# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1039461'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H53 Br Ni P2'
_chemical_formula_sum            'C37 H53 Br Ni P2'
_chemical_formula_weight         698.35

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   9.2153(4)
_cell_length_b                   9.6712(4)
_cell_length_c                   20.4152(7)
_cell_angle_alpha                82.3510(10)
_cell_angle_beta                 85.353(4)
_cell_angle_gamma                68.282(3)
_cell_volume                     1674.28(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    11438
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      26.00

_exptl_crystal_description       Plates
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_absorpt_coefficient_mu    1.893
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8949
_exptl_absorpt_correction_T_max  0.9631
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' ω and φ '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11438
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.87
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6428
_reflns_number_gt                5117
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+6.0984P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6428
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0598
_refine_ls_wR_factor_ref         0.1225
_refine_ls_wR_factor_gt          0.1103
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_restrained_S_all      1.166
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5243(5) 0.6549(5) 0.2835(2) 0.0232(10) Uani 1 1 d . . .
H1 H 0.4983 0.5798 0.3160 0.028 Uiso 1 1 calc R . .
C2 C 0.6378(5) 0.6957(5) 0.3193(2) 0.0222(10) Uani 1 1 d . . .
C3 C 0.5774(5) 0.7778(5) 0.3732(2) 0.0235(10) Uani 1 1 d . . .
C4 C 0.6745(6) 0.8094(5) 0.4126(3) 0.0293(11) Uani 1 1 d . . .
H4 H 0.6328 0.8581 0.4511 0.035 Uiso 1 1 calc R . .
C5 C 0.8307(6) 0.7701(6) 0.3959(3) 0.0371(13) Uani 1 1 d . . .
H5 H 0.8976 0.7920 0.4226 0.045 Uiso 1 1 calc R . .
C6 C 0.8896(6) 0.6991(6) 0.3404(3) 0.0341(12) Uani 1 1 d . . .
H6 H 0.9964 0.6771 0.3274 0.041 Uiso 1 1 calc R . .
C7 C 0.7953(6) 0.6587(5) 0.3030(3) 0.0289(11) Uani 1 1 d . . .
H7 H 0.8392 0.6054 0.2659 0.035 Uiso 1 1 calc R . .
C8 C 0.5914(5) 0.5713(5) 0.2237(2) 0.0241(10) Uani 1 1 d . . .
C9 C 0.5241(6) 0.6304(5) 0.1627(2) 0.0255(10) Uani 1 1 d . . .
C10 C 0.5872(6) 0.5604(6) 0.1063(2) 0.0325(12) Uani 1 1 d . . .
H10 H 0.5433 0.6035 0.0645 0.039 Uiso 1 1 calc R . .
C11 C 0.7140(6) 0.4282(6) 0.1117(3) 0.0335(12) Uani 1 1 d . . .
H11 H 0.7587 0.3808 0.0731 0.040 Uiso 1 1 calc R . .
C12 C 0.7769(6) 0.3639(6) 0.1719(3) 0.0336(12) Uani 1 1 d . . .
H12 H 0.8622 0.2708 0.1752 0.040 Uiso 1 1 calc R . .
C13 C 0.7163(6) 0.4342(5) 0.2277(2) 0.0283(11) Uani 1 1 d . . .
H13 H 0.7600 0.3889 0.2693 0.034 Uiso 1 1 calc R . .
C14 C 0.3519(5) 1.0696(5) 0.3732(2) 0.0239(10) Uani 1 1 d . . .
H14 H 0.4189 1.0684 0.4096 0.029 Uiso 1 1 calc R . .
C15 C 0.4209(6) 1.1226(5) 0.3086(2) 0.0293(11) Uani 1 1 d . . .
H15A H 0.3614 1.1185 0.2711 0.035 Uiso 1 1 calc R . .
H15B H 0.5305 1.0543 0.3024 0.035 Uiso 1 1 calc R . .
C16 C 0.4165(6) 1.2822(6) 0.3080(3) 0.0363(13) Uani 1 1 d . . .
H16A H 0.4887 1.2836 0.3411 0.044 Uiso 1 1 calc R . .
H16B H 0.4526 1.3159 0.2640 0.044 Uiso 1 1 calc R . .
C17 C 0.2536(6) 1.3888(5) 0.3236(3) 0.0333(12) Uani 1 1 d . . .
H17A H 0.2558 1.4897 0.3257 0.040 Uiso 1 1 calc R . .
H17B H 0.1838 1.3963 0.2879 0.040 Uiso 1 1 calc R . .
C18 C 0.1902(6) 1.3365(5) 0.3885(3) 0.0324(12) Uani 1 1 d . . .
H18A H 0.0828 1.4071 0.3971 0.039 Uiso 1 1 calc R . .
H18B H 0.2560 1.3352 0.4247 0.039 Uiso 1 1 calc R . .
C19 C 0.1879(6) 1.1794(5) 0.3873(3) 0.0289(11) Uani 1 1 d . . .
H19A H 0.1474 1.1462 0.4305 0.035 Uiso 1 1 calc R . .
H19B H 0.1174 1.1816 0.3527 0.035 Uiso 1 1 calc R . .
C20 C 0.2700(5) 0.8237(5) 0.4471(2) 0.0233(10) Uani 1 1 d . . .
H20 H 0.1559 0.8840 0.4432 0.028 Uiso 1 1 calc R . .
C21 C 0.3198(6) 0.8596(6) 0.5101(2) 0.0328(12) Uani 1 1 d . . .
H21A H 0.4320 0.8002 0.5167 0.039 Uiso 1 1 calc R . .
H21B H 0.3055 0.9670 0.5058 0.039 Uiso 1 1 calc R . .
C22 C 0.2243(6) 0.8246(6) 0.5699(2) 0.0343(12) Uani 1 1 d . . .
H22A H 0.2611 0.8452 0.6105 0.041 Uiso 1 1 calc R . .
H22B H 0.1129 0.8895 0.5651 0.041 Uiso 1 1 calc R . .
C23 C 0.2411(6) 0.6617(6) 0.5757(2) 0.0358(13) Uani 1 1 d . . .
H23A H 0.3505 0.5979 0.5859 0.043 Uiso 1 1 calc R . .
H23B H 0.1733 0.6421 0.6131 0.043 Uiso 1 1 calc R . .
C24 C 0.1980(7) 0.6188(6) 0.5136(3) 0.0362(13) Uani 1 1 d . . .
H24A H 0.0844 0.6705 0.5073 0.043 Uiso 1 1 calc R . .
H24B H 0.2211 0.5096 0.5187 0.043 Uiso 1 1 calc R . .
C25 C 0.2874(6) 0.6598(5) 0.4525(2) 0.0306(11) Uani 1 1 d . . .
H25A H 0.3994 0.5956 0.4552 0.037 Uiso 1 1 calc R . .
H25B H 0.2471 0.6409 0.4124 0.037 Uiso 1 1 calc R . .
C26 C 0.4040(6) 0.9442(5) 0.1173(2) 0.0278(11) Uani 1 1 d . . .
H26 H 0.4258 0.9145 0.0714 0.033 Uiso 1 1 calc R . .
C27 C 0.2695(6) 1.0962(6) 0.1146(3) 0.0349(12) Uani 1 1 d . . .
H27A H 0.2419 1.1263 0.1598 0.042 Uiso 1 1 calc R . .
H27B H 0.1764 1.0882 0.0968 0.042 Uiso 1 1 calc R . .
C28 C 0.3168(7) 1.2152(7) 0.0705(3) 0.0476(15) Uani 1 1 d . . .
H28A H 0.3360 1.1891 0.0245 0.057 Uiso 1 1 calc R . .
H28B H 0.2305 1.3137 0.0706 0.057 Uiso 1 1 calc R . .
C29 C 0.4631(8) 1.2248(7) 0.0952(3) 0.0488(16) Uani 1 1 d . . .
H29A H 0.4936 1.2999 0.0655 0.059 Uiso 1 1 calc R . .
H29B H 0.4412 1.2584 0.1399 0.059 Uiso 1 1 calc R . .
C30 C 0.5951(7) 1.0765(6) 0.0978(3) 0.0438(14) Uani 1 1 d . . .
H30A H 0.6875 1.0854 0.1158 0.053 Uiso 1 1 calc R . .
H30B H 0.6235 1.0476 0.0525 0.053 Uiso 1 1 calc R . .
C31 C 0.5524(6) 0.9555(6) 0.1406(3) 0.0326(12) Uani 1 1 d . . .
H31A H 0.5360 0.9783 0.1871 0.039 Uiso 1 1 calc R . .
H31B H 0.6396 0.8580 0.1388 0.039 Uiso 1 1 calc R . .
C32 C 0.1879(5) 0.7817(5) 0.1307(2) 0.0240(10) Uani 1 1 d . . .
H32 H 0.0929 0.8668 0.1437 0.029 Uiso 1 1 calc R . .
C33 C 0.1622(6) 0.6395(6) 0.1607(3) 0.0331(12) Uani 1 1 d . . .
H33A H 0.2514 0.5510 0.1479 0.040 Uiso 1 1 calc R . .
H33B H 0.1570 0.6349 0.2095 0.040 Uiso 1 1 calc R . .
C34 C 0.0121(7) 0.6357(7) 0.1371(3) 0.0432(14) Uani 1 1 d . . .
H34A H -0.0779 0.7166 0.1550 0.052 Uiso 1 1 calc R . .
H34B H 0.0022 0.5389 0.1544 0.052 Uiso 1 1 calc R . .
C35 C 0.0076(7) 0.6553(7) 0.0621(3) 0.0400(13) Uani 1 1 d . . .
H35A H 0.0876 0.5666 0.0445 0.048 Uiso 1 1 calc R . .
H35B H -0.0960 0.6618 0.0489 0.048 Uiso 1 1 calc R . .
C36 C 0.0372(6) 0.7941(6) 0.0323(3) 0.0325(12) Uani 1 1 d . . .
H36A H -0.0497 0.8839 0.0455 0.039 Uiso 1 1 calc R . .
H36B H 0.0406 0.7993 -0.0165 0.039 Uiso 1 1 calc R . .
C37 C 0.1915(6) 0.7936(6) 0.0552(2) 0.0293(11) Uani 1 1 d . . .
H37A H 0.2796 0.7078 0.0396 0.035 Uiso 1 1 calc R . .
H37B H 0.2072 0.8870 0.0363 0.035 Uiso 1 1 calc R . .
Br1 Br 0.06131(6) 0.98971(6) 0.27005(3) 0.03460(15) Uani 1 1 d . . .
Ni1 Ni 0.32356(7) 0.82563(7) 0.27342(3) 0.02185(15) Uani 1 1 d . . .
P1 P 0.36698(14) 0.87397(14) 0.37028(6) 0.0226(3) Uani 1 1 d . . .
P2 P 0.35312(14) 0.79828(14) 0.16979(6) 0.0232(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.513(6) . ?
C1 C8 1.516(6) . ?
C1 Ni1 1.975(5) . ?
C1 H1 1.0000 . ?
C2 C7 1.383(7) . ?
C2 C3 1.399(7) . ?
C3 C4 1.387(7) . ?
C3 P1 1.816(5) . ?
C4 C5 1.372(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.372(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(7) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.391(6) . ?
C8 C13 1.396(6) . ?
C9 C10 1.389(7) . ?
C9 P2 1.809(5) . ?
C10 C11 1.375(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.372(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.375(7) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.523(6) . ?
C14 C15 1.527(6) . ?
C14 P1 1.854(5) . ?
C14 H14 1.0000 . ?
C15 C16 1.527(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.510(7) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.505(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.530(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C25 1.523(6) . ?
C20 C21 1.524(6) . ?
C20 P1 1.840(5) . ?
C20 H20 1.0000 . ?
C21 C22 1.521(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.514(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.511(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.527(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C31 1.529(7) . ?
C26 C27 1.530(7) . ?
C26 P2 1.835(5) . ?
C26 H26 1.0000 . ?
C27 C28 1.535(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.516(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.496(8) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.517(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.521(6) . ?
C32 C37 1.529(6) . ?
C32 P2 1.842(5) . ?
C32 H32 1.0000 . ?
C33 C34 1.515(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.521(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.508(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.531(7) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
Br1 Ni1 2.3501(8) . ?
Ni1 P2 2.1499(14) . ?
Ni1 P1 2.1911(14) . ?

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
C2 C1 C8 115.7(4) . . ?
C2 C1 Ni1 110.4(3) . . ?
C8 C1 Ni1 117.2(3) . . ?
C2 C1 H1 103.8 . . ?
C8 C1 H1 103.8 . . ?
Ni1 C1 H1 103.8 . . ?
C7 C2 C3 117.7(4) . . ?
C7 C2 C1 125.4(4) . . ?
C3 C2 C1 116.9(4) . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 P1 124.9(4) . . ?
C2 C3 P1 112.0(3) . . ?
C5 C4 C3 119.9(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C6 C5 C4 119.5(5) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C7 120.9(5) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C2 C7 C6 120.5(5) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C9 C8 C13 118.2(4) . . ?
C9 C8 C1 119.3(4) . . ?
C13 C8 C1 122.4(4) . . ?
C10 C9 C8 120.8(4) . . ?
C10 C9 P2 128.0(4) . . ?
C8 C9 P2 111.2(4) . . ?
C11 C10 C9 119.3(5) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C12 C11 C10 120.9(5) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 120.0(5) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C8 120.7(4) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
C19 C14 C15 110.8(4) . . ?
C19 C14 P1 115.0(3) . . ?
C15 C14 P1 108.8(3) . . ?
C19 C14 H14 107.3 . . ?
C15 C14 H14 107.3 . . ?
P1 C14 H14 107.3 . . ?
C14 C15 C16 111.9(4) . . ?
C14 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C15 111.4(4) . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C18 C17 C16 111.1(4) . . ?
C18 C17 H17A 109.4 . . ?
C16 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
C16 C17 H17B 109.4 . . ?
H17A C17 H17B 108.0 . . ?
C17 C18 C19 110.7(4) . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C14 C19 C18 110.2(4) . . ?
C14 C19 H19A 109.6 . . ?
C18 C19 H19A 109.6 . . ?
C14 C19 H19B 109.6 . . ?
C18 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C25 C20 C21 110.9(4) . . ?
C25 C20 P1 110.3(3) . . ?
C21 C20 P1 115.3(3) . . ?
C25 C20 H20 106.6 . . ?
C21 C20 H20 106.6 . . ?
P1 C20 H20 106.6 . . ?
C22 C21 C20 111.0(4) . . ?
C22 C21 H21A 109.4 . . ?
C20 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C23 C22 C21 109.9(4) . . ?
C23 C22 H22A 109.7 . . ?
C21 C22 H22A 109.7 . . ?
C23 C22 H22B 109.7 . . ?
C21 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C24 C23 C22 112.8(4) . . ?
C24 C23 H23A 109.0 . . ?
C22 C23 H23A 109.0 . . ?
C24 C23 H23B 109.0 . . ?
C22 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C23 C24 C25 112.0(4) . . ?
C23 C24 H24A 109.2 . . ?
C25 C24 H24A 109.2 . . ?
C23 C24 H24B 109.2 . . ?
C25 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
C20 C25 C24 111.0(4) . . ?
C20 C25 H25A 109.4 . . ?
C24 C25 H25A 109.4 . . ?
C20 C25 H25B 109.4 . . ?
C24 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C31 C26 C27 110.8(4) . . ?
C31 C26 P2 110.7(3) . . ?
C27 C26 P2 111.8(3) . . ?
C31 C26 H26 107.8 . . ?
C27 C26 H26 107.8 . . ?
P2 C26 H26 107.8 . . ?
C26 C27 C28 110.3(5) . . ?
C26 C27 H27A 109.6 . . ?
C28 C27 H27A 109.6 . . ?
C26 C27 H27B 109.6 . . ?
C28 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
C29 C28 C27 110.5(5) . . ?
C29 C28 H28A 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
C30 C29 C28 111.2(5) . . ?
C30 C29 H29A 109.4 . . ?
C28 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
C28 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
C29 C30 C31 111.7(5) . . ?
C29 C30 H30A 109.3 . . ?
C31 C30 H30A 109.3 . . ?
C29 C30 H30B 109.3 . . ?
C31 C30 H30B 109.3 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 C26 111.2(4) . . ?
C30 C31 H31A 109.4 . . ?
C26 C31 H31A 109.4 . . ?
C30 C31 H31B 109.4 . . ?
C26 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
C33 C32 C37 110.5(4) . . ?
C33 C32 P2 109.9(3) . . ?
C37 C32 P2 117.5(3) . . ?
C33 C32 H32 106.0 . . ?
C37 C32 H32 106.0 . . ?
P2 C32 H32 106.0 . . ?
C34 C33 C32 110.7(4) . . ?
C34 C33 H33A 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 108.1 . . ?
C33 C34 C35 112.0(5) . . ?
C33 C34 H34A 109.2 . . ?
C35 C34 H34A 109.2 . . ?
C33 C34 H34B 109.2 . . ?
C35 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
C36 C35 C34 111.8(5) . . ?
C36 C35 H35A 109.3 . . ?
C34 C35 H35A 109.3 . . ?
C36 C35 H35B 109.3 . . ?
C34 C35 H35B 109.3 . . ?
H35A C35 H35B 107.9 . . ?
C35 C36 C37 111.0(4) . . ?
C35 C36 H36A 109.4 . . ?
C37 C36 H36A 109.4 . . ?
C35 C36 H36B 109.4 . . ?
C37 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
C32 C37 C36 109.5(4) . . ?
C32 C37 H37A 109.8 . . ?
C36 C37 H37A 109.8 . . ?
C32 C37 H37B 109.8 . . ?
C36 C37 H37B 109.8 . . ?
H37A C37 H37B 108.2 . . ?
C1 Ni1 P2 85.92(14) . . ?
C1 Ni1 P1 85.59(14) . . ?
P2 Ni1 P1 159.63(6) . . ?
C1 Ni1 Br1 167.62(14) . . ?
P2 Ni1 Br1 96.45(4) . . ?
P1 Ni1 Br1 95.80(4) . . ?
C3 P1 C20 110.8(2) . . ?
C3 P1 C14 100.3(2) . . ?
C20 P1 C14 105.9(2) . . ?
C3 P1 Ni1 100.55(16) . . ?
C20 P1 Ni1 122.50(16) . . ?
C14 P1 Ni1 114.49(16) . . ?
C9 P2 C26 103.8(2) . . ?
C9 P2 C32 109.5(2) . . ?
C26 P2 C32 106.0(2) . . ?
C9 P2 Ni1 105.46(16) . . ?
C26 P2 Ni1 114.82(17) . . ?
C32 P2 Ni1 116.45(16) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.096
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1039462'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H45 Cl Ni P2'
_chemical_formula_sum            'C29 H45 Cl Ni P2'
_chemical_formula_weight         549.75

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   18.5050(6)
_cell_length_b                   16.1911(4)
_cell_length_c                   23.0219(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 124.093(2)
_cell_angle_gamma                90.00
_cell_volume                     5712.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    19165
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      26.00

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9153
_exptl_absorpt_correction_T_max  0.9649
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' ω and φ '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19165
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         26.00
_reflns_number_total             10765
_reflns_number_gt                8036
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+23.6462P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10765
_refine_ls_number_parameters     599
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0740
_refine_ls_wR_factor_ref         0.1526
_refine_ls_wR_factor_gt          0.1355
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6787(7) 0.6050(7) 0.3786(5) 0.0291(15) Uani 0.433(8) 1 d P A 1
H1 H 0.7347 0.5910 0.3837 0.035 Uiso 0.433(8) 1 calc PR A 1
C1' C 0.6099(6) 0.6250(5) 0.3606(4) 0.0291(15) Uani 0.567(8) 1 d P A 2
H1' H 0.5515 0.6336 0.3526 0.035 Uiso 0.567(8) 1 calc PR A 2
C2 C 0.5996(5) 0.6314(4) 0.2928(3) 0.0595(19) Uani 1 1 d . . .
C3 C 0.6326(4) 0.6957(3) 0.2749(3) 0.0370(12) Uani 1 1 d . A .
C4 C 0.6048(4) 0.7059(4) 0.2058(3) 0.0496(15) Uani 1 1 d . . .
H4 H 0.6304 0.7473 0.1937 0.060 Uiso 1 1 calc R A .
C5 C 0.5401(5) 0.6561(4) 0.1545(3) 0.065(2) Uani 1 1 d . A .
H5 H 0.5218 0.6628 0.1072 0.079 Uiso 1 1 calc R . .
C6 C 0.5019(4) 0.5973(4) 0.1713(4) 0.0567(17) Uani 1 1 d . . .
H6 H 0.4550 0.5651 0.1355 0.068 Uiso 1 1 calc R A .
C7 C 0.5312(5) 0.5850(4) 0.2391(4) 0.0606(19) Uani 1 1 d . A .
H7 H 0.5045 0.5437 0.2505 0.073 Uiso 1 1 calc R . .
C8 C 0.6449(4) 0.5324(4) 0.3945(3) 0.0512(16) Uani 1 1 d . . .
C9 C 0.6571(3) 0.5250(3) 0.4593(3) 0.0319(11) Uani 1 1 d . A .
C10 C 0.6536(4) 0.4476(3) 0.4836(3) 0.0432(14) Uani 1 1 d . . .
H10 H 0.6584 0.4426 0.5267 0.052 Uiso 1 1 calc R A .
C11 C 0.6430(4) 0.3782(4) 0.4452(3) 0.0594(19) Uani 1 1 d . A .
H11 H 0.6398 0.3254 0.4616 0.071 Uiso 1 1 calc R . .
C12 C 0.6372(4) 0.3855(4) 0.3838(3) 0.0589(18) Uani 1 1 d . . .
H12 H 0.6318 0.3372 0.3581 0.071 Uiso 1 1 calc R A .
C13 C 0.6390(4) 0.4610(4) 0.3587(3) 0.0562(17) Uani 1 1 d . A .
H13 H 0.6363 0.4649 0.3164 0.067 Uiso 1 1 calc R . .
C14 C 0.6425(4) 0.8659(3) 0.3201(3) 0.0404(13) Uani 1 1 d . . .
C15 C 0.5642(4) 0.8563(4) 0.3251(4) 0.0604(18) Uani 1 1 d . . .
H15A H 0.5269 0.8114 0.2943 0.091 Uiso 1 1 calc R . .
H15B H 0.5307 0.9079 0.3107 0.091 Uiso 1 1 calc R . .
H15C H 0.5845 0.8435 0.3736 0.091 Uiso 1 1 calc R . .
C16 C 0.7006(4) 0.9357(3) 0.3687(3) 0.0535(16) Uani 1 1 d . . .
H16A H 0.7509 0.9423 0.3655 0.080 Uiso 1 1 calc R . .
H16B H 0.7209 0.9224 0.4171 0.080 Uiso 1 1 calc R . .
H16C H 0.6672 0.9873 0.3546 0.080 Uiso 1 1 calc R . .
C17 C 0.6088(4) 0.8908(4) 0.2445(3) 0.0567(18) Uani 1 1 d . . .
H17A H 0.5713 0.8470 0.2123 0.085 Uiso 1 1 calc R . .
H17B H 0.6583 0.8993 0.2406 0.085 Uiso 1 1 calc R . .
H17C H 0.5752 0.9422 0.2325 0.085 Uiso 1 1 calc R . .
C18 C 0.8099(4) 0.7660(4) 0.3641(3) 0.0540(17) Uani 1 1 d . . .
C19 C 0.8749(4) 0.8121(6) 0.4322(4) 0.086(3) Uani 1 1 d . . .
H19A H 0.8741 0.7880 0.4709 0.129 Uiso 1 1 calc R . .
H19B H 0.8586 0.8705 0.4270 0.129 Uiso 1 1 calc R . .
H19C H 0.9337 0.8071 0.4423 0.129 Uiso 1 1 calc R . .
C20 C 0.8120(5) 0.8022(6) 0.3042(4) 0.080(2) Uani 1 1 d . . .
H20A H 0.7706 0.7725 0.2608 0.120 Uiso 1 1 calc R . .
H20B H 0.8710 0.7967 0.3147 0.120 Uiso 1 1 calc R . .
H20C H 0.7959 0.8607 0.2986 0.120 Uiso 1 1 calc R . .
C21 C 0.8371(6) 0.6748(5) 0.3731(5) 0.103(3) Uani 1 1 d . . .
H21A H 0.8358 0.6507 0.4116 0.155 Uiso 1 1 calc R . .
H21B H 0.8964 0.6708 0.3840 0.155 Uiso 1 1 calc R . .
H21C H 0.7966 0.6448 0.3296 0.155 Uiso 1 1 calc R . .
C22 C 0.5946(4) 0.6451(4) 0.5177(4) 0.0557(17) Uani 1 1 d . . .
C23 C 0.5936(5) 0.5867(5) 0.5696(4) 0.083(3) Uani 1 1 d . . .
H23A H 0.5902 0.5294 0.5545 0.125 Uiso 1 1 calc R . .
H23B H 0.5429 0.5990 0.5711 0.125 Uiso 1 1 calc R . .
H23C H 0.6471 0.5943 0.6164 0.125 Uiso 1 1 calc R . .
C24 C 0.5997(5) 0.7351(5) 0.5404(5) 0.092(3) Uani 1 1 d . . .
H24A H 0.6001 0.7719 0.5068 0.138 Uiso 1 1 calc R . .
H24B H 0.6532 0.7433 0.5871 0.138 Uiso 1 1 calc R . .
H24C H 0.5489 0.7477 0.5419 0.138 Uiso 1 1 calc R . .
C25 C 0.5088(4) 0.6352(5) 0.4456(4) 0.085(3) Uani 1 1 d . . .
H25A H 0.5032 0.5781 0.4295 0.128 Uiso 1 1 calc R . .
H25B H 0.5086 0.6726 0.4120 0.128 Uiso 1 1 calc R . .
H25C H 0.4597 0.6486 0.4491 0.128 Uiso 1 1 calc R . .
C26 C 0.7923(4) 0.6081(4) 0.5891(3) 0.0452(14) Uani 1 1 d . . .
C27 C 0.8106(4) 0.6756(4) 0.6415(3) 0.0585(18) Uani 1 1 d . . .
H27A H 0.8030 0.7297 0.6197 0.088 Uiso 1 1 calc R . .
H27B H 0.8706 0.6702 0.6827 0.088 Uiso 1 1 calc R . .
H27C H 0.7699 0.6703 0.6558 0.088 Uiso 1 1 calc R . .
C28 C 0.8578(4) 0.6147(4) 0.5685(4) 0.067(2) Uani 1 1 d . . .
H28A H 0.8508 0.6682 0.5459 0.100 Uiso 1 1 calc R . .
H28B H 0.8473 0.5701 0.5359 0.100 Uiso 1 1 calc R . .
H28C H 0.9173 0.6102 0.6107 0.100 Uiso 1 1 calc R . .
C29 C 0.8050(5) 0.5245(4) 0.6240(3) 0.073(2) Uani 1 1 d . . .
H29A H 0.7935 0.4804 0.5907 0.109 Uiso 1 1 calc R . .
H29B H 0.7645 0.5194 0.6385 0.109 Uiso 1 1 calc R . .
H29C H 0.8651 0.5200 0.6652 0.109 Uiso 1 1 calc R . .
C30 C 0.8832(4) 0.3825(3) 0.2935(3) 0.0400(13) Uani 1 1 d . . .
H30 H 0.9430 0.3588 0.3153 0.048 Uiso 1 1 calc R . .
C31 C 0.8929(4) 0.4680(3) 0.2734(3) 0.0375(12) Uani 1 1 d . . .
C32 C 0.8453(3) 0.4909(3) 0.2034(3) 0.0321(11) Uani 1 1 d . . .
C33 C 0.8542(4) 0.5702(3) 0.1847(3) 0.0403(13) Uani 1 1 d . . .
H33 H 0.8194 0.5869 0.1369 0.048 Uiso 1 1 calc R . .
C34 C 0.9128(4) 0.6242(3) 0.2348(3) 0.0445(14) Uani 1 1 d . . .
H34 H 0.9175 0.6787 0.2219 0.053 Uiso 1 1 calc R . .
C35 C 0.9648(4) 0.6001(3) 0.3035(3) 0.0443(14) Uani 1 1 d . . .
H35 H 1.0076 0.6368 0.3378 0.053 Uiso 1 1 calc R . .
C36 C 0.9552(3) 0.5232(3) 0.3229(3) 0.0414(13) Uani 1 1 d . . .
H36 H 0.9914 0.5071 0.3707 0.050 Uiso 1 1 calc R . .
C37 C 0.8703(4) 0.3783(3) 0.3533(3) 0.0394(13) Uani 1 1 d . . .
C38 C 0.8617(3) 0.2993(3) 0.3737(2) 0.0317(11) Uani 1 1 d . . .
C39 C 0.8725(4) 0.2877(4) 0.4378(3) 0.0425(14) Uani 1 1 d . . .
H39 H 0.8731 0.2334 0.4536 0.051 Uiso 1 1 calc R . .
C40 C 0.8823(4) 0.3546(4) 0.4785(3) 0.0569(17) Uani 1 1 d . . .
H40 H 0.8903 0.3465 0.5226 0.068 Uiso 1 1 calc R . .
C41 C 0.8806(4) 0.4329(4) 0.4552(3) 0.0578(17) Uani 1 1 d . . .
H41 H 0.8831 0.4792 0.4816 0.069 Uiso 1 1 calc R . .
C42 C 0.8752(4) 0.4449(4) 0.3933(3) 0.0504(15) Uani 1 1 d . . .
H42 H 0.8747 0.4995 0.3779 0.061 Uiso 1 1 calc R . .
C43 C 0.8292(4) 0.3884(4) 0.0923(3) 0.0457(14) Uani 1 1 d . . .
C44 C 0.9145(5) 0.3425(4) 0.1400(4) 0.073(2) Uani 1 1 d . . .
H44A H 0.9541 0.3767 0.1811 0.109 Uiso 1 1 calc R . .
H44B H 0.9414 0.3306 0.1144 0.109 Uiso 1 1 calc R . .
H44C H 0.9030 0.2906 0.1554 0.109 Uiso 1 1 calc R . .
C45 C 0.7676(5) 0.3345(4) 0.0280(3) 0.069(2) Uani 1 1 d . . .
H45A H 0.7125 0.3640 -0.0030 0.103 Uiso 1 1 calc R . .
H45B H 0.7561 0.2826 0.0434 0.103 Uiso 1 1 calc R . .
H45C H 0.7948 0.3226 0.0027 0.103 Uiso 1 1 calc R . .
C46 C 0.8486(5) 0.4668(4) 0.0664(3) 0.0583(18) Uani 1 1 d . . .
H46A H 0.7942 0.4974 0.0355 0.087 Uiso 1 1 calc R . .
H46B H 0.8743 0.4519 0.0405 0.087 Uiso 1 1 calc R . .
H46C H 0.8896 0.5014 0.1067 0.087 Uiso 1 1 calc R . .
C47 C 0.6670(4) 0.4397(4) 0.0924(3) 0.0537(16) Uani 1 1 d . . .
C48 C 0.6064(4) 0.3670(4) 0.0549(4) 0.068(2) Uani 1 1 d . . .
H48A H 0.6196 0.3232 0.0889 0.101 Uiso 1 1 calc R . .
H48B H 0.6148 0.3459 0.0191 0.101 Uiso 1 1 calc R . .
H48C H 0.5458 0.3849 0.0325 0.101 Uiso 1 1 calc R . .
C49 C 0.6477(4) 0.5087(5) 0.0414(4) 0.087(3) Uani 1 1 d . . .
H49A H 0.6871 0.5551 0.0666 0.130 Uiso 1 1 calc R . .
H49B H 0.5871 0.5269 0.0190 0.130 Uiso 1 1 calc R . .
H49C H 0.6562 0.4889 0.0054 0.130 Uiso 1 1 calc R . .
C50 C 0.6499(5) 0.4704(5) 0.1473(5) 0.083(3) Uani 1 1 d . . .
H50A H 0.6625 0.4258 0.1805 0.124 Uiso 1 1 calc R . .
H50B H 0.5887 0.4870 0.1235 0.124 Uiso 1 1 calc R . .
H50C H 0.6877 0.5177 0.1726 0.124 Uiso 1 1 calc R . .
C51 C 0.9150(4) 0.1427(3) 0.3423(3) 0.0402(13) Uani 1 1 d . . .
C52 C 0.9012(4) 0.0839(4) 0.2844(3) 0.0526(16) Uani 1 1 d . . .
H52A H 0.8465 0.0534 0.2651 0.079 Uiso 1 1 calc R . .
H52B H 0.9499 0.0449 0.3042 0.079 Uiso 1 1 calc R . .
H52C H 0.8983 0.1160 0.2471 0.079 Uiso 1 1 calc R . .
C53 C 1.0000(3) 0.1893(4) 0.3707(3) 0.0495(15) Uani 1 1 d . . .
H53A H 1.0102 0.2274 0.4077 0.074 Uiso 1 1 calc R . .
H53B H 0.9961 0.2207 0.3326 0.074 Uiso 1 1 calc R . .
H53C H 1.0484 0.1499 0.3900 0.074 Uiso 1 1 calc R . .
C54 C 0.9235(4) 0.0917(4) 0.4017(3) 0.0524(16) Uani 1 1 d . . .
H54A H 0.8690 0.0615 0.3841 0.079 Uiso 1 1 calc R . .
H54B H 0.9352 0.1284 0.4399 0.079 Uiso 1 1 calc R . .
H54C H 0.9716 0.0523 0.4191 0.079 Uiso 1 1 calc R . .
C55 C 0.7206(3) 0.1833(3) 0.2838(3) 0.0387(13) Uani 1 1 d . . .
C56 C 0.6949(4) 0.1043(4) 0.2401(3) 0.0464(14) Uani 1 1 d . . .
H56A H 0.6967 0.1141 0.1990 0.070 Uiso 1 1 calc R . .
H56B H 0.6356 0.0882 0.2248 0.070 Uiso 1 1 calc R . .
H56C H 0.7357 0.0600 0.2686 0.070 Uiso 1 1 calc R . .
C57 C 0.6547(4) 0.2513(4) 0.2401(3) 0.0495(15) Uani 1 1 d . . .
H57A H 0.6558 0.2628 0.1988 0.074 Uiso 1 1 calc R . .
H57B H 0.6699 0.3015 0.2684 0.074 Uiso 1 1 calc R . .
H57C H 0.5961 0.2331 0.2250 0.074 Uiso 1 1 calc R . .
C58 C 0.7170(4) 0.1667(4) 0.3473(3) 0.0465(15) Uani 1 1 d . . .
H58A H 0.7330 0.2169 0.3757 0.070 Uiso 1 1 calc R . .
H58B H 0.7580 0.1223 0.3756 0.070 Uiso 1 1 calc R . .
H58C H 0.6578 0.1500 0.3315 0.070 Uiso 1 1 calc R . .
Cl1 Cl 0.75018(11) 0.81232(8) 0.50696(7) 0.0513(4) Uani 1 1 d . A .
Cl2 Cl 0.75093(11) 0.20398(9) 0.13724(7) 0.0509(4) Uani 1 1 d . . .
Ni1 Ni 0.69305(6) 0.70608(4) 0.43270(4) 0.0437(2) Uani 1 1 d . . .
Ni2 Ni 0.80971(5) 0.30327(4) 0.21851(3) 0.03374(17) Uani 1 1 d . . .
P1 P 0.70008(9) 0.76423(8) 0.34907(7) 0.0329(3) Uani 1 1 d . A .
P2 P 0.68348(9) 0.62356(8) 0.50454(6) 0.0308(3) Uani 1 1 d . A .
P3 P 0.78331(9) 0.40498(8) 0.14595(6) 0.0315(3) Uani 1 1 d . . .
P4 P 0.82841(9) 0.22364(8) 0.30478(6) 0.0311(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C8 1.470(12) . ?
C1 C2 1.728(12) . ?
C1 Ni1 1.982(11) . ?
C1 H1 1.0000 . ?
C1' C2 1.465(9) . ?
C1' C8 1.646(10) . ?
C1' Ni1 1.995(8) . ?
C1' H1' 1.0000 . ?
C2 C3 1.382(7) . ?
C2 C7 1.393(9) . ?
C3 C4 1.380(7) . ?
C3 P1 1.822(5) . ?
C4 C5 1.375(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.364(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.350(9) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.384(7) . ?
C8 C13 1.388(8) . ?
C9 C10 1.389(7) . ?
C9 P2 1.817(5) . ?
C10 C11 1.373(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.363(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.361(9) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.525(8) . ?
C14 C16 1.529(8) . ?
C14 C17 1.536(7) . ?
C14 P1 1.870(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
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 C20 1.517(9) . ?
C18 C19 1.533(9) . ?
C18 C21 1.535(10) . ?
C18 P1 1.861(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C25 1.532(9) . ?
C22 C23 1.532(10) . ?
C22 C24 1.533(9) . ?
C22 P2 1.864(6) . ?
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 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.518(8) . ?
C26 C29 1.523(8) . ?
C26 C28 1.532(9) . ?
C26 P2 1.873(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.501(7) . ?
C30 C37 1.525(7) . ?
C30 Ni2 1.960(5) . ?
C30 H30 1.0000 . ?
C31 C32 1.386(7) . ?
C31 C36 1.398(7) . ?
C32 C33 1.393(7) . ?
C32 P3 1.817(5) . ?
C33 C34 1.367(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.369(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.367(8) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.387(8) . ?
C37 C38 1.402(7) . ?
C38 C39 1.386(7) . ?
C38 P4 1.817(5) . ?
C39 C40 1.376(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.370(9) . ?
C40 H40 0.9500 . ?
C41 C42 1.386(8) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.519(9) . ?
C43 C46 1.528(8) . ?
C43 C45 1.536(8) . ?
C43 P3 1.869(6) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C49 1.511(9) . ?
C47 C48 1.517(8) . ?
C47 C50 1.547(10) . ?
C47 P3 1.869(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C53 1.523(7) . ?
C51 C54 1.527(8) . ?
C51 C52 1.538(7) . ?
C51 P4 1.865(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C58 1.524(7) . ?
C55 C57 1.527(7) . ?
C55 C56 1.529(8) . ?
C55 P4 1.887(5) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
Cl1 Ni1 2.2300(15) . ?
Cl2 Ni2 2.2332(15) . ?
Ni1 P2 2.2090(14) . ?
Ni1 P1 2.2116(15) . ?
Ni2 P3 2.1968(15) . ?
Ni2 P4 2.2262(14) . ?

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
C8 C1 C2 106.0(7) . . ?
C8 C1 Ni1 115.4(7) . . ?
C2 C1 Ni1 104.0(6) . . ?
C8 C1 H1 110.3 . . ?
C2 C1 H1 110.3 . . ?
Ni1 C1 H1 110.3 . . ?
C2 C1' C8 110.5(6) . . ?
C2 C1' Ni1 114.8(6) . . ?
C8 C1' Ni1 106.9(5) . . ?
C2 C1' H1' 108.2 . . ?
C8 C1' H1' 108.2 . . ?
Ni1 C1' H1' 108.2 . . ?
C3 C2 C7 118.3(5) . . ?
C3 C2 C1' 123.8(6) . . ?
C7 C2 C1' 114.7(6) . . ?
C3 C2 C1 107.2(6) . . ?
C7 C2 C1 130.3(6) . . ?
C1' C2 C1 40.9(5) . . ?
C4 C3 C2 119.5(5) . . ?
C4 C3 P1 128.6(4) . . ?
C2 C3 P1 111.4(4) . . ?
C5 C4 C3 120.1(6) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 120.4(6) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C7 C6 C5 119.6(6) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C7 C2 121.5(6) . . ?
C6 C7 H7 119.2 . . ?
C2 C7 H7 119.2 . . ?
C9 C8 C13 118.6(5) . . ?
C9 C8 C1 120.2(6) . . ?
C13 C8 C1 114.9(6) . . ?
C9 C8 C1' 111.9(5) . . ?
C13 C8 C1' 126.8(6) . . ?
C1 C8 C1' 42.6(5) . . ?
C8 C9 C10 119.8(5) . . ?
C8 C9 P2 111.8(4) . . ?
C10 C9 P2 128.3(4) . . ?
C11 C10 C9 120.1(6) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C12 C11 C10 119.8(6) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C13 C12 C11 120.7(6) . . ?
C13 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
C12 C13 C8 120.7(6) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
C15 C14 C16 109.2(5) . . ?
C15 C14 C17 108.2(5) . . ?
C16 C14 C17 107.9(5) . . ?
C15 C14 P1 105.0(4) . . ?
C16 C14 P1 111.3(4) . . ?
C17 C14 P1 115.1(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C20 C18 C19 109.6(6) . . ?
C20 C18 C21 108.7(6) . . ?
C19 C18 C21 108.6(6) . . ?
C20 C18 P1 114.8(4) . . ?
C19 C18 P1 110.3(4) . . ?
C21 C18 P1 104.6(5) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C22 C23 108.8(6) . . ?
C25 C22 C24 107.3(6) . . ?
C23 C22 C24 110.2(6) . . ?
C25 C22 P2 106.1(5) . . ?
C23 C22 P2 114.1(5) . . ?
C24 C22 P2 110.0(5) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C29 108.7(5) . . ?
C27 C26 C28 109.4(5) . . ?
C29 C26 C28 108.0(6) . . ?
C27 C26 P2 111.1(4) . . ?
C29 C26 P2 115.1(4) . . ?
C28 C26 P2 104.2(4) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C37 115.1(5) . . ?
C31 C30 Ni2 118.4(4) . . ?
C37 C30 Ni2 112.5(4) . . ?
C31 C30 H30 102.6 . . ?
C37 C30 H30 102.6 . . ?
Ni2 C30 H30 102.6 . . ?
C32 C31 C36 118.2(5) . . ?
C32 C31 C30 119.9(5) . . ?
C36 C31 C30 121.7(5) . . ?
C31 C32 C33 119.9(5) . . ?
C31 C32 P3 111.8(4) . . ?
C33 C32 P3 128.1(4) . . ?
C34 C33 C32 120.2(5) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 120.3(5) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C36 C35 C34 120.1(5) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C31 121.0(5) . . ?
C35 C36 H36 119.5 . . ?
C31 C36 H36 119.5 . . ?
C42 C37 C38 117.6(5) . . ?
C42 C37 C30 125.5(5) . . ?
C38 C37 C30 116.6(5) . . ?
C39 C38 C37 120.4(5) . . ?
C39 C38 P4 127.8(4) . . ?
C37 C38 P4 111.7(4) . . ?
C40 C39 C38 120.2(6) . . ?
C40 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C41 C40 C39 119.8(5) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C40 C41 C42 120.3(6) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C41 C42 C37 121.0(6) . . ?
C41 C42 H42 119.5 . . ?
C37 C42 H42 119.5 . . ?
C44 C43 C46 108.2(5) . . ?
C44 C43 C45 109.1(6) . . ?
C46 C43 C45 107.9(5) . . ?
C44 C43 P3 105.4(4) . . ?
C46 C43 P3 115.6(4) . . ?
C45 C43 P3 110.6(4) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C49 C47 C48 110.8(6) . . ?
C49 C47 C50 109.2(6) . . ?
C48 C47 C50 106.8(6) . . ?
C49 C47 P3 114.7(5) . . ?
C48 C47 P3 110.6(4) . . ?
C50 C47 P3 104.1(4) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C47 C50 H50A 109.5 . . ?
C47 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C47 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C53 C51 C54 108.7(5) . . ?
C53 C51 C52 107.9(5) . . ?
C54 C51 C52 108.9(5) . . ?
C53 C51 P4 105.2(4) . . ?
C54 C51 P4 115.2(4) . . ?
C52 C51 P4 110.5(4) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C58 C55 C57 108.2(5) . . ?
C58 C55 C56 108.5(5) . . ?
C57 C55 C56 109.2(5) . . ?
C58 C55 P4 115.1(4) . . ?
C57 C55 P4 105.0(4) . . ?
C56 C55 P4 110.6(4) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C1 Ni1 C1' 33.4(4) . . ?
C1 Ni1 P2 86.1(3) . . ?
C1' Ni1 P2 82.9(2) . . ?
C1 Ni1 P1 81.8(3) . . ?
C1' Ni1 P1 87.1(2) . . ?
P2 Ni1 P1 167.89(6) . . ?
C1 Ni1 Cl1 163.2(3) . . ?
C1' Ni1 Cl1 163.4(3) . . ?
P2 Ni1 Cl1 95.46(5) . . ?
P1 Ni1 Cl1 96.03(6) . . ?
C30 Ni2 P3 85.86(16) . . ?
C30 Ni2 P4 84.81(16) . . ?
P3 Ni2 P4 165.84(6) . . ?
C30 Ni2 Cl2 168.64(18) . . ?
P3 Ni2 Cl2 96.10(5) . . ?
P4 Ni2 Cl2 95.14(5) . . ?
C3 P1 C18 106.7(3) . . ?
C3 P1 C14 104.3(3) . . ?
C18 P1 C14 113.4(3) . . ?
C3 P1 Ni1 102.28(17) . . ?
C18 P1 Ni1 115.9(2) . . ?
C14 P1 Ni1 112.69(19) . . ?
C9 P2 C22 106.2(3) . . ?
C9 P2 C26 105.4(2) . . ?
C22 P2 C26 112.9(3) . . ?
C9 P2 Ni1 102.16(17) . . ?
C22 P2 Ni1 117.2(2) . . ?
C26 P2 Ni1 111.6(2) . . ?
C32 P3 C47 105.9(3) . . ?
C32 P3 C43 104.8(3) . . ?
C47 P3 C43 112.8(3) . . ?
C32 P3 Ni2 103.91(16) . . ?
C47 P3 Ni2 114.2(2) . . ?
C43 P3 Ni2 113.9(2) . . ?
C38 P4 C51 106.7(2) . . ?
C38 P4 C55 104.4(2) . . ?
C51 P4 C55 112.7(2) . . ?
C38 P4 Ni2 101.25(17) . . ?
C51 P4 Ni2 118.95(19) . . ?
C55 P4 Ni2 111.03(17) . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1039463'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H43 N Ni O P2'
_chemical_formula_sum            'C32 H43 N Ni O P2'
_chemical_formula_weight         578.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   10.6682(3)
_cell_length_b                   13.0871(5)
_cell_length_c                   10.8509(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.579(3)
_cell_angle_gamma                90.00
_cell_volume                     1504.98(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    11685
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.00

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             616
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9405
_exptl_absorpt_correction_T_max  0.9549
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11685
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.47
_diffrn_reflns_theta_max         27.00
_reflns_number_total             6353
_reflns_number_gt                5633
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0149P)²+2.3150P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.031(16)
_refine_ls_number_reflns         6353
_refine_ls_number_parameters     338
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1068
_refine_ls_wR_factor_gt          0.1002
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.1073(4) 0.1273(3) 0.4030(4) 0.0280(9) Uani 1 1 d . . .
H1 H 1.0748 0.1882 0.4450 0.034 Uiso 1 1 calc R . .
C2 C 1.2351(4) 0.1607(3) 0.3700(4) 0.0306(9) Uani 1 1 d . . .
C3 C 1.2614(4) 0.1539(3) 0.2482(4) 0.0312(9) Uani 1 1 d . . .
C4 C 1.3761(4) 0.1858(4) 0.2140(5) 0.0435(11) Uani 1 1 d . . .
H4 H 1.3938 0.1783 0.1306 0.052 Uiso 1 1 calc R . .
C5 C 1.4650(4) 0.2289(4) 0.3017(5) 0.0483(13) Uani 1 1 d . . .
H5 H 1.5439 0.2509 0.2787 0.058 Uiso 1 1 calc R . .
C6 C 1.4391(4) 0.2396(4) 0.4214(5) 0.0487(13) Uani 1 1 d . . .
H6 H 1.4994 0.2707 0.4810 0.058 Uiso 1 1 calc R . .
C7 C 1.3263(4) 0.2059(3) 0.4558(5) 0.0398(11) Uani 1 1 d . . .
H7 H 1.3099 0.2133 0.5396 0.048 Uiso 1 1 calc R . .
C8 C 1.1094(4) 0.0432(3) 0.4986(4) 0.0313(9) Uani 1 1 d . . .
C9 C 0.9916(4) 0.0051(3) 0.5233(4) 0.0318(9) Uani 1 1 d . . .
C10 C 0.9848(5) -0.0663(4) 0.6164(4) 0.0396(11) Uani 1 1 d . . .
H10 H 0.9048 -0.0906 0.6339 0.048 Uiso 1 1 calc R . .
C11 C 1.0928(5) -0.1025(4) 0.6837(4) 0.0460(12) Uani 1 1 d . . .
H11 H 1.0874 -0.1501 0.7491 0.055 Uiso 1 1 calc R . .
C12 C 1.2079(5) -0.0695(4) 0.6559(5) 0.0450(12) Uani 1 1 d . . .
H12 H 1.2826 -0.0964 0.7003 0.054 Uiso 1 1 calc R . .
C13 C 1.2171(4) 0.0024(3) 0.5641(4) 0.0382(10) Uani 1 1 d . . .
H13 H 1.2979 0.0240 0.5457 0.046 Uiso 1 1 calc R . .
C14 C 1.1696(5) -0.0192(3) 0.0915(4) 0.0386(10) Uani 1 1 d . . .
H14 H 1.0945 -0.0445 0.0363 0.046 Uiso 1 1 calc R . .
C15 C 1.2797(5) -0.0202(4) 0.0150(5) 0.0555(15) Uani 1 1 d . . .
H15A H 1.2629 0.0273 -0.0548 0.083 Uiso 1 1 calc R . .
H15B H 1.2909 -0.0893 -0.0166 0.083 Uiso 1 1 calc R . .
H15C H 1.3566 0.0008 0.0670 0.083 Uiso 1 1 calc R . .
C16 C 1.1902(5) -0.0928(4) 0.1994(5) 0.0523(14) Uani 1 1 d . . .
H16A H 1.1174 -0.0907 0.2467 0.079 Uiso 1 1 calc R . .
H16B H 1.2665 -0.0733 0.2533 0.079 Uiso 1 1 calc R . .
H16C H 1.2003 -0.1622 0.1680 0.079 Uiso 1 1 calc R . .
C17 C 1.1194(4) 0.1910(3) 0.0115(4) 0.0356(10) Uani 1 1 d . . .
H17 H 1.2061 0.1951 -0.0148 0.043 Uiso 1 1 calc R . .
C18 C 1.0315(5) 0.1520(4) -0.0989(4) 0.0501(13) Uani 1 1 d . . .
H18A H 1.0576 0.0832 -0.1210 0.075 Uiso 1 1 calc R . .
H18B H 1.0353 0.1980 -0.1696 0.075 Uiso 1 1 calc R . .
H18C H 0.9449 0.1497 -0.0771 0.075 Uiso 1 1 calc R . .
C19 C 1.0829(6) 0.2978(4) 0.0490(5) 0.0553(14) Uani 1 1 d . . .
H19A H 1.1417 0.3211 0.1194 0.083 Uiso 1 1 calc R . .
H19B H 0.9970 0.2968 0.0728 0.083 Uiso 1 1 calc R . .
H19C H 1.0863 0.3446 -0.0211 0.083 Uiso 1 1 calc R . .
C20 C 0.7654(4) -0.0653(3) 0.3780(4) 0.0346(10) Uani 1 1 d . . .
H20 H 0.7500 -0.0966 0.4591 0.042 Uiso 1 1 calc R . .
C21 C 0.6375(5) -0.0389(4) 0.3081(5) 0.0466(12) Uani 1 1 d . . .
H21A H 0.5947 0.0112 0.3559 0.070 Uiso 1 1 calc R . .
H21B H 0.5860 -0.1009 0.2966 0.070 Uiso 1 1 calc R . .
H21C H 0.6495 -0.0101 0.2270 0.070 Uiso 1 1 calc R . .
C22 C 0.8368(5) -0.1432(3) 0.3085(5) 0.0418(11) Uani 1 1 d . . .
H22A H 0.9178 -0.1588 0.3570 0.063 Uiso 1 1 calc R . .
H22B H 0.8518 -0.1151 0.2278 0.063 Uiso 1 1 calc R . .
H22C H 0.7868 -0.2059 0.2960 0.063 Uiso 1 1 calc R . .
C23 C 0.7667(4) 0.1340(3) 0.4959(4) 0.0373(10) Uani 1 1 d . . .
H23 H 0.6995 0.1631 0.4340 0.045 Uiso 1 1 calc R . .
C24 C 0.7015(5) 0.0822(5) 0.5970(5) 0.0598(16) Uani 1 1 d . . .
H24A H 0.6500 0.0253 0.5611 0.090 Uiso 1 1 calc R . .
H24B H 0.6474 0.1318 0.6333 0.090 Uiso 1 1 calc R . .
H24C H 0.7652 0.0563 0.6617 0.090 Uiso 1 1 calc R . .
C25 C 0.8445(5) 0.2224(4) 0.5533(5) 0.0458(12) Uani 1 1 d . . .
H25A H 0.8862 0.2571 0.4891 0.069 Uiso 1 1 calc R . .
H25B H 0.9083 0.1966 0.6179 0.069 Uiso 1 1 calc R . .
H25C H 0.7892 0.2708 0.5900 0.069 Uiso 1 1 calc R . .
C26 C 0.7501(4) 0.1464(3) 0.1102(4) 0.0335(9) Uani 1 1 d . . .
C27 C 0.6498(4) 0.1277(3) 0.0021(4) 0.0350(11) Uani 1 1 d . . .
C28 C 0.5704(5) 0.2076(4) -0.0360(5) 0.0516(14) Uani 1 1 d . . .
H28 H 0.5801 0.2719 0.0046 0.062 Uiso 1 1 calc R . .
C29 C 0.4768(5) 0.1938(6) -0.1333(6) 0.068(2) Uani 1 1 d . . .
H29 H 0.4229 0.2493 -0.1597 0.082 Uiso 1 1 calc R . .
C30 C 0.4605(5) 0.1026(8) -0.1917(4) 0.0713(18) Uani 1 1 d . . .
H30 H 0.3953 0.0939 -0.2582 0.086 Uiso 1 1 calc R . .
C31 C 0.5385(5) 0.0230(5) -0.1542(5) 0.0604(17) Uani 1 1 d . . .
H31 H 0.5274 -0.0411 -0.1949 0.073 Uiso 1 1 calc R . .
C32 C 0.6323(5) 0.0350(5) -0.0588(5) 0.0475(12) Uani 1 1 d . . .
H32 H 0.6862 -0.0209 -0.0338 0.057 Uiso 1 1 calc R . .
N1 N 0.8467(3) 0.0839(3) 0.1290(3) 0.0335(9) Uani 1 1 d . . .
Ni1 Ni 0.97640(4) 0.09938(4) 0.26332(4) 0.02690(12) Uani 1 1 d . . .
O1 O 0.7372(3) 0.2196(3) 0.1789(4) 0.0539(10) Uani 1 1 d . . .
P1 P 1.12764(9) 0.10699(11) 0.14802(9) 0.0285(2) Uani 1 1 d . . .
P2 P 0.86430(10) 0.04913(8) 0.41214(10) 0.0288(2) Uani 1 1 d . . .
H2 H 0.843(4) 0.042(4) 0.078(4) 0.033(14) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C8 1.511(6) . ?
C1 C2 1.513(6) . ?
C1 Ni1 1.973(4) . ?
C1 H1 1.0000 . ?
C2 C3 1.386(6) . ?
C2 C7 1.398(6) . ?
C3 C4 1.383(6) . ?
C3 P1 1.800(4) . ?
C4 C5 1.384(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.365(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.374(7) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.387(6) . ?
C8 C9 1.405(6) . ?
C9 C10 1.384(6) . ?
C9 P2 1.805(4) . ?
C10 C11 1.375(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.368(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(6) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C16 1.513(6) . ?
C14 C15 1.514(7) . ?
C14 P1 1.835(4) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.520(7) . ?
C17 C18 1.522(6) . ?
C17 P1 1.839(4) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.522(6) . ?
C20 C22 1.523(6) . ?
C20 P2 1.845(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.515(6) . ?
C23 C24 1.524(6) . ?
C23 P2 1.833(4) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 O1 1.232(5) . ?
C26 N1 1.313(6) . ?
C26 C27 1.515(6) . ?
C27 C28 1.380(7) . ?
C27 C32 1.383(7) . ?
C28 C29 1.379(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.354(11) . ?
C29 H29 0.9500 . ?
C30 C31 1.365(10) . ?
C30 H30 0.9500 . ?
C31 C32 1.365(7) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
N1 Ni1 1.902(3) . ?
N1 H2 0.78(5) . ?
Ni1 P1 2.1544(10) . ?
Ni1 P2 2.2165(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 C1 C2 115.5(3) . . ?
C8 C1 Ni1 110.3(3) . . ?
C2 C1 Ni1 116.7(3) . . ?
C8 C1 H1 104.2 . . ?
C2 C1 H1 104.2 . . ?
Ni1 C1 H1 104.2 . . ?
C3 C2 C7 117.4(4) . . ?
C3 C2 C1 119.6(4) . . ?
C7 C2 C1 122.8(4) . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 P1 127.3(4) . . ?
C2 C3 P1 111.4(3) . . ?
C3 C4 C5 119.7(5) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 120.0(5) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.3(5) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C2 121.3(5) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
C13 C8 C9 118.1(4) . . ?
C13 C8 C1 125.3(4) . . ?
C9 C8 C1 116.5(4) . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 P2 127.2(4) . . ?
C8 C9 P2 112.3(3) . . ?
C11 C10 C9 120.6(5) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 119.5(4) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 120.9(4) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C8 120.6(5) . . ?
C12 C13 H13 119.7 . . ?
C8 C13 H13 119.7 . . ?
C16 C14 C15 111.4(4) . . ?
C16 C14 P1 109.5(3) . . ?
C15 C14 P1 115.2(3) . . ?
C16 C14 H14 106.8 . . ?
C15 C14 H14 106.8 . . ?
P1 C14 H14 106.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C19 C17 C18 111.4(4) . . ?
C19 C17 P1 108.9(3) . . ?
C18 C17 P1 113.7(3) . . ?
C19 C17 H17 107.5 . . ?
C18 C17 H17 107.5 . . ?
P1 C17 H17 107.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C22 112.1(4) . . ?
C21 C20 P2 112.0(3) . . ?
C22 C20 P2 109.6(3) . . ?
C21 C20 H20 107.6 . . ?
C22 C20 H20 107.6 . . ?
P2 C20 H20 107.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C24 108.5(4) . . ?
C25 C23 P2 110.6(3) . . ?
C24 C23 P2 114.8(3) . . ?
C25 C23 H23 107.6 . . ?
C24 C23 H23 107.6 . . ?
P2 C23 H23 107.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O1 C26 N1 122.1(4) . . ?
O1 C26 C27 118.4(4) . . ?
N1 C26 C27 119.5(4) . . ?
C28 C27 C32 118.5(4) . . ?
C28 C27 C26 117.7(4) . . ?
C32 C27 C26 123.8(4) . . ?
C29 C28 C27 119.7(6) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C30 C29 C28 121.1(6) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C29 C30 C31 119.4(5) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
C32 C31 C30 120.5(6) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C27 120.7(6) . . ?
C31 C32 H32 119.7 . . ?
C27 C32 H32 119.7 . . ?
C26 N1 Ni1 122.8(3) . . ?
C26 N1 H2 111(3) . . ?
Ni1 N1 H2 126(4) . . ?
N1 Ni1 C1 175.38(18) . . ?
N1 Ni1 P1 95.01(11) . . ?
C1 Ni1 P1 85.77(12) . . ?
N1 Ni1 P2 96.94(11) . . ?
C1 Ni1 P2 83.62(12) . . ?
P1 Ni1 P2 159.94(5) . . ?
C3 P1 C14 107.6(2) . . ?
C3 P1 C17 104.1(2) . . ?
C14 P1 C17 105.0(2) . . ?
C3 P1 Ni1 105.06(14) . . ?
C14 P1 Ni1 112.35(15) . . ?
C17 P1 Ni1 121.71(15) . . ?
C9 P2 C23 106.8(2) . . ?
C9 P2 C20 104.1(2) . . ?
C23 P2 C20 104.3(2) . . ?
C9 P2 Ni1 98.86(14) . . ?
C23 P2 Ni1 124.45(15) . . ?
C20 P2 Ni1 116.02(15) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.065
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1039464'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H43 N Ni O P2, 2(C7 H7 N O)'
_chemical_formula_sum            'C46 H57 N3 Ni O3 P2'
_chemical_formula_weight         820.60

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.0173(4)
_cell_length_b                   24.8752(7)
_cell_length_c                   17.1986(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.3580(10)
_cell_angle_gamma                90.00
_cell_volume                     4713.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    21795
_cell_measurement_theta_min      2.02
_cell_measurement_theta_max      26.00

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9500
_exptl_absorpt_correction_T_max  0.9846
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' ω and φ '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21795
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0532
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         26.00
_reflns_number_total             9009
_reflns_number_gt                7090
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0325P)²+9.3774P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9009
_refine_ls_number_parameters     520
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.1549
_refine_ls_wR_factor_gt          0.1458
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_restrained_S_all      1.168
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8901(4) 0.21581(17) 0.0654(3) 0.0382(9) Uani 1 1 d . . .
C2 C 0.9605(4) 0.17129(17) 0.1042(2) 0.0458(11) Uani 1 1 d . . .
C3 C 1.0857(5) 0.17795(18) 0.1155(2) 0.0476(11) Uani 1 1 d . . .
C4 C 1.1537(6) 0.1400(2) 0.1575(3) 0.0684(16) Uani 1 1 d . . .
H4 H 1.2381 0.1458 0.1657 0.082 Uiso 1 1 calc R . .
C5 C 1.1003(7) 0.0950(2) 0.1869(4) 0.0824(19) Uani 1 1 d . . .
H5 H 1.1471 0.0692 0.2147 0.099 Uiso 1 1 calc R . .
C6 C 0.9774(7) 0.0873(2) 0.1757(3) 0.0719(18) Uani 1 1 d . . .
H6 H 0.9399 0.0560 0.1961 0.086 Uiso 1 1 calc R . .
C7 C 0.9077(5) 0.12459(19) 0.1353(3) 0.0582(14) Uani 1 1 d . . .
H7 H 0.8232 0.1185 0.1285 0.070 Uiso 1 1 calc R . .
C8 C 0.8066(4) 0.20074(17) -0.0009(3) 0.0428(10) Uani 1 1 d . . .
C9 C 0.7473(4) 0.24209(18) -0.0394(3) 0.0448(11) Uani 1 1 d . . .
C10 C 0.6611(4) 0.2314(2) -0.0970(3) 0.0604(14) Uani 1 1 d . . .
H10 H 0.6176 0.2603 -0.1202 0.072 Uiso 1 1 calc R . .
C11 C 0.6385(5) 0.1799(2) -0.1206(4) 0.0701(16) Uani 1 1 d . . .
H11 H 0.5792 0.1728 -0.1595 0.084 Uiso 1 1 calc R . .
C12 C 0.7026(5) 0.1388(2) -0.0871(3) 0.0698(16) Uani 1 1 d . . .
H12 H 0.6902 0.1030 -0.1048 0.084 Uiso 1 1 calc R . .
C13 C 0.7857(5) 0.1486(2) -0.0276(3) 0.0573(13) Uani 1 1 d . . .
H13 H 0.8288 0.1194 -0.0048 0.069 Uiso 1 1 calc R . .
C14 C 1.2524(4) 0.2650(2) 0.1446(3) 0.0614(14) Uani 1 1 d . . .
H14 H 1.3155 0.2366 0.1524 0.074 Uiso 1 1 calc R . .
C15 C 1.3164(5) 0.3156(3) 0.1138(5) 0.104(3) Uani 1 1 d . . .
H15A H 1.3538 0.3076 0.0635 0.157 Uiso 1 1 calc R . .
H15B H 1.3793 0.3269 0.1509 0.157 Uiso 1 1 calc R . .
H15C H 1.2570 0.3446 0.1073 0.157 Uiso 1 1 calc R . .
C16 C 1.1943(5) 0.2760(2) 0.2231(3) 0.0743(17) Uani 1 1 d . . .
H16A H 1.1552 0.2431 0.2421 0.111 Uiso 1 1 calc R . .
H16B H 1.1335 0.3045 0.2175 0.111 Uiso 1 1 calc R . .
H16C H 1.2569 0.2874 0.2604 0.111 Uiso 1 1 calc R . .
C17 C 1.2258(5) 0.2192(2) -0.0124(3) 0.0716(18) Uani 1 1 d . . .
H17 H 1.2522 0.2531 -0.0386 0.086 Uiso 1 1 calc R . .
C18 C 1.3410(6) 0.1867(3) 0.0051(4) 0.112(3) Uani 1 1 d . . .
H18A H 1.3939 0.2073 0.0402 0.168 Uiso 1 1 calc R . .
H18B H 1.3839 0.1794 -0.0435 0.168 Uiso 1 1 calc R . .
H18C H 1.3189 0.1526 0.0298 0.168 Uiso 1 1 calc R . .
C19 C 1.1402(7) 0.1904(3) -0.0685(3) 0.091(2) Uani 1 1 d . . .
H19A H 1.0686 0.2129 -0.0781 0.137 Uiso 1 1 calc R . .
H19B H 1.1148 0.1561 -0.0458 0.137 Uiso 1 1 calc R . .
H19C H 1.1820 0.1837 -0.1177 0.137 Uiso 1 1 calc R . .
C20 C 0.6956(4) 0.34910(17) 0.0311(3) 0.0425(10) Uani 1 1 d . . .
H20 H 0.7355 0.3835 0.0471 0.051 Uiso 1 1 calc R . .
C21 C 0.5848(4) 0.3636(2) -0.0188(3) 0.0557(13) Uani 1 1 d . . .
H21A H 0.6114 0.3824 -0.0659 0.084 Uiso 1 1 calc R . .
H21B H 0.5307 0.3871 0.0108 0.084 Uiso 1 1 calc R . .
H21C H 0.5414 0.3307 -0.0335 0.084 Uiso 1 1 calc R . .
C22 C 0.6562(4) 0.32030(19) 0.1048(3) 0.0484(11) Uani 1 1 d . . .
H22A H 0.7279 0.3117 0.1364 0.073 Uiso 1 1 calc R . .
H22B H 0.6137 0.2870 0.0909 0.073 Uiso 1 1 calc R . .
H22C H 0.6018 0.3436 0.1345 0.073 Uiso 1 1 calc R . .
C23 C 0.8266(4) 0.33760(18) -0.1164(2) 0.0422(10) Uani 1 1 d . . .
H23 H 0.7456 0.3352 -0.1427 0.051 Uiso 1 1 calc R . .
C24 C 0.8625(5) 0.39693(19) -0.1140(3) 0.0520(12) Uani 1 1 d . . .
H24A H 0.8034 0.4170 -0.0830 0.078 Uiso 1 1 calc R . .
H24B H 0.8638 0.4113 -0.1670 0.078 Uiso 1 1 calc R . .
H24C H 0.9433 0.4005 -0.0904 0.078 Uiso 1 1 calc R . .
C25 C 0.9160(4) 0.30483(19) -0.1647(2) 0.0480(11) Uani 1 1 d . . .
H25A H 0.8906 0.2671 -0.1654 0.072 Uiso 1 1 calc R . .
H25B H 0.9974 0.3076 -0.1418 0.072 Uiso 1 1 calc R . .
H25C H 0.9172 0.3187 -0.2180 0.072 Uiso 1 1 calc R . .
C26 C 1.0657(3) 0.39645(15) 0.0389(2) 0.0292(8) Uani 1 1 d . . .
C27 C 0.9821(3) 0.41024(16) 0.1045(2) 0.0313(8) Uani 1 1 d . . .
C28 C 0.9483(4) 0.37229(17) 0.1598(2) 0.0369(9) Uani 1 1 d . . .
H28 H 0.9756 0.3362 0.1550 0.044 Uiso 1 1 calc R . .
C29 C 0.8758(4) 0.38658(19) 0.2213(2) 0.0445(11) Uani 1 1 d . . .
H29 H 0.8552 0.3606 0.2596 0.053 Uiso 1 1 calc R . .
C30 C 0.8331(4) 0.4383(2) 0.2275(3) 0.0502(12) Uani 1 1 d . . .
H30 H 0.7827 0.4482 0.2698 0.060 Uiso 1 1 calc R . .
C31 C 0.8636(4) 0.47580(19) 0.1722(3) 0.0475(11) Uani 1 1 d . . .
H31 H 0.8324 0.5113 0.1757 0.057 Uiso 1 1 calc R . .
C32 C 0.9392(4) 0.46220(16) 0.1115(2) 0.0392(10) Uani 1 1 d . . .
H32 H 0.9617 0.4887 0.0745 0.047 Uiso 1 1 calc R . .
C33 C 1.3138(4) 0.36427(17) -0.1404(2) 0.0379(9) Uani 1 1 d . . .
C34 C 1.4129(4) 0.3558(2) -0.1987(3) 0.0458(11) Uani 1 1 d . . .
C35 C 1.4740(5) 0.3975(3) -0.2333(3) 0.0765(18) Uani 1 1 d . . .
H35 H 1.4553 0.4337 -0.2203 0.092 Uiso 1 1 calc R . .
C36 C 1.5635(7) 0.3862(3) -0.2876(5) 0.119(3) Uani 1 1 d . . .
H36 H 1.6066 0.4148 -0.3117 0.143 Uiso 1 1 calc R . .
C37 C 1.5899(6) 0.3337(3) -0.3067(4) 0.104(3) Uani 1 1 d . . .
H37 H 1.6494 0.3263 -0.3449 0.125 Uiso 1 1 calc R . .
C38 C 1.5316(4) 0.2923(3) -0.2713(3) 0.0700(17) Uani 1 1 d . . .
H38 H 1.5515 0.2562 -0.2836 0.084 Uiso 1 1 calc R . .
C39 C 1.4429(4) 0.3036(2) -0.2170(3) 0.0516(12) Uani 1 1 d . . .
H39 H 1.4020 0.2748 -0.1920 0.062 Uiso 1 1 calc R . .
C40 C 1.5779(4) 0.51656(17) -0.1072(3) 0.0412(10) Uani 1 1 d . . .
C41 C 1.6315(4) 0.53573(16) -0.1817(2) 0.0380(9) Uani 1 1 d . . .
C42 C 1.5559(4) 0.5537(2) -0.2400(3) 0.0522(12) Uani 1 1 d . . .
H42 H 1.4705 0.5535 -0.2325 0.063 Uiso 1 1 calc R . .
C43 C 1.6029(5) 0.5720(2) -0.3091(3) 0.0636(14) Uani 1 1 d . . .
H43 H 1.5501 0.5848 -0.3488 0.076 Uiso 1 1 calc R . .
C44 C 1.7276(5) 0.5715(2) -0.3205(3) 0.0588(13) Uani 1 1 d . . .
H44 H 1.7603 0.5839 -0.3683 0.071 Uiso 1 1 calc R . .
C45 C 1.8039(4) 0.55317(19) -0.2626(3) 0.0486(11) Uani 1 1 d . . .
H45 H 1.8892 0.5527 -0.2705 0.058 Uiso 1 1 calc R . .
C46 C 1.7567(4) 0.53545(17) -0.1934(3) 0.0415(10) Uani 1 1 d . . .
H46 H 1.8095 0.5229 -0.1535 0.050 Uiso 1 1 calc R . .
N1 N 1.0680(3) 0.34671(13) 0.0143(2) 0.0317(7) Uani 1 1 d . . .
N2 N 1.3008(3) 0.41292(16) -0.1102(2) 0.0423(9) Uani 1 1 d . . .
N3 N 1.6484(4) 0.51313(17) -0.0453(2) 0.0462(10) Uani 1 1 d . . .
Ni1 Ni 0.97985(4) 0.282834(19) 0.03960(3) 0.02986(14) Uani 1 1 d . . .
O1 O 1.1290(2) 0.43443(11) 0.01066(16) 0.0357(6) Uani 1 1 d . . .
O2 O 1.2473(3) 0.32655(12) -0.12295(17) 0.0462(7) Uani 1 1 d . . .
O3 O 1.4676(3) 0.50483(13) -0.10540(18) 0.0511(8) Uani 1 1 d . . .
P1 P 1.14028(10) 0.23925(5) 0.07436(7) 0.0409(3) Uani 1 1 d . . .
P2 P 0.81088(9) 0.30772(4) -0.01887(6) 0.0366(3) Uani 1 1 d . . .
H1 H 0.838(3) 0.2276(15) 0.104(2) 0.032(11) Uiso 1 1 d . . .
H2 H 1.117(3) 0.3466(15) -0.024(2) 0.025(10) Uiso 1 1 d . . .
H8A H 1.612(4) 0.5022(17) 0.003(2) 0.041(12) Uiso 1 1 d . . .
H2B H 1.351(4) 0.4361(16) -0.116(2) 0.027(11) Uiso 1 1 d . . .
H2A H 1.243(4) 0.4185(19) -0.072(3) 0.060(15) Uiso 1 1 d . . .
H8B H 1.713(4) 0.527(2) -0.042(3) 0.050(15) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.505(6) . ?
C1 C8 1.509(6) . ?
C1 Ni1 1.990(4) . ?
C1 H1 0.93(4) . ?
C2 C3 1.401(7) . ?
C2 C7 1.406(6) . ?
C3 C4 1.402(6) . ?
C3 P1 1.787(5) . ?
C4 C5 1.365(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(8) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.385(6) . ?
C8 C13 1.395(6) . ?
C9 C10 1.393(6) . ?
C9 P2 1.810(4) . ?
C10 C11 1.367(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.369(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.391(7) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C16 1.522(8) . ?
C14 C15 1.539(8) . ?
C14 P1 1.839(5) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.524(9) . ?
C17 C18 1.533(7) . ?
C17 P1 1.838(5) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.521(6) . ?
C20 C21 1.531(6) . ?
C20 P2 1.851(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.528(6) . ?
C23 C24 1.528(6) . ?
C23 P2 1.844(4) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 O1 1.272(4) . ?
C26 N1 1.308(5) . ?
C26 C27 1.501(5) . ?
C27 C32 1.382(5) . ?
C27 C28 1.393(5) . ?
C28 C29 1.377(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.375(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.376(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.381(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 O2 1.229(5) . ?
C33 N2 1.325(5) . ?
C33 C34 1.501(6) . ?
C34 C35 1.375(7) . ?
C34 C39 1.378(6) . ?
C35 C36 1.391(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.379(10) . ?
C36 H36 0.9500 . ?
C37 C38 1.358(9) . ?
C37 H37 0.9500 . ?
C38 C39 1.384(6) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 O3 1.250(5) . ?
C40 N3 1.317(6) . ?
C40 C41 1.493(6) . ?
C41 C42 1.374(6) . ?
C41 C46 1.395(6) . ?
C42 C43 1.376(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.390(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.377(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.374(6) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
N1 Ni1 1.914(3) . ?
N1 H2 0.86(4) . ?
N2 H2B 0.80(4) . ?
N2 H2A 0.93(5) . ?
N3 H8A 0.96(4) . ?
N3 H8B 0.80(5) . ?
Ni1 P1 2.1550(12) . ?
Ni1 P2 2.1992(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C8 117.5(4) . . ?
C2 C1 Ni1 117.4(3) . . ?
C8 C1 Ni1 109.9(3) . . ?
C2 C1 H1 103(2) . . ?
C8 C1 H1 104(2) . . ?
Ni1 C1 H1 102(2) . . ?
C3 C2 C7 117.0(4) . . ?
C3 C2 C1 118.6(4) . . ?
C7 C2 C1 124.2(5) . . ?
C2 C3 C4 120.9(5) . . ?
C2 C3 P1 112.3(3) . . ?
C4 C3 P1 126.7(4) . . ?
C5 C4 C3 120.9(6) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 119.1(6) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C5 C6 C7 121.1(5) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C6 C7 C2 120.9(6) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
C9 C8 C13 117.2(4) . . ?
C9 C8 C1 117.4(4) . . ?
C13 C8 C1 125.3(4) . . ?
C8 C9 C10 121.1(4) . . ?
C8 C9 P2 113.3(3) . . ?
C10 C9 P2 124.8(4) . . ?
C11 C10 C9 120.7(5) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C11 C12 119.0(5) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C11 C12 C13 120.9(5) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C8 120.8(5) . . ?
C12 C13 H13 119.6 . . ?
C8 C13 H13 119.6 . . ?
C16 C14 C15 110.8(5) . . ?
C16 C14 P1 111.2(3) . . ?
C15 C14 P1 111.5(4) . . ?
C16 C14 H14 107.7 . . ?
C15 C14 H14 107.7 . . ?
P1 C14 H14 107.7 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C19 C17 C18 112.6(5) . . ?
C19 C17 P1 108.8(4) . . ?
C18 C17 P1 114.4(4) . . ?
C19 C17 H17 106.9 . . ?
C18 C17 H17 106.9 . . ?
P1 C17 H17 106.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C20 C21 110.4(4) . . ?
C22 C20 P2 109.0(3) . . ?
C21 C20 P2 114.7(3) . . ?
C22 C20 H20 107.5 . . ?
C21 C20 H20 107.5 . . ?
P2 C20 H20 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C24 111.3(4) . . ?
C25 C23 P2 110.1(3) . . ?
C24 C23 P2 113.0(3) . . ?
C25 C23 H23 107.4 . . ?
C24 C23 H23 107.4 . . ?
P2 C23 H23 107.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O1 C26 N1 124.6(3) . . ?
O1 C26 C27 117.2(3) . . ?
N1 C26 C27 118.2(3) . . ?
C32 C27 C28 118.8(4) . . ?
C32 C27 C26 119.5(4) . . ?
C28 C27 C26 121.8(3) . . ?
C29 C28 C27 120.6(4) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C30 C29 C28 120.1(4) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C31 119.7(4) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C30 C31 C32 120.5(4) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C27 120.3(4) . . ?
C31 C32 H32 119.9 . . ?
C27 C32 H32 119.9 . . ?
O2 C33 N2 122.3(4) . . ?
O2 C33 C34 119.5(4) . . ?
N2 C33 C34 118.1(4) . . ?
C35 C34 C39 119.6(4) . . ?
C35 C34 C33 122.9(4) . . ?
C39 C34 C33 117.5(4) . . ?
C34 C35 C36 119.3(6) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
C37 C36 C35 120.2(6) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C38 C37 C36 120.7(6) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C37 C38 C39 119.2(6) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C34 C39 C38 121.1(5) . . ?
C34 C39 H39 119.5 . . ?
C38 C39 H39 119.5 . . ?
O3 C40 N3 122.3(4) . . ?
O3 C40 C41 119.0(4) . . ?
N3 C40 C41 118.6(4) . . ?
C42 C41 C46 119.4(4) . . ?
C42 C41 C40 119.3(4) . . ?
C46 C41 C40 121.3(4) . . ?
C41 C42 C43 120.5(4) . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
C42 C43 C44 119.9(5) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C45 C44 C43 119.9(5) . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
C46 C45 C44 120.0(4) . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C45 C46 C41 120.3(4) . . ?
C45 C46 H46 119.9 . . ?
C41 C46 H46 119.9 . . ?
C26 N1 Ni1 134.6(3) . . ?
C26 N1 H2 105(2) . . ?
Ni1 N1 H2 120(2) . . ?
C33 N2 H2B 122(3) . . ?
C33 N2 H2A 119(3) . . ?
H2B N2 H2A 117(4) . . ?
C40 N3 H8A 118(2) . . ?
C40 N3 H8B 123(3) . . ?
H8A N3 H8B 116(4) . . ?
N1 Ni1 C1 179.23(17) . . ?
N1 Ni1 P1 93.69(10) . . ?
C1 Ni1 P1 85.66(13) . . ?
N1 Ni1 P2 95.26(10) . . ?
C1 Ni1 P2 85.27(13) . . ?
P1 Ni1 P2 163.53(5) . . ?
C3 P1 C17 105.4(2) . . ?
C3 P1 C14 105.3(2) . . ?
C17 P1 C14 106.4(3) . . ?
C3 P1 Ni1 105.17(17) . . ?
C17 P1 Ni1 109.58(19) . . ?
C14 P1 Ni1 123.62(17) . . ?
C9 P2 C23 103.0(2) . . ?
C9 P2 C20 109.0(2) . . ?
C23 P2 C20 105.5(2) . . ?
C9 P2 Ni1 99.26(16) . . ?
C23 P2 Ni1 116.43(14) . . ?
C20 P2 Ni1 121.72(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H2 O2 0.86(4) 2.28(4) 3.129(4) 167(3) .
N2 H2A O1 0.93(5) 1.94(5) 2.870(5) 176(4) .
N2 H2B O3 0.80(4) 2.15(4) 2.934(5) 167(4) .
N3 H8B O1 0.80(5) 2.05(5) 2.837(5) 168(5) 3_865
N3 H8A O3 0.96(4) 1.99(4) 2.931(5) 169(4) 3_865

_diffrn_measured_fraction_theta_max 0.971
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.971
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.068

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.019 0.000 0.000 291 61 ' '
2 -0.034 0.500 0.500 291 61 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1039465'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H40 Ni O2 P2'
_chemical_formula_sum            'C27 H40 Ni O2 P2'
_chemical_formula_weight         517.24

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   9.2432(4)
_cell_length_b                   15.3651(5)
_cell_length_c                   9.4633(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.045(3)
_cell_angle_gamma                90.00
_cell_volume                     1309.32(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    10175
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      27.00

_exptl_crystal_description       'Triangular Prism'
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             552
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9655
_exptl_absorpt_correction_T_max  0.9825
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10175
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         27.00
_reflns_number_total             5636
_reflns_number_gt                4782
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0134P)²+3.2889P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(2)
_refine_ls_number_reflns         5636
_refine_ls_number_parameters     289
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1323
_refine_ls_wR_factor_gt          0.1196
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.161
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0233(6) 0.2966(3) 0.1876(6) 0.0259(12) Uani 1 1 d . . .
H1 H -0.0251 0.3296 0.0984 0.031 Uiso 1 1 calc R . .
C2 C 0.0096(6) 0.3563(3) 0.3087(6) 0.0278(12) Uani 1 1 d . . .
C3 C 0.1346(6) 0.3754(4) 0.4161(6) 0.0291(12) Uani 1 1 d . . .
C4 C 0.1256(7) 0.4274(4) 0.5345(7) 0.0361(14) Uani 1 1 d . . .
H4 H 0.2111 0.4374 0.6098 0.043 Uiso 1 1 calc R . .
C5 C -0.0092(8) 0.4643(4) 0.5409(7) 0.0407(15) Uani 1 1 d . . .
H5 H -0.0168 0.5001 0.6207 0.049 Uiso 1 1 calc R . .
C6 C -0.1315(7) 0.4489(4) 0.4320(7) 0.0377(14) Uani 1 1 d . . .
H6 H -0.2232 0.4761 0.4348 0.045 Uiso 1 1 calc R . .
C7 C -0.1237(7) 0.3948(4) 0.3187(7) 0.0388(15) Uani 1 1 d . . .
H7 H -0.2108 0.3835 0.2459 0.047 Uiso 1 1 calc R . .
C8 C -0.0666(6) 0.2130(4) 0.1765(6) 0.0284(12) Uani 1 1 d . . .
C9 C -0.0460(6) 0.1528(4) 0.0720(6) 0.0296(12) Uani 1 1 d . . .
C10 C -0.1322(7) 0.0775(4) 0.0480(6) 0.0346(13) Uani 1 1 d . . .
H10 H -0.1197 0.0379 -0.0255 0.041 Uiso 1 1 calc R . .
C11 C -0.2350(7) 0.0593(4) 0.1286(7) 0.0369(14) Uani 1 1 d . . .
H11 H -0.2943 0.0082 0.1113 0.044 Uiso 1 1 calc R . .
C12 C -0.2496(7) 0.1176(4) 0.2354(7) 0.0356(14) Uani 1 1 d . . .
H12 H -0.3187 0.1052 0.2934 0.043 Uiso 1 1 calc R . .
C13 C -0.1677(7) 0.1928(4) 0.2610(6) 0.0337(13) Uani 1 1 d . . .
H13 H -0.1799 0.2311 0.3363 0.040 Uiso 1 1 calc R . .
C14 C 0.4415(6) 0.4156(4) 0.3882(6) 0.0323(13) Uani 1 1 d . . .
H14 H 0.5300 0.3881 0.3620 0.039 Uiso 1 1 calc R . .
C15 C 0.4952(8) 0.4542(4) 0.5389(8) 0.0477(17) Uani 1 1 d . . .
H15A H 0.5311 0.4075 0.6086 0.072 Uiso 1 1 calc R . .
H15B H 0.4130 0.4848 0.5671 0.072 Uiso 1 1 calc R . .
H15C H 0.5762 0.4953 0.5382 0.072 Uiso 1 1 calc R . .
C16 C 0.3864(8) 0.4848(4) 0.2755(8) 0.0487(17) Uani 1 1 d . . .
H16A H 0.3540 0.4575 0.1800 0.073 Uiso 1 1 calc R . .
H16B H 0.4667 0.5260 0.2734 0.073 Uiso 1 1 calc R . .
H16C H 0.3026 0.5158 0.3001 0.073 Uiso 1 1 calc R . .
C17 C 0.3729(7) 0.2518(3) 0.5168(6) 0.0351(14) Uani 1 1 d . . .
H17 H 0.3817 0.2819 0.6121 0.042 Uiso 1 1 calc R . .
C18 C 0.2625(8) 0.1776(4) 0.5081(7) 0.0494(17) Uani 1 1 d . . .
H18A H 0.1660 0.2009 0.5159 0.074 Uiso 1 1 calc R . .
H18B H 0.2984 0.1366 0.5877 0.074 Uiso 1 1 calc R . .
H18C H 0.2520 0.1474 0.4152 0.074 Uiso 1 1 calc R . .
C19 C 0.5258(8) 0.2202(5) 0.5077(8) 0.0561(19) Uani 1 1 d . . .
H19A H 0.5932 0.2699 0.5146 0.084 Uiso 1 1 calc R . .
H19B H 0.5194 0.1903 0.4150 0.084 Uiso 1 1 calc R . .
H19C H 0.5635 0.1797 0.5876 0.084 Uiso 1 1 calc R . .
C20 C 0.0396(7) 0.2114(4) -0.1934(6) 0.0344(13) Uani 1 1 d . . .
H20 H 0.1277 0.2211 -0.2363 0.041 Uiso 1 1 calc R . .
C21 C -0.0423(8) 0.2972(4) -0.2011(7) 0.0530(19) Uani 1 1 d . . .
H21A H 0.0220 0.3406 -0.1420 0.079 Uiso 1 1 calc R . .
H21B H -0.1324 0.2895 -0.1643 0.079 Uiso 1 1 calc R . .
H21C H -0.0694 0.3171 -0.3021 0.079 Uiso 1 1 calc R . .
C22 C -0.0565(8) 0.1426(5) -0.2855(7) 0.0488(17) Uani 1 1 d . . .
H22A H -0.0012 0.0878 -0.2793 0.073 Uiso 1 1 calc R . .
H22B H -0.0832 0.1620 -0.3867 0.073 Uiso 1 1 calc R . .
H22C H -0.1470 0.1336 -0.2499 0.073 Uiso 1 1 calc R . .
C23 C 0.2046(7) 0.0736(4) -0.0092(6) 0.0370(14) Uani 1 1 d . . .
H23 H 0.1303 0.0314 -0.0638 0.044 Uiso 1 1 calc R . .
C24 C 0.3319(7) 0.0796(4) -0.0848(7) 0.0447(16) Uani 1 1 d . . .
H24A H 0.2950 0.1011 -0.1839 0.067 Uiso 1 1 calc R . .
H24B H 0.3760 0.0219 -0.0880 0.067 Uiso 1 1 calc R . .
H24C H 0.4072 0.1198 -0.0316 0.067 Uiso 1 1 calc R . .
C25 C 0.2605(9) 0.0391(4) 0.1432(7) 0.0489(18) Uani 1 1 d . . .
H25A H 0.1776 0.0349 0.1916 0.073 Uiso 1 1 calc R . .
H25B H 0.3359 0.0787 0.1977 0.073 Uiso 1 1 calc R . .
H25C H 0.3043 -0.0187 0.1389 0.073 Uiso 1 1 calc R . .
C26 C 0.4283(7) 0.3027(4) 0.0020(7) 0.0363(14) Uani 1 1 d . . .
C27 C 0.5747(7) 0.2911(5) -0.0425(7) 0.0456(17) Uani 1 1 d . . .
H27A H 0.6409 0.2545 0.0288 0.068 Uiso 1 1 calc R . .
H27B H 0.6209 0.3482 -0.0472 0.068 Uiso 1 1 calc R . .
H27C H 0.5569 0.2633 -0.1380 0.068 Uiso 1 1 calc R . .
O2 O 0.3299(5) 0.3458(3) -0.0739(6) 0.0635(16) Uani 1 1 d . . .
Ni1 Ni 0.22427(8) 0.27344(4) 0.16028(7) 0.02759(17) Uani 1 1 d . . .
O1 O 0.4188(4) 0.2650(3) 0.1198(4) 0.0352(9) Uani 1 1 d . . .
P1 P 0.29969(16) 0.33006(9) 0.37189(16) 0.0265(3) Uani 1 1 d . . .
P2 P 0.11040(17) 0.17935(9) -0.00362(16) 0.0295(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.496(7) . ?
C1 C8 1.521(7) . ?
C1 Ni1 1.965(5) . ?
C1 H1 1.0000 . ?
C2 C3 1.387(8) . ?
C2 C7 1.389(8) . ?
C3 C4 1.393(8) . ?
C3 P1 1.810(6) . ?
C4 C5 1.383(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.368(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.371(9) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.396(8) . ?
C8 C9 1.398(8) . ?
C9 C10 1.394(8) . ?
C9 P2 1.799(6) . ?
C10 C11 1.375(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.379(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.373(8) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C16 1.511(9) . ?
C14 C15 1.521(8) . ?
C14 P1 1.838(6) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.515(9) . ?
C17 C18 1.520(8) . ?
C17 P1 1.835(6) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.514(9) . ?
C20 C22 1.522(8) . ?
C20 P2 1.835(6) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.512(8) . ?
C23 C25 1.514(8) . ?
C23 P2 1.849(6) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 O2 1.219(7) . ?
C26 O1 1.277(7) . ?
C26 C27 1.516(8) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
Ni1 O1 1.926(4) . ?
Ni1 P1 2.1501(16) . ?
Ni1 P2 2.2061(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C8 115.6(5) . . ?
C2 C1 Ni1 117.3(4) . . ?
C8 C1 Ni1 110.9(3) . . ?
C2 C1 H1 103.7 . . ?
C8 C1 H1 103.7 . . ?
Ni1 C1 H1 103.7 . . ?
C3 C2 C7 117.7(5) . . ?
C3 C2 C1 119.4(5) . . ?
C7 C2 C1 122.9(5) . . ?
C2 C3 C4 121.3(5) . . ?
C2 C3 P1 110.8(4) . . ?
C4 C3 P1 127.8(5) . . ?
C5 C4 C3 119.2(6) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 119.7(6) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 120.9(6) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C6 C7 C2 121.0(6) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
C13 C8 C9 118.3(5) . . ?
C13 C8 C1 125.0(5) . . ?
C9 C8 C1 116.6(5) . . ?
C10 C9 C8 120.0(5) . . ?
C10 C9 P2 127.2(5) . . ?
C8 C9 P2 112.4(4) . . ?
C11 C10 C9 121.3(5) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 118.0(6) . . ?
C10 C11 H11 121.0 . . ?
C12 C11 H11 121.0 . . ?
C13 C12 C11 122.3(6) . . ?
C13 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
C12 C13 C8 120.0(6) . . ?
C12 C13 H13 120.0 . . ?
C8 C13 H13 120.0 . . ?
C16 C14 C15 111.9(5) . . ?
C16 C14 P1 108.9(4) . . ?
C15 C14 P1 115.7(4) . . ?
C16 C14 H14 106.6 . . ?
C15 C14 H14 106.6 . . ?
P1 C14 H14 106.6 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C19 C17 C18 112.3(6) . . ?
C19 C17 P1 111.0(4) . . ?
C18 C17 P1 108.7(4) . . ?
C19 C17 H17 108.2 . . ?
C18 C17 H17 108.2 . . ?
P1 C17 H17 108.2 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C22 110.9(5) . . ?
C21 C20 P2 110.2(4) . . ?
C22 C20 P2 114.0(4) . . ?
C21 C20 H20 107.1 . . ?
C22 C20 H20 107.1 . . ?
P2 C20 H20 107.1 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C25 109.7(6) . . ?
C24 C23 P2 112.4(5) . . ?
C25 C23 P2 110.0(4) . . ?
C24 C23 H23 108.2 . . ?
C25 C23 H23 108.2 . . ?
P2 C23 H23 108.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O2 C26 O1 124.8(6) . . ?
O2 C26 C27 119.6(6) . . ?
O1 C26 C27 115.5(5) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O1 Ni1 C1 172.5(2) . . ?
O1 Ni1 P1 95.25(12) . . ?
C1 Ni1 P1 85.50(16) . . ?
O1 Ni1 P2 97.75(14) . . ?
C1 Ni1 P2 84.03(16) . . ?
P1 Ni1 P2 157.36(6) . . ?
C26 O1 Ni1 113.2(4) . . ?
C3 P1 C17 105.5(3) . . ?
C3 P1 C14 109.1(3) . . ?
C17 P1 C14 105.7(3) . . ?
C3 P1 Ni1 105.0(2) . . ?
C17 P1 Ni1 114.74(19) . . ?
C14 P1 Ni1 116.29(19) . . ?
C9 P2 C20 108.0(3) . . ?
C9 P2 C23 103.8(3) . . ?
C20 P2 C23 105.9(3) . . ?
C9 P2 Ni1 99.66(19) . . ?
C20 P2 Ni1 121.4(2) . . ?
C23 P2 Ni1 116.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.090
####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1039466'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H37 N Ni P2'
_chemical_formula_sum            'C26 H37 N Ni P2'
_chemical_formula_weight         484.22

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   11.1512(6)
_cell_length_b                   13.4171(5)
_cell_length_c                   17.6730(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.081(3)
_cell_angle_gamma                90.00
_cell_volume                     2483.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7770
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      25.00

_exptl_crystal_description       Plates
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    0.923
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9298
_exptl_absorpt_correction_T_max  0.9818
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' ω and φ '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7770
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4271
_reflns_number_gt                3574
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0336P)²+8.9007P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4271
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.1422
_refine_ls_wR_factor_gt          0.1308
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3685(4) 0.2091(4) 0.9385(3) 0.0360(11) Uani 1 1 d . . .
H1 H 0.3980 0.1483 0.9725 0.043 Uiso 1 1 calc R . .
C2 C 0.2429(5) 0.2360(4) 0.9486(3) 0.0354(11) Uani 1 1 d . . .
C3 C 0.1394(4) 0.1721(4) 0.9110(3) 0.0341(11) Uani 1 1 d . . .
C4 C 0.0238(5) 0.1855(4) 0.9217(3) 0.0436(12) Uani 1 1 d . . .
H4 H -0.0441 0.1399 0.8983 0.052 Uiso 1 1 calc R . .
C5 C 0.0063(5) 0.2654(4) 0.9665(3) 0.0479(13) Uani 1 1 d . . .
H5 H -0.0740 0.2755 0.9730 0.057 Uiso 1 1 calc R . .
C6 C 0.1050(5) 0.3295(4) 1.0012(3) 0.0470(13) Uani 1 1 d . . .
H6 H 0.0928 0.3847 1.0315 0.056 Uiso 1 1 calc R . .
C7 C 0.2217(5) 0.3152(4) 0.9929(3) 0.0401(12) Uani 1 1 d . . .
H7 H 0.2893 0.3605 1.0179 0.048 Uiso 1 1 calc R . .
C8 C 0.4754(5) 0.2830(4) 0.9718(3) 0.0372(11) Uani 1 1 d . . .
C9 C 0.5329(4) 0.3246(3) 0.9211(3) 0.0329(10) Uani 1 1 d . . .
C10 C 0.6311(5) 0.3935(4) 0.9498(3) 0.0388(12) Uani 1 1 d . . .
H10 H 0.6676 0.4239 0.9142 0.047 Uiso 1 1 calc R . .
C11 C 0.6746(5) 0.4171(4) 1.0303(3) 0.0466(13) Uani 1 1 d . . .
H11 H 0.7430 0.4630 1.0507 0.056 Uiso 1 1 calc R . .
C12 C 0.6206(5) 0.3753(4) 1.0813(3) 0.0503(14) Uani 1 1 d . . .
H12 H 0.6519 0.3919 1.1369 0.060 Uiso 1 1 calc R . .
C13 C 0.5216(5) 0.3098(4) 1.0527(3) 0.0492(14) Uani 1 1 d . . .
H13 H 0.4837 0.2821 1.0885 0.059 Uiso 1 1 calc R . .
C14 C 0.0256(4) 0.0835(4) 0.7537(3) 0.0369(11) Uani 1 1 d . . .
H14 H -0.0469 0.0712 0.7736 0.044 Uiso 1 1 calc R . .
C15 C 0.0039(5) 0.1839(4) 0.7113(3) 0.0478(14) Uani 1 1 d . . .
H15A H 0.0023 0.2364 0.7495 0.072 Uiso 1 1 calc R . .
H15B H -0.0779 0.1830 0.6666 0.072 Uiso 1 1 calc R . .
H15C H 0.0731 0.1972 0.6904 0.072 Uiso 1 1 calc R . .
C16 C 0.0265(5) -0.0003(4) 0.6956(3) 0.0436(13) Uani 1 1 d . . .
H16A H 0.0392 -0.0643 0.7241 0.065 Uiso 1 1 calc R . .
H16B H 0.0961 0.0107 0.6746 0.065 Uiso 1 1 calc R . .
H16C H -0.0552 -0.0013 0.6509 0.065 Uiso 1 1 calc R . .
C17 C 0.1894(5) -0.0404(4) 0.8838(3) 0.0428(12) Uani 1 1 d . . .
H17 H 0.1906 -0.0870 0.8399 0.051 Uiso 1 1 calc R . .
C18 C 0.0797(6) -0.0711(5) 0.9093(4) 0.0637(17) Uani 1 1 d . . .
H18A H -0.0005 -0.0628 0.8640 0.096 Uiso 1 1 calc R . .
H18B H 0.0780 -0.0295 0.9545 0.096 Uiso 1 1 calc R . .
H18C H 0.0897 -0.1411 0.9260 0.096 Uiso 1 1 calc R . .
C19 C 0.3165(6) -0.0522(5) 0.9517(4) 0.0608(16) Uani 1 1 d . . .
H19A H 0.3859 -0.0322 0.9328 0.091 Uiso 1 1 calc R . .
H19B H 0.3281 -0.1221 0.9689 0.091 Uiso 1 1 calc R . .
H19C H 0.3176 -0.0101 0.9972 0.091 Uiso 1 1 calc R . .
C20 C 0.3872(5) 0.3830(4) 0.7583(3) 0.0362(11) Uani 1 1 d . . .
H20 H 0.4478 0.4406 0.7711 0.043 Uiso 1 1 calc R . .
C21 C 0.3465(6) 0.3616(4) 0.6682(3) 0.0488(14) Uani 1 1 d . . .
H21A H 0.4219 0.3453 0.6541 0.073 Uiso 1 1 calc R . .
H21B H 0.3043 0.4205 0.6379 0.073 Uiso 1 1 calc R . .
H21C H 0.2871 0.3051 0.6548 0.073 Uiso 1 1 calc R . .
C22 C 0.2729(5) 0.4100(4) 0.7825(3) 0.0440(13) Uani 1 1 d . . .
H22A H 0.3017 0.4239 0.8405 0.066 Uiso 1 1 calc R . .
H22B H 0.2124 0.3542 0.7701 0.066 Uiso 1 1 calc R . .
H22C H 0.2308 0.4692 0.7526 0.066 Uiso 1 1 calc R . .
C23 C 0.5937(4) 0.2353(4) 0.7843(3) 0.0350(11) Uani 1 1 d . . .
H23 H 0.5506 0.2073 0.7292 0.042 Uiso 1 1 calc R . .
C24 C 0.6857(5) 0.3150(4) 0.7756(4) 0.0475(14) Uani 1 1 d . . .
H24A H 0.6372 0.3692 0.7415 0.071 Uiso 1 1 calc R . .
H24B H 0.7437 0.2856 0.7508 0.071 Uiso 1 1 calc R . .
H24C H 0.7353 0.3414 0.8289 0.071 Uiso 1 1 calc R . .
C25 C 0.6639(5) 0.1497(4) 0.8360(3) 0.0478(13) Uani 1 1 d . . .
H25A H 0.6022 0.0998 0.8401 0.072 Uiso 1 1 calc R . .
H25B H 0.7132 0.1744 0.8899 0.072 Uiso 1 1 calc R . .
H25C H 0.7218 0.1193 0.8116 0.072 Uiso 1 1 calc R . .
C26 C 0.3277(4) 0.1054(3) 0.7276(3) 0.0332(11) Uani 1 1 d . . .
N1 N 0.3302(4) 0.0698(3) 0.6719(3) 0.0448(11) Uani 1 1 d . . .
Ni1 Ni 0.33642(5) 0.16245(5) 0.82703(3) 0.03169(19) Uani 1 1 d . . .
P1 P 0.17365(11) 0.08721(9) 0.84160(7) 0.0315(3) Uani 1 1 d . . .
P2 P 0.46639(11) 0.27640(9) 0.82007(7) 0.0303(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C8 1.506(6) . ?
C1 C2 1.515(7) . ?
C1 Ni1 1.979(5) . ?
C1 H1 1.0000 . ?
C2 C7 1.388(7) . ?
C2 C3 1.407(6) . ?
C3 C4 1.378(7) . ?
C3 P1 1.808(5) . ?
C4 C5 1.386(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.366(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.373(7) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.385(6) . ?
C8 C13 1.390(7) . ?
C9 C10 1.389(6) . ?
C9 P2 1.803(5) . ?
C10 C11 1.374(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.365(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.365(7) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.521(7) . ?
C14 C16 1.526(7) . ?
C14 P1 1.838(5) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.500(7) . ?
C17 C19 1.518(7) . ?
C17 P1 1.852(5) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.522(7) . ?
C20 C21 1.525(7) . ?
C20 P2 1.832(5) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.508(7) . ?
C23 C24 1.526(7) . ?
C23 P2 1.826(5) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 N1 1.104(6) . ?
C26 Ni1 1.888(5) . ?
Ni1 P2 2.1390(13) . ?
Ni1 P1 2.1681(13) . ?

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
C8 C1 C2 115.9(4) . . ?
C8 C1 Ni1 116.4(3) . . ?
C2 C1 Ni1 109.5(3) . . ?
C8 C1 H1 104.5 . . ?
C2 C1 H1 104.5 . . ?
Ni1 C1 H1 104.5 . . ?
C7 C2 C3 117.5(5) . . ?
C7 C2 C1 126.3(4) . . ?
C3 C2 C1 116.2(4) . . ?
C4 C3 C2 120.7(5) . . ?
C4 C3 P1 126.9(4) . . ?
C2 C3 P1 112.0(3) . . ?
C3 C4 C5 120.1(5) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 119.6(5) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 120.7(5) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C6 C7 C2 121.3(5) . . ?
C6 C7 H7 119.4 . . ?
C2 C7 H7 119.4 . . ?
C9 C8 C13 118.1(4) . . ?
C9 C8 C1 119.5(4) . . ?
C13 C8 C1 122.4(4) . . ?
C8 C9 C10 121.0(4) . . ?
C8 C9 P2 111.8(3) . . ?
C10 C9 P2 127.2(4) . . ?
C11 C10 C9 119.0(5) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C12 C11 C10 120.7(5) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 120.3(5) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C12 C13 C8 121.0(5) . . ?
C12 C13 H13 119.5 . . ?
C8 C13 H13 119.5 . . ?
C15 C14 C16 111.0(4) . . ?
C15 C14 P1 109.7(3) . . ?
C16 C14 P1 112.1(3) . . ?
C15 C14 H14 107.9 . . ?
C16 C14 H14 107.9 . . ?
P1 C14 H14 107.9 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C19 111.8(5) . . ?
C18 C17 P1 113.6(4) . . ?
C19 C17 P1 110.4(4) . . ?
C18 C17 H17 106.9 . . ?
C19 C17 H17 106.9 . . ?
P1 C17 H17 106.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C20 C21 111.1(4) . . ?
C22 C20 P2 107.3(3) . . ?
C21 C20 P2 112.6(3) . . ?
C22 C20 H20 108.6 . . ?
C21 C20 H20 108.6 . . ?
P2 C20 H20 108.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C24 111.6(4) . . ?
C25 C23 P2 108.9(3) . . ?
C24 C23 P2 116.9(3) . . ?
C25 C23 H23 106.2 . . ?
C24 C23 H23 106.2 . . ?
P2 C23 H23 106.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N1 C26 Ni1 175.5(5) . . ?
C26 Ni1 C1 171.3(2) . . ?
C26 Ni1 P2 93.19(14) . . ?
C1 Ni1 P2 86.36(14) . . ?
C26 Ni1 P1 98.28(14) . . ?
C1 Ni1 P1 84.36(14) . . ?
P2 Ni1 P1 161.99(5) . . ?
C3 P1 C14 104.6(2) . . ?
C3 P1 C17 108.8(2) . . ?
C14 P1 C17 104.4(2) . . ?
C3 P1 Ni1 99.63(16) . . ?
C14 P1 Ni1 117.26(17) . . ?
C17 P1 Ni1 120.71(18) . . ?
C9 P2 C23 110.3(2) . . ?
C9 P2 C20 105.1(2) . . ?
C23 P2 C20 107.6(2) . . ?
C9 P2 Ni1 104.83(16) . . ?
C23 P2 Ni1 115.26(16) . . ?
C20 P2 Ni1 113.27(17) . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.606
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.082
