# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

####################################################################### 
# 
# 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_HL
_database_code_depnum_ccdc_archive 'CCDC 1453155'
_audit_update_record             
;
2016-02-12 deposited with the CCDC.
2016-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H25 N2 O2 P S2'
_chemical_formula_sum            'C23 H25 N2 O2 P S2'
_chemical_formula_weight         456.54

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'
S S 0.1246 0.1234 '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                   10.244(2)
_cell_length_b                   10.4376(19)
_cell_length_c                   11.148(2)
_cell_angle_alpha                104.961(15)
_cell_angle_beta                 90.250(16)
_cell_angle_gamma                103.255(15)
_cell_volume                     1118.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6472
_cell_measurement_theta_min      3.3
_cell_measurement_theta_max      25.9

_exptl_crystal_description       block
_exptl_crystal_colour            'light brown'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             480
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9156
_exptl_absorpt_correction_T_max  0.9305
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'

_exptl_special_details           
;
 ;
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  'Genix 3D multilayer optics'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10227
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_sigmaI/netI    0.1161
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.25
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3924
_reflns_number_gt                2445
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008) '
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008) '
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL97

_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)+(0.0439P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3924
_refine_ls_number_parameters     279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1057
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1223
_refine_ls_wR_factor_gt          0.1091
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_restrained_S_all      0.924
_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
P1 P 0.24790(9) 0.80229(10) 0.11848(10) 0.0257(3) Uani 1 1 d . . .
S1 S 0.09819(9) 0.38662(9) 0.08861(10) 0.0303(3) Uani 1 1 d . . .
S2 S 0.43983(9) 0.86929(11) 0.14026(11) 0.0376(3) Uani 1 1 d . . .
N1 N 0.3298(3) 0.5593(4) 0.1732(4) 0.0318(8) Uani 1 1 d . . .
H1 H 0.377(4) 0.623(5) 0.175(4) 0.032(13) Uiso 1 1 d . . .
N2 N 0.1927(3) 0.6350(3) 0.0579(3) 0.0265(8) Uani 1 1 d . . .
H2 H 0.128(5) 0.625(5) 0.030(5) 0.047(16) Uiso 1 1 d . . .
O1 O 0.1734(2) 0.8613(3) 0.0312(3) 0.0305(7) Uani 1 1 d . . .
O2 O 0.1693(3) 0.8199(3) 0.2398(3) 0.0342(7) Uani 1 1 d . . .
C1 C 0.2132(3) 0.5329(4) 0.1089(4) 0.0254(8) Uani 1 1 d . . .
C2 C 0.3685(3) 0.4703(4) 0.2378(4) 0.0287(9) Uani 1 1 d . . .
C3 C 0.3171(3) 0.4623(4) 0.3525(4) 0.0268(9) Uani 1 1 d . . .
C4 C 0.2229(4) 0.5368(4) 0.4101(4) 0.0339(10) Uani 1 1 d . . .
H4 H 0.1930 0.5959 0.3699 0.041 Uiso 1 1 calc R . .
C5 C 0.1762(4) 0.5250(4) 0.5197(4) 0.0381(10) Uani 1 1 d . . .
H5 H 0.1143 0.5768 0.5557 0.046 Uiso 1 1 calc R . .
C6 C 0.2160(4) 0.4370(4) 0.5843(4) 0.0351(10) Uani 1 1 d . . .
C7 C 0.1645(4) 0.4195(5) 0.6965(4) 0.0434(11) Uani 1 1 d . . .
H7 H 0.0986 0.4659 0.7322 0.052 Uiso 1 1 calc R . .
C8 C 0.2095(5) 0.3347(5) 0.7553(4) 0.0529(13) Uani 1 1 d . . .
H8 H 0.1742 0.3241 0.8318 0.063 Uiso 1 1 calc R . .
C9 C 0.3034(4) 0.2658(5) 0.7059(4) 0.0451(12) Uani 1 1 d . . .
H9 H 0.3330 0.2088 0.7487 0.054 Uiso 1 1 calc R . .
C10 C 0.3563(4) 0.2779(4) 0.5939(4) 0.0334(10) Uani 1 1 d . . .
C11 C 0.4534(4) 0.2060(4) 0.5381(4) 0.0369(10) Uani 1 1 d . . .
H11 H 0.4852 0.1493 0.5799 0.044 Uiso 1 1 calc R . .
C12 C 0.5007(4) 0.2167(4) 0.4275(4) 0.0331(10) Uani 1 1 d . . .
H12 H 0.5649 0.1672 0.3929 0.040 Uiso 1 1 calc R . .
C13 C 0.4564(3) 0.3013(4) 0.3612(4) 0.0275(9) Uani 1 1 d . . .
C14 C 0.5017(4) 0.3125(4) 0.2464(4) 0.0333(9) Uani 1 1 d . . .
H14 H 0.5637 0.2615 0.2093 0.040 Uiso 1 1 calc R . .
C15 C 0.4588(4) 0.3960(4) 0.1849(4) 0.0313(9) Uani 1 1 d . . .
H15 H 0.4913 0.4023 0.1065 0.038 Uiso 1 1 calc R . .
C16 C 0.3113(4) 0.3641(4) 0.5317(4) 0.0311(9) Uani 1 1 d . . .
C17 C 0.3622(3) 0.3759(4) 0.4146(4) 0.0279(9) Uani 1 1 d . . .
C18 C 0.2361(4) 0.9308(4) -0.0615(4) 0.0321(9) Uani 1 1 d . . .
H18 H 0.3354 0.9400 -0.0555 0.039 Uiso 1 1 calc R . .
C19 C 0.1787(5) 0.8426(5) -0.1876(5) 0.0488(12) Uani 1 1 d . . .
H19A H 0.2023 0.7542 -0.2021 0.073 Uiso 1 1 calc R . .
H19B H 0.2156 0.8875 -0.2513 0.073 Uiso 1 1 calc R . .
H19C H 0.0807 0.8283 -0.1918 0.073 Uiso 1 1 calc R . .
C20 C 0.2083(5) 1.0692(5) -0.0285(6) 0.0553(14) Uani 1 1 d . . .
H20A H 0.2494 1.1201 0.0547 0.083 Uiso 1 1 calc R . .
H20B H 0.1109 1.0605 -0.0294 0.083 Uiso 1 1 calc R . .
H20C H 0.2462 1.1182 -0.0893 0.083 Uiso 1 1 calc R . .
C21 C 0.1935(4) 0.9476(4) 0.3395(4) 0.0409(10) Uani 1 1 d . . .
H21 H 0.2888 0.9997 0.3413 0.049 Uiso 1 1 calc R . .
C22 C 0.1708(6) 0.9052(5) 0.4572(5) 0.0564(13) Uani 1 1 d . . .
H22A H 0.2348 0.8515 0.4679 0.085 Uiso 1 1 calc R . .
H22B H 0.0789 0.8498 0.4533 0.085 Uiso 1 1 calc R . .
H22C H 0.1838 0.9866 0.5278 0.085 Uiso 1 1 calc R . .
C23 C 0.1004(6) 1.0316(5) 0.3152(6) 0.0623(15) Uani 1 1 d . . .
H23A H 0.1205 1.0562 0.2371 0.093 Uiso 1 1 calc R . .
H23B H 0.1128 1.1149 0.3837 0.093 Uiso 1 1 calc R . .
H23C H 0.0072 0.9786 0.3091 0.093 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1 1.558(2) . ?
P1 O2 1.568(3) . ?
P1 N2 1.661(3) . ?
P1 S2 1.9213(13) . ?
S1 C1 1.663(4) . ?
N1 C1 1.325(5) . ?
N1 C2 1.432(5) . ?
N1 H1 0.72(4) . ?
N2 C1 1.385(5) . ?
N2 H2 0.71(5) . ?
O1 C18 1.478(4) . ?
O2 C21 1.468(5) . ?
C2 C15 1.380(6) . ?
C2 C3 1.400(6) . ?
C3 C17 1.419(5) . ?
C3 C4 1.428(6) . ?
C4 C5 1.340(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.427(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.398(6) . ?
C6 C16 1.411(6) . ?
C7 C8 1.382(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.365(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(6) . ?
C9 H9 0.9500 . ?
C10 C16 1.418(6) . ?
C10 C11 1.430(6) . ?
C11 C12 1.348(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.432(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(6) . ?
C13 C17 1.415(6) . ?
C14 C15 1.380(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.431(6) . ?
C18 C20 1.490(6) . ?
C18 C19 1.499(6) . ?
C18 H18 1.0000 . ?
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 C22 1.492(6) . ?
C21 C23 1.502(6) . ?
C21 H21 1.0000 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 O2 104.46(15) . . ?
O1 P1 N2 102.23(16) . . ?
O2 P1 N2 99.63(16) . . ?
O1 P1 S2 116.05(11) . . ?
O2 P1 S2 116.54(12) . . ?
N2 P1 S2 115.64(14) . . ?
C1 N1 C2 124.7(3) . . ?
C1 N1 H1 117(3) . . ?
C2 N1 H1 118(3) . . ?
C1 N2 P1 126.8(3) . . ?
C1 N2 H2 116(4) . . ?
P1 N2 H2 106(4) . . ?
C18 O1 P1 125.7(2) . . ?
C21 O2 P1 123.5(2) . . ?
N1 C1 N2 115.7(3) . . ?
N1 C1 S1 122.8(3) . . ?
N2 C1 S1 121.5(3) . . ?
C15 C2 C3 121.7(3) . . ?
C15 C2 N1 118.1(4) . . ?
C3 C2 N1 120.2(4) . . ?
C2 C3 C17 117.9(4) . . ?
C2 C3 C4 123.4(3) . . ?
C17 C3 C4 118.7(4) . . ?
C5 C4 C3 121.1(4) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 122.3(4) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C7 C6 C16 118.7(4) . . ?
C7 C6 C5 123.1(4) . . ?
C16 C6 C5 118.2(4) . . ?
C8 C7 C6 120.0(5) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C9 C8 C7 121.4(4) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C10 120.9(4) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C9 C10 C16 118.6(4) . . ?
C9 C10 C11 122.6(4) . . ?
C16 C10 C11 118.7(4) . . ?
C12 C11 C10 121.6(4) . . ?
C12 C11 H11 119.2 . . ?
C10 C11 H11 119.2 . . ?
C11 C12 C13 121.3(4) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C17 118.8(3) . . ?
C14 C13 C12 122.5(4) . . ?
C17 C13 C12 118.7(4) . . ?
C15 C14 C13 121.5(4) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C2 119.8(4) . . ?
C14 C15 H15 120.1 . . ?
C2 C15 H15 120.1 . . ?
C6 C16 C10 120.3(4) . . ?
C6 C16 C17 120.1(4) . . ?
C10 C16 C17 119.7(4) . . ?
C13 C17 C3 120.4(4) . . ?
C13 C17 C16 120.0(3) . . ?
C3 C17 C16 119.6(4) . . ?
O1 C18 C20 106.8(3) . . ?
O1 C18 C19 107.3(3) . . ?
C20 C18 C19 114.7(4) . . ?
O1 C18 H18 109.3 . . ?
C20 C18 H18 109.3 . . ?
C19 C18 H18 109.3 . . ?
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 . . ?
O2 C21 C22 105.5(3) . . ?
O2 C21 C23 109.0(4) . . ?
C22 C21 C23 113.5(4) . . ?
O2 C21 H21 109.6 . . ?
C22 C21 H21 109.6 . . ?
C23 C21 H21 109.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 P1 N2 C1 -170.9(3) . . . . ?
O2 P1 N2 C1 -63.6(4) . . . . ?
S2 P1 N2 C1 62.1(4) . . . . ?
O2 P1 O1 C18 148.1(3) . . . . ?
N2 P1 O1 C18 -108.5(3) . . . . ?
S2 P1 O1 C18 18.3(3) . . . . ?
O1 P1 O2 C21 -83.0(3) . . . . ?
N2 P1 O2 C21 171.6(3) . . . . ?
S2 P1 O2 C21 46.5(3) . . . . ?
C2 N1 C1 N2 177.1(4) . . . . ?
C2 N1 C1 S1 -3.5(6) . . . . ?
P1 N2 C1 N1 -33.8(5) . . . . ?
P1 N2 C1 S1 146.8(3) . . . . ?
C1 N1 C2 C15 103.9(5) . . . . ?
C1 N1 C2 C3 -77.3(5) . . . . ?
C15 C2 C3 C17 0.8(5) . . . . ?
N1 C2 C3 C17 -178.0(3) . . . . ?
C15 C2 C3 C4 -179.6(4) . . . . ?
N1 C2 C3 C4 1.6(6) . . . . ?
C2 C3 C4 C5 179.6(4) . . . . ?
C17 C3 C4 C5 -0.8(6) . . . . ?
C3 C4 C5 C6 -0.7(6) . . . . ?
C4 C5 C6 C7 -177.6(4) . . . . ?
C4 C5 C6 C16 2.1(6) . . . . ?
C16 C6 C7 C8 1.6(6) . . . . ?
C5 C6 C7 C8 -178.8(4) . . . . ?
C6 C7 C8 C9 -0.5(7) . . . . ?
C7 C8 C9 C10 -0.5(7) . . . . ?
C8 C9 C10 C16 0.3(6) . . . . ?
C8 C9 C10 C11 -179.0(4) . . . . ?
C9 C10 C11 C12 178.3(4) . . . . ?
C16 C10 C11 C12 -1.1(6) . . . . ?
C10 C11 C12 C13 0.3(6) . . . . ?
C11 C12 C13 C14 -178.9(4) . . . . ?
C11 C12 C13 C17 0.8(6) . . . . ?
C17 C13 C14 C15 1.1(6) . . . . ?
C12 C13 C14 C15 -179.2(4) . . . . ?
C13 C14 C15 C2 -0.2(6) . . . . ?
C3 C2 C15 C14 -0.8(6) . . . . ?
N1 C2 C15 C14 177.9(4) . . . . ?
C7 C6 C16 C10 -1.8(6) . . . . ?
C5 C6 C16 C10 178.5(3) . . . . ?
C7 C6 C16 C17 177.7(4) . . . . ?
C5 C6 C16 C17 -2.0(6) . . . . ?
C9 C10 C16 C6 0.9(6) . . . . ?
C11 C10 C16 C6 -179.7(4) . . . . ?
C9 C10 C16 C17 -178.6(4) . . . . ?
C11 C10 C16 C17 0.8(5) . . . . ?
C14 C13 C17 C3 -1.1(5) . . . . ?
C12 C13 C17 C3 179.2(3) . . . . ?
C14 C13 C17 C16 178.6(3) . . . . ?
C12 C13 C17 C16 -1.1(5) . . . . ?
C2 C3 C17 C13 0.2(5) . . . . ?
C4 C3 C17 C13 -179.4(3) . . . . ?
C2 C3 C17 C16 -179.5(3) . . . . ?
C4 C3 C17 C16 0.8(5) . . . . ?
C6 C16 C17 C13 -179.2(3) . . . . ?
C10 C16 C17 C13 0.3(5) . . . . ?
C6 C16 C17 C3 0.6(5) . . . . ?
C10 C16 C17 C3 -179.9(3) . . . . ?
P1 O1 C18 C20 -122.0(3) . . . . ?
P1 O1 C18 C19 114.5(3) . . . . ?
P1 O2 C21 C22 -146.1(3) . . . . ?
P1 O2 C21 C23 91.6(4) . . . . ?

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 H1 S2 0.72(4) 2.64(4) 3.289(4) 152(4) .
N2 H2 S1 0.71(5) 2.62(5) 3.325(4) 172(5) 2_565

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.068
####################################################################### 
# 
# 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_NiL2
_database_code_depnum_ccdc_archive 'CCDC 1453156'
_audit_update_record             
;
2016-02-12 deposited with the CCDC.
2016-09-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H48 N4 Ni O4 P2 S4'
_chemical_formula_sum            'C46 H48 N4 Ni O4 P2 S4'
_chemical_formula_weight         969.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 '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 0.0050 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0100 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0960 0.0880 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1170 0.1150 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3430 1.0390 '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                   10.2046(6)
_cell_length_b                   10.7201(7)
_cell_length_c                   10.8463(5)
_cell_angle_alpha                90.022(5)
_cell_angle_beta                 108.105(5)
_cell_angle_gamma                105.302(5)
_cell_volume                     1083.40(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5520
_cell_measurement_theta_min      1.8986
_cell_measurement_theta_max      32.5716

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             506
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_min  0.99996
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.68239
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  Si(111)
_diffrn_measurement_device_type  'pilatus 2M'
_diffrn_measurement_method       '359 images, ΔΦ 1.0° '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9801
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         31.65
_reflns_number_total             5086
_reflns_number_gt                4649
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SNBL Pilatus control'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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)+(0.0423P)²+0.6082P] 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         5086
_refine_ls_number_parameters     284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0840
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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
Ni1 Ni 1.0000 1.0000 0.5000 0.01286(8) Uani 1 2 d S . .
S2 S 1.12374(4) 0.91761(3) 0.40148(4) 0.01518(10) Uani 1 1 d . . .
C3 C 0.97053(18) 0.79278(14) 0.37714(17) 0.0141(3) Uani 1 1 d . . .
N4 N 0.88318(15) 0.82886(12) 0.43114(14) 0.0145(3) Uani 1 1 d . . .
P5 P 0.71204(5) 0.76276(4) 0.41128(4) 0.01408(10) Uani 1 1 d . . .
S6 S 0.63551(5) 0.57957(3) 0.35357(5) 0.01855(11) Uani 1 1 d . . .
O7 O 0.70880(13) 0.80076(11) 0.54966(12) 0.0178(3) Uani 1 1 d . . .
C8 C 0.58426(19) 0.74688(15) 0.59302(18) 0.0189(4) Uani 1 1 d . . .
H8 H 0.5593 0.6499 0.5833 0.023 Uiso 1 1 calc R . .
C9 C 0.6374(2) 0.79337(17) 0.73557(19) 0.0235(4) Uani 1 1 d . . .
H9A H 0.7228 0.7653 0.7798 0.035 Uiso 1 1 calc R . .
H9B H 0.5621 0.7567 0.7742 0.035 Uiso 1 1 calc R . .
H9C H 0.6616 0.8884 0.7455 0.035 Uiso 1 1 calc R . .
C10 C 0.4561(2) 0.7897(2) 0.5170(2) 0.0286(4) Uani 1 1 d . . .
H10A H 0.4811 0.8848 0.5238 0.043 Uiso 1 1 calc R . .
H10B H 0.3772 0.7556 0.5520 0.043 Uiso 1 1 calc R . .
H10C H 0.4261 0.7568 0.4253 0.043 Uiso 1 1 calc R . .
O11 O 0.63048(14) 0.85372(11) 0.32422(13) 0.0195(3) Uani 1 1 d . . .
C12 C 0.5428(2) 0.82277(15) 0.18747(19) 0.0191(4) Uani 1 1 d . . .
H12 H 0.4753 0.7338 0.1757 0.023 Uiso 1 1 calc R . .
C13 C 0.6367(2) 0.82753(19) 0.1027(2) 0.0268(4) Uani 1 1 d . . .
H13A H 0.7058 0.9136 0.1168 0.040 Uiso 1 1 calc R . .
H13B H 0.5767 0.8108 0.0109 0.040 Uiso 1 1 calc R . .
H13C H 0.6885 0.7613 0.1253 0.040 Uiso 1 1 calc R . .
C14 C 0.4583(2) 0.92131(18) 0.1587(2) 0.0269(4) Uani 1 1 d . . .
H14A H 0.3970 0.9115 0.2139 0.040 Uiso 1 1 calc R . .
H14B H 0.3985 0.9075 0.0669 0.040 Uiso 1 1 calc R . .
H14C H 0.5246 1.0090 0.1765 0.040 Uiso 1 1 calc R . .
N15 N 0.94242(16) 0.67799(12) 0.31245(15) 0.0172(3) Uani 1 1 d . . .
H15 H 0.870(3) 0.627(2) 0.310(2) 0.021 Uiso 1 1 d . . .
C51 C 1.05290(18) 0.68891(14) 0.13977(17) 0.0151(3) Uani 1 1 d . . .
C52 C 1.20597(18) 0.54481(14) 0.14109(17) 0.0153(3) Uani 1 1 d . . .
C53 C 1.15259(18) 0.68298(14) -0.03884(17) 0.0151(3) Uani 1 1 d . . .
C54 C 1.03750(18) 0.64055(14) 0.25638(17) 0.0155(3) Uani 1 1 d . . .
C55 C 1.30389(19) 0.53773(15) -0.03598(18) 0.0176(4) Uani 1 1 d . . .
H55 H 1.3599 0.5036 -0.0752 0.021 Uiso 1 1 calc R . .
C56 C 1.28961(19) 0.49606(14) 0.07775(18) 0.0175(4) Uani 1 1 d . . .
H56 H 1.3358 0.4331 0.1170 0.021 Uiso 1 1 calc R . .
C57 C 1.10510(19) 0.54922(15) 0.31465(18) 0.0176(4) Uani 1 1 d . . .
H57 H 1.0937 0.5186 0.3939 0.021 Uiso 1 1 calc R . .
C58 C 1.13835(17) 0.63928(13) 0.08159(17) 0.0138(3) Uani 1 1 d . . .
C59 C 1.23619(18) 0.63249(14) -0.09859(17) 0.0160(3) Uani 1 1 d . . .
C60 C 1.18924(19) 0.50219(15) 0.25813(18) 0.0179(4) Uani 1 1 d . . .
H60 H 1.2359 0.4403 0.2996 0.021 Uiso 1 1 calc R . .
C61 C 1.2488(2) 0.67722(16) -0.21688(18) 0.0201(4) Uani 1 1 d . . .
H61 H 1.3041 0.6442 -0.2578 0.024 Uiso 1 1 calc R . .
C62 C 1.00338(19) 0.82731(15) -0.03580(18) 0.0178(4) Uani 1 1 d . . .
H62 H 0.9592 0.8917 -0.0745 0.021 Uiso 1 1 calc R . .
C63 C 0.98718(19) 0.78496(15) 0.07727(18) 0.0175(4) Uani 1 1 d . . .
H63 H 0.9311 0.8195 0.1161 0.021 Uiso 1 1 calc R . .
C64 C 1.08589(19) 0.77725(14) -0.09868(18) 0.0169(3) Uani 1 1 d . . .
C65 C 1.1003(2) 0.81807(16) -0.21709(19) 0.0210(4) Uani 1 1 d . . .
H65 H 1.0540 0.8802 -0.2586 0.025 Uiso 1 1 calc R . .
C66 C 1.1822(2) 0.76822(17) -0.27458(19) 0.0231(4) Uani 1 1 d . . .
H66 H 1.1923 0.7974 -0.3547 0.028 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N4 1.9068(13) 2_776 ?
Ni1 N4 1.9068(13) . ?
Ni1 S2 2.2233(4) . ?
Ni1 S2 2.2233(4) 2_776 ?
Ni1 C3 2.4894(14) 2_776 ?
Ni1 C3 2.4894(14) . ?
S2 C3 1.7158(15) . ?
C3 N15 1.3329(19) . ?
C3 N4 1.3392(18) . ?
N4 P5 1.6466(14) . ?
P5 O7 1.5675(12) . ?
P5 O11 1.5734(14) . ?
P5 S6 1.9350(5) . ?
O7 C8 1.4678(18) . ?
C8 C10 1.500(3) . ?
C8 C9 1.506(3) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
O11 C12 1.459(2) . ?
C12 C14 1.507(3) . ?
C12 C13 1.513(2) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N15 C54 1.4299(19) . ?
N15 H15 0.79(2) . ?
C51 C54 1.405(2) . ?
C51 C58 1.424(2) . ?
C51 C63 1.432(2) . ?
C52 C60 1.394(2) . ?
C52 C58 1.418(2) . ?
C52 C56 1.440(2) . ?
C53 C64 1.412(2) . ?
C53 C59 1.424(2) . ?
C53 C58 1.425(2) . ?
C54 C57 1.386(2) . ?
C55 C56 1.349(2) . ?
C55 C59 1.432(2) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C60 1.387(2) . ?
C57 H57 0.9500 . ?
C59 C61 1.401(2) . ?
C60 H60 0.9500 . ?
C61 C66 1.375(3) . ?
C61 H61 0.9500 . ?
C62 C63 1.351(2) . ?
C62 C64 1.434(2) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 C65 1.395(2) . ?
C65 C66 1.390(2) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?

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
N4 Ni1 N4 180.0 2_776 . ?
N4 Ni1 S2 105.64(4) 2_776 . ?
N4 Ni1 S2 74.36(4) . . ?
N4 Ni1 S2 74.36(4) 2_776 2_776 ?
N4 Ni1 S2 105.64(4) . 2_776 ?
S2 Ni1 S2 179.999(16) . 2_776 ?
N4 Ni1 C3 32.13(5) 2_776 2_776 ?
N4 Ni1 C3 147.87(5) . 2_776 ?
S2 Ni1 C3 137.77(4) . 2_776 ?
S2 Ni1 C3 42.23(3) 2_776 2_776 ?
N4 Ni1 C3 147.87(5) 2_776 . ?
N4 Ni1 C3 32.13(5) . . ?
S2 Ni1 C3 42.23(3) . . ?
S2 Ni1 C3 137.77(4) 2_776 . ?
C3 Ni1 C3 180.00(3) 2_776 . ?
C3 S2 Ni1 77.20(5) . . ?
N15 C3 N4 125.37(14) . . ?
N15 C3 S2 124.84(11) . . ?
N4 C3 S2 109.79(11) . . ?
N15 C3 Ni1 174.58(11) . . ?
N4 C3 Ni1 49.23(7) . . ?
S2 C3 Ni1 60.57(4) . . ?
C3 N4 P5 130.30(12) . . ?
C3 N4 Ni1 98.64(9) . . ?
P5 N4 Ni1 129.30(7) . . ?
O7 P5 O11 102.09(7) . . ?
O7 P5 N4 99.82(7) . . ?
O11 P5 N4 105.48(7) . . ?
O7 P5 S6 115.12(5) . . ?
O11 P5 S6 115.19(5) . . ?
N4 P5 S6 117.01(5) . . ?
C8 O7 P5 122.68(11) . . ?
O7 C8 C10 112.12(14) . . ?
O7 C8 C9 103.93(14) . . ?
C10 C8 C9 112.97(14) . . ?
O7 C8 H8 109.2 . . ?
C10 C8 H8 109.2 . . ?
C9 C8 H8 109.2 . . ?
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 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 O11 P5 125.50(10) . . ?
O11 C12 C14 105.13(14) . . ?
O11 C12 C13 110.49(15) . . ?
C14 C12 C13 113.08(16) . . ?
O11 C12 H12 109.3 . . ?
C14 C12 H12 109.3 . . ?
C13 C12 H12 109.3 . . ?
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 . . ?
C3 N15 C54 124.66(13) . . ?
C3 N15 H15 115.6(16) . . ?
C54 N15 H15 119.7(16) . . ?
C54 C51 C58 117.87(15) . . ?
C54 C51 C63 123.30(13) . . ?
C58 C51 C63 118.83(14) . . ?
C60 C52 C58 119.20(13) . . ?
C60 C52 C56 122.30(15) . . ?
C58 C52 C56 118.50(14) . . ?
C64 C53 C59 119.71(14) . . ?
C64 C53 C58 120.50(13) . . ?
C59 C53 C58 119.79(15) . . ?
C57 C54 C51 121.34(13) . . ?
C57 C54 N15 118.37(14) . . ?
C51 C54 N15 120.13(15) . . ?
C56 C55 C59 121.17(14) . . ?
C56 C55 H55 119.4 . . ?
C59 C55 H55 119.4 . . ?
C55 C56 C52 121.54(16) . . ?
C55 C56 H56 119.2 . . ?
C52 C56 H56 119.2 . . ?
C54 C57 C60 120.49(15) . . ?
C54 C57 H57 119.8 . . ?
C60 C57 H57 119.8 . . ?
C52 C58 C51 120.45(14) . . ?
C52 C58 C53 120.10(13) . . ?
C51 C58 C53 119.43(15) . . ?
C61 C59 C53 118.69(15) . . ?
C61 C59 C55 122.41(14) . . ?
C53 C59 C55 118.90(14) . . ?
C57 C60 C52 120.62(16) . . ?
C57 C60 H60 119.7 . . ?
C52 C60 H60 119.7 . . ?
C66 C61 C59 120.96(15) . . ?
C66 C61 H61 119.5 . . ?
C59 C61 H61 119.5 . . ?
C63 C62 C64 121.44(15) . . ?
C63 C62 H62 119.3 . . ?
C64 C62 H62 119.3 . . ?
C62 C63 C51 121.23(14) . . ?
C62 C63 H63 119.4 . . ?
C51 C63 H63 119.4 . . ?
C65 C64 C53 119.60(14) . . ?
C65 C64 C62 121.85(16) . . ?
C53 C64 C62 118.55(15) . . ?
C66 C65 C64 120.23(17) . . ?
C66 C65 H65 119.9 . . ?
C64 C65 H65 119.9 . . ?
C61 C66 C65 120.80(16) . . ?
C61 C66 H66 119.6 . . ?
C65 C66 H66 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 Ni1 S2 C3 179.67(8) 2_776 . . . ?
N4 Ni1 S2 C3 -0.33(8) . . . . ?
C3 Ni1 S2 C3 180.0 2_776 . . . ?
Ni1 S2 C3 N15 179.59(17) . . . . ?
Ni1 S2 C3 N4 0.49(11) . . . . ?
N4 Ni1 C3 N4 180.0 2_776 . . . ?
S2 Ni1 C3 N4 -179.40(14) . . . . ?
S2 Ni1 C3 N4 0.61(14) 2_776 . . . ?
N4 Ni1 C3 S2 -0.60(14) 2_776 . . . ?
N4 Ni1 C3 S2 179.40(14) . . . . ?
S2 Ni1 C3 S2 180.0 2_776 . . . ?
N15 C3 N4 P5 -13.9(3) . . . . ?
S2 C3 N4 P5 165.15(11) . . . . ?
Ni1 C3 N4 P5 165.71(19) . . . . ?
N15 C3 N4 Ni1 -179.66(16) . . . . ?
S2 C3 N4 Ni1 -0.56(13) . . . . ?
S2 Ni1 N4 C3 0.42(10) . . . . ?
S2 Ni1 N4 C3 -179.58(10) 2_776 . . . ?
C3 Ni1 N4 C3 180.0 2_776 . . . ?
S2 Ni1 N4 P5 -165.50(12) . . . . ?
S2 Ni1 N4 P5 14.50(12) 2_776 . . . ?
C3 Ni1 N4 P5 14.08(19) 2_776 . . . ?
C3 Ni1 N4 P5 -165.92(19) . . . . ?
C3 N4 P5 O7 149.21(16) . . . . ?
Ni1 N4 P5 O7 -49.17(12) . . . . ?
C3 N4 P5 O11 -105.22(16) . . . . ?
Ni1 N4 P5 O11 56.40(12) . . . . ?
C3 N4 P5 S6 24.34(18) . . . . ?
Ni1 N4 P5 S6 -174.04(8) . . . . ?
O11 P5 O7 C8 82.14(13) . . . . ?
N4 P5 O7 C8 -169.56(12) . . . . ?
S6 P5 O7 C8 -43.39(14) . . . . ?
P5 O7 C8 C10 -66.21(17) . . . . ?
P5 O7 C8 C9 171.46(11) . . . . ?
O7 P5 O11 C12 -148.86(12) . . . . ?
N4 P5 O11 C12 107.24(13) . . . . ?
S6 P5 O11 C12 -23.37(14) . . . . ?
P5 O11 C12 C14 165.47(12) . . . . ?
P5 O11 C12 C13 -72.22(17) . . . . ?
N4 C3 N15 C54 -179.39(17) . . . . ?
S2 C3 N15 C54 1.6(3) . . . . ?
C58 C51 C54 C57 1.1(2) . . . . ?
C63 C51 C54 C57 -178.87(16) . . . . ?
C58 C51 C54 N15 -174.21(14) . . . . ?
C63 C51 C54 N15 5.8(2) . . . . ?
C3 N15 C54 C57 108.4(2) . . . . ?
C3 N15 C54 C51 -76.2(2) . . . . ?
C59 C55 C56 C52 0.0(3) . . . . ?
C60 C52 C56 C55 179.54(17) . . . . ?
C58 C52 C56 C55 -0.3(2) . . . . ?
C51 C54 C57 C60 -0.6(3) . . . . ?
N15 C54 C57 C60 174.86(15) . . . . ?
C60 C52 C58 C51 -0.8(2) . . . . ?
C56 C52 C58 C51 179.11(15) . . . . ?
C60 C52 C58 C53 -179.22(16) . . . . ?
C56 C52 C58 C53 0.7(2) . . . . ?
C54 C51 C58 C52 -0.5(2) . . . . ?
C63 C51 C58 C52 179.54(15) . . . . ?
C54 C51 C58 C53 177.99(15) . . . . ?
C63 C51 C58 C53 -2.0(2) . . . . ?
C64 C53 C58 C52 -179.86(15) . . . . ?
C59 C53 C58 C52 -0.7(2) . . . . ?
C64 C53 C58 C51 1.7(2) . . . . ?
C59 C53 C58 C51 -179.12(14) . . . . ?
C64 C53 C59 C61 -0.7(2) . . . . ?
C58 C53 C59 C61 -179.87(16) . . . . ?
C64 C53 C59 C55 179.53(15) . . . . ?
C58 C53 C59 C55 0.3(2) . . . . ?
C56 C55 C59 C61 -179.79(17) . . . . ?
C56 C55 C59 C53 0.0(2) . . . . ?
C54 C57 C60 C52 -0.7(3) . . . . ?
C58 C52 C60 C57 1.4(3) . . . . ?
C56 C52 C60 C57 -178.50(16) . . . . ?
C53 C59 C61 C66 0.1(3) . . . . ?
C55 C59 C61 C66 179.91(17) . . . . ?
C64 C62 C63 C51 0.5(3) . . . . ?
C54 C51 C63 C62 -179.09(17) . . . . ?
C58 C51 C63 C62 0.9(2) . . . . ?
C59 C53 C64 C65 1.3(2) . . . . ?
C58 C53 C64 C65 -179.55(16) . . . . ?
C59 C53 C64 C62 -179.44(15) . . . . ?
C58 C53 C64 C62 -0.2(2) . . . . ?
C63 C62 C64 C65 178.40(17) . . . . ?
C63 C62 C64 C53 -0.9(2) . . . . ?
C53 C64 C65 C66 -1.3(3) . . . . ?
C62 C64 C65 C66 179.44(17) . . . . ?
C59 C61 C66 C65 -0.1(3) . . . . ?
C64 C65 C66 C61 0.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.615
_diffrn_reflns_theta_full        24.26
_diffrn_measured_fraction_theta_full 0.801
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.063
