# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
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data_E500
_database_code_depnum_ccdc_archive 'CCDC 1828489'
_audit_update_record             
;
2018-03-09 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H35 N4 Ni O6 P'
_chemical_formula_weight         505.19

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   15.0308(10)
_cell_length_b                   10.8450(7)
_cell_length_c                   14.9367(10)
_cell_angle_alpha                90
_cell_angle_beta                 105.677(2)
_cell_angle_gamma                90
_cell_volume                     2344.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9900
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      28.32

_exptl_crystal_description       Plate
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_F_000             1072
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.937
_shelx_estimated_absorpt_T_min   0.706
_shelx_estimated_absorpt_T_max   0.880
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22665
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.347
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5813
_reflns_number_gt                4840
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0440P)²+3.2647P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5813
_refine_ls_number_parameters     288
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.1114
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.21845(2) 0.32515(3) 0.71984(2) 0.01558(10) Uani 1 1 d . . . . .
P1 P 0.24221(4) 0.52432(6) 0.72289(4) 0.01537(14) Uani 1 1 d . . . . .
O1 O 0.10649(13) 0.34183(18) 0.75297(13) 0.0237(4) Uani 1 1 d . . . . .
O2 O 0.16399(15) 0.2805(2) 0.89631(14) 0.0318(5) Uani 1 1 d . . . . .
O3 O 0.02085(15) 0.3424(2) 0.84756(17) 0.0371(5) Uani 1 1 d . . . . .
O4 O 0.41739(15) 0.7262(2) 0.57507(15) 0.0319(5) Uani 1 1 d . . . . .
O5 O 0.50574(16) 0.8867(2) 0.59757(17) 0.0397(6) Uani 1 1 d . . . . .
O6 O 0.40438(16) 0.8649(2) 0.67455(16) 0.0406(6) Uani 1 1 d . . . . .
N1 N 0.21072(15) 0.1422(2) 0.70413(15) 0.0204(5) Uani 1 1 d . . . . .
N2 N 0.31881(15) 0.3147(2) 0.66900(14) 0.0182(4) Uani 1 1 d . . . . .
N3 N 0.09738(16) 0.3203(2) 0.83543(17) 0.0242(5) Uani 1 1 d . . . . .
N4 N 0.44319(15) 0.8260(2) 0.61648(15) 0.0225(5) Uani 1 1 d . . . . .
C1 C 0.2631(2) 0.1077(3) 0.6369(2) 0.0263(6) Uani 1 1 d . . . . .
H1A H 0.2197 0.0965 0.5745 0.032 Uiso 1 1 calc R U . . .
H1B H 0.2952 0.0284 0.6559 0.032 Uiso 1 1 calc R U . . .
C2 C 0.33222(19) 0.2042(3) 0.63210(18) 0.0226(6) Uani 1 1 d . . . . .
C3 C 0.40112(19) 0.1875(3) 0.5878(2) 0.0278(6) Uani 1 1 d . . . . .
H3 H 0.4114 0.1086 0.5648 0.033 Uiso 1 1 calc R U . . .
C4 C 0.45445(19) 0.2866(3) 0.5773(2) 0.0303(7) Uani 1 1 d . . . . .
H4 H 0.4999 0.2776 0.5442 0.036 Uiso 1 1 calc R U . . .
C5 C 0.44176(19) 0.3991(3) 0.61501(19) 0.0269(6) Uani 1 1 d . . . . .
H5 H 0.4786 0.4679 0.6084 0.032 Uiso 1 1 calc R U . . .
C6 C 0.37443(17) 0.4113(3) 0.66306(17) 0.0190(5) Uani 1 1 d . . . . .
C7 C 0.35968(17) 0.5268(3) 0.71049(18) 0.0194(5) Uani 1 1 d . . . . .
H7A H 0.3682 0.5992 0.6733 0.023 Uiso 1 1 calc R U . . .
H7B H 0.4048 0.5323 0.7724 0.023 Uiso 1 1 calc R U . . .
C8 C 0.1127(2) 0.0933(3) 0.6693(2) 0.0274(6) Uani 1 1 d . . . . .
H8A H 0.1154 0.0044 0.6552 0.033 Uiso 1 1 calc R U . . .
H8B H 0.0817 0.1014 0.7196 0.033 Uiso 1 1 calc R U . . .
C9 C 0.0555(2) 0.1581(3) 0.5840(2) 0.0335(7) Uani 1 1 d . . . . .
H9A H 0.0417 0.2421 0.6004 0.050 Uiso 1 1 calc R U . . .
H9B H -0.0025 0.1130 0.5592 0.050 Uiso 1 1 calc R U . . .
H9C H 0.0898 0.1615 0.5368 0.050 Uiso 1 1 calc R U . . .
C10 C 0.2518(2) 0.0798(3) 0.7962(2) 0.0337(7) Uani 1 1 d . . . . .
H10A H 0.2502 -0.0106 0.7867 0.040 Uiso 1 1 calc R U . . .
H10B H 0.2134 0.0990 0.8388 0.040 Uiso 1 1 calc R U . . .
C11 C 0.3509(2) 0.1192(4) 0.8416(2) 0.0452(9) Uani 1 1 d . . . . .
H11A H 0.3893 0.1008 0.7997 0.068 Uiso 1 1 calc R U . . .
H11B H 0.3746 0.0743 0.9001 0.068 Uiso 1 1 calc R U . . .
H11C H 0.3526 0.2080 0.8542 0.068 Uiso 1 1 calc R U . . .
C12 C 0.24792(18) 0.6118(2) 0.83153(17) 0.0188(5) Uani 1 1 d . . . . .
C13 C 0.29937(19) 0.5293(3) 0.91291(17) 0.0228(6) Uani 1 1 d . . . . .
H13A H 0.3038 0.5718 0.9718 0.034 Uiso 1 1 calc R U . . .
H13B H 0.3616 0.5118 0.9073 0.034 Uiso 1 1 calc R U . . .
H13C H 0.2655 0.4517 0.9114 0.034 Uiso 1 1 calc R U . . .
C14 C 0.1518(2) 0.6412(3) 0.8418(2) 0.0282(6) Uani 1 1 d . . . . .
H14A H 0.1162 0.5647 0.8378 0.042 Uiso 1 1 calc R U . . .
H14B H 0.1201 0.6973 0.7919 0.042 Uiso 1 1 calc R U . . .
H14C H 0.1575 0.6804 0.9022 0.042 Uiso 1 1 calc R U . . .
C15 C 0.3035(2) 0.7316(3) 0.8355(2) 0.0287(6) Uani 1 1 d . . . . .
H15A H 0.2708 0.7870 0.7856 0.043 Uiso 1 1 calc R U . . .
H15B H 0.3646 0.7124 0.8275 0.043 Uiso 1 1 calc R U . . .
H15C H 0.3106 0.7718 0.8958 0.043 Uiso 1 1 calc R U . . .
C16 C 0.16606(19) 0.5968(2) 0.61611(17) 0.0205(5) Uani 1 1 d . . . . .
C17 C 0.06484(19) 0.5672(3) 0.61085(19) 0.0257(6) Uani 1 1 d . . . . .
H17A H 0.0495 0.6008 0.6657 0.039 Uiso 1 1 calc R U . . .
H17B H 0.0560 0.4776 0.6089 0.039 Uiso 1 1 calc R U . . .
H17C H 0.0245 0.6043 0.5546 0.039 Uiso 1 1 calc R U . . .
C18 C 0.1792(2) 0.7364(3) 0.6136(2) 0.0267(6) Uani 1 1 d . . . . .
H18A H 0.1421 0.7689 0.5540 0.040 Uiso 1 1 calc R U . . .
H18B H 0.2446 0.7549 0.6207 0.040 Uiso 1 1 calc R U . . .
H18C H 0.1595 0.7748 0.6644 0.040 Uiso 1 1 calc R U . . .
C19 C 0.1903(2) 0.5392(3) 0.53151(18) 0.0286(6) Uani 1 1 d . . . . .
H19A H 0.1464 0.5682 0.4743 0.043 Uiso 1 1 calc R U . . .
H19B H 0.1870 0.4492 0.5350 0.043 Uiso 1 1 calc R U . . .
H19C H 0.2530 0.5637 0.5314 0.043 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.867(2) . ?
Ni1 O1 1.8866(18) . ?
Ni1 N1 1.998(2) . ?
Ni1 P1 2.1878(7) . ?
P1 C7 1.825(3) . ?
P1 C12 1.862(3) . ?
P1 C16 1.867(3) . ?
O1 N3 1.297(3) . ?
O2 N3 1.234(3) . ?
O3 N3 1.235(3) . ?
O4 N4 1.255(3) . ?
O5 N4 1.241(3) . ?
O6 N4 1.243(3) . ?
N1 C1 1.482(3) . ?
N1 C10 1.508(4) . ?
N1 C8 1.519(4) . ?
N2 C2 1.357(3) . ?
N2 C6 1.358(3) . ?
C1 C2 1.490(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.384(4) . ?
C3 C4 1.375(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.396(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.485(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.505(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.522(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.527(4) . ?
C12 C15 1.537(4) . ?
C12 C13 1.539(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C18 1.528(4) . ?
C16 C17 1.536(4) . ?
C16 C19 1.539(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 O1 171.37(9) . . ?
N2 Ni1 N1 85.40(9) . . ?
O1 Ni1 N1 95.65(9) . . ?
N2 Ni1 P1 85.57(7) . . ?
O1 Ni1 P1 92.98(6) . . ?
N1 Ni1 P1 170.76(7) . . ?
C7 P1 C12 105.25(12) . . ?
C7 P1 C16 107.09(12) . . ?
C12 P1 C16 113.78(12) . . ?
C7 P1 Ni1 99.74(9) . . ?
C12 P1 Ni1 119.35(9) . . ?
C16 P1 Ni1 109.82(9) . . ?
N3 O1 Ni1 124.23(17) . . ?
C1 N1 C10 110.1(2) . . ?
C1 N1 C8 108.9(2) . . ?
C10 N1 C8 106.0(2) . . ?
C1 N1 Ni1 107.77(17) . . ?
C10 N1 Ni1 110.01(17) . . ?
C8 N1 Ni1 114.01(17) . . ?
C2 N2 C6 119.5(2) . . ?
C2 N2 Ni1 116.35(19) . . ?
C6 N2 Ni1 124.02(18) . . ?
O2 N3 O3 124.2(2) . . ?
O2 N3 O1 119.3(2) . . ?
O3 N3 O1 116.5(2) . . ?
O5 N4 O6 120.4(3) . . ?
O5 N4 O4 119.8(2) . . ?
O6 N4 O4 119.7(2) . . ?
N1 C1 C2 111.1(2) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C3 121.5(3) . . ?
N2 C2 C1 114.8(2) . . ?
C3 C2 C1 123.5(3) . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
N2 C6 C5 120.3(2) . . ?
N2 C6 C7 116.5(2) . . ?
C5 C6 C7 123.2(3) . . ?
C6 C7 P1 108.03(18) . . ?
C6 C7 H7A 110.1 . . ?
P1 C7 H7A 110.1 . . ?
C6 C7 H7B 110.1 . . ?
P1 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
C9 C8 N1 114.0(2) . . ?
C9 C8 H8A 108.7 . . ?
N1 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
N1 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C11 113.0(3) . . ?
N1 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
N1 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C15 109.8(2) . . ?
C14 C12 C13 109.2(2) . . ?
C15 C12 C13 108.0(2) . . ?
C14 C12 P1 111.81(18) . . ?
C15 C12 P1 111.14(18) . . ?
C13 C12 P1 106.68(18) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C16 C17 109.8(2) . . ?
C18 C16 C19 108.7(2) . . ?
C17 C16 C19 108.9(2) . . ?
C18 C16 P1 112.62(19) . . ?
C17 C16 P1 109.01(18) . . ?
C19 C16 P1 107.70(18) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_refine_diff_density_max         1.202
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.095

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_E559
_database_code_depnum_ccdc_archive 'CCDC 1828491'
_audit_update_record             
;
2018-03-09 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H51 N2 Ni O4 P S2'
_chemical_formula_weight         693.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4946(6)
_cell_length_b                   14.6252(9)
_cell_length_c                   24.2697(14)
_cell_angle_alpha                77.195(2)
_cell_angle_beta                 86.842(2)
_cell_angle_gamma                70.793(2)
_cell_volume                     3429.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9980
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      26.21

_exptl_crystal_description       Block
_exptl_crystal_colour            Dark_Green
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_F_000             1480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    0.773
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sadabs, (Sheldrick 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60257
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.055
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15675
_reflns_number_gt                9666
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0838P)²+7.5208P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         15675
_refine_ls_number_parameters     880
_refine_ls_number_restraints     298
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0750
_refine_ls_wR_factor_ref         0.1977
_refine_ls_wR_factor_gt          0.1742
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.80144(5) 0.16710(4) 0.83870(2) 0.02540(15) Uani 1 1 d . . . . .
Ni2 Ni 0.75684(5) 0.76153(4) 0.64557(3) 0.03210(17) Uani 1 1 d . . . . .
P1 P 1.01251(10) 0.14986(8) 0.85475(4) 0.0255(3) Uani 1 1 d . . . . .
P2 P 0.53735(11) 0.80219(8) 0.64249(5) 0.0314(3) Uani 1 1 d . . . . .
S1 S 0.80873(11) 0.05001(9) 0.91381(5) 0.0333(3) Uani 1 1 d . . . . .
S2 S 0.75068(13) 0.88820(10) 0.57651(6) 0.0452(3) Uani 1 1 d . . . . .
S3 S 0.26400(14) 0.32708(10) 0.65773(6) 0.0471(3) Uani 1 1 d . . . . .
N1 N 0.6070(4) 0.2018(3) 0.81472(16) 0.0364(9) Uani 1 1 d . . . . .
N2 N 0.8046(3) 0.2741(3) 0.77789(14) 0.0271(8) Uani 1 1 d . . . . .
N3 N 0.9590(4) 0.7120(3) 0.65969(18) 0.0393(10) Uani 1 1 d . . . . .
N4 N 0.7525(4) 0.6667(3) 0.71260(17) 0.0337(9) Uani 1 1 d . . . . .
C1 C 0.5667(5) 0.3023(4) 0.7750(2) 0.0455(13) Uani 1 1 d . . . . .
H1A H 0.5098 0.3020 0.7439 0.055 Uiso 1 1 calc R U . . .
H1B H 0.5122 0.3529 0.7956 0.055 Uiso 1 1 calc R U . . .
C2 C 0.6855(4) 0.3294(3) 0.75085(18) 0.0303(10) Uani 1 1 d . . . . .
C3 C 0.6757(4) 0.4067(3) 0.70506(19) 0.0357(11) Uani 1 1 d . . . . .
H3 H 0.5914 0.4430 0.6862 0.043 Uiso 1 1 calc R U . . .
C4 C 0.7900(5) 0.4304(3) 0.6871(2) 0.0371(11) Uani 1 1 d . . . . .
H4 H 0.7855 0.4839 0.6560 0.045 Uiso 1 1 calc R U . . .
C5 C 0.9124(4) 0.3748(3) 0.71527(19) 0.0347(11) Uani 1 1 d . . . . .
H5 H 0.9921 0.3904 0.7037 0.042 Uiso 1 1 calc R U . . .
C6 C 0.9168(4) 0.2973(3) 0.75986(17) 0.0271(9) Uani 1 1 d . . . . .
C7 C 1.0465(4) 0.2304(3) 0.78981(18) 0.0334(11) Uani 1 1 d . . . . .
H7A H 1.0976 0.2709 0.7995 0.040 Uiso 1 1 calc R U . . .
H7B H 1.1024 0.1890 0.7645 0.040 Uiso 1 1 calc R U . . .
C8 C 0.5932(6) 0.1268(5) 0.7840(3) 0.0560(15) Uani 1 1 d . . . . .
H8A H 0.5027 0.1517 0.7657 0.067 Uiso 1 1 calc R U . . .
H8B H 0.6004 0.0643 0.8116 0.067 Uiso 1 1 calc R U . . .
C9 C 0.6995(6) 0.1055(5) 0.7395(3) 0.0652(17) Uani 1 1 d . . . . .
H9A H 0.6889 0.1661 0.7105 0.098 Uiso 1 1 calc R U . . .
H9B H 0.6890 0.0540 0.7220 0.098 Uiso 1 1 calc R U . . .
H9C H 0.7895 0.0826 0.7572 0.098 Uiso 1 1 calc R U . . .
C10 C 0.5073(5) 0.2064(4) 0.8615(2) 0.0439(13) Uani 1 1 d . . . . .
H10A H 0.4151 0.2318 0.8448 0.053 Uiso 1 1 calc R U . . .
H10B H 0.5215 0.1384 0.8840 0.053 Uiso 1 1 calc R U . . .
C11 C 0.5173(6) 0.2706(4) 0.9001(2) 0.0612(17) Uani 1 1 d . . . . .
H11A H 0.6089 0.2468 0.9164 0.092 Uiso 1 1 calc R U . . .
H11B H 0.4524 0.2680 0.9306 0.092 Uiso 1 1 calc R U . . .
H11C H 0.4971 0.3392 0.8788 0.092 Uiso 1 1 calc R U . . .
C12 C 1.1482(4) 0.0279(3) 0.85566(19) 0.0316(10) Uani 1 1 d . . . . .
C13 C 1.0998(5) -0.0190(4) 0.8135(2) 0.0428(12) Uani 1 1 d . . . . .
H13A H 1.1692 -0.0816 0.8104 0.064 Uiso 1 1 calc R U . . .
H13B H 1.0831 0.0265 0.7764 0.064 Uiso 1 1 calc R U . . .
H13C H 1.0162 -0.0318 0.8269 0.064 Uiso 1 1 calc R U . . .
C14 C 1.1677(5) -0.0424(3) 0.91423(19) 0.0387(12) Uani 1 1 d . . . . .
H14A H 1.2326 -0.1071 0.9118 0.058 Uiso 1 1 calc R U . . .
H14B H 1.0811 -0.0503 0.9271 0.058 Uiso 1 1 calc R U . . .
H14C H 1.2020 -0.0145 0.9411 0.058 Uiso 1 1 calc R U . . .
C15 C 1.2844(4) 0.0407(4) 0.8362(2) 0.0386(12) Uani 1 1 d . . . . .
H15A H 1.3151 0.0720 0.8622 0.058 Uiso 1 1 calc R U . . .
H15B H 1.2739 0.0825 0.7981 0.058 Uiso 1 1 calc R U . . .
H15C H 1.3511 -0.0245 0.8360 0.058 Uiso 1 1 calc R U . . .
C16 C 1.0315(4) 0.2095(3) 0.91301(18) 0.0291(10) Uani 1 1 d . . . . .
C17 C 0.9840(5) 0.1611(3) 0.96973(18) 0.0324(10) Uani 1 1 d . . . . .
H17A H 1.0394 0.0911 0.9803 0.049 Uiso 1 1 calc R U . . .
H17B H 0.8893 0.1661 0.9660 0.049 Uiso 1 1 calc R U . . .
H17C H 0.9930 0.1953 0.9990 0.049 Uiso 1 1 calc R U . . .
C18 C 1.1753(5) 0.2095(4) 0.9208(2) 0.0391(12) Uani 1 1 d . . . . .
H18A H 1.1758 0.2483 0.9489 0.059 Uiso 1 1 calc R U . . .
H18B H 1.2071 0.2391 0.8847 0.059 Uiso 1 1 calc R U . . .
H18C H 1.2351 0.1412 0.9338 0.059 Uiso 1 1 calc R U . . .
C19 C 0.9383(5) 0.3187(3) 0.8964(2) 0.0376(11) Uani 1 1 d . . . . .
H19A H 0.9388 0.3524 0.9271 0.056 Uiso 1 1 calc R U . . .
H19B H 0.8462 0.3205 0.8899 0.056 Uiso 1 1 calc R U . . .
H19C H 0.9711 0.3523 0.8619 0.056 Uiso 1 1 calc R U . . .
C20 C 0.7269(5) -0.0351(4) 0.9071(2) 0.0436(12) Uani 1 1 d . . . . .
C21 C 0.7672(9) -0.0985(6) 0.8703(3) 0.100(3) Uani 1 1 d . . . . .
H21 H 0.8370 -0.0935 0.8443 0.120 Uiso 1 1 calc R U . . .
C22 C 0.7054(12) -0.1705(7) 0.8711(4) 0.132(5) Uani 1 1 d . . . . .
H22 H 0.7324 -0.2120 0.8446 0.158 Uiso 1 1 calc R U . . .
C23 C 0.6083(9) -0.1831(6) 0.9085(3) 0.082(2) Uani 1 1 d . . . . .
C24 C 0.5684(6) -0.1206(4) 0.9447(3) 0.0549(15) Uani 1 1 d . . . . .
H24 H 0.4991 -0.1269 0.9707 0.066 Uiso 1 1 calc R U . . .
C25 C 0.6266(5) -0.0477(4) 0.9447(2) 0.0405(12) Uani 1 1 d . . . . .
H25 H 0.5970 -0.0058 0.9709 0.049 Uiso 1 1 calc R U . . .
C26 C 0.5457(11) -0.2633(7) 0.9104(4) 0.119(3) Uani 1 1 d . . . . .
H26A H 0.4848 -0.2646 0.9424 0.179 Uiso 1 1 calc R U . . .
H26B H 0.6170 -0.3278 0.9147 0.179 Uiso 1 1 calc R U . . .
H26C H 0.4947 -0.2496 0.8752 0.179 Uiso 1 1 calc R U . . .
C27 C 0.9926(5) 0.6292(4) 0.7115(2) 0.0460(13) Uani 1 1 d . . . . .
H27A H 1.0417 0.5659 0.7002 0.055 Uiso 1 1 calc R U . . .
H27B H 1.0529 0.6415 0.7369 0.055 Uiso 1 1 calc R U . . .
C28 C 0.8690(5) 0.6203(3) 0.7426(2) 0.0386(12) Uani 1 1 d . . . . .
C29 C 0.8737(5) 0.5652(4) 0.7972(2) 0.0521(15) Uani 1 1 d . . . . .
H29 H 0.9568 0.5343 0.8177 0.062 Uiso 1 1 calc R U . . .
C30 C 0.7544(5) 0.5562(4) 0.8210(3) 0.0561(17) Uani 1 1 d . . . . .
H30 H 0.7541 0.5208 0.8589 0.067 Uiso 1 1 calc R U . . .
C31 C 0.6354(5) 0.5989(4) 0.7894(2) 0.0521(15) Uani 1 1 d . . . . .
H31 H 0.5540 0.5901 0.8048 0.063 Uiso 1 1 calc R U . . .
C32 C 0.6356(4) 0.6541(3) 0.7354(2) 0.0375(12) Uani 1 1 d . . . . .
C33 C 0.5144(5) 0.6993(3) 0.6974(2) 0.0404(12) Uani 1 1 d . . . . .
H33A H 0.4334 0.7246 0.7195 0.048 Uiso 1 1 calc R U . . .
H33B H 0.5010 0.6486 0.6794 0.048 Uiso 1 1 calc R U . . .
C34 C 1.0342(5) 0.6747(4) 0.6106(2) 0.0443(13) Uani 1 1 d . . . . .
H34A H 1.1306 0.6413 0.6215 0.053 Uiso 1 1 calc R U . . .
H34B H 1.0281 0.7318 0.5789 0.053 Uiso 1 1 calc R U . . .
C35 C 0.9809(5) 0.6032(4) 0.5908(2) 0.0521(15) Uani 1 1 d . . . . .
H35A H 0.9930 0.5440 0.6210 0.078 Uiso 1 1 calc R U . . .
H35B H 1.0303 0.5840 0.5574 0.078 Uiso 1 1 calc R U . . .
H35C H 0.8847 0.6350 0.5810 0.078 Uiso 1 1 calc R U . . .
C36 C 1.0060(5) 0.7934(4) 0.6701(3) 0.0498(14) Uani 1 1 d . . . . .
H36A H 0.9961 0.8441 0.6346 0.060 Uiso 1 1 calc R U . . .
H36B H 1.1030 0.7655 0.6808 0.060 Uiso 1 1 calc R U . . .
C37 C 0.9294(6) 0.8424(5) 0.7157(3) 0.0649(17) Uani 1 1 d . . . . .
H37A H 0.8338 0.8733 0.7045 0.097 Uiso 1 1 calc R U . . .
H37B H 0.9661 0.8933 0.7214 0.097 Uiso 1 1 calc R U . . .
H37C H 0.9383 0.7926 0.7510 0.097 Uiso 1 1 calc R U . . .
C38 C 0.4599(5) 0.7918(3) 0.5774(2) 0.0380(11) Uani 1 1 d . . . . .
C39 C 0.5598(6) 0.7017(4) 0.5584(3) 0.0552(15) Uani 1 1 d . . . . .
H39A H 0.5220 0.6902 0.5256 0.083 Uiso 1 1 calc R U . . .
H39B H 0.5762 0.6431 0.5894 0.083 Uiso 1 1 calc R U . . .
H39C H 0.6451 0.7144 0.5482 0.083 Uiso 1 1 calc R U . . .
C40 C 0.4361(6) 0.8847(4) 0.5300(2) 0.0511(14) Uani 1 1 d . . . . .
H40A H 0.4041 0.8733 0.4958 0.077 Uiso 1 1 calc R U . . .
H40B H 0.5208 0.8994 0.5222 0.077 Uiso 1 1 calc R U . . .
H40C H 0.3681 0.9410 0.5416 0.077 Uiso 1 1 calc R U . . .
C41 C 0.3254(5) 0.7714(4) 0.5887(3) 0.0576(16) Uani 1 1 d . . . . .
H41A H 0.2601 0.8265 0.6023 0.086 Uiso 1 1 calc R U . . .
H41B H 0.3395 0.7098 0.6173 0.086 Uiso 1 1 calc R U . . .
H41C H 0.2908 0.7647 0.5536 0.086 Uiso 1 1 calc R U . . .
C42 C 0.4461(5) 0.9144(4) 0.6711(2) 0.0466(14) Uani 1 1 d . . . . .
C43 C 0.4692(7) 1.0073(4) 0.6351(3) 0.0655(19) Uani 1 1 d . . . . .
H43A H 0.4299 1.0209 0.5972 0.098 Uiso 1 1 calc R U . . .
H43B H 0.5663 0.9967 0.6322 0.098 Uiso 1 1 calc R U . . .
H43C H 0.4261 1.0638 0.6527 0.098 Uiso 1 1 calc R U . . .
C44 C 0.2939(5) 0.9312(4) 0.6753(3) 0.0543(15) Uani 1 1 d . . . . .
H44A H 0.2513 0.9856 0.6945 0.081 Uiso 1 1 calc R U . . .
H44B H 0.2788 0.8706 0.6967 0.081 Uiso 1 1 calc R U . . .
H44C H 0.2543 0.9482 0.6372 0.081 Uiso 1 1 calc R U . . .
C45 C 0.5050(6) 0.8946(4) 0.7313(3) 0.0596(16) Uani 1 1 d . . . . .
H45A H 0.6036 0.8755 0.7297 0.089 Uiso 1 1 calc R U . . .
H45B H 0.4793 0.8409 0.7559 0.089 Uiso 1 1 calc R U . . .
H45C H 0.4694 0.9549 0.7463 0.089 Uiso 1 1 calc R U . . .
C46 C 0.8418(6) 0.8672(5) 0.5150(3) 0.0628(17) Uani 1 1 d . . . . .
C47 C 0.8119(8) 0.8168(6) 0.4769(4) 0.085(2) Uani 1 1 d . . . . .
H47 H 0.7455 0.7850 0.4860 0.102 Uiso 1 1 calc R U . . .
C48 C 0.8760(9) 0.8134(7) 0.4280(3) 0.094(3) Uani 1 1 d . . . . .
H48 H 0.8526 0.7770 0.4045 0.113 Uiso 1 1 calc R U . . .
C49 C 0.9657(8) 0.8537(6) 0.4092(3) 0.086(2) Uani 1 1 d . . . . .
C50 C 1.0008(9) 0.9062(7) 0.4454(4) 0.106(3) Uani 1 1 d . . . . .
H50 H 1.0666 0.9379 0.4337 0.127 Uiso 1 1 calc R U . . .
C51 C 0.9391(9) 0.9122(8) 0.4986(4) 0.107(3) Uani 1 1 d . . . . .
H51 H 0.9645 0.9466 0.5227 0.128 Uiso 1 1 calc R U . . .
C52 C 1.0305(9) 0.8565(7) 0.3512(3) 0.129(4) Uani 1 1 d . . . . .
H52A H 1.1093 0.7968 0.3528 0.193 Uiso 1 1 calc R U . . .
H52B H 1.0589 0.9154 0.3404 0.193 Uiso 1 1 calc R U . . .
H52C H 0.9650 0.8590 0.3232 0.193 Uiso 1 1 calc R U . . .
C56 C 0.4100(5) 0.3399(4) 0.6195(2) 0.0373(11) Uani 1 1 d . . . . .
C57 C 0.4172(6) 0.4329(4) 0.5956(2) 0.0446(13) Uani 1 1 d . . . . .
H57 H 0.3436 0.4903 0.5989 0.054 Uiso 1 1 calc R U . . .
C58 C 0.5313(6) 0.4431(4) 0.5670(2) 0.0495(14) Uani 1 1 d . . . . .
H58 H 0.5349 0.5076 0.5509 0.059 Uiso 1 1 calc R U . . .
C59 C 0.6401(6) 0.3611(4) 0.5612(2) 0.0475(13) Uani 1 1 d . . . . .
C61 C 0.5160(5) 0.2567(4) 0.6134(2) 0.0446(12) Uani 1 1 d . . . . .
H61 H 0.5114 0.1924 0.6291 0.053 Uiso 1 1 calc R U . . .
C62 C 0.7651(7) 0.3728(6) 0.5310(3) 0.074(2) Uani 1 1 d . . . . .
H62A H 0.8309 0.3072 0.5310 0.111 Uiso 1 1 calc R U . . .
H62B H 0.7412 0.4093 0.4919 0.111 Uiso 1 1 calc R U . . .
H62C H 0.8045 0.4096 0.5503 0.111 Uiso 1 1 calc R U . . .
C60 C 0.6298(5) 0.2681(4) 0.5841(2) 0.0502(14) Uani 1 1 d . . . . .
H60 H 0.7021 0.2108 0.5797 0.060 Uiso 1 1 calc R U . . .
O1 O 0.2306(4) 0.4068(3) 0.68933(18) 0.0602(11) Uani 1 1 d . . . . .
O2 O 0.1680(11) 0.3589(11) 0.6159(6) 0.272(7) Uani 1 1 d . . . . .
O3 O 0.3067(4) 0.2286(3) 0.69377(19) 0.0629(11) Uani 1 1 d . . . . .
S1X S 0.2665(9) 0.6301(7) 0.8346(4) 0.0804(10) Uani 0.5 1 d . U P A -1
O1X O 0.3378(12) 0.5358(10) 0.8209(5) 0.0818(14) Uani 0.5 1 d . U P A -1
O2X O 0.1921(12) 0.7067(9) 0.7871(5) 0.0879(13) Uani 0.5 1 d . U P A -1
O3X O 0.3391(11) 0.6784(8) 0.8550(4) 0.0850(12) Uani 0.5 1 d . U P A -1
C1X C 0.1506(9) 0.6042(7) 0.8886(4) 0.0807(11) Uani 0.5 1 d G U P A -1
C2X C 0.1710(8) 0.5081(7) 0.9194(4) 0.0811(14) Uani 0.5 1 d G U P A -1
H2XA H 0.2462 0.4551 0.9118 0.097 Uiso 0.5 1 calc R U P A -1
C3X C 0.0815(10) 0.4897(6) 0.9614(4) 0.0809(15) Uani 0.5 1 d G U P A -1
H3XA H 0.0954 0.4240 0.9824 0.097 Uiso 0.5 1 calc R U P A -1
C4X C -0.0286(9) 0.5672(8) 0.9725(4) 0.0812(15) Uani 0.5 1 d G U P A -1
C5X C -0.0490(8) 0.6633(7) 0.9416(4) 0.0809(15) Uani 0.5 1 d G U P A -1
H5XA H -0.1242 0.7163 0.9492 0.097 Uiso 0.5 1 calc R U P A -1
C6X C 0.0406(10) 0.6817(6) 0.8997(4) 0.0817(13) Uani 0.5 1 d G U P A -1
H6XA H 0.0266 0.7474 0.8787 0.098 Uiso 0.5 1 calc R U P A -1
C7X C -0.1267(16) 0.5425(13) 1.0186(6) 0.083(2) Uani 0.5 1 d . U P A -1
H7XA H -0.1990 0.6035 1.0220 0.125 Uiso 0.5 1 calc R U P A -1
H7XB H -0.1656 0.4961 1.0082 0.125 Uiso 0.5 1 calc R U P A -1
H7XC H -0.0776 0.5121 1.0548 0.125 Uiso 0.5 1 calc R U P A -1
S1S S 0.2379(9) 0.6526(7) 0.8274(5) 0.0803(10) Uani 0.5 1 d . U P B -2
O1S O 0.0971(11) 0.6838(8) 0.8341(4) 0.0885(12) Uani 0.5 1 d . U P B -2
O2S O 0.2876(12) 0.5621(10) 0.8032(5) 0.0840(13) Uani 0.5 1 d . U P B -2
O3S O 0.2828(11) 0.7299(8) 0.7950(4) 0.0849(13) Uani 0.5 1 d . U P B -2
C1S C 0.3054(9) 0.6171(7) 0.8925(3) 0.0814(11) Uani 0.5 1 d G U P B -2
C2S C 0.4162(10) 0.5310(7) 0.9041(3) 0.0830(14) Uani 0.5 1 d G U P B -2
H2SA H 0.4518 0.4956 0.8753 0.100 Uiso 0.5 1 calc R U P B -2
C3S C 0.4748(9) 0.4968(7) 0.9580(4) 0.0833(16) Uani 0.5 1 d G U P B -2
H3SA H 0.5506 0.4380 0.9659 0.100 Uiso 0.5 1 calc R U P B -2
C4S C 0.4227(10) 0.5487(8) 1.0001(3) 0.0832(15) Uani 0.5 1 d G U P B -2
C5S C 0.3119(10) 0.6348(7) 0.9885(3) 0.0822(15) Uani 0.5 1 d G U P B -2
H5SA H 0.2762 0.6702 1.0173 0.099 Uiso 0.5 1 calc R U P B -2
C6S C 0.2532(8) 0.6690(6) 0.9347(4) 0.0814(14) Uani 0.5 1 d G U P B -2
H6SA H 0.1775 0.7278 0.9267 0.098 Uiso 0.5 1 calc R U P B -2
C7S C 0.4686(18) 0.5155(13) 1.0586(6) 0.091(2) Uani 0.5 1 d . U P B -2
H7SA H 0.4167 0.5645 1.0801 0.136 Uiso 0.5 1 calc R U P B -2
H7SB H 0.4556 0.4516 1.0745 0.136 Uiso 0.5 1 calc R U P B -2
H7SC H 0.5646 0.5081 1.0607 0.136 Uiso 0.5 1 calc R U P B -2
O1W O 0.3521(3) 0.5497(3) 0.69614(16) 0.0423(8) Uani 1 1 d D . . C -2
H1W H 0.315(5) 0.510(3) 0.690(2) 0.051 Uiso 1 1 d D U . D -2
H2W H 0.330(6) 0.565(4) 0.7270(13) 0.051 Uiso 1 1 d D U . E -2
O2W O 0.2008(4) 0.3983(3) 0.80596(18) 0.0533(10) Uani 1 1 d D . . F -2
H21W H 0.218(6) 0.388(5) 0.7730(13) 0.064 Uiso 1 1 d D U . G -2
H22W H 0.238(6) 0.435(4) 0.816(3) 0.064 Uiso 1 1 d D U . H -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.906(3) . ?
Ni1 N1 2.019(4) . ?
Ni1 P1 2.1923(12) . ?
Ni1 S1 2.1926(12) . ?
Ni2 N4 1.899(4) . ?
Ni2 N3 2.025(4) . ?
Ni2 P2 2.1825(12) . ?
Ni2 S2 2.1914(13) . ?
P1 C7 1.841(4) . ?
P1 C16 1.868(5) . ?
P1 C12 1.877(4) . ?
P2 C33 1.847(4) . ?
P2 C42 1.869(5) . ?
P2 C38 1.873(5) . ?
S1 C20 1.768(5) . ?
S2 C46 1.757(7) . ?
S3 O2 1.363(11) . ?
S3 O3 1.449(4) . ?
S3 O1 1.473(4) . ?
S3 C56 1.788(5) . ?
N1 C10 1.499(6) . ?
N1 C8 1.504(7) . ?
N1 C1 1.508(6) . ?
N2 C6 1.354(5) . ?
N2 C2 1.355(5) . ?
N3 C34 1.498(6) . ?
N3 C36 1.503(7) . ?
N3 C27 1.504(6) . ?
N4 C28 1.349(6) . ?
N4 C32 1.369(5) . ?
C1 C2 1.482(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.379(6) . ?
C3 C4 1.378(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.373(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.502(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.515(8) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.496(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C15 1.537(6) . ?
C12 C14 1.538(6) . ?
C12 C13 1.542(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C18 1.532(6) . ?
C16 C17 1.539(6) . ?
C16 C19 1.549(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
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 1.380(9) . ?
C20 C25 1.387(7) . ?
C21 C22 1.403(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.357(10) . ?
C22 H22 0.9500 . ?
C23 C24 1.359(9) . ?
C23 C26 1.513(9) . ?
C24 C25 1.393(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.493(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.384(7) . ?
C29 C30 1.384(7) . ?
C29 H29 0.9500 . ?
C30 C31 1.386(8) . ?
C30 H30 0.9500 . ?
C31 C32 1.378(7) . ?
C31 H31 0.9500 . ?
C32 C33 1.488(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.509(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.504(8) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C40 1.533(6) . ?
C38 C39 1.534(7) . ?
C38 C41 1.535(7) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.528(7) . ?
C42 C44 1.535(7) . ?
C42 C45 1.546(8) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
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 C51 1.385(10) . ?
C46 C47 1.409(10) . ?
C47 C48 1.334(10) . ?
C47 H47 0.9500 . ?
C48 C49 1.281(12) . ?
C48 H48 0.9500 . ?
C49 C50 1.420(12) . ?
C49 C52 1.527(11) . ?
C50 C51 1.421(11) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C56 C57 1.381(7) . ?
C56 C61 1.382(7) . ?
C57 C58 1.385(8) . ?
C57 H57 0.9500 . ?
C58 C59 1.384(8) . ?
C58 H58 0.9500 . ?
C59 C60 1.388(8) . ?
C59 C62 1.508(8) . ?
C61 C60 1.395(7) . ?
C61 H61 0.9500 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C60 H60 0.9500 . ?
S1X O3X 1.370(15) . ?
S1X O1X 1.439(14) . ?
S1X O2X 1.465(16) . ?
S1X C1X 1.802(13) . ?
C1X C2X 1.3900 . ?
C1X C6X 1.3900 . ?
C2X C3X 1.3900 . ?
C2X H2XA 0.9500 . ?
C3X C4X 1.3900 . ?
C3X H3XA 0.9500 . ?
C4X C5X 1.3900 . ?
C4X C7X 1.543(14) . ?
C5X C6X 1.3900 . ?
C5X H5XA 0.9500 . ?
C6X H6XA 0.9500 . ?
C7X H7XA 0.9800 . ?
C7X H7XB 0.9800 . ?
C7X H7XC 0.9800 . ?
S1S O1S 1.408(14) . ?
S1S O3S 1.427(14) . ?
S1S O2S 1.492(14) . ?
S1S C1S 1.668(13) . ?
C1S C2S 1.3900 . ?
C1S C6S 1.3900 . ?
C2S C3S 1.3900 . ?
C2S H2SA 0.9500 . ?
C3S C4S 1.3900 . ?
C3S H3SA 0.9500 . ?
C4S C5S 1.3900 . ?
C4S C7S 1.448(17) . ?
C5S C6S 1.3900 . ?
C5S H5SA 0.9500 . ?
C6S H6SA 0.9500 . ?
C7S H7SA 0.9800 . ?
C7S H7SB 0.9800 . ?
C7S H7SC 0.9800 . ?
O1W H1W 0.836(19) . ?
O1W H2W 0.829(19) . ?
O2W H21W 0.84(2) . ?
O2W H22W 0.84(2) . ?

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
N2 Ni1 N1 84.95(14) . . ?
N2 Ni1 P1 86.17(11) . . ?
N1 Ni1 P1 171.08(11) . . ?
N2 Ni1 S1 174.17(12) . . ?
N1 Ni1 S1 99.18(11) . . ?
P1 Ni1 S1 89.62(4) . . ?
N4 Ni2 N3 85.06(15) . . ?
N4 Ni2 P2 86.79(12) . . ?
N3 Ni2 P2 171.74(11) . . ?
N4 Ni2 S2 170.99(12) . . ?
N3 Ni2 S2 96.90(11) . . ?
P2 Ni2 S2 90.95(5) . . ?
C7 P1 C16 104.8(2) . . ?
C7 P1 C12 103.0(2) . . ?
C16 P1 C12 113.4(2) . . ?
C7 P1 Ni1 100.16(14) . . ?
C16 P1 Ni1 112.45(14) . . ?
C12 P1 Ni1 120.27(16) . . ?
C33 P2 C42 103.3(2) . . ?
C33 P2 C38 103.8(2) . . ?
C42 P2 C38 115.5(2) . . ?
C33 P2 Ni2 99.80(15) . . ?
C42 P2 Ni2 114.32(18) . . ?
C38 P2 Ni2 116.98(16) . . ?
C20 S1 Ni1 115.89(18) . . ?
C46 S2 Ni2 119.2(2) . . ?
O2 S3 O3 124.7(6) . . ?
O2 S3 O1 105.3(7) . . ?
O3 S3 O1 113.3(3) . . ?
O2 S3 C56 102.2(6) . . ?
O3 S3 C56 105.9(2) . . ?
O1 S3 C56 102.9(2) . . ?
C10 N1 C8 106.7(4) . . ?
C10 N1 C1 107.7(4) . . ?
C8 N1 C1 108.8(4) . . ?
C10 N1 Ni1 115.7(3) . . ?
C8 N1 Ni1 109.8(3) . . ?
C1 N1 Ni1 107.9(3) . . ?
C6 N2 C2 118.5(4) . . ?
C6 N2 Ni1 124.6(3) . . ?
C2 N2 Ni1 116.9(3) . . ?
C34 N3 C36 108.3(4) . . ?
C34 N3 C27 109.1(4) . . ?
C36 N3 C27 108.2(4) . . ?
C34 N3 Ni2 111.6(3) . . ?
C36 N3 Ni2 110.6(3) . . ?
C27 N3 Ni2 108.9(3) . . ?
C28 N4 C32 119.1(4) . . ?
C28 N4 Ni2 117.0(3) . . ?
C32 N4 Ni2 123.3(3) . . ?
C2 C1 N1 112.1(4) . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
N1 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
N2 C2 C3 122.2(4) . . ?
N2 C2 C1 115.1(4) . . ?
C3 C2 C1 122.7(4) . . ?
C4 C3 C2 119.0(4) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 119.0(4) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 119.5(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
N2 C6 C5 121.7(4) . . ?
N2 C6 C7 115.9(4) . . ?
C5 C6 C7 122.3(4) . . ?
C6 C7 P1 110.6(3) . . ?
C6 C7 H7A 109.5 . . ?
P1 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
P1 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N1 C8 C9 112.6(5) . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 N1 113.7(4) . . ?
C11 C10 H10A 108.8 . . ?
N1 C10 H10A 108.8 . . ?
C11 C10 H10B 108.8 . . ?
N1 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C15 C12 C14 109.0(4) . . ?
C15 C12 C13 108.8(4) . . ?
C14 C12 C13 108.7(4) . . ?
C15 C12 P1 112.3(3) . . ?
C14 C12 P1 112.4(3) . . ?
C13 C12 P1 105.5(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C16 C17 108.9(4) . . ?
C18 C16 C19 108.0(4) . . ?
C17 C16 C19 108.2(4) . . ?
C18 C16 P1 113.9(3) . . ?
C17 C16 P1 111.7(3) . . ?
C19 C16 P1 105.9(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C25 117.2(5) . . ?
C21 C20 S1 123.5(4) . . ?
C25 C20 S1 119.0(4) . . ?
C20 C21 C22 120.1(6) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C23 C22 C21 122.4(7) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C22 C23 C24 117.5(6) . . ?
C22 C23 C26 121.9(7) . . ?
C24 C23 C26 120.6(7) . . ?
C23 C24 C25 121.7(6) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C20 C25 C24 121.1(5) . . ?
C20 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 N3 111.9(4) . . ?
C28 C27 H27A 109.2 . . ?
N3 C27 H27A 109.2 . . ?
C28 C27 H27B 109.2 . . ?
N3 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
N4 C28 C29 122.3(4) . . ?
N4 C28 C27 114.9(4) . . ?
C29 C28 C27 122.8(4) . . ?
C28 C29 C30 118.4(5) . . ?
C28 C29 H29 120.8 . . ?
C30 C29 H29 120.8 . . ?
C29 C30 C31 119.6(5) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C32 C31 C30 119.8(5) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
N4 C32 C31 120.6(5) . . ?
N4 C32 C33 115.6(4) . . ?
C31 C32 C33 123.7(4) . . ?
C32 C33 P2 109.5(3) . . ?
C32 C33 H33A 109.8 . . ?
P2 C33 H33A 109.8 . . ?
C32 C33 H33B 109.8 . . ?
P2 C33 H33B 109.8 . . ?
H33A C33 H33B 108.2 . . ?
N3 C34 C35 112.9(4) . . ?
N3 C34 H34A 109.0 . . ?
C35 C34 H34A 109.0 . . ?
N3 C34 H34B 109.0 . . ?
C35 C34 H34B 109.0 . . ?
H34A C34 H34B 107.8 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N3 C36 C37 113.2(4) . . ?
N3 C36 H36A 108.9 . . ?
C37 C36 H36A 108.9 . . ?
N3 C36 H36B 108.9 . . ?
C37 C36 H36B 108.9 . . ?
H36A C36 H36B 107.8 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C40 C38 C39 110.1(4) . . ?
C40 C38 C41 108.1(4) . . ?
C39 C38 C41 107.3(4) . . ?
C40 C38 P2 112.5(4) . . ?
C39 C38 P2 105.8(4) . . ?
C41 C38 P2 112.9(4) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C44 109.3(4) . . ?
C43 C42 C45 109.4(5) . . ?
C44 C42 C45 108.7(4) . . ?
C43 C42 P2 111.3(3) . . ?
C44 C42 P2 111.9(4) . . ?
C45 C42 P2 106.2(4) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C51 C46 C47 116.4(7) . . ?
C51 C46 S2 118.9(6) . . ?
C47 C46 S2 124.2(5) . . ?
C48 C47 C46 120.6(8) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C49 C48 C47 127.1(9) . . ?
C49 C48 H48 116.4 . . ?
C47 C48 H48 116.4 . . ?
C48 C49 C50 115.5(8) . . ?
C48 C49 C52 126.8(10) . . ?
C50 C49 C52 117.6(9) . . ?
C49 C50 C51 121.1(8) . . ?
C49 C50 H50 119.5 . . ?
C51 C50 H50 119.5 . . ?
C46 C51 C50 119.3(9) . . ?
C46 C51 H51 120.3 . . ?
C50 C51 H51 120.3 . . ?
C49 C52 H52A 109.5 . . ?
C49 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C49 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C57 C56 C61 119.5(5) . . ?
C57 C56 S3 120.3(4) . . ?
C61 C56 S3 120.2(4) . . ?
C56 C57 C58 120.4(5) . . ?
C56 C57 H57 119.8 . . ?
C58 C57 H57 119.8 . . ?
C59 C58 C57 121.3(5) . . ?
C59 C58 H58 119.3 . . ?
C57 C58 H58 119.3 . . ?
C58 C59 C60 117.6(5) . . ?
C58 C59 C62 121.0(5) . . ?
C60 C59 C62 121.4(5) . . ?
C56 C61 C60 119.4(5) . . ?
C56 C61 H61 120.3 . . ?
C60 C61 H61 120.3 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C59 C60 C61 121.7(5) . . ?
C59 C60 H60 119.2 . . ?
C61 C60 H60 119.2 . . ?
O3X S1X O1X 118.4(8) . . ?
O3X S1X O2X 101.6(9) . . ?
O1X S1X O2X 114.6(9) . . ?
O3X S1X C1X 107.4(8) . . ?
O1X S1X C1X 104.7(7) . . ?
O2X S1X C1X 109.8(7) . . ?
C2X C1X C6X 120.0 . . ?
C2X C1X S1X 120.8(6) . . ?
C6X C1X S1X 119.2(6) . . ?
C1X C2X C3X 120.0 . . ?
C1X C2X H2XA 120.0 . . ?
C3X C2X H2XA 120.0 . . ?
C4X C3X C2X 120.0 . . ?
C4X C3X H3XA 120.0 . . ?
C2X C3X H3XA 120.0 . . ?
C3X C4X C5X 120.0 . . ?
C3X C4X C7X 118.0(8) . . ?
C5X C4X C7X 122.0(8) . . ?
C4X C5X C6X 120.0 . . ?
C4X C5X H5XA 120.0 . . ?
C6X C5X H5XA 120.0 . . ?
C5X C6X C1X 120.0 . . ?
C5X C6X H6XA 120.0 . . ?
C1X C6X H6XA 120.0 . . ?
C4X C7X H7XA 109.5 . . ?
C4X C7X H7XB 109.5 . . ?
H7XA C7X H7XB 109.5 . . ?
C4X C7X H7XC 109.5 . . ?
H7XA C7X H7XC 109.5 . . ?
H7XB C7X H7XC 109.5 . . ?
O1S S1S O3S 112.1(9) . . ?
O1S S1S O2S 112.5(9) . . ?
O3S S1S O2S 110.7(9) . . ?
O1S S1S C1S 106.1(8) . . ?
O3S S1S C1S 110.1(9) . . ?
O2S S1S C1S 105.0(7) . . ?
C2S C1S C6S 120.0 . . ?
C2S C1S S1S 117.5(7) . . ?
C6S C1S S1S 122.5(7) . . ?
C1S C2S C3S 120.0 . . ?
C1S C2S H2SA 120.0 . . ?
C3S C2S H2SA 120.0 . . ?
C4S C3S C2S 120.0 . . ?
C4S C3S H3SA 120.0 . . ?
C2S C3S H3SA 120.0 . . ?
C3S C4S C5S 120.0 . . ?
C3S C4S C7S 124.5(10) . . ?
C5S C4S C7S 115.3(10) . . ?
C6S C5S C4S 120.0 . . ?
C6S C5S H5SA 120.0 . . ?
C4S C5S H5SA 120.0 . . ?
C5S C6S C1S 120.0 . . ?
C5S C6S H6SA 120.0 . . ?
C1S C6S H6SA 120.0 . . ?
C4S C7S H7SA 109.5 . . ?
C4S C7S H7SB 109.5 . . ?
H7SA C7S H7SB 109.5 . . ?
C4S C7S H7SC 109.5 . . ?
H7SA C7S H7SC 109.5 . . ?
H7SB C7S H7SC 109.5 . . ?
H1W O1W H2W 111(6) . . ?
H21W O2W H22W 117(7) . . ?

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
O1W H1W O1 0.836(19) 1.99(2) 2.820(5) 171(5) .
O2W H21W O1 0.84(2) 1.99(3) 2.810(6) 163(6) .

_refine_diff_density_max         1.061
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.097

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_E423
_database_code_depnum_ccdc_archive 'CCDC 1828490'
_audit_update_record             
;
2018-03-09 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H37 Cl2 N2 Ni O P'
_chemical_formula_weight         470.08

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'
P P 0.1023 0.0942 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   31.456(5)
_cell_length_b                   10.5339(17)
_cell_length_c                   13.821(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4579.7(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      26.52

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      'Not Measured'
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_F_000             2000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.162
_shelx_estimated_absorpt_T_min   0.722
_shelx_estimated_absorpt_T_max   0.893
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'Sababs, (Sheldrick 2012)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Microfocusing Source'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62283
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.962
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11348
_reflns_number_gt                10708
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.921
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

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

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

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0333P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 4818 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.010(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         11348
_refine_ls_number_parameters     497
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0731
_refine_ls_wR_factor_gt          0.0717
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.58010(2) 0.41828(3) 0.47724(3) 0.00704(9) Uani 1 1 d . . . . .
Ni2 Ni 0.84621(2) 0.63902(3) 0.48321(3) 0.00796(9) Uani 1 1 d . . . . .
P1 P 0.55965(2) 0.61457(7) 0.49700(6) 0.00730(16) Uani 1 1 d . . . . .
P2 P 0.85924(2) 0.43626(7) 0.49260(6) 0.00771(15) Uani 1 1 d . . . . .
Cl1 Cl 0.52273(2) 0.36399(7) 0.40259(6) 0.01403(16) Uani 1 1 d . . . . .
Cl2 Cl 0.90243(2) 0.69072(7) 0.56312(6) 0.01385(16) Uani 1 1 d . . . . .
Cl3 Cl 0.74090(3) 0.11585(9) 0.39327(10) 0.0349(3) Uani 1 1 d . . . . .
Cl4 Cl 0.65296(3) 0.94732(8) 0.66543(6) 0.01922(18) Uani 1 1 d . . . . .
N1 N 0.60382(8) 0.2412(2) 0.4766(2) 0.0091(5) Uani 1 1 d . . . . .
N2 N 0.63007(8) 0.4645(2) 0.54204(19) 0.0080(5) Uani 1 1 d . . . . .
N3 N 0.82490(8) 0.8188(2) 0.4733(2) 0.0115(5) Uani 1 1 d . . . . .
N4 N 0.79653(8) 0.5942(2) 0.4167(2) 0.0092(5) Uani 1 1 d . . . . .
C1 C 0.64608(10) 0.2416(3) 0.5274(2) 0.0107(6) Uani 1 1 d . . . . .
H1A H 0.6458 0.1775 0.5798 0.013 Uiso 1 1 calc R U . . .
H1B H 0.6687 0.2177 0.4809 0.013 Uiso 1 1 calc R U . . .
C2 C 0.65594(10) 0.3692(3) 0.5693(2) 0.0099(6) Uani 1 1 d . . . . .
C3 C 0.68991(10) 0.3901(3) 0.6307(2) 0.0107(6) Uani 1 1 d . . . . .
H3 H 0.7077 0.3217 0.6497 0.013 Uiso 1 1 calc R U . . .
C4 C 0.69760(10) 0.5114(3) 0.6638(2) 0.0121(6) Uani 1 1 d . . . . .
H4 H 0.7202 0.5270 0.7077 0.015 Uiso 1 1 calc R U . . .
C5 C 0.67209(10) 0.6104(3) 0.6325(2) 0.0125(7) Uani 1 1 d . . . . .
H5 H 0.6775 0.6947 0.6536 0.015 Uiso 1 1 calc R U . . .
C6 C 0.63858(10) 0.5857(3) 0.5704(2) 0.0103(6) Uani 1 1 d . . . . .
C7 C 0.61071(10) 0.6858(3) 0.5298(2) 0.0112(6) Uani 1 1 d . . . . .
H7A H 0.6242 0.7238 0.4720 0.013 Uiso 1 1 calc R U . . .
H7B H 0.6063 0.7537 0.5783 0.013 Uiso 1 1 calc R U . . .
C8 C 0.60937(11) 0.1947(3) 0.3752(2) 0.0126(7) Uani 1 1 d . . . . .
H8A H 0.5810 0.1807 0.3460 0.015 Uiso 1 1 calc R U . . .
H8B H 0.6244 0.1122 0.3765 0.015 Uiso 1 1 calc R U . . .
C9 C 0.63415(12) 0.2865(3) 0.3127(3) 0.0184(8) Uani 1 1 d . . . . .
H9A H 0.6200 0.3694 0.3131 0.028 Uiso 1 1 calc R U . . .
H9B H 0.6354 0.2541 0.2463 0.028 Uiso 1 1 calc R U . . .
H9C H 0.6631 0.2953 0.3382 0.028 Uiso 1 1 calc R U . . .
C10 C 0.57469(10) 0.1493(3) 0.5270(3) 0.0116(7) Uani 1 1 d . . . . .
H10A H 0.5890 0.0657 0.5314 0.014 Uiso 1 1 calc R U . . .
H10B H 0.5487 0.1383 0.4876 0.014 Uiso 1 1 calc R U . . .
C11 C 0.56210(13) 0.1917(4) 0.6281(3) 0.0207(8) Uani 1 1 d . . . . .
H11A H 0.5877 0.2065 0.6667 0.031 Uiso 1 1 calc R U . . .
H11B H 0.5448 0.1255 0.6588 0.031 Uiso 1 1 calc R U . . .
H11C H 0.5456 0.2704 0.6239 0.031 Uiso 1 1 calc R U . . .
C12 C 0.52537(11) 0.6328(3) 0.6059(2) 0.0121(7) Uani 1 1 d . . . . .
C13 C 0.55089(11) 0.5760(3) 0.6903(2) 0.0166(7) Uani 1 1 d . . . . .
H13A H 0.5334 0.5767 0.7490 0.025 Uiso 1 1 calc R U . . .
H13B H 0.5766 0.6267 0.7010 0.025 Uiso 1 1 calc R U . . .
H13C H 0.5589 0.4885 0.6747 0.025 Uiso 1 1 calc R U . . .
C14 C 0.48387(11) 0.5576(3) 0.5954(3) 0.0157(7) Uani 1 1 d . . . . .
H14A H 0.4671 0.5656 0.6549 0.024 Uiso 1 1 calc R U . . .
H14B H 0.4905 0.4679 0.5839 0.024 Uiso 1 1 calc R U . . .
H14C H 0.4675 0.5911 0.5408 0.024 Uiso 1 1 calc R U . . .
C15 C 0.51520(12) 0.7725(3) 0.6294(3) 0.0178(7) Uani 1 1 d . . . . .
H15A H 0.4972 0.8081 0.5782 0.027 Uiso 1 1 calc R U . . .
H15B H 0.5417 0.8210 0.6335 0.027 Uiso 1 1 calc R U . . .
H15C H 0.5002 0.7772 0.6913 0.027 Uiso 1 1 calc R U . . .
C16 C 0.54137(11) 0.7079(3) 0.3897(2) 0.0111(6) Uani 1 1 d . . . . .
C17 C 0.56674(12) 0.6571(3) 0.3037(3) 0.0166(7) Uani 1 1 d . . . . .
H17A H 0.5597 0.5674 0.2934 0.025 Uiso 1 1 calc R U . . .
H17B H 0.5972 0.6654 0.3170 0.025 Uiso 1 1 calc R U . . .
H17C H 0.5595 0.7058 0.2456 0.025 Uiso 1 1 calc R U . . .
C18 C 0.55085(11) 0.8511(3) 0.4014(3) 0.0165(7) Uani 1 1 d . . . . .
H18A H 0.5425 0.8961 0.3423 0.025 Uiso 1 1 calc R U . . .
H18B H 0.5813 0.8633 0.4129 0.025 Uiso 1 1 calc R U . . .
H18C H 0.5347 0.8846 0.4564 0.025 Uiso 1 1 calc R U . . .
C19 C 0.49382(11) 0.6899(3) 0.3715(3) 0.0164(7) Uani 1 1 d . . . . .
H19A H 0.4862 0.7273 0.3090 0.025 Uiso 1 1 calc R U . . .
H19B H 0.4776 0.7318 0.4230 0.025 Uiso 1 1 calc R U . . .
H19C H 0.4871 0.5991 0.3710 0.025 Uiso 1 1 calc R U . . .
C20 C 0.78702(11) 0.8189(3) 0.4085(3) 0.0148(7) Uani 1 1 d . . . . .
H20A H 0.7653 0.8776 0.4346 0.018 Uiso 1 1 calc R U . . .
H20B H 0.7954 0.8494 0.3435 0.018 Uiso 1 1 calc R U . . .
C21 C 0.76866(10) 0.6894(3) 0.4004(2) 0.0114(6) Uani 1 1 d . . . . .
C22 C 0.72747(11) 0.6653(3) 0.3722(2) 0.0149(7) Uani 1 1 d . . . . .
H22 H 0.7078 0.7328 0.3634 0.018 Uiso 1 1 calc R U . . .
C23 C 0.71528(11) 0.5411(3) 0.3571(3) 0.0170(7) Uani 1 1 d . . . . .
H23 H 0.6869 0.5223 0.3388 0.020 Uiso 1 1 calc R U . . .
C24 C 0.74439(10) 0.4441(3) 0.3687(2) 0.0138(7) Uani 1 1 d . . . . .
H24 H 0.7364 0.3586 0.3566 0.017 Uiso 1 1 calc R U . . .
C25 C 0.78525(10) 0.4729(3) 0.3979(2) 0.0100(6) Uani 1 1 d . . . . .
C26 C 0.82009(10) 0.3772(3) 0.4058(2) 0.0099(6) Uani 1 1 d . . . . .
H26A H 0.8336 0.3643 0.3419 0.012 Uiso 1 1 calc R U . . .
H26B H 0.8085 0.2949 0.4281 0.012 Uiso 1 1 calc R U . . .
C27 C 0.81198(12) 0.8667(3) 0.5711(3) 0.0176(7) Uani 1 1 d . . . . .
H27A H 0.8009 0.9542 0.5642 0.021 Uiso 1 1 calc R U . . .
H27B H 0.8375 0.8706 0.6130 0.021 Uiso 1 1 calc R U . . .
C28 C 0.77862(13) 0.7858(4) 0.6202(3) 0.0250(9) Uani 1 1 d . . . . .
H28A H 0.7531 0.7820 0.5795 0.037 Uiso 1 1 calc R U . . .
H28B H 0.7713 0.8232 0.6830 0.037 Uiso 1 1 calc R U . . .
H28C H 0.7898 0.6999 0.6299 0.037 Uiso 1 1 calc R U . . .
C29 C 0.85716(11) 0.9092(3) 0.4338(3) 0.0190(8) Uani 1 1 d . . . . .
H29A H 0.8784 0.9275 0.4847 0.023 Uiso 1 1 calc R U . . .
H29B H 0.8429 0.9900 0.4172 0.023 Uiso 1 1 calc R U . . .
C30 C 0.87977(13) 0.8598(4) 0.3455(3) 0.0275(9) Uani 1 1 d . . . . .
H30A H 0.8949 0.7813 0.3618 0.041 Uiso 1 1 calc R U . . .
H30B H 0.9002 0.9234 0.3227 0.041 Uiso 1 1 calc R U . . .
H30C H 0.8590 0.8424 0.2944 0.041 Uiso 1 1 calc R U . . .
C31 C 0.84328(10) 0.3663(3) 0.6113(2) 0.0120(7) Uani 1 1 d . . . . .
C32 C 0.79576(11) 0.3938(3) 0.6229(3) 0.0165(7) Uani 1 1 d . . . . .
H32A H 0.7864 0.3668 0.6873 0.025 Uiso 1 1 calc R U . . .
H32B H 0.7798 0.3471 0.5735 0.025 Uiso 1 1 calc R U . . .
H32C H 0.7907 0.4850 0.6153 0.025 Uiso 1 1 calc R U . . .
C33 C 0.84905(12) 0.2209(3) 0.6139(3) 0.0183(8) Uani 1 1 d . . . . .
H33A H 0.8794 0.2004 0.6144 0.027 Uiso 1 1 calc R U . . .
H33B H 0.8358 0.1832 0.5566 0.027 Uiso 1 1 calc R U . . .
H33C H 0.8356 0.1867 0.6723 0.027 Uiso 1 1 calc R U . . .
C34 C 0.86680(12) 0.4292(3) 0.6954(2) 0.0161(7) Uani 1 1 d . . . . .
H34A H 0.8565 0.3941 0.7567 0.024 Uiso 1 1 calc R U . . .
H34B H 0.8617 0.5209 0.6941 0.024 Uiso 1 1 calc R U . . .
H34C H 0.8974 0.4128 0.6893 0.024 Uiso 1 1 calc R U . . .
C35 C 0.91169(11) 0.3776(3) 0.4484(2) 0.0135(7) Uani 1 1 d . . . . .
C36 C 0.90767(11) 0.2431(3) 0.4058(3) 0.0200(8) Uani 1 1 d . . . . .
H36A H 0.9357 0.2132 0.3852 0.030 Uiso 1 1 calc R U . . .
H36B H 0.8885 0.2450 0.3500 0.030 Uiso 1 1 calc R U . . .
H36C H 0.8962 0.1856 0.4551 0.030 Uiso 1 1 calc R U . . .
C37 C 0.94553(11) 0.3767(3) 0.5282(3) 0.0176(7) Uani 1 1 d . . . . .
H37A H 0.9734 0.3581 0.4997 0.026 Uiso 1 1 calc R U . . .
H37B H 0.9385 0.3115 0.5761 0.026 Uiso 1 1 calc R U . . .
H37C H 0.9464 0.4600 0.5597 0.026 Uiso 1 1 calc R U . . .
C38 C 0.92572(11) 0.4688(4) 0.3674(3) 0.0189(8) Uani 1 1 d . . . . .
H38A H 0.9306 0.5535 0.3947 0.028 Uiso 1 1 calc R U . . .
H38B H 0.9034 0.4736 0.3180 0.028 Uiso 1 1 calc R U . . .
H38C H 0.9521 0.4375 0.3380 0.028 Uiso 1 1 calc R U . . .
O1W O 0.73857(11) 0.1100(3) 0.6282(3) 0.0384(8) Uani 1 1 d D . . . .
H1X H 0.7392(18) 0.119(5) 0.566(2) 0.046 Uiso 1 1 d D U . . .
H1Y H 0.7179(12) 0.062(4) 0.642(4) 0.046 Uiso 1 1 d D U . . .
O2W O 0.66850(10) 0.9130(3) 0.4394(2) 0.0203(6) Uani 1 1 d D . . . .
H2X H 0.6865(11) 0.970(3) 0.430(3) 0.024 Uiso 1 1 d D U . . .
H2Y H 0.6658(14) 0.925(4) 0.4985(19) 0.024 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 1.873(3) . ?
Ni1 N1 2.009(2) . ?
Ni1 Cl1 2.1562(9) . ?
Ni1 P1 2.1827(9) . ?
Ni2 N4 1.873(3) . ?
Ni2 N3 2.014(2) . ?
Ni2 Cl2 2.1549(9) . ?
Ni2 P2 2.1786(9) . ?
P1 C7 1.830(3) . ?
P1 C12 1.861(3) . ?
P1 C16 1.870(3) . ?
P2 C26 1.828(3) . ?
P2 C35 1.865(3) . ?
P2 C31 1.867(3) . ?
N1 C8 1.495(4) . ?
N1 C1 1.503(4) . ?
N1 C10 1.504(4) . ?
N2 C2 1.346(4) . ?
N2 C6 1.362(4) . ?
N3 C20 1.490(4) . ?
N3 C29 1.495(4) . ?
N3 C27 1.499(5) . ?
N4 C21 1.351(4) . ?
N4 C25 1.351(4) . ?
C1 C2 1.497(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.381(5) . ?
C3 C4 1.379(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.481(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.513(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.519(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C14 1.534(5) . ?
C12 C13 1.537(5) . ?
C12 C15 1.540(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C19 1.528(5) . ?
C16 C17 1.528(5) . ?
C16 C18 1.546(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
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 1.485(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.377(5) . ?
C22 C23 1.379(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.493(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.513(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.506(6) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C34 1.529(5) . ?
C31 C32 1.531(5) . ?
C31 C33 1.543(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C37 1.532(5) . ?
C35 C36 1.539(5) . ?
C35 C38 1.540(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O1W H1X 0.86(3) . ?
O1W H1Y 0.84(3) . ?
O2W H2X 0.84(2) . ?
O2W H2Y 0.83(2) . ?

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
N2 Ni1 N1 86.10(11) . . ?
N2 Ni1 Cl1 179.68(9) . . ?
N1 Ni1 Cl1 93.58(8) . . ?
N2 Ni1 P1 86.63(8) . . ?
N1 Ni1 P1 171.73(8) . . ?
Cl1 Ni1 P1 93.69(3) . . ?
N4 Ni2 N3 85.75(11) . . ?
N4 Ni2 Cl2 178.53(9) . . ?
N3 Ni2 Cl2 94.04(8) . . ?
N4 Ni2 P2 86.51(8) . . ?
N3 Ni2 P2 171.38(8) . . ?
Cl2 Ni2 P2 93.60(3) . . ?
C7 P1 C12 105.41(16) . . ?
C7 P1 C16 104.56(15) . . ?
C12 P1 C16 114.13(15) . . ?
C7 P1 Ni1 99.23(11) . . ?
C12 P1 Ni1 111.71(11) . . ?
C16 P1 Ni1 119.30(10) . . ?
C26 P2 C35 105.58(15) . . ?
C26 P2 C31 105.12(15) . . ?
C35 P2 C31 113.26(15) . . ?
C26 P2 Ni2 99.65(10) . . ?
C35 P2 Ni2 118.16(11) . . ?
C31 P2 Ni2 112.87(11) . . ?
C8 N1 C1 109.6(2) . . ?
C8 N1 C10 107.1(2) . . ?
C1 N1 C10 108.9(3) . . ?
C8 N1 Ni1 110.6(2) . . ?
C1 N1 Ni1 108.89(18) . . ?
C10 N1 Ni1 111.68(19) . . ?
C2 N2 C6 120.0(3) . . ?
C2 N2 Ni1 116.6(2) . . ?
C6 N2 Ni1 123.1(2) . . ?
C20 N3 C29 108.9(3) . . ?
C20 N3 C27 109.0(3) . . ?
C29 N3 C27 107.4(3) . . ?
C20 N3 Ni2 107.91(19) . . ?
C29 N3 Ni2 113.5(2) . . ?
C27 N3 Ni2 110.2(2) . . ?
C21 N4 C25 120.0(3) . . ?
C21 N4 Ni2 115.9(2) . . ?
C25 N4 Ni2 123.5(2) . . ?
C2 C1 N1 111.5(2) . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
N1 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N2 C2 C3 121.4(3) . . ?
N2 C2 C1 115.8(3) . . ?
C3 C2 C1 122.7(3) . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
N2 C6 C5 120.3(3) . . ?
N2 C6 C7 116.2(3) . . ?
C5 C6 C7 123.5(3) . . ?
C6 C7 P1 108.8(2) . . ?
C6 C7 H7A 109.9 . . ?
P1 C7 H7A 109.9 . . ?
C6 C7 H7B 109.9 . . ?
P1 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N1 C8 C9 112.8(3) . . ?
N1 C8 H8A 109.0 . . ?
C9 C8 H8A 109.0 . . ?
N1 C8 H8B 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C11 113.3(3) . . ?
N1 C10 H10A 108.9 . . ?
C11 C10 H10A 108.9 . . ?
N1 C10 H10B 108.9 . . ?
C11 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C14 C12 C13 108.3(3) . . ?
C14 C12 C15 109.7(3) . . ?
C13 C12 C15 108.7(3) . . ?
C14 C12 P1 111.3(2) . . ?
C13 C12 P1 105.7(2) . . ?
C15 C12 P1 112.9(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C19 C16 C17 109.9(3) . . ?
C19 C16 C18 109.1(3) . . ?
C17 C16 C18 108.8(3) . . ?
C19 C16 P1 111.5(2) . . ?
C17 C16 P1 105.8(2) . . ?
C18 C16 P1 111.7(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 N3 110.8(3) . . ?
C21 C20 H20A 109.5 . . ?
N3 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
N3 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
N4 C21 C22 121.4(3) . . ?
N4 C21 C20 114.6(3) . . ?
C22 C21 C20 123.8(3) . . ?
C21 C22 C23 118.7(3) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
C22 C23 C24 120.0(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 119.2(3) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
N4 C25 C24 120.6(3) . . ?
N4 C25 C26 115.6(3) . . ?
C24 C25 C26 123.8(3) . . ?
C25 C26 P2 108.2(2) . . ?
C25 C26 H26A 110.1 . . ?
P2 C26 H26A 110.1 . . ?
C25 C26 H26B 110.1 . . ?
P2 C26 H26B 110.1 . . ?
H26A C26 H26B 108.4 . . ?
N3 C27 C28 113.8(3) . . ?
N3 C27 H27A 108.8 . . ?
C28 C27 H27A 108.8 . . ?
N3 C27 H27B 108.8 . . ?
C28 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 C30 113.3(3) . . ?
N3 C29 H29A 108.9 . . ?
C30 C29 H29A 108.9 . . ?
N3 C29 H29B 108.9 . . ?
C30 C29 H29B 108.9 . . ?
H29A C29 H29B 107.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C34 C31 C32 108.1(3) . . ?
C34 C31 C33 110.8(3) . . ?
C32 C31 C33 107.5(3) . . ?
C34 C31 P2 111.5(2) . . ?
C32 C31 P2 106.3(2) . . ?
C33 C31 P2 112.4(2) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C37 C35 C36 109.1(3) . . ?
C37 C35 C38 109.1(3) . . ?
C36 C35 C38 108.6(3) . . ?
C37 C35 P2 112.4(2) . . ?
C36 C35 P2 111.0(2) . . ?
C38 C35 P2 106.6(2) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
H1X O1W H1Y 107(5) . . ?
H2X O2W H2Y 97(4) . . ?

_refine_diff_density_max         0.615
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.072

_shelxl_version_number           2014-3

