2_2 120.7 . . ?
C2_2 C3_2 C4_2 126.3(15) . . ?
C2_2 C3_2 Ni1_2 70.5(7) . . ?
C4_2 C3_2 Ni1_2 106.1(9) . . ?
C2_2 C3_2 H3_2 114.7 . . ?
C4_2 C3_2 H3_2 114.7 . . ?
Ni1_2 C3_2 H3_2 114.7 . . ?
C3_2 C4_2 C5_2 118.0(10) . . ?
C3_2 C4_2 H4A_2 107.8 . . ?
C5_2 C4_2 H4A_2 107.8 . . ?
C3_2 C4_2 H4B_2 107.8 . . ?
C5_2 C4_2 H4B_2 107.8 . . ?
H4A_2 C4_2 H4B_2 107.1 . . ?
O6_2 C5_2 O5_2 125.1(12) . . ?
O6_2 C5_2 C4_2 118.7(12) . . ?
O5_2 C5_2 C4_2 116.3(10) . . ?
C5_2 O5_2 Ni1_2 109.3(8) . . ?
C9_2 C10_2 P1_2 116.6(11) . . ?
C9_2 C10_2 H10A_2 108.1 . . ?
P1_2 C10_2 H10A_2 108.1 . . ?
C9_2 C10_2 H10B_2 108.1 . . ?
P1_2 C10_2 H10B_2 108.1 . . ?
H10A_2 C10_2 H10B_2 107.3 . . ?
C10_2 C9_2 P1_2 103.3(10) . 7_565 ?
C10_2 C9_2 H9A_2 111.1 . . ?
P1_2 C9_2 H9A_2 111.1 7_565 . ?
C10_2 C9_2 H9B_2 111.1 . . ?
P1_2 C9_2 H9B_2 111.1 7_565 . ?
H9A_2 C9_2 H9B_2 109.1 . . ?
C16_2 C11_2 C12_2 110.2(6) . . ?
C16_2 C11_2 P1_2 112.3(6) . . ?
C12_2 C11_2 P1_2 110.9(4) . . ?
C16_2 C11_2 H11_2 107.7 . . ?
C12_2 C11_2 H11_2 107.7 . . ?
P1_2 C11_2 H11_2 107.7 . . ?
C11_2 C12_2 C13_2 112.4(6) . . ?
C11_2 C12_2 H12A_2 109.1 . . ?
C13_2 C12_2 H12A_2 109.1 . . ?
C11_2 C12_2 H12B_2 109.1 . . ?
C13_2 C12_2 H12B_2 109.1 . . ?
H12A_2 C12_2 H12B_2 107.9 . . ?
C14_2 C13_2 C12_2 110.8(7) . . ?
C14_2 C13_2 H13A_2 109.5 . . ?
C12_2 C13_2 H13A_2 109.5 . . ?
C14_2 C13_2 H13B_2 109.5 . . ?
C12_2 C13_2 H13B_2 109.5 . . ?
H13A_2 C13_2 H13B_2 108.1 . . ?
C15_2 C14_2 C13_2 111.7(7) . . ?
C15_2 C14_2 H14A_2 109.3 . . ?
C13_2 C14_2 H14A_2 109.3 . . ?
C15_2 C14_2 H14B_2 109.3 . . ?
C13_2 C14_2 H14B_2 109.3 . . ?
H14A_2 C14_2 H14B_2 107.9 . . ?
C14_2 C15_2 C16_2 109.9(6) . . ?
C14_2 C15_2 H15A_2 109.7 . . ?
C16_2 C15_2 H15A_2 109.7 . . ?
C14_2 C15_2 H15B_2 109.7 . . ?
C16_2 C15_2 H15B_2 109.7 . . ?
H15A_2 C15_2 H15B_2 108.2 . . ?
C11_2 C16_2 C15_2 113.0(7) . . ?
C11_2 C16_2 H16A_2 109.0 . . ?
C15_2 C16_2 H16A_2 109.0 . . ?
C11_2 C16_2 H16B_2 109.0 . . ?
C15_2 C16_2 H16B_2 109.0 . . ?
H16A_2 C16_2 H16B_2 107.8 . . ?
C26_2 C21_2 C22_2 111.8(7) . . ?
C26_2 C21_2 P1_2 115.7(8) . . ?
C22_2 C21_2 P1_2 114.7(6) . . ?
C26_2 C21_2 H21_2 104.3 . . ?
C22_2 C21_2 H21_2 104.3 . . ?
P1_2 C21_2 H21_2 104.3 . . ?
C21_2 C22_2 C23_2 110.9(8) . . ?
C21_2 C22_2 H22A_2 109.5 . . ?
C23_2 C22_2 H22A_2 109.5 . . ?
C21_2 C22_2 H22B_2 109.5 . . ?
C23_2 C22_2 H22B_2 109.5 . . ?
H22A_2 C22_2 H22B_2 108.1 . . ?
C24_2 C23_2 C22_2 115.8(13) . . ?
C24_2 C23_2 H23A_2 108.3 . . ?
C22_2 C23_2 H23A_2 108.3 . . ?
C24_2 C23_2 H23B_2 108.3 . . ?
C22_2 C23_2 H23B_2 108.3 . . ?
H23A_2 C23_2 H23B_2 107.4 . . ?
C23_2 C24_2 C25_2 111.2(10) . . ?
C23_2 C24_2 H24A_2 109.4 . . ?
C25_2 C24_2 H24A_2 109.4 . . ?
C23_2 C24_2 H24B_2 109.4 . . ?
C25_2 C24_2 H24B_2 109.4 . . ?
H24A_2 C24_2 H24B_2 108.0 . . ?
C26_2 C25_2 C24_2 113.0(9) . . ?
C26_2 C25_2 H25A_2 109.0 . . ?
C24_2 C25_2 H25A_2 109.0 . . ?
C26_2 C25_2 H25B_2 109.0 . . ?
C24_2 C25_2 H25B_2 109.0 . . ?
H25A_2 C25_2 H25B_2 107.8 . . ?
C21_2 C26_2 C25_2 114.4(11) . . ?
C21_2 C26_2 H26A_2 108.7 . . ?
C25_2 C26_2 H26A_2 108.7 . . ?
C21_2 C26_2 H26B_2 108.7 . . ?
C25_2 C26_2 H26B_2 108.7 . . ?
H26A_2 C26_2 H26B_2 107.6 . . ?

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
Ni1_1 C1_1 C2_1 C3_1 57.9(9) . . . . ?
C1_1 C2_1 C3_1 C4_1 33.9(15) . . . . ?
Ni1_1 C2_1 C3_1 C4_1 95.6(12) . . . . ?
C1_1 C2_1 C3_1 Ni1_1 -61.7(9) . . . . ?
C2_1 C3_1 C4_1 C5_1 -85.2(17) . . . . ?
Ni1_1 C3_1 C4_1 C5_1 -8.8(16) . . . . ?
C3_1 C4_1 C5_1 O6_1 -157.7(14) . . . . ?
C3_1 C4_1 C5_1 O5_1 23(2) . . . . ?
O6_1 C5_1 O5_1 Ni1_1 157.5(13) . . . . ?
C4_1 C5_1 O5_1 Ni1_1 -23.4(15) . . . . ?
P1_1 C10_1 C9_1 P1_1 -37.8(18) . . . 7_575 ?
C9_1 P1_1 C11_1 C12_1 166.2(7) 7_575 . . . ?
C21_1 P1_1 C11_1 C12_1 66.2(7) . . . . ?
C10_1 P1_1 C11_1 C12_1 -175.8(7) . . . . ?
Ni1_1 P1_1 C11_1 C12_1 -64.2(6) . . . . ?
C9_1 P1_1 C11_1 C16_1 -71.9(8) 7_575 . . . ?
C21_1 P1_1 C11_1 C16_1 -171.9(6) . . . . ?
C10_1 P1_1 C11_1 C16_1 -53.9(8) . . . . ?
Ni1_1 P1_1 C11_1 C16_1 57.7(6) . . . . ?
C16_1 C11_1 C12_1 C13_1 57.3(9) . . . . ?
P1_1 C11_1 C12_1 C13_1 -179.6(6) . . . . ?
C11_1 C12_1 C13_1 C14_1 -57.7(11) . . . . ?
C12_1 C13_1 C14_1 C15_1 57.3(11) . . . . ?
C13_1 C14_1 C15_1 C16_1 -57.6(11) . . . . ?
C12_1 C11_1 C16_1 C15_1 -56.7(9) . . . . ?
P1_1 C11_1 C16_1 C15_1 -178.6(6) . . . . ?
C14_1 C15_1 C16_1 C11_1 57.1(11) . . . . ?
C9_1 P1_1 C21_1 C26_1 75.2(10) 7_575 . . . ?
C11_1 P1_1 C21_1 C26_1 -174.5(7) . . . . ?
C10_1 P1_1 C21_1 C26_1 77.7(9) . . . . ?
Ni1_1 P1_1 C21_1 C26_1 -44.0(8) . . . . ?
C9_1 P1_1 C21_1 C22_1 -53.5(10) 7_575 . . . ?
C11_1 P1_1 C21_1 C22_1 56.8(8) . . . . ?
C10_1 P1_1 C21_1 C22_1 -51.0(9) . . . . ?
Ni1_1 P1_1 C21_1 C22_1 -172.7(6) . . . . ?
C26_1 C21_1 C22_1 C23_1 52.6(12) . . . . ?
P1_1 C21_1 C22_1 C23_1 -178.0(9) . . . . ?
C21_1 C22_1 C23_1 C24_1 -52.2(16) . . . . ?
C22_1 C23_1 C24_1 C25_1 51.8(18) . . . . ?
C23_1 C24_1 C25_1 C26_1 -52.2(17) . . . . ?
C22_1 C21_1 C26_1 C25_1 -54.7(12) . . . . ?
P1_1 C21_1 C26_1 C25_1 175.4(7) . . . . ?
C24_1 C25_1 C26_1 C21_1 53.3(14) . . . . ?
Ni1_2 C1_2 C2_2 C3_2 57.2(9) . . . . ?
C1_2 C2_2 C3_2 C4_2 34.5(15) . . . . ?
Ni1_2 C2_2 C3_2 C4_2 96.0(13) . . . . ?
C1_2 C2_2 C3_2 Ni1_2 -61.4(9) . . . . ?
C2_2 C3_2 C4_2 C5_2 -82.4(19) . . . . ?
Ni1_2 C3_2 C4_2 C5_2 -5.2(18) . . . . ?
C3_2 C4_2 C5_2 O6_2 -160.5(15) . . . . ?
C3_2 C4_2 C5_2 O5_2 19(2) . . . . ?
O6_2 C5_2 O5_2 Ni1_2 158.6(14) . . . . ?
C4_2 C5_2 O5_2 Ni1_2 -21.1(15) . . . . ?
P1_2 C10_2 C9_2 P1_2 -41.6(11) . . . 7_565 ?
C9_2 P1_2 C11_2 C16_2 -75.9(8) 7_565 . . . ?
C21_2 P1_2 C11_2 C16_2 -172.8(6) . . . . ?
C10_2 P1_2 C11_2 C16_2 -52.2(7) . . . . ?
Ni1_2 P1_2 C11_2 C16_2 55.5(6) . . . . ?
C9_2 P1_2 C11_2 C12_2 160.3(7) 7_565 . . . ?
C21_2 P1_2 C11_2 C12_2 63.4(7) . . . . ?
C10_2 P1_2 C11_2 C12_2 -176.0(7) . . . . ?
Ni1_2 P1_2 C11_2 C12_2 -68.3(6) . . . . ?
C16_2 C11_2 C12_2 C13_2 52.6(9) . . . . ?
P1_2 C11_2 C12_2 C13_2 177.6(6) . . . . ?
C11_2 C12_2 C13_2 C14_2 -54.3(9) . . . . ?
C12_2 C13_2 C14_2 C15_2 56.4(9) . . . . ?
C13_2 C14_2 C15_2 C16_2 -57.0(10) . . . . ?
C12_2 C11_2 C16_2 C15_2 -54.0(9) . . . . ?
P1_2 C11_2 C16_2 C15_2 -178.2(6) . . . . ?
C14_2 C15_2 C16_2 C11_2 56.3(10) . . . . ?
C9_2 P1_2 C21_2 C26_2 78.0(9) 7_565 . . . ?
C11_2 P1_2 C21_2 C26_2 -174.3(7) . . . . ?
C10_2 P1_2 C21_2 C26_2 76.6(9) . . . . ?
Ni1_2 P1_2 C21_2 C26_2 -42.6(9) . . . . ?
C9_2 P1_2 C21_2 C22_2 -54.5(10) 7_565 . . . ?
C11_2 P1_2 C21_2 C22_2 53.2(9) . . . . ?
C10_2 P1_2 C21_2 C22_2 -55.9(10) . . . . ?
Ni1_2 P1_2 C21_2 C22_2 -175.1(7) . . . . ?
C26_2 C21_2 C22_2 C23_2 48.5(15) . . . . ?
P1_2 C21_2 C22_2 C23_2 -177.2(9) . . . . ?
C21_2 C22_2 C23_2 C24_2 -50.8(16) . . . . ?
C22_2 C23_2 C24_2 C25_2 51.1(19) . . . . ?
C23_2 C24_2 C25_2 C26_2 -50.4(19) . . . . ?
C22_2 C21_2 C26_2 C25_2 -51.1(14) . . . . ?
P1_2 C21_2 C26_2 C25_2 175.1(8) . . . . ?
C24_2 C25_2 C26_2 C21_2 51.9(16) . . . . ?

_refine_diff_density_max         0.527
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.070

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_THETM01_ij21                
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: We have cut the dataset at a resolution of 0.91  due to 
I/sigma and R(int) criteria. Despite of using a high intensity source 
and long irradiation times this was the best achievable resolution. 
The data to parameter ratio is still acceptable. In 
order to compensate for the lack of information we used similarity 
restraints among the two independent molecules (SHELX SAME command) 
and rigid bond restraints (SHELX RIGU command) for all atoms.
;
####################################################################### 
# 
# 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_ij4
_database_code_depnum_ccdc_archive 'CCDC 1052345'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '5b in manuscript'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H64 Ni O3 P2'
_chemical_formula_weight         701.55

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   16.78(3)
_cell_length_b                   8.692(16)
_cell_length_c                   27.13(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.38(3)
_cell_angle_gamma                90
_cell_volume                     3850(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_F_000             1520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.621
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8574
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2008). SADABS. University of Göttingen, Germany.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'ImuS microsource'
_diffrn_measurement_device_type  'Bruker APEX-II Quazar'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18748
_diffrn_reflns_av_unetI/netI     0.1512
_diffrn_reflns_av_R_equivalents  0.1386
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.247
_diffrn_reflns_theta_max         22.463
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.719
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.719
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.719
_reflns_number_total             5010
_reflns_number_gt                2827
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0587P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5010
_refine_ls_number_parameters     410
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1446
_refine_ls_R_factor_gt           0.0663
_refine_ls_wR_factor_ref         0.1540
_refine_ls_wR_factor_gt          0.1271
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.024
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.26264(5) 0.67630(10) 0.39835(3) 0.0241(3) Uani 1 1 d . . . . .
P1 P 0.32139(11) 0.7909(2) 0.34493(7) 0.0261(5) Uani 1 1 d . . . . .
P2 P 0.16973(11) 0.8542(2) 0.38860(6) 0.0237(5) Uani 1 1 d . . . . .
C1 C 0.2356(4) 0.5165(8) 0.4436(3) 0.0310(19) Uani 1 1 d . . . . .
H1A H 0.2482 0.5457 0.4803 0.037 Uiso 1 1 calc R U . . .
C2 C 0.3068(4) 0.4722(8) 0.4248(3) 0.0296(19) Uani 1 1 d . . . . .
H2 H 0.2985 0.3860 0.3997 0.036 Uiso 1 1 calc R U . . .
C3 C 0.3884(5) 0.4863(8) 0.4574(3) 0.0334(19) Uani 1 1 d . . . . .
O1 O 0.4484(3) 0.4184(6) 0.44191(18) 0.0447(14) Uani 1 1 d . . . . .
H1 H 0.521(7) 0.442(11) 0.471(4) 0.12(3) Uiso 1 1 d . . . . .
O2 O 0.4026(3) 0.5596(6) 0.49933(19) 0.0412(14) Uani 1 1 d . . . . .
C9 C 0.2426(4) 0.9252(8) 0.3076(2) 0.0303(19) Uani 1 1 d . . . . .
H9A H 0.2697 1.0065 0.2917 0.036 Uiso 1 1 calc R U . . .
H9B H 0.2047 0.8681 0.2803 0.036 Uiso 1 1 calc R U . . .
C10 C 0.1947(4) 0.9983(7) 0.3437(2) 0.0275(18) Uani 1 1 d . . . . .
H10A H 0.1434 1.0438 0.3235 0.033 Uiso 1 1 calc R U . . .
H10B H 0.2278 1.0821 0.3631 0.033 Uiso 1 1 calc R U . . .
C11 C 0.3563(4) 0.6829(8) 0.2947(2) 0.0273(17) Uani 1 1 d . . . . .
H11 H 0.3704 0.7584 0.2703 0.033 Uiso 1 1 calc R U . . .
C12 C 0.2879(4) 0.5767(9) 0.2657(3) 0.041(2) Uani 1 1 d . . . . .
H12A H 0.2401 0.6396 0.2491 0.049 Uiso 1 1 calc R U . . .
H12B H 0.2704 0.5063 0.2899 0.049 Uiso 1 1 calc R U . . .
C13 C 0.3172(5) 0.4810(9) 0.2251(3) 0.047(2) Uani 1 1 d . . . . .
H13A H 0.2730 0.4097 0.2086 0.056 Uiso 1 1 calc R U . . .
H13B H 0.3288 0.5508 0.1988 0.056 Uiso 1 1 calc R U . . .
C14 C 0.3933(4) 0.3897(9) 0.2483(3) 0.048(2) Uani 1 1 d . . . . .
H14A H 0.4127 0.3360 0.2211 0.058 Uiso 1 1 calc R U . . .
H14B H 0.3798 0.3109 0.2714 0.058 Uiso 1 1 calc R U . . .
C15 C 0.4619(4) 0.4933(8) 0.2778(3) 0.038(2) Uani 1 1 d . . . . .
H15A H 0.5092 0.4290 0.2944 0.046 Uiso 1 1 calc R U . . .
H15B H 0.4802 0.5640 0.2540 0.046 Uiso 1 1 calc R U . . .
C16 C 0.4331(4) 0.5857(8) 0.3173(2) 0.0311(19) Uani 1 1 d . . . . .
H16A H 0.4778 0.6548 0.3345 0.037 Uiso 1 1 calc R U . . .
H16B H 0.4205 0.5148 0.3431 0.037 Uiso 1 1 calc R U . . .
C21 C 0.4031(4) 0.9304(8) 0.3724(2) 0.0297(19) Uani 1 1 d . . . . .
H21 H 0.3746 1.0185 0.3847 0.036 Uiso 1 1 calc R U . . .
C22 C 0.4485(4) 1.0009(8) 0.3342(2) 0.0338(19) Uani 1 1 d . . . . .
H22A H 0.4796 0.9192 0.3214 0.041 Uiso 1 1 calc R U . . .
H22B H 0.4080 1.0435 0.3049 0.041 Uiso 1 1 calc R U . . .
C23 C 0.5077(4) 1.1294(8) 0.3589(3) 0.042(2) Uani 1 1 d . . . . .
H23A H 0.5366 1.1710 0.3338 0.050 Uiso 1 1 calc R U . . .
H23B H 0.4764 1.2142 0.3697 0.050 Uiso 1 1 calc R U . . .
C24 C 0.5698(4) 1.0673(9) 0.4043(3) 0.046(2) Uani 1 1 d . . . . .
H24A H 0.6064 1.1516 0.4204 0.056 Uiso 1 1 calc R U . . .
H24B H 0.6038 0.9876 0.3930 0.056 Uiso 1 1 calc R U . . .
C25 C 0.5262(5) 0.9974(9) 0.4432(3) 0.049(2) Uani 1 1 d . . . . .
H25A H 0.5676 0.9539 0.4719 0.058 Uiso 1 1 calc R U . . .
H25B H 0.4963 1.0795 0.4567 0.058 Uiso 1 1 calc R U . . .
C26 C 0.4656(4) 0.8701(8) 0.4193(3) 0.039(2) Uani 1 1 d . . . . .
H26A H 0.4362 0.8324 0.4447 0.047 Uiso 1 1 calc R U . . .
H26B H 0.4962 0.7826 0.4094 0.047 Uiso 1 1 calc R U . . .
C31 C 0.0626(4) 0.7947(7) 0.3593(2) 0.0247(17) Uani 1 1 d . . . . .
H31 H 0.0488 0.7109 0.3811 0.030 Uiso 1 1 calc R U . . .
C32 C 0.0547(4) 0.7238(8) 0.3061(2) 0.0293(18) Uani 1 1 d . . . . .
H32A H 0.0686 0.8028 0.2832 0.035 Uiso 1 1 calc R U . . .
H32B H 0.0945 0.6385 0.3085 0.035 Uiso 1 1 calc R U . . .
C33 C -0.0315(4) 0.6627(9) 0.2836(3) 0.040(2) Uani 1 1 d . . . . .
H33A H -0.0342 0.6223 0.2491 0.047 Uiso 1 1 calc R U . . .
H33B H -0.0437 0.5769 0.3047 0.047 Uiso 1 1 calc R U . . .
C34 C -0.0958(4) 0.7893(9) 0.2809(3) 0.043(2) Uani 1 1 d . . . . .
H34A H -0.0873 0.8699 0.2568 0.052 Uiso 1 1 calc R U . . .
H34B H -0.1512 0.7454 0.2682 0.052 Uiso 1 1 calc R U . . .
C35 C -0.0896(4) 0.8603(9) 0.3329(3) 0.047(2) Uani 1 1 d . . . . .
H35A H -0.1049 0.7822 0.3556 0.057 Uiso 1 1 calc R U . . .
H35B H -0.1289 0.9466 0.3298 0.057 Uiso 1 1 calc R U . . .
C36 C -0.0031(4) 0.9198(8) 0.3565(3) 0.035(2) Uani 1 1 d . . . . .
H36A H -0.0013 0.9582 0.3911 0.042 Uiso 1 1 calc R U . . .
H36B H 0.0094 1.0072 0.3361 0.042 Uiso 1 1 calc R U . . .
C41 C 0.1624(4) 0.9738(8) 0.4445(2) 0.0260(18) Uani 1 1 d . . . . .
H41 H 0.1275 1.0655 0.4321 0.031 Uiso 1 1 calc R U . . .
C42 C 0.2474(4) 1.0303(8) 0.4721(2) 0.0337(19) Uani 1 1 d . . . . .
H42A H 0.2711 1.0932 0.4486 0.040 Uiso 1 1 calc R U . . .
H42B H 0.2837 0.9407 0.4827 0.040 Uiso 1 1 calc R U . . .
C43 C 0.2433(4) 1.1272(8) 0.5191(2) 0.0342(19) Uani 1 1 d . . . . .
H43A H 0.2995 1.1556 0.5373 0.041 Uiso 1 1 calc R U . . .
H43B H 0.2127 1.2234 0.5081 0.041 Uiso 1 1 calc R U . . .
C44 C 0.2025(5) 1.0418(9) 0.5542(3) 0.044(2) Uani 1 1 d . . . . .
H44A H 0.1965 1.1109 0.5821 0.053 Uiso 1 1 calc R U . . .
H44B H 0.2375 0.9542 0.5693 0.053 Uiso 1 1 calc R U . . .
C45 C 0.1176(4) 0.9811(9) 0.5270(3) 0.041(2) Uani 1 1 d . . . . .
H45A H 0.0947 0.9186 0.5509 0.049 Uiso 1 1 calc R U . . .
H45B H 0.0804 1.0691 0.5159 0.049 Uiso 1 1 calc R U . . .
C46 C 0.1223(4) 0.8832(8) 0.4810(2) 0.0297(18) Uani 1 1 d . . . . .
H46A H 0.0664 0.8514 0.4632 0.036 Uiso 1 1 calc R U . . .
H46B H 0.1546 0.7892 0.4924 0.036 Uiso 1 1 calc R U . . .
C51 C 0.1543(4) 0.4485(8) 0.4248(3) 0.0275(18) Uani 1 1 d . . . . .
C52 C 0.1272(5) 0.3855(7) 0.3763(3) 0.033(2) Uani 1 1 d . . . . .
H52 H 0.1636 0.3825 0.3541 0.040 Uiso 1 1 calc R U . . .
C53 C 0.0478(5) 0.3269(8) 0.3596(3) 0.044(2) Uani 1 1 d . . . . .
H53 H 0.0311 0.2848 0.3265 0.053 Uiso 1 1 calc R U . . .
C54 C -0.0061(5) 0.3296(9) 0.3906(3) 0.049(2) Uani 1 1 d . . . . .
H54 H -0.0601 0.2906 0.3788 0.058 Uiso 1 1 calc R U . . .
C55 C 0.0182(5) 0.3894(8) 0.4389(3) 0.042(2) Uani 1 1 d . . . . .
H55 H -0.0187 0.3892 0.4607 0.051 Uiso 1 1 calc R U . . .
C56 C 0.0969(4) 0.4503(8) 0.4559(3) 0.035(2) Uani 1 1 d . . . . .
H56 H 0.1123 0.4936 0.4889 0.042 Uiso 1 1 calc R U . . .
O61 O 0.2831(9) 1.0422(17) 0.1779(5) 0.253(7) Uani 1 1 d . U . . .
C62 C 0.2389(11) 0.909(2) 0.1601(6) 0.194(8) Uani 1 1 d . U . . .
H62A H 0.2643 0.8187 0.1797 0.233 Uiso 1 1 calc R U . . .
H62B H 0.1818 0.9188 0.1638 0.233 Uiso 1 1 calc R U . . .
C63 C 0.2402(11) 0.893(2) 0.1099(6) 0.208(8) Uani 1 1 d . U . . .
H63A H 0.1862 0.9211 0.0882 0.250 Uiso 1 1 calc R U . . .
H63B H 0.2524 0.7853 0.1027 0.250 Uiso 1 1 calc R U . . .
C64 C 0.3004(12) 0.9901(19) 0.0999(6) 0.194(8) Uani 1 1 d . U . . .
H64A H 0.3494 0.9295 0.0977 0.233 Uiso 1 1 calc R U . . .
H64B H 0.2799 1.0436 0.0672 0.233 Uiso 1 1 calc R U . . .
C65 C 0.3206(9) 1.0961(16) 0.1386(5) 0.149(5) Uani 1 1 d . U . . .
H65A H 0.2995 1.1992 0.1268 0.178 Uiso 1 1 calc R U . . .
H65B H 0.3808 1.1026 0.1512 0.178 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.976(7) . ?
Ni1 C2 1.991(7) . ?
Ni1 P2 2.168(4) . ?
Ni1 P1 2.174(3) . ?
P1 C21 1.852(7) . ?
P1 C11 1.858(7) . ?
P1 C9 1.875(7) . ?
P2 C10 1.862(7) . ?
P2 C31 1.863(7) . ?
P2 C41 1.865(7) . ?
C1 C2 1.456(8) . ?
C1 C51 1.467(9) . ?
C1 H1A 1.0000 . ?
C2 C3 1.453(10) . ?
C2 H2 1.0000 . ?
C3 O2 1.277(8) . ?
C3 O1 1.317(8) . ?
O1 H1 1.31(11) . ?
C9 C10 1.540(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.539(9) . ?
C11 C16 1.545(9) . ?
C11 H11 1.0000 . ?
C12 C13 1.546(9) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.512(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.532(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.506(9) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C21 C26 1.543(9) . ?
C21 C22 1.548(8) . ?
C21 H21 1.0000 . ?
C22 C23 1.542(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.517(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.542(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.541(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C31 C36 1.538(8) . ?
C31 C32 1.545(8) . ?
C31 H31 1.0000 . ?
C32 C33 1.530(9) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.530(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.521(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.534(9) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C41 C42 1.530(9) . ?
C41 C46 1.538(8) . ?
C41 H41 1.0000 . ?
C42 C43 1.543(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.495(9) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.538(9) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.526(9) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C51 C52 1.401(9) . ?
C51 C56 1.420(9) . ?
C52 C53 1.401(9) . ?
C52 H52 0.9500 . ?
C53 C54 1.370(10) . ?
C53 H53 0.9500 . ?
C54 C55 1.382(10) . ?
C54 H54 0.9500 . ?
C55 C56 1.399(10) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
O61 C62 1.395(16) . ?
O61 C65 1.436(14) . ?
C62 C63 1.374(17) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.389(18) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C65 1.378(16) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Ni1 C2 43.1(2) . . ?
C1 Ni1 P2 108.4(2) . . ?
C2 Ni1 P2 151.22(19) . . ?
C1 Ni1 P1 160.3(2) . . ?
C2 Ni1 P1 117.4(2) . . ?
P2 Ni1 P1 90.94(13) . . ?
C21 P1 C11 107.2(3) . . ?
C21 P1 C9 100.0(3) . . ?
C11 P1 C9 102.7(3) . . ?
C21 P1 Ni1 116.1(2) . . ?
C11 P1 Ni1 121.7(3) . . ?
C9 P1 Ni1 105.9(2) . . ?
C10 P2 C31 104.4(3) . . ?
C10 P2 C41 103.0(3) . . ?
C31 P2 C41 105.2(3) . . ?
C10 P2 Ni1 107.1(2) . . ?
C31 P2 Ni1 116.7(2) . . ?
C41 P2 Ni1 118.6(2) . . ?
C2 C1 C51 123.0(6) . . ?
C2 C1 Ni1 69.0(4) . . ?
C51 C1 Ni1 113.3(5) . . ?
C2 C1 H1A 114.5 . . ?
C51 C1 H1A 114.5 . . ?
Ni1 C1 H1A 114.5 . . ?
C3 C2 C1 119.9(6) . . ?
C3 C2 Ni1 111.4(5) . . ?
C1 C2 Ni1 67.9(4) . . ?
C3 C2 H2 116.1 . . ?
C1 C2 H2 116.1 . . ?
Ni1 C2 H2 116.1 . . ?
O2 C3 O1 120.6(7) . . ?
O2 C3 C2 122.7(7) . . ?
O1 C3 C2 116.7(7) . . ?
C3 O1 H1 114(4) . . ?
C10 C9 P1 108.6(4) . . ?
C10 C9 H9A 110.0 . . ?
P1 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
P1 C9 H9B 110.0 . . ?
H9A C9 H9B 108.3 . . ?
C9 C10 P2 111.6(4) . . ?
C9 C10 H10A 109.3 . . ?
P2 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
P2 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C16 109.2(6) . . ?
C12 C11 P1 110.7(4) . . ?
C16 C11 P1 111.1(4) . . ?
C12 C11 H11 108.6 . . ?
C16 C11 H11 108.6 . . ?
P1 C11 H11 108.6 . . ?
C11 C12 C13 111.4(6) . . ?
C11 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C14 C13 C12 111.3(6) . . ?
C14 C13 H13A 109.4 . . ?
C12 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C13 C14 C15 111.7(6) . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C14 111.1(6) . . ?
C16 C15 H15A 109.4 . . ?
C14 C15 H15A 109.4 . . ?
C16 C15 H15B 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C15 C16 C11 112.6(6) . . ?
C15 C16 H16A 109.1 . . ?
C11 C16 H16A 109.1 . . ?
C15 C16 H16B 109.1 . . ?
C11 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C26 C21 C22 109.9(6) . . ?
C26 C21 P1 114.1(5) . . ?
C22 C21 P1 115.0(5) . . ?
C26 C21 H21 105.6 . . ?
C22 C21 H21 105.6 . . ?
P1 C21 H21 105.6 . . ?
C23 C22 C21 111.3(6) . . ?
C23 C22 H22A 109.4 . . ?
C21 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
C21 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C24 C23 C22 110.4(6) . . ?
C24 C23 H23A 109.6 . . ?
C22 C23 H23A 109.6 . . ?
C24 C23 H23B 109.6 . . ?
C22 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
C23 C24 C25 110.6(6) . . ?
C23 C24 H24A 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
C26 C25 C24 111.5(6) . . ?
C26 C25 H25A 109.3 . . ?
C24 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
C24 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
C25 C26 C21 111.1(6) . . ?
C25 C26 H26A 109.4 . . ?
C21 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
C21 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C36 C31 C32 109.3(5) . . ?
C36 C31 P2 115.8(5) . . ?
C32 C31 P2 112.0(4) . . ?
C36 C31 H31 106.4 . . ?
C32 C31 H31 106.4 . . ?
P2 C31 H31 106.4 . . ?
C33 C32 C31 112.4(5) . . ?
C33 C32 H32A 109.1 . . ?
C31 C32 H32A 109.1 . . ?
C33 C32 H32B 109.1 . . ?
C31 C32 H32B 109.1 . . ?
H32A C32 H32B 107.9 . . ?
C34 C33 C32 111.1(6) . . ?
C34 C33 H33A 109.4 . . ?
C32 C33 H33A 109.4 . . ?
C34 C33 H33B 109.4 . . ?
C32 C33 H33B 109.4 . . ?
H33A C33 H33B 108.0 . . ?
C35 C34 C33 110.6(6) . . ?
C35 C34 H34A 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
C34 C35 C36 112.3(6) . . ?
C34 C35 H35A 109.2 . . ?
C36 C35 H35A 109.2 . . ?
C34 C35 H35B 109.2 . . ?
C36 C35 H35B 109.2 . . ?
H35A C35 H35B 107.9 . . ?
C35 C36 C31 112.4(6) . . ?
C35 C36 H36A 109.1 . . ?
C31 C36 H36A 109.1 . . ?
C35 C36 H36B 109.1 . . ?
C31 C36 H36B 109.1 . . ?
H36A C36 H36B 107.9 . . ?
C42 C41 C46 110.3(6) . . ?
C42 C41 P2 110.3(4) . . ?
C46 C41 P2 111.1(5) . . ?
C42 C41 H41 108.4 . . ?
C46 C41 H41 108.4 . . ?
P2 C41 H41 108.4 . . ?
C41 C42 C43 111.4(5) . . ?
C41 C42 H42A 109.3 . . ?
C43 C42 H42A 109.3 . . ?
C41 C42 H42B 109.3 . . ?
C43 C42 H42B 109.3 . . ?
H42A C42 H42B 108.0 . . ?
C44 C43 C42 111.7(6) . . ?
C44 C43 H43A 109.3 . . ?
C42 C43 H43A 109.3 . . ?
C44 C43 H43B 109.3 . . ?
C42 C43 H43B 109.3 . . ?
H43A C43 H43B 107.9 . . ?
C43 C44 C45 112.0(6) . . ?
C43 C44 H44A 109.2 . . ?
C45 C44 H44A 109.2 . . ?
C43 C44 H44B 109.2 . . ?
C45 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
C46 C45 C44 111.5(6) . . ?
C46 C45 H45A 109.3 . . ?
C44 C45 H45A 109.3 . . ?
C46 C45 H45B 109.3 . . ?
C44 C45 H45B 109.3 . . ?
H45A C45 H45B 108.0 . . ?
C45 C46 C41 110.8(6) . . ?
C45 C46 H46A 109.5 . . ?
C41 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C41 C46 H46B 109.5 . . ?
H46A C46 H46B 108.1 . . ?
C52 C51 C56 116.5(7) . . ?
C52 C51 C1 123.9(6) . . ?
C56 C51 C1 119.5(7) . . ?
C53 C52 C51 121.5(7) . . ?
C53 C52 H52 119.2 . . ?
C51 C52 H52 119.2 . . ?
C54 C53 C52 120.7(7) . . ?
C54 C53 H53 119.7 . . ?
C52 C53 H53 119.7 . . ?
C53 C54 C55 119.8(7) . . ?
C53 C54 H54 120.1 . . ?
C55 C54 H54 120.1 . . ?
C54 C55 C56 120.2(7) . . ?
C54 C55 H55 119.9 . . ?
C56 C55 H55 119.9 . . ?
C55 C56 C51 121.2(7) . . ?
C55 C56 H56 119.4 . . ?
C51 C56 H56 119.4 . . ?
C62 O61 C65 107.6(13) . . ?
C63 C62 O61 107.3(15) . . ?
C63 C62 H62A 110.3 . . ?
O61 C62 H62A 110.3 . . ?
C63 C62 H62B 110.3 . . ?
O61 C62 H62B 110.3 . . ?
H62A C62 H62B 108.5 . . ?
C62 C63 C64 108.1(16) . . ?
C62 C63 H63A 110.1 . . ?
C64 C63 H63A 110.1 . . ?
C62 C63 H63B 110.1 . . ?
C64 C63 H63B 110.1 . . ?
H63A C63 H63B 108.4 . . ?
C65 C64 C63 108.5(14) . . ?
C65 C64 H64A 110.0 . . ?
C63 C64 H64A 110.0 . . ?
C65 C64 H64B 110.0 . . ?
C63 C64 H64B 110.0 . . ?
H64A C64 H64B 108.4 . . ?
C64 C65 O61 105.9(13) . . ?
C64 C65 H65A 110.6 . . ?
O61 C65 H65A 110.6 . . ?
C64 C65 H65B 110.6 . . ?
O61 C65 H65B 110.6 . . ?
H65A C65 H65B 108.7 . . ?

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
C51 C1 C2 C3 -152.4(6) . . . . ?
Ni1 C1 C2 C3 102.7(6) . . . . ?
C51 C1 C2 Ni1 104.9(6) . . . . ?
C1 C2 C3 O2 -12.0(10) . . . . ?
Ni1 C2 C3 O2 64.0(8) . . . . ?
C1 C2 C3 O1 167.7(6) . . . . ?
Ni1 C2 C3 O1 -116.3(6) . . . . ?
C21 P1 C9 C10 -81.7(5) . . . . ?
C11 P1 C9 C10 167.9(5) . . . . ?
Ni1 P1 C9 C10 39.2(5) . . . . ?
P1 C9 C10 P2 -42.2(6) . . . . ?
C31 P2 C10 C9 -97.4(5) . . . . ?
C41 P2 C10 C9 152.8(5) . . . . ?
Ni1 P2 C10 C9 27.0(5) . . . . ?
C21 P1 C11 C12 -173.6(5) . . . . ?
C9 P1 C11 C12 -68.8(6) . . . . ?
Ni1 P1 C11 C12 49.2(6) . . . . ?
C21 P1 C11 C16 64.8(5) . . . . ?
C9 P1 C11 C16 169.6(5) . . . . ?
Ni1 P1 C11 C16 -72.4(5) . . . . ?
C16 C11 C12 C13 -55.0(8) . . . . ?
P1 C11 C12 C13 -177.7(5) . . . . ?
C11 C12 C13 C14 55.7(9) . . . . ?
C12 C13 C14 C15 -54.8(8) . . . . ?
C13 C14 C15 C16 55.1(8) . . . . ?
C14 C15 C16 C11 -56.1(8) . . . . ?
C12 C11 C16 C15 56.1(7) . . . . ?
P1 C11 C16 C15 178.5(5) . . . . ?
C11 P1 C21 C26 -92.9(5) . . . . ?
C9 P1 C21 C26 160.4(5) . . . . ?
Ni1 P1 C21 C26 47.1(5) . . . . ?
C11 P1 C21 C22 35.5(6) . . . . ?
C9 P1 C21 C22 -71.3(5) . . . . ?
Ni1 P1 C21 C22 175.4(4) . . . . ?
C26 C21 C22 C23 -56.5(8) . . . . ?
P1 C21 C22 C23 173.1(5) . . . . ?
C21 C22 C23 C24 58.3(8) . . . . ?
C22 C23 C24 C25 -57.6(8) . . . . ?
C23 C24 C25 C26 56.8(9) . . . . ?
C24 C25 C26 C21 -55.5(8) . . . . ?
C22 C21 C26 C25 54.9(8) . . . . ?
P1 C21 C26 C25 -174.2(5) . . . . ?
C10 P2 C31 C36 -66.5(5) . . . . ?
C41 P2 C31 C36 41.6(5) . . . . ?
Ni1 P2 C31 C36 175.5(4) . . . . ?
C10 P2 C31 C32 59.8(5) . . . . ?
C41 P2 C31 C32 167.8(4) . . . . ?
Ni1 P2 C31 C32 -58.3(5) . . . . ?
C36 C31 C32 C33 -55.0(7) . . . . ?
P2 C31 C32 C33 175.3(5) . . . . ?
C31 C32 C33 C34 56.8(8) . . . . ?
C32 C33 C34 C35 -55.6(8) . . . . ?
C33 C34 C35 C36 54.9(9) . . . . ?
C34 C35 C36 C31 -55.0(8) . . . . ?
C32 C31 C36 C35 53.6(7) . . . . ?
P2 C31 C36 C35 -178.8(5) . . . . ?
C10 P2 C41 C42 -70.9(5) . . . . ?
C31 P2 C41 C42 -180.0(4) . . . . ?
Ni1 P2 C41 C42 47.2(5) . . . . ?
C10 P2 C41 C46 166.6(5) . . . . ?
C31 P2 C41 C46 57.5(5) . . . . ?
Ni1 P2 C41 C46 -75.4(5) . . . . ?
C46 C41 C42 C43 -55.9(7) . . . . ?
P2 C41 C42 C43 -179.0(4) . . . . ?
C41 C42 C43 C44 55.0(8) . . . . ?
C42 C43 C44 C45 -53.7(8) . . . . ?
C43 C44 C45 C46 54.6(8) . . . . ?
C44 C45 C46 C41 -55.7(8) . . . . ?
C42 C41 C46 C45 56.6(7) . . . . ?
P2 C41 C46 C45 179.2(5) . . . . ?
C2 C1 C51 C52 -26.5(10) . . . . ?
Ni1 C1 C51 C52 52.9(8) . . . . ?
C2 C1 C51 C56 156.2(6) . . . . ?
Ni1 C1 C51 C56 -124.4(6) . . . . ?
C56 C51 C52 C53 -0.3(10) . . . . ?
C1 C51 C52 C53 -177.7(6) . . . . ?
C51 C52 C53 C54 0.1(11) . . . . ?
C52 C53 C54 C55 -0.6(11) . . . . ?
C53 C54 C55 C56 1.5(11) . . . . ?
C54 C55 C56 C51 -1.8(11) . . . . ?
C52 C51 C56 C55 1.1(10) . . . . ?
C1 C51 C56 C55 178.7(6) . . . . ?
C65 O61 C62 C63 -7(2) . . . . ?
O61 C62 C63 C64 15(2) . . . . ?
C62 C63 C64 C65 -17(2) . . . . ?
C63 C64 C65 O61 12(2) . . . . ?
C62 O61 C65 C64 -3(2) . . . . ?

_refine_diff_density_max         0.620
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.081

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_THETM01_ij4                 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Yes, it is. And the data to parameter ratio is more than 12.
;
_vrf_PLAT305_ij4                 
;
PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??) H1 Check
RESPONSE: This is a hydrogen atom of a dimerized carboxyl group. 
For this situation its typical to find rather symmetric C-O distances 
and hydrogen positions. Either this is the real or the average 
hydrogen position. However, with this dataset its not sensible 
trying to refine disordered hydrogen positions. 
;
####################################################################### 
# 
# 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_ij20
_database_code_depnum_ccdc_archive 'CCDC 1052346'
_audit_update_record             
;
2015-03-05 deposited with the CCDC.
2015-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            'dtbpe carbonate in manuscript'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H40 Ni O3 P2'
_chemical_formula_weight         437.16

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   9.9880(9)
_cell_length_b                   14.3032(12)
_cell_length_c                   16.3855(13)
_cell_angle_alpha                90
_cell_angle_beta                 106.4993(14)
_cell_angle_gamma                90
_cell_volume                     2244.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    3594
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      26.66

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.021
_shelx_estimated_absorpt_T_min   0.846
_shelx_estimated_absorpt_T_max   0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8619
_exptl_absorpt_correction_T_max  0.9632
_exptl_absorpt_process_details   
;
Sheldrick, G. M. (2008). SADABS. University of Göttingen, Germany.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'ImuS microsource'
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19179
_diffrn_reflns_av_unetI/netI     0.0710
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.925
_diffrn_reflns_theta_max         29.612
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6295
_reflns_number_gt                4243
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0413P)²+0.3936P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6295
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1111
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.53040(3) 0.78243(2) 0.30565(2) 0.01877(10) Uani 1 1 d . . . . .
P1 P 0.61783(7) 0.72689(5) 0.43345(4) 0.01867(15) Uani 1 1 d . . . . .
P2 P 0.32735(7) 0.72663(5) 0.30211(4) 0.01937(15) Uani 1 1 d . . . . .
C1 C 0.6108(3) 0.86924(18) 0.21153(17) 0.0238(6) Uani 1 1 d . . . . .
O1 O 0.48191(19) 0.83983(13) 0.19786(11) 0.0279(4) Uani 1 1 d . . . . .
O2 O 0.68901(19) 0.83976(13) 0.28633(11) 0.0280(4) Uani 1 1 d . . . . .
O3 O 0.6525(2) 0.91674(13) 0.16134(12) 0.0314(5) Uani 1 1 d . . . . .
C9 C 0.4709(3) 0.68598(19) 0.47143(16) 0.0225(6) Uani 1 1 d . . . . .
H9A H 0.5032 0.6349 0.5131 0.027 Uiso 1 1 calc R U . . .
H9B H 0.4376 0.7379 0.5005 0.027 Uiso 1 1 calc R U . . .
C10 C 0.3495(3) 0.65045(19) 0.39648(16) 0.0239(6) Uani 1 1 d . . . . .
H10A H 0.2620 0.6499 0.4135 0.029 Uiso 1 1 calc R U . . .
H10B H 0.3690 0.5857 0.3819 0.029 Uiso 1 1 calc R U . . .
C11 C 0.7024(3) 0.82410(19) 0.50741(16) 0.0247(6) Uani 1 1 d . . . . .
C12 C 0.6019(3) 0.90772(19) 0.4867(2) 0.0355(7) Uani 1 1 d . . . . .
H12A H 0.6464 0.9623 0.5196 0.053 Uiso 1 1 calc R U . . .
H12B H 0.5161 0.8924 0.5016 0.053 Uiso 1 1 calc R U . . .
H12C H 0.5791 0.9218 0.4258 0.053 Uiso 1 1 calc R U . . .
C13 C 0.7257(3) 0.8014(2) 0.60165(17) 0.0321(7) Uani 1 1 d . . . . .
H13A H 0.7629 0.8566 0.6360 0.048 Uiso 1 1 calc R U . . .
H13B H 0.7924 0.7497 0.6180 0.048 Uiso 1 1 calc R U . . .
H13C H 0.6368 0.7833 0.6113 0.048 Uiso 1 1 calc R U . . .
C14 C 0.8384(3) 0.8539(2) 0.4891(2) 0.0381(8) Uani 1 1 d . . . . .
H14A H 0.8749 0.9103 0.5218 0.057 Uiso 1 1 calc R U . . .
H14B H 0.8202 0.8669 0.4282 0.057 Uiso 1 1 calc R U . . .
H14C H 0.9072 0.8034 0.5055 0.057 Uiso 1 1 calc R U . . .
C15 C 0.7422(3) 0.62539(18) 0.44145(17) 0.0246(6) Uani 1 1 d . . . . .
C16 C 0.6552(3) 0.5354(2) 0.4177(2) 0.0441(8) Uani 1 1 d . . . . .
H16A H 0.7175 0.4826 0.4171 0.066 Uiso 1 1 calc R U . . .
H16B H 0.5888 0.5426 0.3611 0.066 Uiso 1 1 calc R U . . .
H16C H 0.6042 0.5238 0.4597 0.066 Uiso 1 1 calc R U . . .
C17 C 0.8440(3) 0.6102(2) 0.52910(19) 0.0355(7) Uani 1 1 d . . . . .
H17A H 0.8990 0.5536 0.5284 0.053 Uiso 1 1 calc R U . . .
H17B H 0.7919 0.6030 0.5712 0.053 Uiso 1 1 calc R U . . .
H17C H 0.9066 0.6641 0.5442 0.053 Uiso 1 1 calc R U . . .
C18 C 0.8238(4) 0.6410(2) 0.3763(2) 0.0428(8) Uani 1 1 d . . . . .
H18A H 0.8885 0.5888 0.3789 0.064 Uiso 1 1 calc R U . . .
H18B H 0.8767 0.6995 0.3893 0.064 Uiso 1 1 calc R U . . .
H18C H 0.7585 0.6446 0.3190 0.064 Uiso 1 1 calc R U . . .
C21 C 0.1917(3) 0.8172(2) 0.30565(17) 0.0265(6) Uani 1 1 d . . . . .
C22 C 0.0422(3) 0.7805(2) 0.2765(2) 0.0436(8) Uani 1 1 d . . . . .
H22A H -0.0220 0.8289 0.2850 0.065 Uiso 1 1 calc R U . . .
H22B H 0.0341 0.7250 0.3098 0.065 Uiso 1 1 calc R U . . .
H22C H 0.0185 0.7640 0.2160 0.065 Uiso 1 1 calc R U . . .
C23 C 0.2186(4) 0.8505(3) 0.3970(2) 0.0482(9) Uani 1 1 d . . . . .
H23A H 0.1506 0.8990 0.3995 0.072 Uiso 1 1 calc R U . . .
H23B H 0.3132 0.8762 0.4171 0.072 Uiso 1 1 calc R U . . .
H23C H 0.2093 0.7977 0.4331 0.072 Uiso 1 1 calc R U . . .
C24 C 0.2062(4) 0.9018(2) 0.2508(2) 0.0476(9) Uani 1 1 d . . . . .
H24A H 0.1345 0.9482 0.2517 0.071 Uiso 1 1 calc R U . . .
H24B H 0.1945 0.8813 0.1921 0.071 Uiso 1 1 calc R U . . .
H24C H 0.2989 0.9297 0.2736 0.071 Uiso 1 1 calc R U . . .
C25 C 0.2624(3) 0.6488(2) 0.20628(16) 0.0281(6) Uani 1 1 d . . . . .
C26 C 0.1480(3) 0.5796(2) 0.2130(2) 0.0407(8) Uani 1 1 d . . . . .
H26A H 0.1280 0.5363 0.1647 0.061 Uiso 1 1 calc R U . . .
H26B H 0.0630 0.6141 0.2125 0.061 Uiso 1 1 calc R U . . .
H26C H 0.1803 0.5442 0.2662 0.061 Uiso 1 1 calc R U . . .
C27 C 0.3898(3) 0.5925(2) 0.19904(19) 0.0357(7) Uani 1 1 d . . . . .
H27A H 0.3629 0.5532 0.1480 0.054 Uiso 1 1 calc R U . . .
H27B H 0.4238 0.5529 0.2495 0.054 Uiso 1 1 calc R U . . .
H27C H 0.4639 0.6356 0.1950 0.054 Uiso 1 1 calc R U . . .
C28 C 0.2121(3) 0.7079(2) 0.12550(18) 0.0396(8) Uani 1 1 d . . . . .
H28A H 0.1910 0.6670 0.0755 0.059 Uiso 1 1 calc R U . . .
H28B H 0.2854 0.7523 0.1226 0.059 Uiso 1 1 calc R U . . .
H28C H 0.1278 0.7423 0.1266 0.059 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.8821(17) . ?
Ni1 O2 1.8887(18) . ?
Ni1 P2 2.1648(7) . ?
Ni1 P1 2.1772(7) . ?
Ni1 C1 2.295(3) . ?
P1 C9 1.844(3) . ?
P1 C11 1.880(3) . ?
P1 C15 1.891(3) . ?
P2 C10 1.853(3) . ?
P2 C25 1.883(3) . ?
P2 C21 1.888(3) . ?
C1 O3 1.227(3) . ?
C1 O1 1.312(3) . ?
C1 O2 1.321(3) . ?
C9 C10 1.547(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C13 1.530(4) . ?
C11 C14 1.533(4) . ?
C11 C12 1.536(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C17 1.521(4) . ?
C15 C18 1.533(4) . ?
C15 C16 1.539(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C21 C23 1.520(4) . ?
C21 C22 1.526(4) . ?
C21 C24 1.538(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C28 1.530(4) . ?
C25 C27 1.539(4) . ?
C25 C26 1.540(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O2 69.99(8) . . ?
O1 Ni1 P2 98.41(6) . . ?
O2 Ni1 P2 168.40(6) . . ?
O1 Ni1 P1 171.04(6) . . ?
O2 Ni1 P1 101.14(6) . . ?
P2 Ni1 P1 90.46(3) . . ?
O1 Ni1 C1 34.86(9) . . ?
O2 Ni1 C1 35.15(8) . . ?
P2 Ni1 C1 133.26(7) . . ?
P1 Ni1 C1 136.25(7) . . ?
C9 P1 C11 105.78(12) . . ?
C9 P1 C15 107.63(12) . . ?
C11 P1 C15 110.94(12) . . ?
C9 P1 Ni1 107.47(8) . . ?
C11 P1 Ni1 109.52(9) . . ?
C15 P1 Ni1 115.02(9) . . ?
C10 P2 C25 106.24(13) . . ?
C10 P2 C21 107.12(12) . . ?
C25 P2 C21 110.54(13) . . ?
C10 P2 Ni1 107.80(9) . . ?
C25 P2 Ni1 109.78(9) . . ?
C21 P2 Ni1 114.93(9) . . ?
O3 C1 O1 124.5(3) . . ?
O3 C1 O2 125.1(3) . . ?
O1 C1 O2 110.4(2) . . ?
O3 C1 Ni1 179.0(2) . . ?
O1 C1 Ni1 55.08(12) . . ?
O2 C1 Ni1 55.36(12) . . ?
C1 O1 Ni1 90.07(15) . . ?
C1 O2 Ni1 89.49(15) . . ?
C10 C9 P1 110.86(17) . . ?
C10 C9 H9A 109.5 . . ?
P1 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
P1 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C9 C10 P2 110.50(17) . . ?
C9 C10 H10A 109.6 . . ?
P2 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
P2 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C13 C11 C14 111.5(2) . . ?
C13 C11 C12 106.9(2) . . ?
C14 C11 C12 107.5(2) . . ?
C13 C11 P1 113.92(19) . . ?
C14 C11 P1 109.88(19) . . ?
C12 C11 P1 106.74(18) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C15 C18 109.5(2) . . ?
C17 C15 C16 107.3(2) . . ?
C18 C15 C16 108.6(3) . . ?
C17 C15 P1 115.15(19) . . ?
C18 C15 P1 107.99(19) . . ?
C16 C15 P1 108.19(19) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C23 C21 C22 107.4(3) . . ?
C23 C21 C24 108.0(3) . . ?
C22 C21 C24 109.5(3) . . ?
C23 C21 P2 108.52(19) . . ?
C22 C21 P2 113.7(2) . . ?
C24 C21 P2 109.51(19) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C28 C25 C27 107.3(2) . . ?
C28 C25 C26 110.5(2) . . ?
C27 C25 C26 108.4(2) . . ?
C28 C25 P2 110.2(2) . . ?
C27 C25 P2 106.07(18) . . ?
C26 C25 P2 114.0(2) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

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
O3 C1 O1 Ni1 -178.9(3) . . . . ?
O2 C1 O1 Ni1 1.6(2) . . . . ?
O2 Ni1 O1 C1 -1.15(15) . . . . ?
P2 Ni1 O1 C1 179.19(14) . . . . ?
O3 C1 O2 Ni1 178.9(3) . . . . ?
O1 C1 O2 Ni1 -1.6(2) . . . . ?
O1 Ni1 O2 C1 1.14(14) . . . . ?
P2 Ni1 O2 C1 2.8(4) . . . . ?
P1 Ni1 O2 C1 -177.53(13) . . . . ?
C11 P1 C9 C10 148.36(19) . . . . ?
C15 P1 C9 C10 -93.0(2) . . . . ?
Ni1 P1 C9 C10 31.4(2) . . . . ?
P1 C9 C10 P2 -39.5(2) . . . . ?
C25 P2 C10 C9 148.30(19) . . . . ?
C21 P2 C10 C9 -93.5(2) . . . . ?
Ni1 P2 C10 C9 30.7(2) . . . . ?
C9 P1 C11 C13 46.0(2) . . . . ?
C15 P1 C11 C13 -70.4(2) . . . . ?
Ni1 P1 C11 C13 161.58(18) . . . . ?
C9 P1 C11 C14 172.03(19) . . . . ?
C15 P1 C11 C14 55.6(2) . . . . ?
Ni1 P1 C11 C14 -72.4(2) . . . . ?
C9 P1 C11 C12 -71.7(2) . . . . ?
C15 P1 C11 C12 171.87(19) . . . . ?
Ni1 P1 C11 C12 43.8(2) . . . . ?
C9 P1 C15 C17 -82.7(2) . . . . ?
C11 P1 C15 C17 32.6(2) . . . . ?
Ni1 P1 C15 C17 157.62(18) . . . . ?
C9 P1 C15 C18 154.7(2) . . . . ?
C11 P1 C15 C18 -90.0(2) . . . . ?
Ni1 P1 C15 C18 35.0(2) . . . . ?
C9 P1 C15 C16 37.3(2) . . . . ?
C11 P1 C15 C16 152.6(2) . . . . ?
Ni1 P1 C15 C16 -82.4(2) . . . . ?
C10 P2 C21 C23 41.7(2) . . . . ?
C25 P2 C21 C23 157.0(2) . . . . ?
Ni1 P2 C21 C23 -78.0(2) . . . . ?
C10 P2 C21 C22 -77.8(2) . . . . ?
C25 P2 C21 C22 37.6(2) . . . . ?
Ni1 P2 C21 C22 162.50(19) . . . . ?
C10 P2 C21 C24 159.4(2) . . . . ?
C25 P2 C21 C24 -85.3(2) . . . . ?
Ni1 P2 C21 C24 39.7(2) . . . . ?
C10 P2 C25 C28 168.3(2) . . . . ?
C21 P2 C25 C28 52.4(2) . . . . ?
Ni1 P2 C25 C28 -75.4(2) . . . . ?
C10 P2 C25 C27 -75.8(2) . . . . ?
C21 P2 C25 C27 168.29(19) . . . . ?
Ni1 P2 C25 C27 40.5(2) . . . . ?
C10 P2 C25 C26 43.4(2) . . . . ?
C21 P2 C25 C26 -72.5(2) . . . . ?
Ni1 P2 C25 C26 159.68(19) . . . . ?

_refine_diff_density_max         0.527
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.087

_shelxl_version_number           2014-3

