# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_nipl16de
_database_code_depnum_ccdc_archive 'CCDC 1510789'
_audit_update_record             
;
2016-10-20 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_audit_creation_date             2015-08-18
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2015.06.29 svn.r3191 for OlexSys, GUI svn.r3563)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C56 H50 N6 Ni2 O4 P2 S2, 2(C3 H6 O)'
_chemical_formula_sum            'C62 H62 N6 Ni2 O6 P2 S2'
_chemical_formula_weight         1230.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C62 H62 N6 Ni2 O6 P2 S2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6317(7)
_cell_length_b                   11.2106(7)
_cell_length_c                   13.6662(8)
_cell_angle_alpha                102.602(5)
_cell_angle_beta                 91.453(5)
_cell_angle_gamma                101.450(6)
_cell_volume                     1407.79(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6421
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      32.5100
_cell_measurement_theta_min      2.5710
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.38.7t (release 04-09-2014 CrysAlis171 .NET)
(compiled Sep  4 2014,14:28:23)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             642
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of water and acetone by slow evaporation'
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.181
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12955
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.903
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1511
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -14.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679    0.0000  -90.0000 113

#__ type_ start__ end____ width___ exp.time_
  2 omega   21.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679   77.0000  -90.0000 76

#__ type_ start__ end____ width___ exp.time_
  3 omega  -22.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000   90.0000 91

#__ type_ start__ end____ width___ exp.time_
  4 omega    7.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000    0.0000 60

#__ type_ start__ end____ width___ exp.time_
  5 omega   10.00   71.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -103.0000 -154.0000 61

#__ type_ start__ end____ width___ exp.time_
  6 omega  -24.00   19.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000  150.0000 43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0727933000
_diffrn_orient_matrix_UB_12      -0.0025406000
_diffrn_orient_matrix_UB_13      -0.0119019000
_diffrn_orient_matrix_UB_21      0.0151928000
_diffrn_orient_matrix_UB_22      0.0041302000
_diffrn_orient_matrix_UB_23      -0.0498133000
_diffrn_orient_matrix_UB_31      -0.0120522000
_diffrn_orient_matrix_UB_32      -0.0661209000
_diffrn_orient_matrix_UB_33      -0.0148342000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           35
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5779
_reflns_number_total             6799
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.38.7t (release 04-09-2014 CrysAlis171 .NET)
(compiled Sep  4 2014,14:28:23)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.38.7t (release 04-09-2014 CrysAlis171 .NET)
(compiled Sep  4 2014,14:28:23)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.38.7t (release 04-09-2014 CrysAlis171 .NET)
(compiled Sep  4 2014,14:28:23)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         6799
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0401
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0467P)²+0.9172P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1045
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C22(H22), C8(H8), C19(H19), C12(H12), C26(H26), C20(H20), C13(H13),
 C27(H27), C25(H25), C2(H2), C11(H11), C24(H24), C28(H28), C7(H7), C21(H21),
 C14(H14), C9(H9), C15(H15)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.45769(3) 0.35334(2) 0.68047(2) 0.01505(8) Uani 1 1 d . . . . .
S1 S 0.58533(6) 0.47008(5) 0.80813(4) 0.01893(12) Uani 1 1 d . . . . .
P1 P 0.38584(6) 0.51126(5) 0.64267(4) 0.01458(12) Uani 1 1 d . . . . .
O2 O 0.13992(17) 0.15712(14) 0.42112(11) 0.0239(3) Uani 1 1 d . . . . .
O1 O 0.34121(16) 0.25787(13) 0.56794(11) 0.0193(3) Uani 1 1 d . . . . .
N1 N 0.6317(2) 0.23767(17) 0.78895(14) 0.0207(4) Uani 1 1 d . . . . .
N2 N 0.52728(18) 0.22047(16) 0.71147(13) 0.0173(3) Uani 1 1 d . . . . .
N3 N 0.7580(2) 0.39029(17) 0.92151(14) 0.0214(4) Uani 1 1 d . . . . .
H3 H 0.7745 0.4688 0.9491 0.026 Uiso 1 1 d R . . . .
C18 C 0.1279(2) 0.5813(2) 0.61131(17) 0.0226(5) Uani 1 1 d . . . . .
H18 H 0.1808 0.6455 0.5863 0.027 Uiso 1 1 calc R . . . .
C17 C 0.1950(2) 0.49711(19) 0.64480(15) 0.0170(4) Uani 1 1 d . . . . .
C6 C 0.0273(3) 0.0997(2) 0.34484(18) 0.0290(5) Uani 1 1 d . . . . .
H6A H 0.0628 0.0482 0.2896 0.043 Uiso 1 1 calc GR . . . .
H6B H -0.0090 0.1633 0.3217 0.043 Uiso 1 1 calc GR . . . .
H6C H -0.0474 0.0491 0.3721 0.043 Uiso 1 1 calc GR . . . .
C22 C 0.1159(2) 0.4037(2) 0.68506(16) 0.0216(4) Uani 1 1 d . . . . .
H22 H 0.1602 0.3472 0.7077 0.026 Uiso 1 1 calc R . . . .
C8 C 0.2324(3) -0.1280(2) 0.47597(18) 0.0268(5) Uani 1 1 d . . . . .
H8 H 0.2067 -0.2145 0.4544 0.032 Uiso 1 1 calc R . . . .
C19 C -0.0178(3) 0.5697(2) 0.61518(18) 0.0277(5) Uani 1 1 d . . . . .
H19 H -0.0629 0.6246 0.5909 0.033 Uiso 1 1 calc R . . . .
C12 C 0.9053(3) 0.1301(2) 0.98245(19) 0.0312(5) Uani 1 1 d . . . . .
H12 H 0.9008 0.0451 0.9584 0.037 Uiso 1 1 calc R . . . .
C10 C 0.8335(2) 0.3195(2) 0.96690(16) 0.0191(4) Uani 1 1 d . . . . .
C26 C 0.5421(3) 0.9070(2) 0.84023(19) 0.0322(6) Uani 1 1 d . . . . .
H26 H 0.5724 0.9870 0.8806 0.039 Uiso 1 1 calc R . . . .
C20 C -0.0960(2) 0.4767(2) 0.65516(18) 0.0281(5) Uani 1 1 d . . . . .
H20 H -0.1937 0.4689 0.6577 0.034 Uiso 1 1 calc R . . . .
C13 C 0.9868(3) 0.1922(2) 1.07007(19) 0.0319(6) Uani 1 1 d . . . . .
H13 H 1.0367 0.1494 1.1047 0.038 Uiso 1 1 calc R . . . .
C4 C 0.3091(2) 0.13553(18) 0.54101(15) 0.0174(4) Uani 1 1 d . . . . .
C27 C 0.4219(3) 0.8295(3) 0.8607(2) 0.0417(7) Uani 1 1 d . . . . .
H27 H 0.3700 0.8574 0.9143 0.050 Uiso 1 1 calc R . . . .
C25 C 0.6171(3) 0.8659(2) 0.76003(18) 0.0258(5) Uani 1 1 d . . . . .
H25 H 0.6991 0.9179 0.7471 0.031 Uiso 1 1 calc R . . . .
C23 C 0.4518(2) 0.66834(18) 0.71855(15) 0.0175(4) Uani 1 1 d . . . . .
C5 C 0.2009(2) 0.0770(2) 0.46205(16) 0.0196(4) Uani 1 1 d . . . . .
C3 C 0.3751(2) 0.05669(19) 0.58528(16) 0.0197(4) Uani 1 1 d . . . . .
C2 C 0.4850(2) 0.10447(19) 0.66427(16) 0.0210(4) Uani 1 1 d . . . . .
H2 H 0.5308 0.0469 0.6838 0.025 Uiso 1 1 calc R . . . .
C1 C 0.6621(2) 0.35257(19) 0.83981(16) 0.0188(4) Uani 1 1 d . . . . .
C11 C 0.8298(3) 0.1924(2) 0.92957(18) 0.0254(5) Uani 1 1 d . . . . .
H11 H 0.7773 0.1497 0.8698 0.030 Uiso 1 1 calc R . . . .
C24 C 0.5720(2) 0.7476(2) 0.69815(17) 0.0217(4) Uani 1 1 d . . . . .
H24 H 0.6222 0.7216 0.6431 0.026 Uiso 1 1 calc R . . . .
C28 C 0.3787(3) 0.7096(2) 0.80112(19) 0.0351(6) Uani 1 1 d . . . . .
H28 H 0.2997 0.6563 0.8167 0.042 Uiso 1 1 calc R . . . .
C16 C 0.4275(2) 0.51580(19) 0.51242(15) 0.0168(4) Uani 1 1 d . . . . .
H16A H 0.3542 0.4568 0.4665 0.020 Uiso 1 1 calc R . . . .
H16B H 0.4268 0.5986 0.5021 0.020 Uiso 1 1 calc R . . . .
C7 C 0.1646(3) -0.0517(2) 0.43115(17) 0.0241(5) Uani 1 1 d . . . . .
H7 H 0.0940 -0.0883 0.3797 0.029 Uiso 1 1 calc R . . . .
C21 C -0.0289(2) 0.3951(2) 0.69141(18) 0.0266(5) Uani 1 1 d . . . . .
H21 H -0.0813 0.3342 0.7202 0.032 Uiso 1 1 calc R . . . .
C14 C 0.9934(3) 0.3180(2) 1.10566(17) 0.0270(5) Uani 1 1 d . . . . .
H14 H 1.0493 0.3606 1.1641 0.032 Uiso 1 1 calc R . . . .
C9 C 0.3364(3) -0.0748(2) 0.55132(17) 0.0251(5) Uani 1 1 d . . . . .
H9 H 0.3821 -0.1254 0.5806 0.030 Uiso 1 1 calc R . . . .
C15 C 0.9175(2) 0.3819(2) 1.05535(16) 0.0226(4) Uani 1 1 d . . . . .
H15 H 0.9223 0.4668 1.0804 0.027 Uiso 1 1 calc R . . . .
O3 O 0.2134(3) 0.36643(19) 0.92431(15) 0.0482(5) Uani 1 1 d . . . . .
C30 C 0.3653(4) 0.2455(3) 0.9703(2) 0.0540(8) Uani 1 1 d . . . . .
H30A H 0.4172 0.3236 1.0106 0.081 Uiso 1 1 calc GR . . . .
H30B H 0.4282 0.2061 0.9270 0.081 Uiso 1 1 calc GR . . . .
H30C H 0.3261 0.1920 1.0132 0.081 Uiso 1 1 calc GR . . . .
C31 C 0.1787(4) 0.1600(3) 0.8243(2) 0.0471(8) Uani 1 1 d . . . . .
H31A H 0.0865 0.1721 0.8061 0.071 Uiso 1 1 calc GR . . . .
H31B H 0.1691 0.0830 0.8459 0.071 Uiso 1 1 calc GR . . . .
H31C H 0.2351 0.1568 0.7673 0.071 Uiso 1 1 calc GR . . . .
C29 C 0.2509(3) 0.2680(3) 0.9095(2) 0.0354(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.1269(6) . ?
Ni1 P1 2.1790(6) . ?
Ni1 O1 1.8673(14) . ?
Ni1 N2 1.8720(18) . ?
S1 C1 1.757(2) . ?
P1 C17 1.814(2) . ?
P1 C23 1.818(2) . ?
P1 C16 1.844(2) . ?
O2 C6 1.432(3) . ?
O2 C5 1.370(3) . ?
O1 C4 1.311(2) . ?
N1 N2 1.396(2) . ?
N1 C1 1.295(3) . ?
N2 C2 1.298(3) . ?
N3 H3 0.8597 . ?
N3 C10 1.401(3) . ?
N3 C1 1.366(3) . ?
C18 H18 0.9300 . ?
C18 C17 1.391(3) . ?
C18 C19 1.387(3) . ?
C17 C22 1.391(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C22 H22 0.9300 . ?
C22 C21 1.385(3) . ?
C8 H8 0.9300 . ?
C8 C7 1.401(3) . ?
C8 C9 1.364(3) . ?
C19 H19 0.9300 . ?
C19 C20 1.383(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.380(3) . ?
C12 C11 1.390(3) . ?
C10 C11 1.398(3) . ?
C10 C15 1.401(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.377(4) . ?
C26 C25 1.374(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.384(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.377(3) . ?
C4 C5 1.429(3) . ?
C4 C3 1.410(3) . ?
C27 H27 0.9300 . ?
C27 C28 1.388(3) . ?
C25 H25 0.9300 . ?
C25 C24 1.387(3) . ?
C23 C24 1.387(3) . ?
C23 C28 1.388(3) . ?
C5 C7 1.382(3) . ?
C3 C2 1.427(3) . ?
C3 C9 1.415(3) . ?
C2 H2 0.9300 . ?
C11 H11 0.9300 . ?
C24 H24 0.9300 . ?
C28 H28 0.9300 . ?
C16 C16 1.535(4) 2_666 ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C7 H7 0.9300 . ?
C21 H21 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.384(3) . ?
C9 H9 0.9300 . ?
C15 H15 0.9300 . ?
O3 C29 1.205(3) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30 C29 1.458(4) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C31 C29 1.521(4) . ?

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
S1 Ni1 P1 92.06(2) . . ?
O1 Ni1 S1 176.99(5) . . ?
O1 Ni1 P1 84.99(5) . . ?
O1 Ni1 N2 95.93(7) . . ?
N2 Ni1 S1 87.03(5) . . ?
N2 Ni1 P1 177.52(6) . . ?
C1 S1 Ni1 96.16(7) . . ?
C17 P1 Ni1 113.04(7) . . ?
C17 P1 C23 101.93(10) . . ?
C17 P1 C16 105.82(9) . . ?
C23 P1 Ni1 120.07(7) . . ?
C23 P1 C16 106.60(10) . . ?
C16 P1 Ni1 108.35(7) . . ?
C5 O2 C6 115.86(17) . . ?
C4 O1 Ni1 126.08(13) . . ?
C1 N1 N2 111.33(18) . . ?
N1 N2 Ni1 122.50(13) . . ?
C2 N2 Ni1 124.32(15) . . ?
C2 N2 N1 113.18(18) . . ?
C10 N3 H3 115.3 . . ?
C1 N3 H3 115.3 . . ?
C1 N3 C10 129.36(18) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C19 C18 C17 120.1(2) . . ?
C18 C17 P1 121.18(16) . . ?
C18 C17 C22 119.6(2) . . ?
C22 C17 P1 119.12(17) . . ?
O2 C6 H6A 109.5 . . ?
O2 C6 H6B 109.5 . . ?
O2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C17 C22 H22 120.1 . . ?
C21 C22 C17 119.9(2) . . ?
C21 C22 H22 120.1 . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C9 C8 C7 119.7(2) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.0(2) . . ?
C20 C19 H19 120.0 . . ?
C13 C12 H12 119.4 . . ?
C13 C12 C11 121.2(2) . . ?
C11 C12 H12 119.4 . . ?
C11 C10 N3 124.30(19) . . ?
C11 C10 C15 118.8(2) . . ?
C15 C10 N3 116.92(19) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C25 C26 C27 119.8(2) . . ?
C19 C20 H20 120.0 . . ?
C19 C20 C21 120.0(2) . . ?
C21 C20 H20 120.0 . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.3(2) . . ?
C14 C13 H13 120.3 . . ?
O1 C4 C5 118.78(19) . . ?
O1 C4 C3 123.95(18) . . ?
C3 C4 C5 117.28(18) . . ?
C26 C27 H27 120.1 . . ?
C26 C27 C28 119.7(2) . . ?
C28 C27 H27 120.1 . . ?
C26 C25 H25 119.6 . . ?
C26 C25 C24 120.8(2) . . ?
C24 C25 H25 119.6 . . ?
C24 C23 P1 123.04(17) . . ?
C24 C23 C28 118.88(19) . . ?
C28 C23 P1 118.07(16) . . ?
O2 C5 C4 115.29(18) . . ?
O2 C5 C7 124.23(19) . . ?
C7 C5 C4 120.5(2) . . ?
C4 C3 C2 122.28(19) . . ?
C4 C3 C9 120.87(19) . . ?
C9 C3 C2 116.8(2) . . ?
N2 C2 C3 126.3(2) . . ?
N2 C2 H2 116.8 . . ?
C3 C2 H2 116.8 . . ?
N1 C1 S1 122.72(16) . . ?
N1 C1 N3 121.63(19) . . ?
N3 C1 S1 115.65(15) . . ?
C12 C11 C10 119.6(2) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C25 C24 H24 120.0 . . ?
C23 C24 C25 119.9(2) . . ?
C23 C24 H24 120.0 . . ?
C27 C28 H28 119.6 . . ?
C23 C28 C27 120.8(2) . . ?
C23 C28 H28 119.6 . . ?
P1 C16 H16A 109.0 . . ?
P1 C16 H16B 109.0 . . ?
C16 C16 P1 112.73(18) 2_666 . ?
C16 C16 H16A 109.0 2_666 . ?
C16 C16 H16B 109.0 2_666 . ?
H16A C16 H16B 107.8 . . ?
C8 C7 H7 119.4 . . ?
C5 C7 C8 121.1(2) . . ?
C5 C7 H7 119.4 . . ?
C22 C21 H21 119.9 . . ?
C20 C21 C22 120.3(2) . . ?
C20 C21 H21 119.9 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.6(2) . . ?
C15 C14 H14 119.7 . . ?
C8 C9 C3 120.5(2) . . ?
C8 C9 H9 119.7 . . ?
C3 C9 H9 119.7 . . ?
C10 C15 H15 119.8 . . ?
C14 C15 C10 120.4(2) . . ?
C14 C15 H15 119.8 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
O3 C29 C30 122.9(3) . . ?
O3 C29 C31 120.4(3) . . ?
C30 C29 C31 116.7(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S1 C1 N1 -0.2(2) . . . . ?
Ni1 S1 C1 N3 179.05(15) . . . . ?
Ni1 P1 C17 C18 -172.34(15) . . . . ?
Ni1 P1 C17 C22 10.68(18) . . . . ?
Ni1 P1 C23 C24 90.64(19) . . . . ?
Ni1 P1 C23 C28 -88.7(2) . . . . ?
Ni1 P1 C16 C16 -39.5(2) . . . 2_666 ?
Ni1 O1 C4 C5 170.20(14) . . . . ?
Ni1 O1 C4 C3 -9.9(3) . . . . ?
Ni1 N2 C2 C3 -3.4(3) . . . . ?
S1 Ni1 N2 N1 -4.99(15) . . . . ?
S1 Ni1 N2 C2 175.11(19) . . . . ?
P1 Ni1 O1 C4 -171.37(17) . . . . ?
P1 C17 C22 C21 177.10(16) . . . . ?
P1 C23 C24 C25 -179.26(18) . . . . ?
P1 C23 C28 C27 -178.6(2) . . . . ?
O2 C5 C7 C8 179.5(2) . . . . ?
O1 Ni1 N2 N1 175.50(16) . . . . ?
O1 Ni1 N2 C2 -4.4(2) . . . . ?
O1 C4 C5 O2 0.1(3) . . . . ?
O1 C4 C5 C7 179.6(2) . . . . ?
O1 C4 C3 C2 -0.3(3) . . . . ?
O1 C4 C3 C9 -179.1(2) . . . . ?
N1 N2 C2 C3 176.7(2) . . . . ?
N2 Ni1 O1 C4 10.94(18) . . . . ?
N2 N1 C1 S1 -3.1(3) . . . . ?
N2 N1 C1 N3 177.71(19) . . . . ?
N3 C10 C11 C12 -177.9(2) . . . . ?
N3 C10 C15 C14 178.9(2) . . . . ?
C18 C17 C22 C21 0.1(3) . . . . ?
C18 C19 C20 C21 0.1(3) . . . . ?
C17 P1 C23 C24 -143.59(19) . . . . ?
C17 P1 C23 C28 37.1(2) . . . . ?
C17 P1 C16 C16 -160.99(19) . . . 2_666 ?
C17 C18 C19 C20 1.9(3) . . . . ?
C17 C22 C21 C20 1.9(3) . . . . ?
C6 O2 C5 C4 -177.46(19) . . . . ?
C6 O2 C5 C7 3.0(3) . . . . ?
C19 C18 C17 P1 -178.96(17) . . . . ?
C19 C18 C17 C22 -2.0(3) . . . . ?
C19 C20 C21 C22 -2.0(3) . . . . ?
C12 C13 C14 C15 1.1(4) . . . . ?
C10 N3 C1 S1 178.02(18) . . . . ?
C10 N3 C1 N1 -2.7(4) . . . . ?
C26 C27 C28 C23 -2.6(5) . . . . ?
C26 C25 C24 C23 -1.6(4) . . . . ?
C13 C12 C11 C10 -1.6(4) . . . . ?
C13 C14 C15 C10 -0.4(4) . . . . ?
C4 C5 C7 C8 -0.1(4) . . . . ?
C4 C3 C2 N2 7.5(4) . . . . ?
C4 C3 C9 C8 -1.1(4) . . . . ?
C27 C26 C25 C24 1.1(4) . . . . ?
C25 C26 C27 C28 1.0(5) . . . . ?
C23 P1 C17 C18 57.39(19) . . . . ?
C23 P1 C17 C22 -119.59(17) . . . . ?
C23 P1 C16 C16 91.0(2) . . . 2_666 ?
C5 C4 C3 C2 179.6(2) . . . . ?
C5 C4 C3 C9 0.9(3) . . . . ?
C3 C4 C5 O2 -179.88(19) . . . . ?
C3 C4 C5 C7 -0.3(3) . . . . ?
C2 C3 C9 C8 -179.9(2) . . . . ?
C1 N1 N2 Ni1 5.8(2) . . . . ?
C1 N1 N2 C2 -174.3(2) . . . . ?
C1 N3 C10 C11 4.9(4) . . . . ?
C1 N3 C10 C15 -175.2(2) . . . . ?
C11 C12 C13 C14 0.0(4) . . . . ?
C11 C10 C15 C14 -1.2(3) . . . . ?
C24 C23 C28 C27 2.0(4) . . . . ?
C28 C23 C24 C25 0.1(3) . . . . ?
C16 P1 C17 C18 -53.92(19) . . . . ?
C16 P1 C17 C22 129.10(17) . . . . ?
C16 P1 C23 C24 -32.9(2) . . . . ?
C16 P1 C23 C28 147.8(2) . . . . ?
C7 C8 C9 C3 0.7(4) . . . . ?
C9 C8 C7 C5 -0.1(4) . . . . ?
C9 C3 C2 N2 -173.7(2) . . . . ?
C15 C10 C11 C12 2.2(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 -15 0 0.1194 -1.2105 -14.6434 -0.4733 0.1310 -0.0553 0.9898
13 -1 -3 0.0902 13.4216 -1.1632 -2.6467 -0.9425 0.3309 -0.0456
-1 15 1 0.1361 -1.1560 15.1118 0.9527 0.0344 -0.0026 -0.9994
-13 2 3 0.0852 -13.4742 2.0017 2.6973 0.9436 -0.3308 -0.0100
1 -15 0 0.1214 0.8620 -15.1690 -0.4637 -0.0187 -0.0265 0.9995
-1 1 -19 0.1165 -1.3605 0.9817 -18.7827 0.3201 0.9190 0.2301
-1 16 -6 0.1251 -1.3284 15.6713 -5.8354 0.1263 0.3352 -0.9336
1 -1 19 0.1121 1.3316 -0.5943 18.6942 -0.3179 -0.9134 -0.2541

_olex2_date_sample_data_collection 2015-08-17
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id NiPL16DE
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_rpn14de
_database_code_depnum_ccdc_archive 'CCDC 1510790'
_audit_update_record             
;
2016-10-20 deposited with the CCDC.
2017-02-16 downloaded from the CCDC.
;
_audit_creation_date             2014-09-10
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r3563)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H42 N6 Ni2 O4 P2 S2, 2(C3 H7 N O)'
_chemical_formula_sum            'C50 H56 N8 Ni2 O6 P2 S2'
_chemical_formula_weight         1108.50
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5619(11)
_cell_length_b                   11.0171(12)
_cell_length_c                   11.3222(12)
_cell_angle_alpha                93.080(4)
_cell_angle_beta                 108.522(3)
_cell_angle_gamma                98.363(3)
_cell_volume                     1228.9(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4581
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.304
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1338 before and 0.1036 after correction.
The Ratio of minimum to maximum transmission is 0.7395.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             578
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 
'The material was recrystallised from DMF by slow evaporation'
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.024
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0980
_diffrn_reflns_av_unetI/netI     0.1143
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16394
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.304
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3848
_reflns_number_total             5617
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5617
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0609
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0704P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1582
_refine_special_details          
'This structure was refined with olex2.refine. Owing to the ShelXL specific world-view of CheckCif, this causes some spurious CheckCif Alerts. All hydrogen atoms have been refined as constrained, using the riding model. Their coordinates are reported with e.s.d. values as they should. CheckCif takes the presence of these e.s.d values as a marker that these atoms have been refined freely, which is not the case: they value "constr" provided in the cif is correct.'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H3B \\sim N3-H3A
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C1S(H1S)
3.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.09434(5) 0.66906(4) 0.78209(4) 0.01651(16) Uani 1 1 d . . . . .
S3 S -0.07606(9) 0.66143(8) 0.84388(9) 0.0199(2) Uani 1 1 d . . . . .
P2 P 0.04263(9) 0.47538(9) 0.70323(9) 0.0158(2) Uani 1 1 d . . . . .
O1 O 0.2402(3) 0.6666(2) 0.7261(2) 0.0208(6) Uani 1 1 d . . . . .
O2 O 0.4427(3) 0.5990(2) 0.6735(2) 0.0260(6) Uani 1 1 d . . . . .
N1 N 0.1518(3) 0.8318(3) 0.8619(3) 0.0171(7) Uani 1 1 d . . . . .
N2 N 0.0758(3) 0.8869(3) 0.9242(3) 0.0191(7) Uani 1 1 d . . . . .
N3 N -0.1113(3) 0.8452(3) 0.9853(3) 0.0254(8) Uani 1 1 d . . . . .
C1 C -0.0316(4) 0.8101(3) 0.9235(3) 0.0188(8) Uani 1 1 d . . . . .
C2 C 0.2647(4) 0.9024(3) 0.8674(3) 0.0198(8) Uani 1 1 d . . . . .
H2 H 0.2805 0.9846 0.9058 0.024 Uiso 1 1 calc R . . . .
C3 C 0.3666(4) 0.8672(3) 0.8210(3) 0.0192(8) Uani 1 1 d . . . . .
C4 C 0.4871(4) 0.9519(3) 0.8439(3) 0.0200(8) Uani 1 1 d . . . . .
H4 H 0.4957 1.0321 0.8839 0.024 Uiso 1 1 calc R . . . .
C5 C 0.5925(4) 0.9207(4) 0.8098(4) 0.0225(9) Uani 1 1 d . . . . .
H5 H 0.6728 0.9794 0.8254 0.027 Uiso 1 1 calc R . . . .
C6 C 0.5819(4) 0.8021(4) 0.7518(4) 0.0243(9) Uani 1 1 d . . . . .
H6 H 0.6557 0.7801 0.7297 0.029 Uiso 1 1 calc R . . . .
C7 C 0.4640(4) 0.7173(3) 0.7266(3) 0.0199(8) Uani 1 1 d . . . . .
C8 C 0.3511(4) 0.7490(3) 0.7565(3) 0.0185(8) Uani 1 1 d . . . . .
C10 C 0.0418(4) 0.4574(3) 0.5410(3) 0.0168(8) Uani 1 1 d . . . . .
H10A H 0.1362 0.4753 0.5403 0.020 Uiso 1 1 calc R . . . .
H10B H 0.0041 0.3707 0.5051 0.020 Uiso 1 1 calc R . . . .
C11 C -0.1120(4) 0.3807(3) 0.7057(3) 0.0157(7) Uani 1 1 d . . . . .
C12 C -0.1251(4) 0.3575(3) 0.8215(4) 0.0214(8) Uani 1 1 d . . . . .
H12 H -0.0537 0.3905 0.8964 0.026 Uiso 1 1 calc R . . . .
C13 C -0.2426(4) 0.2860(4) 0.8279(4) 0.0243(9) Uani 1 1 d . . . . .
H13 H -0.2504 0.2700 0.9071 0.029 Uiso 1 1 calc R . . . .
C14 C -0.3463(4) 0.2392(4) 0.7208(4) 0.0264(9) Uani 1 1 d . . . . .
H14 H -0.4265 0.1910 0.7256 0.032 Uiso 1 1 calc R . . . .
C15 C -0.3348(4) 0.2618(4) 0.6051(4) 0.0258(9) Uani 1 1 d . . . . .
H15 H -0.4074 0.2290 0.5308 0.031 Uiso 1 1 calc R . . . .
C16 C -0.2190(4) 0.3313(3) 0.5969(3) 0.0188(8) Uani 1 1 d . . . . .
H16 H -0.2118 0.3458 0.5171 0.023 Uiso 1 1 calc R . . . .
C21 C 0.1773(4) 0.3974(3) 0.7913(3) 0.0170(8) Uani 1 1 d . . . . .
C22 C 0.2572(4) 0.4455(4) 0.9127(4) 0.0240(9) Uani 1 1 d . . . . .
H22 H 0.2391 0.5179 0.9493 0.029 Uiso 1 1 calc R . . . .
C23 C 0.3623(4) 0.3898(4) 0.9810(4) 0.0275(9) Uani 1 1 d . . . . .
H23 H 0.4141 0.4224 1.0647 0.033 Uiso 1 1 calc R . . . .
C24 C 0.3917(4) 0.2872(4) 0.9275(4) 0.0305(10) Uani 1 1 d . . . . .
H24 H 0.4657 0.2503 0.9732 0.037 Uiso 1 1 calc R . . . .
C25 C 0.3145(4) 0.2384(4) 0.8086(4) 0.0325(10) Uani 1 1 d . . . . .
H25 H 0.3341 0.1665 0.7728 0.039 Uiso 1 1 calc R . . . .
C26 C 0.2070(4) 0.2930(4) 0.7388(4) 0.0253(9) Uani 1 1 d . . . . .
H26 H 0.1545 0.2587 0.6558 0.030 Uiso 1 1 calc R . . . .
C29 C 0.5586(4) 0.5559(4) 0.6590(4) 0.0357(11) Uani 1 1 d . . . . .
H29A H 0.5883 0.6014 0.5977 0.054 Uiso 1 1 calc GR . . . .
H29B H 0.5349 0.4677 0.6295 0.054 Uiso 1 1 calc GR . . . .
H29C H 0.6320 0.5692 0.7397 0.054 Uiso 1 1 calc GR . . . .
O1S O 0.0172(4) -0.1486(3) 0.5058(3) 0.0499(9) Uani 1 1 d . . . . .
N1S N 0.1774(4) -0.0222(4) 0.4530(4) 0.0431(10) Uani 1 1 d . . . . .
C1S C 0.1286(5) -0.0834(4) 0.5322(4) 0.0391(11) Uani 1 1 d . . . . .
H1S H 0.1857 -0.0756 0.6171 0.047 Uiso 1 1 calc R . . . .
C2S C 0.3071(5) 0.0544(6) 0.4956(5) 0.0635(17) Uani 1 1 d . . . . .
H2SA H 0.2962 0.1410 0.4914 0.095 Uiso 1 1 calc GR . . . .
H2SB H 0.3597 0.0335 0.4423 0.095 Uiso 1 1 calc GR . . . .
H2SC H 0.3548 0.0414 0.5823 0.095 Uiso 1 1 calc GR . . . .
C3S C 0.0950(5) -0.0255(6) 0.3222(5) 0.0607(16) Uani 1 1 d . . . . .
H3SA H 0.0137 -0.0886 0.3035 0.091 Uiso 1 1 calc GR . . . .
H3SB H 0.1475 -0.0454 0.2685 0.091 Uiso 1 1 calc GR . . . .
H3SC H 0.0683 0.0552 0.3066 0.091 Uiso 1 1 calc GR . . . .
H3A H -0.094(4) 0.921(3) 1.026(4) 0.029(12) Uiso 1 1 d . . . . .
H3B H -0.191(3) 0.798(4) 0.977(4) 0.040(13) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S3 2.1209(10) . ?
Ni1 P2 2.1897(10) . ?
Ni1 O1 1.846(3) . ?
Ni1 N1 1.887(3) . ?
S3 C1 1.751(4) . ?
P2 C10 1.834(3) . ?
P2 C11 1.815(4) . ?
P2 C21 1.817(4) . ?
O1 C8 1.310(4) . ?
O2 C7 1.362(4) . ?
O2 C29 1.427(4) . ?
N1 N2 1.403(4) . ?
N1 C2 1.308(4) . ?
N2 C1 1.310(5) . ?
N3 C1 1.337(5) . ?
N3 H3A 0.90(3) . ?
N3 H3B 0.90(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.429(5) . ?
C3 C4 1.406(5) . ?
C3 C8 1.420(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.370(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.403(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(5) . ?
C7 C8 1.423(5) . ?
C10 C10 1.529(7) 2_566 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.394(5) . ?
C11 C16 1.399(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.394(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.364(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.386(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.378(5) . ?
C16 H16 0.9500 . ?
C21 C22 1.392(5) . ?
C21 C26 1.387(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.383(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.374(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.364(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.399(5) . ?
C26 H26 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O1S C1S 1.224(5) . ?
N1S C1S 1.335(6) . ?
N1S C2S 1.422(6) . ?
N1S C3S 1.455(6) . ?
C1S H1S 0.9500 . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 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
S3 Ni1 P2 94.21(4) . . ?
O1 Ni1 S3 176.90(8) . . ?
O1 Ni1 P2 82.72(8) . . ?
O1 Ni1 N1 95.68(12) . . ?
N1 Ni1 S3 87.35(9) . . ?
N1 Ni1 P2 174.77(10) . . ?
C1 S3 Ni1 96.75(13) . . ?
C10 P2 Ni1 112.07(12) . . ?
C11 P2 Ni1 120.19(12) . . ?
C11 P2 C10 106.30(16) . . ?
C11 P2 C21 104.48(16) . . ?
C21 P2 Ni1 107.38(12) . . ?
C21 P2 C10 105.22(16) . . ?
C8 O1 Ni1 127.1(2) . . ?
C7 O2 C29 116.1(3) . . ?
N2 N1 Ni1 121.7(2) . . ?
C2 N1 Ni1 124.5(3) . . ?
C2 N1 N2 113.7(3) . . ?
C1 N2 N1 111.6(3) . . ?
C1 N3 H3A 121(3) . . ?
C1 N3 H3B 120(3) . . ?
H3A N3 H3B 118(4) . . ?
N2 C1 S3 122.4(3) . . ?
N2 C1 N3 119.6(3) . . ?
N3 C1 S3 118.0(3) . . ?
N1 C2 H2 117.1 . . ?
N1 C2 C3 125.9(3) . . ?
C3 C2 H2 117.1 . . ?
C4 C3 C2 118.3(3) . . ?
C4 C3 C8 119.6(3) . . ?
C8 C3 C2 122.1(3) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 C3 121.2(4) . . ?
C5 C4 H4 119.4 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.1(3) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.1(3) . . ?
C7 C6 H6 119.9 . . ?
O2 C7 C6 125.5(3) . . ?
O2 C7 C8 113.6(3) . . ?
C6 C7 C8 120.9(3) . . ?
O1 C8 C3 123.8(3) . . ?
O1 C8 C7 118.3(3) . . ?
C3 C8 C7 118.0(3) . . ?
P2 C10 H10A 109.1 . . ?
P2 C10 H10B 109.1 . . ?
C10 C10 P2 112.4(3) 2_566 . ?
C10 C10 H10A 109.1 2_566 . ?
C10 C10 H10B 109.1 2_566 . ?
H10A C10 H10B 107.9 . . ?
C12 C11 P2 118.4(3) . . ?
C12 C11 C16 118.6(3) . . ?
C16 C11 P2 123.0(3) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.4(4) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.3(4) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C15 120.0(4) . . ?
C15 C14 H14 120.0 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.6(4) . . ?
C16 C15 H15 119.7 . . ?
C11 C16 H16 119.9 . . ?
C15 C16 C11 120.2(3) . . ?
C15 C16 H16 119.9 . . ?
C22 C21 P2 119.8(3) . . ?
C26 C21 P2 121.6(3) . . ?
C26 C21 C22 118.5(4) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 C21 121.2(4) . . ?
C23 C22 H22 119.4 . . ?
C22 C23 H23 120.1 . . ?
C24 C23 C22 119.8(4) . . ?
C24 C23 H23 120.1 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.0(4) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 119.6 . . ?
C24 C25 C26 120.9(4) . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C25 119.7(4) . . ?
C21 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
O2 C29 H29A 109.5 . . ?
O2 C29 H29B 109.5 . . ?
O2 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C1S N1S C2S 121.1(4) . . ?
C1S N1S C3S 120.6(4) . . ?
C2S N1S C3S 118.2(4) . . ?
O1S C1S N1S 126.1(5) . . ?
O1S C1S H1S 116.9 . . ?
N1S C1S H1S 116.9 . . ?
N1S C2S H2SA 109.5 . . ?
N1S C2S H2SB 109.5 . . ?
N1S C2S H2SC 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
N1S C3S H3SA 109.5 . . ?
N1S C3S H3SB 109.5 . . ?
N1S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?

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
N3 H3A N2 0.90(3) 2.12(3) 3.002(5) 165(4) 2_577

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 S3 C1 N2 3.2(3) . . . . ?
Ni1 S3 C1 N3 -176.9(3) . . . . ?
Ni1 P2 C10 C10 -50.0(4) . . . 2_566 ?
Ni1 P2 C11 C12 -64.0(3) . . . . ?
Ni1 P2 C11 C16 115.1(3) . . . . ?
Ni1 P2 C21 C22 23.9(3) . . . . ?
Ni1 P2 C21 C26 -153.4(3) . . . . ?
Ni1 O1 C8 C3 -12.4(5) . . . . ?
Ni1 O1 C8 C7 165.8(3) . . . . ?
Ni1 N1 N2 C1 2.9(4) . . . . ?
Ni1 N1 C2 C3 -3.7(5) . . . . ?
S3 Ni1 N1 N2 -0.8(2) . . . . ?
S3 Ni1 N1 C2 177.7(3) . . . . ?
P2 Ni1 O1 C8 -165.4(3) . . . . ?
P2 C11 C12 C13 179.5(3) . . . . ?
P2 C11 C16 C15 -178.9(3) . . . . ?
P2 C21 C22 C23 -178.5(3) . . . . ?
P2 C21 C26 C25 177.8(3) . . . . ?
O1 Ni1 N1 N2 179.8(2) . . . . ?
O1 Ni1 N1 C2 -1.7(3) . . . . ?
O2 C7 C8 O1 -2.9(5) . . . . ?
O2 C7 C8 C3 175.3(3) . . . . ?
N1 Ni1 O1 C8 9.6(3) . . . . ?
N1 N2 C1 S3 -4.0(4) . . . . ?
N1 N2 C1 N3 176.0(3) . . . . ?
N1 C2 C3 C4 -174.8(3) . . . . ?
N1 C2 C3 C8 3.1(6) . . . . ?
N2 N1 C2 C3 174.9(3) . . . . ?
C2 N1 N2 C1 -175.7(3) . . . . ?
C2 C3 C4 C5 175.3(4) . . . . ?
C2 C3 C8 O1 5.3(6) . . . . ?
C2 C3 C8 C7 -172.9(3) . . . . ?
C3 C4 C5 C6 -0.6(6) . . . . ?
C4 C3 C8 O1 -176.7(3) . . . . ?
C4 C3 C8 C7 5.1(5) . . . . ?
C4 C5 C6 C7 1.3(6) . . . . ?
C5 C6 C7 O2 -178.5(3) . . . . ?
C5 C6 C7 C8 1.3(6) . . . . ?
C6 C7 C8 O1 177.3(3) . . . . ?
C6 C7 C8 C3 -4.4(5) . . . . ?
C8 C3 C4 C5 -2.7(6) . . . . ?
C10 P2 C11 C12 167.5(3) . . . . ?
C10 P2 C11 C16 -13.4(4) . . . . ?
C10 P2 C21 C22 143.4(3) . . . . ?
C10 P2 C21 C26 -33.8(4) . . . . ?
C11 P2 C10 C10 83.2(4) . . . 2_566 ?
C11 P2 C21 C22 -104.8(3) . . . . ?
C11 P2 C21 C26 77.9(3) . . . . ?
C11 C12 C13 C14 -0.6(6) . . . . ?
C12 C11 C16 C15 0.3(5) . . . . ?
C12 C13 C14 C15 0.4(6) . . . . ?
C13 C14 C15 C16 0.1(6) . . . . ?
C14 C15 C16 C11 -0.5(6) . . . . ?
C16 C11 C12 C13 0.3(5) . . . . ?
C21 P2 C10 C10 -166.4(3) . . . 2_566 ?
C21 P2 C11 C12 56.5(3) . . . . ?
C21 P2 C11 C16 -124.4(3) . . . . ?
C21 C22 C23 C24 1.9(6) . . . . ?
C22 C21 C26 C25 0.5(6) . . . . ?
C22 C23 C24 C25 -2.0(6) . . . . ?
C23 C24 C25 C26 1.4(6) . . . . ?
C24 C25 C26 C21 -0.6(6) . . . . ?
C26 C21 C22 C23 -1.2(6) . . . . ?
C29 O2 C7 C6 9.0(5) . . . . ?
C29 O2 C7 C8 -170.8(3) . . . . ?
C2S N1S C1S O1S 177.8(5) . . . . ?
C3S N1S C1S O1S 2.2(8) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems 700 Series'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id NiPL14DE
_olex2_submission_special_instructions 'No special instructions were received'
