# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1532640'
_audit_update_record             
;
2019-12-24 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H36 Ni O3 P2 S3'
_chemical_formula_weight         769.51

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.9263(10)
_cell_length_b                   18.2168(15)
_cell_length_c                   18.4634(13)
_cell_angle_alpha                90
_cell_angle_beta                 98.987(6)
_cell_angle_gamma                90
_cell_volume                     3629.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    22755
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.24
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_reflns_number            22750
_diffrn_reflns_av_unetI/netI     0.1764
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.335
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             10292
_reflns_number_gt                4825
_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_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_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)+(0.0820P)²] 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         10292
_refine_ls_number_parameters     439
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1788
_refine_ls_R_factor_gt           0.0814
_refine_ls_wR_factor_ref         0.2102
_refine_ls_wR_factor_gt          0.1661
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_restrained_S_all      0.882
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.25438(6) 0.12468(4) 0.17190(3) 0.03038(19) Uani 1 1 d . . . . .
S2 S 0.31798(14) 0.07940(8) 0.07135(6) 0.0399(4) Uani 1 1 d . . . . .
P2 P 0.26703(13) 0.15474(7) -0.00770(6) 0.0311(3) Uani 1 1 d . . . . .
P1 P 0.15531(12) 0.21631(7) 0.11409(6) 0.0295(3) Uani 1 1 d . . . . .
S11 S 0.33739(12) 0.03268(7) 0.23920(6) 0.0351(3) Uani 1 1 d . . . . .
S13 S 0.20405(13) 0.14892(8) 0.27833(6) 0.0375(3) Uani 1 1 d . . . . .
C2 C 0.2336(5) 0.2392(3) 0.0358(2) 0.0321(11) Uani 1 1 d . . . . .
H2A H 0.180596 0.270057 0.001362 0.039 Uiso 1 1 calc R U . . .
H2B H 0.309792 0.265714 0.052605 0.039 Uiso 1 1 calc R U . . .
C12 C 0.2739(4) 0.0692(3) 0.3116(2) 0.0301(11) Uani 1 1 d . . . . .
C14 C 0.2781(5) 0.0382(3) 0.3819(2) 0.0312(11) Uani 1 1 d . . . . .
C15 C 0.3415(6) -0.0310(3) 0.4002(3) 0.0466(15) Uani 1 1 d . . . . .
O15 O 0.4013(4) -0.0627(2) 0.3581(2) 0.0624(13) Uani 1 1 d . . . . .
C16A C 0.3297(7) -0.0664(4) 0.4730(3) 0.065(2) Uani 0.507(16) 1 d D . P A 1
H16A H 0.271021 -0.106567 0.463489 0.078 Uiso 0.507(16) 1 calc R U P A 1
H16B H 0.409333 -0.087789 0.492574 0.078 Uiso 0.507(16) 1 calc R U P A 1
C17A C 0.2915(15) -0.0213(7) 0.5294(6) 0.044(3) Uani 0.507(16) 1 d D . P A 1
H17A H 0.368714 0.001767 0.552848 0.053 Uiso 0.507(16) 1 calc R U P A 1
C18A C 0.2121(8) 0.0390(4) 0.5080(3) 0.073(2) Uani 0.507(16) 1 d D . P A 1
H18A H 0.229710 0.076326 0.545702 0.088 Uiso 0.507(16) 1 calc R U P A 1
H18B H 0.127835 0.022600 0.508510 0.088 Uiso 0.507(16) 1 calc R U P A 1
C16B C 0.3297(7) -0.0664(4) 0.4730(3) 0.065(2) Uani 0.493(16) 1 d D . P A 2
H16C H 0.312995 -0.118240 0.464253 0.078 Uiso 0.493(16) 1 calc R U P A 2
H16D H 0.409479 -0.062758 0.504314 0.078 Uiso 0.493(16) 1 calc R U P A 2
C17B C 0.2376(15) -0.0383(7) 0.5132(6) 0.044(3) Uani 0.493(16) 1 d D . P A 2
H17B H 0.160606 -0.060620 0.488567 0.053 Uiso 0.493(16) 1 calc R U P A 2
C18B C 0.2121(8) 0.0390(4) 0.5080(3) 0.073(2) Uani 0.493(16) 1 d D . P A 2
H18C H 0.271611 0.063747 0.544438 0.088 Uiso 0.493(16) 1 calc R U P A 2
H18D H 0.130760 0.047082 0.521335 0.088 Uiso 0.493(16) 1 calc R U P A 2
C19 C 0.2150(5) 0.0757(3) 0.4356(2) 0.0384(13) Uani 1 1 d . . . . .
O19 O 0.1641(4) 0.1355(2) 0.42357(17) 0.0442(10) Uani 1 1 d . . . . .
C21 C 0.2505(6) -0.0690(3) 0.5919(3) 0.0489(16) Uani 1 1 d D . . . .
C22 C 0.3468(6) -0.0694(3) 0.6509(3) 0.0509(16) Uani 1 1 d . . . . .
H22 H 0.420202 -0.044766 0.647560 0.061 Uiso 1 1 calc R U . . .
C23 C 0.3334(6) -0.1068(3) 0.7149(3) 0.0470(15) Uani 1 1 d . . . . .
H23 H 0.398343 -0.107087 0.754051 0.056 Uiso 1 1 calc R U . . .
C24 C 0.2263(6) -0.1429(3) 0.7211(3) 0.0451(15) Uani 1 1 d . . . . .
H24 H 0.218329 -0.168385 0.763741 0.054 Uiso 1 1 calc R U . . .
C25 C 0.1289(6) -0.1411(3) 0.6626(3) 0.0478(15) Uani 1 1 d . . . . .
H25 H 0.054621 -0.164823 0.666172 0.057 Uiso 1 1 calc R U . . .
C26 C 0.1433(7) -0.1043(3) 0.6001(3) 0.0547(17) Uani 1 1 d . . . . .
H26 H 0.077540 -0.103235 0.561472 0.066 Uiso 1 1 calc R U . . .
C31 C 0.1282(5) 0.1308(3) -0.0708(2) 0.0299(11) Uani 1 1 d . . . . .
C32 C 0.0638(5) 0.0669(3) -0.0634(3) 0.0416(13) Uani 1 1 d . . . . .
H32 H 0.092983 0.032839 -0.027288 0.050 Uiso 1 1 calc R U . . .
C33 C -0.0455(5) 0.0544(3) -0.1111(3) 0.0471(15) Uani 1 1 d . . . . .
H33 H -0.090709 0.011961 -0.106082 0.057 Uiso 1 1 calc R U . . .
C34 C -0.0888(5) 0.1042(3) -0.1661(3) 0.0457(15) Uani 1 1 d . . . . .
H34 H -0.161705 0.094934 -0.198017 0.055 Uiso 1 1 calc R U . . .
C35 C -0.0229(5) 0.1671(3) -0.1728(2) 0.0389(13) Uani 1 1 d . . . . .
H35 H -0.052513 0.200810 -0.209132 0.047 Uiso 1 1 calc R U . . .
C36 C 0.0874(5) 0.1817(3) -0.1264(2) 0.0336(12) Uani 1 1 d . . . . .
H36 H 0.132777 0.223963 -0.131983 0.040 Uiso 1 1 calc R U . . .
C41 C 0.3860(5) 0.1684(3) -0.0634(2) 0.0374(13) Uani 1 1 d . . . . .
C42 C 0.4454(5) 0.1087(4) -0.0876(3) 0.0490(15) Uani 1 1 d . . . . .
H42 H 0.429716 0.061879 -0.071215 0.059 Uiso 1 1 calc R U . . .
C43 C 0.5287(6) 0.1181(5) -0.1364(3) 0.064(2) Uani 1 1 d . . . . .
H43 H 0.568084 0.077697 -0.153164 0.076 Uiso 1 1 calc R U . . .
C44 C 0.5529(6) 0.1875(5) -0.1599(3) 0.061(2) Uani 1 1 d . . . . .
H44 H 0.608873 0.193928 -0.192514 0.073 Uiso 1 1 calc R U . . .
C45 C 0.4966(6) 0.2455(4) -0.1362(3) 0.0589(18) Uani 1 1 d . . . . .
H45 H 0.513932 0.292157 -0.152459 0.071 Uiso 1 1 calc R U . . .
C46 C 0.4124(5) 0.2375(4) -0.0876(3) 0.0482(15) Uani 1 1 d . . . . .
H46 H 0.373917 0.278553 -0.071466 0.058 Uiso 1 1 calc R U . . .
C51 C 0.1425(5) 0.3056(3) 0.1558(2) 0.0322(12) Uani 1 1 d . . . . .
C52 C 0.0352(5) 0.3486(3) 0.1452(3) 0.0420(14) Uani 1 1 d . . . . .
H52 H -0.036088 0.329944 0.117045 0.050 Uiso 1 1 calc R U . . .
C53 C 0.0320(6) 0.4165(3) 0.1746(3) 0.0443(14) Uani 1 1 d . . . . .
H53 H -0.041389 0.443252 0.167457 0.053 Uiso 1 1 calc R U . . .
C54 C 0.1375(6) 0.4462(3) 0.2154(3) 0.0472(15) Uani 1 1 d . . . . .
H54 H 0.136455 0.493615 0.233844 0.057 Uiso 1 1 calc R U . . .
C55 C 0.2444(6) 0.4045(3) 0.2283(3) 0.0509(16) Uani 1 1 d . . . . .
H55 H 0.314754 0.423603 0.256920 0.061 Uiso 1 1 calc R U . . .
C56 C 0.2480(5) 0.3348(3) 0.1990(2) 0.0431(14) Uani 1 1 d . . . . .
H56 H 0.320461 0.307305 0.208099 0.052 Uiso 1 1 calc R U . . .
C61 C -0.0034(5) 0.1912(3) 0.0764(2) 0.0353(12) Uani 1 1 d . . . . .
C62 C -0.0680(5) 0.2261(3) 0.0136(3) 0.0431(14) Uani 1 1 d . . . . .
H62 H -0.030105 0.262864 -0.009916 0.052 Uiso 1 1 calc R U . . .
C63 C -0.1872(6) 0.2051(4) -0.0124(3) 0.0592(18) Uani 1 1 d . . . . .
H63 H -0.230419 0.227897 -0.053733 0.071 Uiso 1 1 calc R U . . .
C64 C -0.2433(6) 0.1507(5) 0.0222(3) 0.072(2) Uani 1 1 d . . . . .
H64 H -0.323796 0.136469 0.003598 0.086 Uiso 1 1 calc R U . . .
C65 C -0.1812(6) 0.1167(4) 0.0847(3) 0.0600(18) Uani 1 1 d . . . . .
H65 H -0.220183 0.080680 0.108516 0.072 Uiso 1 1 calc R U . . .
C66 C -0.0613(5) 0.1371(3) 0.1109(3) 0.0455(15) Uani 1 1 d . . . . .
H66 H -0.018814 0.114190 0.152360 0.055 Uiso 1 1 calc R U . . .
C1S C 0.5744(9) 0.2539(6) 0.1284(5) 0.113(4) Uani 1 1 d . . . . .
H1S1 H 0.644112 0.274504 0.159974 0.169 Uiso 1 1 calc R U . . .
H1S2 H 0.600488 0.236109 0.084360 0.169 Uiso 1 1 calc R U . . .
H1S3 H 0.540810 0.214066 0.153136 0.169 Uiso 1 1 calc R U . . .
O1S O 0.4921(5) 0.3029(3) 0.1124(3) 0.0899(17) Uani 1 1 d . . . . .
H1S H 0.516700 0.341794 0.131780 0.135 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 S13 2.1670(13) . ?
Ni1 P1 2.1763(14) . ?
Ni1 S11 2.1962(14) . ?
Ni1 S2 2.2390(14) . ?
S2 P2 2.0174(17) . ?
P2 C41 1.797(5) . ?
P2 C2 1.800(5) . ?
P2 C31 1.816(5) . ?
P1 C51 1.815(5) . ?
P1 C61 1.823(5) . ?
P1 C2 1.838(5) . ?
S11 C12 1.732(5) . ?
S13 C12 1.709(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C12 C14 1.411(6) . ?
C14 C15 1.453(7) . ?
C14 C19 1.462(7) . ?
C15 O15 1.234(6) . ?
C15 C16B 1.516(7) . ?
C15 C16A 1.516(7) . ?
C16A C17A 1.438(11) . ?
C16A H16A 0.9700 . ?
C16A H16B 0.9700 . ?
C17A C18A 1.418(11) . ?
C17A C21 1.565(12) . ?
C17A H17A 0.9800 . ?
C18A C19 1.499(7) . ?
C18A H18A 0.9700 . ?
C18A H18B 0.9700 . ?
C16B C17B 1.434(11) . ?
C16B H16C 0.9700 . ?
C16B H16D 0.9700 . ?
C17B C18B 1.437(11) . ?
C17B C21 1.543(11) . ?
C17B H17B 0.9800 . ?
C18B C19 1.499(7) . ?
C18B H18C 0.9700 . ?
C18B H18D 0.9700 . ?
C19 O19 1.226(6) . ?
C21 C26 1.365(9) . ?
C21 C22 1.391(8) . ?
C22 C23 1.391(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.363(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.393(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.367(8) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C31 C32 1.378(7) . ?
C31 C36 1.403(6) . ?
C32 C33 1.387(7) . ?
C32 H32 0.9300 . ?
C33 C34 1.388(8) . ?
C33 H33 0.9300 . ?
C34 C35 1.369(7) . ?
C34 H34 0.9300 . ?
C35 C36 1.391(7) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C41 C42 1.377(8) . ?
C41 C46 1.381(8) . ?
C42 C43 1.388(8) . ?
C42 H42 0.9300 . ?
C43 C44 1.375(9) . ?
C43 H43 0.9300 . ?
C44 C45 1.330(9) . ?
C44 H44 0.9300 . ?
C45 C46 1.390(8) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C51 C52 1.398(7) . ?
C51 C56 1.400(7) . ?
C52 C53 1.354(7) . ?
C52 H52 0.9300 . ?
C53 C54 1.385(8) . ?
C53 H53 0.9300 . ?
C54 C55 1.382(8) . ?
C54 H54 0.9300 . ?
C55 C56 1.383(8) . ?
C55 H55 0.9300 . ?
C56 H56 0.9300 . ?
C61 C66 1.379(7) . ?
C61 C62 1.412(6) . ?
C62 C63 1.369(7) . ?
C62 H62 0.9300 . ?
C63 C64 1.375(9) . ?
C63 H63 0.9300 . ?
C64 C65 1.389(9) . ?
C64 H64 0.9300 . ?
C65 C66 1.374(8) . ?
C65 H65 0.9300 . ?
C66 H66 0.9300 . ?
C1S O1S 1.269(9) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
O1S H1S 0.8200 . ?

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
S13 Ni1 P1 96.39(5) . . ?
S13 Ni1 S11 77.49(5) . . ?
P1 Ni1 S11 173.03(6) . . ?
S13 Ni1 S2 169.27(6) . . ?
P1 Ni1 S2 94.07(5) . . ?
S11 Ni1 S2 91.93(5) . . ?
P2 S2 Ni1 105.25(7) . . ?
C41 P2 C2 110.6(2) . . ?
C41 P2 C31 105.8(2) . . ?
C2 P2 C31 106.5(2) . . ?
C41 P2 S2 111.48(18) . . ?
C2 P2 S2 108.11(15) . . ?
C31 P2 S2 114.17(17) . . ?
C51 P1 C61 104.8(2) . . ?
C51 P1 C2 101.9(2) . . ?
C61 P1 C2 106.8(2) . . ?
C51 P1 Ni1 123.00(15) . . ?
C61 P1 Ni1 111.42(19) . . ?
C2 P1 Ni1 107.63(17) . . ?
C12 S11 Ni1 87.89(17) . . ?
C12 S13 Ni1 89.43(17) . . ?
P2 C2 P1 108.0(2) . . ?
P2 C2 H2A 110.1 . . ?
P1 C2 H2A 110.1 . . ?
P2 C2 H2B 110.1 . . ?
P1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C14 C12 S13 128.3(4) . . ?
C14 C12 S11 126.7(4) . . ?
S13 C12 S11 105.1(3) . . ?
C12 C14 C15 120.5(4) . . ?
C12 C14 C19 119.1(5) . . ?
C15 C14 C19 120.5(4) . . ?
O15 C15 C14 122.7(5) . . ?
O15 C15 C16B 119.1(5) . . ?
C14 C15 C16B 118.2(5) . . ?
O15 C15 C16A 119.1(5) . . ?
C14 C15 C16A 118.2(5) . . ?
C17A C16A C15 118.2(6) . . ?
C17A C16A H16A 107.8 . . ?
C15 C16A H16A 107.8 . . ?
C17A C16A H16B 107.8 . . ?
C15 C16A H16B 107.8 . . ?
H16A C16A H16B 107.1 . . ?
C18A C17A C16A 118.4(8) . . ?
C18A C17A C21 113.7(8) . . ?
C16A C17A C21 111.4(8) . . ?
C18A C17A H17A 103.8 . . ?
C16A C17A H17A 103.8 . . ?
C21 C17A H17A 103.8 . . ?
C17A C18A C19 119.8(6) . . ?
C17A C18A H18A 107.4 . . ?
C19 C18A H18A 107.4 . . ?
C17A C18A H18B 107.4 . . ?
C19 C18A H18B 107.4 . . ?
H18A C18A H18B 106.9 . . ?
C17B C16B C15 118.1(6) . . ?
C17B C16B H16C 107.8 . . ?
C15 C16B H16C 107.8 . . ?
C17B C16B H16D 107.8 . . ?
C15 C16B H16D 107.8 . . ?
H16C C16B H16D 107.1 . . ?
C16B C17B C18B 117.4(10) . . ?
C16B C17B C21 112.9(8) . . ?
C18B C17B C21 114.0(8) . . ?
C16B C17B H17B 103.4 . . ?
C18B C17B H17B 103.4 . . ?
C21 C17B H17B 103.4 . . ?
C17B C18B C19 117.8(6) . . ?
C17B C18B H18C 107.9 . . ?
C19 C18B H18C 107.9 . . ?
C17B C18B H18D 107.9 . . ?
C19 C18B H18D 107.9 . . ?
H18C C18B H18D 107.2 . . ?
O19 C19 C14 122.7(4) . . ?
O19 C19 C18A 119.0(5) . . ?
C14 C19 C18A 118.3(5) . . ?
O19 C19 C18B 119.0(5) . . ?
C14 C19 C18B 118.3(5) . . ?
C26 C21 C22 117.9(5) . . ?
C26 C21 C17B 108.7(8) . . ?
C22 C21 C17B 133.4(9) . . ?
C26 C21 C17A 133.8(8) . . ?
C22 C21 C17A 108.2(8) . . ?
C21 C22 C23 120.1(6) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.8(5) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 119.1(5) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C26 C25 C24 119.4(6) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
C21 C26 C25 122.6(5) . . ?
C21 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
C32 C31 C36 121.5(5) . . ?
C32 C31 P2 121.8(4) . . ?
C36 C31 P2 116.6(4) . . ?
C31 C32 C33 118.5(5) . . ?
C31 C32 H32 120.7 . . ?
C33 C32 H32 120.7 . . ?
C32 C33 C34 121.2(5) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
C35 C34 C33 119.3(5) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
C34 C35 C36 121.4(5) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 H35 119.3 . . ?
C35 C36 C31 118.0(5) . . ?
C35 C36 H36 121.0 . . ?
C31 C36 H36 121.0 . . ?
C42 C41 C46 118.8(5) . . ?
C42 C41 P2 119.7(5) . . ?
C46 C41 P2 121.2(4) . . ?
C41 C42 C43 120.2(6) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C44 C43 C42 119.8(6) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C45 C44 C43 120.3(6) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 121.0(7) . . ?
C44 C45 H45 119.5 . . ?
C46 C45 H45 119.5 . . ?
C41 C46 C45 119.9(6) . . ?
C41 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C52 C51 C56 117.8(5) . . ?
C52 C51 P1 124.1(4) . . ?
C56 C51 P1 118.1(4) . . ?
C53 C52 C51 121.9(5) . . ?
C53 C52 H52 119.0 . . ?
C51 C52 H52 119.0 . . ?
C52 C53 C54 120.2(6) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C55 C54 C53 119.3(5) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C54 C55 C56 120.8(5) . . ?
C54 C55 H55 119.6 . . ?
C56 C55 H55 119.6 . . ?
C55 C56 C51 120.0(6) . . ?
C55 C56 H56 120.0 . . ?
C51 C56 H56 120.0 . . ?
C66 C61 C62 119.6(5) . . ?
C66 C61 P1 118.8(4) . . ?
C62 C61 P1 121.6(4) . . ?
C63 C62 C61 119.3(6) . . ?
C63 C62 H62 120.4 . . ?
C61 C62 H62 120.4 . . ?
C62 C63 C64 120.4(6) . . ?
C62 C63 H63 119.8 . . ?
C64 C63 H63 119.8 . . ?
C63 C64 C65 120.8(6) . . ?
C63 C64 H64 119.6 . . ?
C65 C64 H64 119.6 . . ?
C66 C65 C64 119.1(6) . . ?
C66 C65 H65 120.4 . . ?
C64 C65 H65 120.4 . . ?
C65 C66 C61 120.8(5) . . ?
C65 C66 H66 119.6 . . ?
C61 C66 H66 119.6 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C1S O1S H1S 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
C2 H2A O19 0.97 2.23 3.097(6) 148.1 4_565
C2 H2B O1S 0.97 2.23 3.173(7) 165.0 .

_refine_diff_density_max         0.579
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.107

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1919578'
_audit_update_record             
;
2019-12-24 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H32 Ni O2 P2 S3'
_chemical_formula_weight         689.42

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'
Ni Ni 0.3393 1.1124 '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'
P P 0.1023 0.0942 '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/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   12.9389(5)
_cell_length_b                   18.1214(11)
_cell_length_c                   14.0593(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.926(5)
_cell_angle_gamma                90
_cell_volume                     3170.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    19059
_cell_measurement_theta_min      3.275
_cell_measurement_theta_max      30.000

_exptl_crystal_description       needle
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    0.942
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_T_max  1.000

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            19068
_diffrn_reflns_av_unetI/netI     0.1502
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.275
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             9023
_reflns_number_gt                5217
_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       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'
_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)+(0.0330P)²] 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         9023
_refine_ls_number_parameters     381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.0855
_refine_ls_wR_factor_ref         0.1446
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.43181(4) 0.26861(3) 0.74472(4) 0.02286(15) Uani 1 1 d . . . . .
S11 S 0.57363(9) 0.31971(7) 0.71440(9) 0.0278(3) Uani 1 1 d . . . . .
S2 S 0.51604(9) 0.15817(7) 0.76270(10) 0.0331(3) Uani 1 1 d . . . . .
S13 S 0.38469(9) 0.38417(6) 0.71855(8) 0.0263(3) Uani 1 1 d . . . . .
P2 P 0.39541(9) 0.08850(6) 0.76055(8) 0.0226(3) Uani 1 1 d . . . . .
P1 P 0.28312(8) 0.22787(6) 0.77519(7) 0.0195(2) Uani 1 1 d . . . . .
C2 C 0.3087(3) 0.1334(2) 0.8218(3) 0.0236(10) Uani 1 1 d . . . . .
H2A H 0.342071 0.134254 0.892591 0.028 Uiso 1 1 calc R U . . .
H2B H 0.241392 0.106683 0.809694 0.028 Uiso 1 1 calc R U . . .
C12 C 0.5065(3) 0.4027(3) 0.6969(3) 0.0252(10) Uani 1 1 d . . . . .
C14 C 0.5421(3) 0.4697(2) 0.6658(3) 0.0220(10) Uani 1 1 d . . . . .
C15 C 0.6502(4) 0.4746(3) 0.6516(3) 0.0322(11) Uani 1 1 d . . . . .
C16 C 0.6790(4) 0.5431(3) 0.6033(3) 0.0352(12) Uani 1 1 d . . . . .
H16A H 0.658213 0.535784 0.532217 0.042 Uiso 1 1 calc R U . . .
H16B H 0.756388 0.549268 0.624377 0.042 Uiso 1 1 calc R U . . .
C17 C 0.6267(3) 0.6143(3) 0.6261(3) 0.0274(11) Uani 1 1 d . . . . .
C18 C 0.5067(3) 0.6005(3) 0.5991(3) 0.0287(11) Uani 1 1 d . . . . .
H18A H 0.480793 0.595507 0.527820 0.034 Uiso 1 1 calc R U . . .
H18B H 0.472310 0.643699 0.617628 0.034 Uiso 1 1 calc R U . . .
C19 C 0.4711(3) 0.5334(3) 0.6460(3) 0.0268(11) Uani 1 1 d . . . . .
C21 C 0.1704(3) 0.2145(2) 0.6664(3) 0.0217(10) Uani 1 1 d . . . . .
C22 C 0.1886(3) 0.2233(2) 0.5736(3) 0.0238(10) Uani 1 1 d . . . . .
H22 H 0.254235 0.241299 0.568773 0.029 Uiso 1 1 calc R U . . .
C23 C 0.1087(4) 0.2053(2) 0.4889(3) 0.0297(11) Uani 1 1 d . . . . .
H23 H 0.120747 0.211060 0.427062 0.036 Uiso 1 1 calc R U . . .
C24 C 0.0122(4) 0.1789(3) 0.4962(3) 0.0320(12) Uani 1 1 d . . . . .
H24 H -0.040622 0.166190 0.439018 0.038 Uiso 1 1 calc R U . . .
C25 C -0.0081(4) 0.1708(3) 0.5865(3) 0.0308(12) Uani 1 1 d . . . . .
H25 H -0.074392 0.153464 0.590530 0.037 Uiso 1 1 calc R U . . .
C26 C 0.0723(3) 0.1891(2) 0.6724(3) 0.0257(10) Uani 1 1 d . . . . .
H26 H 0.059217 0.183992 0.733899 0.031 Uiso 1 1 calc R U . . .
C31 C 0.2245(3) 0.2704(2) 0.8653(3) 0.0194(9) Uani 1 1 d . . . . .
C32 C 0.2291(3) 0.2385(3) 0.9566(3) 0.0300(11) Uani 1 1 d . . . . .
H32 H 0.262592 0.193007 0.972953 0.036 Uiso 1 1 calc R U . . .
C33 C 0.1841(4) 0.2737(3) 1.0232(3) 0.0367(12) Uani 1 1 d . . . . .
H33 H 0.187142 0.251516 1.083611 0.044 Uiso 1 1 calc R U . . .
C34 C 0.1355(4) 0.3406(3) 1.0007(3) 0.0369(12) Uani 1 1 d . . . . .
H34 H 0.106345 0.364545 1.045895 0.044 Uiso 1 1 calc R U . . .
C35 C 0.1298(4) 0.3726(3) 0.9105(4) 0.0404(13) Uani 1 1 d . . . . .
H35 H 0.095780 0.417911 0.894455 0.049 Uiso 1 1 calc R U . . .
C36 C 0.1745(4) 0.3378(3) 0.8434(3) 0.0315(11) Uani 1 1 d . . . . .
H36 H 0.170616 0.360121 0.783022 0.038 Uiso 1 1 calc R U . . .
C41 C 0.3191(4) 0.0642(2) 0.6359(3) 0.0262(10) Uani 1 1 d . . . . .
C42 C 0.2230(3) 0.0261(3) 0.6237(3) 0.0306(11) Uani 1 1 d . . . . .
H42 H 0.199386 0.012837 0.678121 0.037 Uiso 1 1 calc R U . . .
C43 C 0.1629(4) 0.0082(3) 0.5281(4) 0.0452(15) Uani 1 1 d . . . . .
H43 H 0.098164 -0.016948 0.518339 0.054 Uiso 1 1 calc R U . . .
C44 C 0.1986(5) 0.0274(3) 0.4493(4) 0.0551(18) Uani 1 1 d . . . . .
H44 H 0.157310 0.015427 0.385898 0.066 Uiso 1 1 calc R U . . .
C45 C 0.2942(5) 0.0640(3) 0.4609(4) 0.0520(16) Uani 1 1 d . . . . .
H45 H 0.318122 0.076100 0.406179 0.062 Uiso 1 1 calc R U . . .
C46 C 0.3544(4) 0.0827(3) 0.5552(3) 0.0379(13) Uani 1 1 d . . . . .
H46 H 0.419001 0.107812 0.564146 0.045 Uiso 1 1 calc R U . . .
C51 C 0.4382(3) 0.0042(2) 0.8270(3) 0.0221(10) Uani 1 1 d . . . . .
C52 C 0.5292(3) -0.0322(2) 0.8161(3) 0.0299(11) Uani 1 1 d . . . . .
H52 H 0.569444 -0.011806 0.777124 0.036 Uiso 1 1 calc R U . . .
C53 C 0.5592(3) -0.0989(3) 0.8639(4) 0.0326(12) Uani 1 1 d . . . . .
H53 H 0.618736 -0.124053 0.855669 0.039 Uiso 1 1 calc R U . . .
C54 C 0.5005(3) -0.1280(3) 0.9237(3) 0.0309(12) Uani 1 1 d . . . . .
H54 H 0.521532 -0.172420 0.956477 0.037 Uiso 1 1 calc R U . . .
C55 C 0.4122(4) -0.0921(3) 0.9350(3) 0.0314(11) Uani 1 1 d . . . . .
H55 H 0.373469 -0.112212 0.975497 0.038 Uiso 1 1 calc R U . . .
C56 C 0.3796(3) -0.0261(2) 0.8868(3) 0.0276(11) Uani 1 1 d . . . . .
H56 H 0.318841 -0.002133 0.894339 0.033 Uiso 1 1 calc R U . . .
C171 C 0.6700(4) 0.6336(3) 0.7364(3) 0.0409(13) Uani 1 1 d . . . . .
H17A H 0.746686 0.639186 0.752840 0.061 Uiso 1 1 calc R U . . .
H17B H 0.652295 0.594753 0.775642 0.061 Uiso 1 1 calc R U . . .
H17C H 0.638189 0.678944 0.749683 0.061 Uiso 1 1 calc R U . . .
C172 C 0.6527(4) 0.6774(3) 0.5659(4) 0.0415(13) Uani 1 1 d . . . . .
H17D H 0.621965 0.667716 0.496754 0.062 Uiso 1 1 calc R U . . .
H17E H 0.729214 0.682204 0.579299 0.062 Uiso 1 1 calc R U . . .
H17F H 0.623274 0.722430 0.583447 0.062 Uiso 1 1 calc R U . . .
O15 O 0.7159(3) 0.4248(2) 0.6787(3) 0.0655(13) Uani 1 1 d . . . . .
O19 O 0.3834(2) 0.53367(18) 0.6636(2) 0.0381(9) 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 S13 2.1838(13) . ?
Ni1 S11 2.1991(13) . ?
Ni1 P1 2.2096(13) . ?
Ni1 S2 2.2597(13) . ?
S11 C12 1.720(5) . ?
S2 P2 2.0012(17) . ?
S13 C12 1.719(5) . ?
P2 C2 1.788(4) . ?
P2 C51 1.797(4) . ?
P2 C41 1.814(4) . ?
P1 C21 1.817(4) . ?
P1 C31 1.817(4) . ?
P1 C2 1.830(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C12 C14 1.409(6) . ?
C14 C19 1.454(6) . ?
C14 C15 1.469(6) . ?
C15 O15 1.227(5) . ?
C15 C16 1.510(6) . ?
C16 C17 1.531(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.514(6) . ?
C17 C172 1.516(6) . ?
C17 C171 1.538(6) . ?
C18 C19 1.515(6) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 O19 1.226(5) . ?
C21 C26 1.374(6) . ?
C21 C22 1.397(6) . ?
C22 C23 1.385(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.367(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.373(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.401(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C31 C36 1.376(6) . ?
C31 C32 1.394(6) . ?
C32 C33 1.386(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.363(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.378(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.385(6) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C41 C46 1.375(6) . ?
C41 C42 1.391(6) . ?
C42 C43 1.393(6) . ?
C42 H42 0.9300 . ?
C43 C44 1.358(8) . ?
C43 H43 0.9300 . ?
C44 C45 1.374(8) . ?
C44 H44 0.9300 . ?
C45 C46 1.383(6) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C51 C56 1.390(6) . ?
C51 C52 1.393(6) . ?
C52 C53 1.385(6) . ?
C52 H52 0.9300 . ?
C53 C54 1.383(7) . ?
C53 H53 0.9300 . ?
C54 C55 1.361(6) . ?
C54 H54 0.9300 . ?
C55 C56 1.382(6) . ?
C55 H55 0.9300 . ?
C56 H56 0.9300 . ?
C171 H17A 0.9600 . ?
C171 H17B 0.9600 . ?
C171 H17C 0.9600 . ?
C172 H17D 0.9600 . ?
C172 H17E 0.9600 . ?
C172 H17F 0.9600 . ?

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
S13 Ni1 S11 76.87(5) . . ?
S13 Ni1 P1 97.78(5) . . ?
S11 Ni1 P1 174.60(5) . . ?
S13 Ni1 S2 166.39(5) . . ?
S11 Ni1 S2 89.55(5) . . ?
P1 Ni1 S2 95.81(5) . . ?
C12 S11 Ni1 88.88(16) . . ?
P2 S2 Ni1 101.93(6) . . ?
C12 S13 Ni1 89.41(16) . . ?
C2 P2 C51 106.3(2) . . ?
C2 P2 C41 109.2(2) . . ?
C51 P2 C41 107.75(19) . . ?
C2 P2 S2 107.18(15) . . ?
C51 P2 S2 113.60(14) . . ?
C41 P2 S2 112.53(17) . . ?
C21 P1 C31 104.55(19) . . ?
C21 P1 C2 101.62(19) . . ?
C31 P1 C2 102.47(19) . . ?
C21 P1 Ni1 114.97(15) . . ?
C31 P1 Ni1 123.05(13) . . ?
C2 P1 Ni1 107.49(14) . . ?
P2 C2 P1 109.2(2) . . ?
P2 C2 H2A 109.8 . . ?
P1 C2 H2A 109.8 . . ?
P2 C2 H2B 109.8 . . ?
P1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
C14 C12 S13 128.0(3) . . ?
C14 C12 S11 127.0(4) . . ?
S13 C12 S11 104.8(2) . . ?
C12 C14 C19 120.1(4) . . ?
C12 C14 C15 119.9(4) . . ?
C19 C14 C15 120.0(4) . . ?
O15 C15 C14 121.2(5) . . ?
O15 C15 C16 120.6(4) . . ?
C14 C15 C16 118.2(4) . . ?
C15 C16 C17 114.9(4) . . ?
C15 C16 H16A 108.6 . . ?
C17 C16 H16A 108.6 . . ?
C15 C16 H16B 108.6 . . ?
C17 C16 H16B 108.6 . . ?
H16A C16 H16B 107.5 . . ?
C18 C17 C172 110.7(4) . . ?
C18 C17 C16 106.9(4) . . ?
C172 C17 C16 109.9(4) . . ?
C18 C17 C171 110.8(4) . . ?
C172 C17 C171 108.4(4) . . ?
C16 C17 C171 110.1(4) . . ?
C17 C18 C19 115.8(4) . . ?
C17 C18 H18A 108.3 . . ?
C19 C18 H18A 108.3 . . ?
C17 C18 H18B 108.3 . . ?
C19 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
O19 C19 C14 122.4(4) . . ?
O19 C19 C18 119.5(4) . . ?
C14 C19 C18 118.1(4) . . ?
C26 C21 C22 119.4(4) . . ?
C26 C21 P1 122.4(3) . . ?
C22 C21 P1 118.0(3) . . ?
C23 C22 C21 120.0(4) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 119.9(4) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 121.2(4) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C24 C25 C26 119.2(4) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C21 C26 C25 120.4(4) . . ?
C21 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C36 C31 C32 118.2(4) . . ?
C36 C31 P1 118.7(3) . . ?
C32 C31 P1 123.0(3) . . ?
C33 C32 C31 120.7(4) . . ?
C33 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C34 C33 C32 120.3(4) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 119.5(5) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C36 120.5(5) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C31 C36 C35 120.7(4) . . ?
C31 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C46 C41 C42 120.4(4) . . ?
C46 C41 P2 121.5(4) . . ?
C42 C41 P2 118.1(4) . . ?
C41 C42 C43 118.6(5) . . ?
C41 C42 H42 120.7 . . ?
C43 C42 H42 120.7 . . ?
C44 C43 C42 120.2(5) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 121.6(5) . . ?
C43 C44 H44 119.2 . . ?
C45 C44 H44 119.2 . . ?
C44 C45 C46 118.9(5) . . ?
C44 C45 H45 120.6 . . ?
C46 C45 H45 120.6 . . ?
C41 C46 C45 120.3(5) . . ?
C41 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C56 C51 C52 119.8(4) . . ?
C56 C51 P2 120.6(3) . . ?
C52 C51 P2 119.6(3) . . ?
C53 C52 C51 119.5(4) . . ?
C53 C52 H52 120.3 . . ?
C51 C52 H52 120.3 . . ?
C54 C53 C52 120.0(4) . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C55 C54 C53 120.4(4) . . ?
C55 C54 H54 119.8 . . ?
C53 C54 H54 119.8 . . ?
C54 C55 C56 120.6(5) . . ?
C54 C55 H55 119.7 . . ?
C56 C55 H55 119.7 . . ?
C55 C56 C51 119.6(4) . . ?
C55 C56 H56 120.2 . . ?
C51 C56 H56 120.2 . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 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
C2 H2B O19 0.97 2.20 3.126(5) 159.5 2_546
C46 H46 S2 0.93 2.88 3.377(5) 115.0 .
C56 H56 O19 0.93 2.60 3.455(5) 153.0 2_546
C53 H53 O15 0.93 2.48 3.157(6) 129.6 2_646

_refine_diff_density_max         0.580
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1974370'
_audit_update_record             
;
2019-12-24 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;
_audit_creation_date             2019-12-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C35 H34 Ni O2 P2 S2, H2 O'
_chemical_formula_sum            'C35 H36 Ni O3 P2 S2'
_chemical_formula_weight         689.41
_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'
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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   19.7845(9)
_cell_length_b                   15.2433(6)
_cell_length_c                   22.3400(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6737.3(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            103324
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.307
_diffrn_reflns_theta_min         2.094
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5963
_reflns_number_total             8373
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    ?
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8373
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0451
_refine_ls_restrained_S_all      1.189
_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)+(0.0664P)²+8.4018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1569
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1W-H1WB = O1W-H1WA
 0.85 with sigma of 0.02
 H1WB-H1WA
 1.375 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C16(H16A,H16B), C18(H18A,H18B)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
 C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
3.c Idealised Me refined as rotating group:
 C171(H17A,H17B,H17C), C172(H17D,H17E,H17F)
;
_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
C3 C 0.59116(17) 0.7817(2) 0.21747(15) 0.0261(7) Uani 1 1 d . . . . .
H3A H 0.578387 0.830834 0.242646 0.031 Uiso 1 1 calc R . . . .
H3B H 0.623956 0.802271 0.188402 0.031 Uiso 1 1 calc R . . . .
C2 C 0.52871(16) 0.7459(2) 0.18510(15) 0.0258(7) Uani 1 1 d . . . . .
H2A H 0.542529 0.710642 0.151095 0.031 Uiso 1 1 calc R . . . .
H2B H 0.501311 0.794135 0.170472 0.031 Uiso 1 1 calc R . . . .
C12 C 0.53183(16) 0.48369(19) 0.38458(14) 0.0208(6) Uani 1 1 d . . . . .
C14 C 0.52118(16) 0.42874(19) 0.43310(13) 0.0193(6) Uani 1 1 d . . . . .
C15 C 0.45646(16) 0.3826(2) 0.43979(14) 0.0210(6) Uani 1 1 d . . . . .
C16 C 0.44804(17) 0.3218(2) 0.49293(15) 0.0257(7) Uani 1 1 d . . . . .
H16A H 0.415862 0.276411 0.482302 0.031 Uiso 1 1 calc R . . . .
H16B H 0.428793 0.355080 0.525791 0.031 Uiso 1 1 calc R . . . .
C17 C 0.51281(17) 0.2779(2) 0.51478(14) 0.0248(7) Uani 1 1 d . . . . .
C18 C 0.56366(17) 0.3508(2) 0.52853(14) 0.0234(7) Uani 1 1 d . . . . .
H18A H 0.548495 0.382158 0.563844 0.028 Uiso 1 1 calc R . . . .
H18B H 0.606818 0.324023 0.538063 0.028 Uiso 1 1 calc R . . . .
C19 C 0.57424(16) 0.4163(2) 0.47856(14) 0.0215(6) Uani 1 1 d . . . . .
C171 C 0.49673(19) 0.2253(2) 0.57161(16) 0.0318(8) Uani 1 1 d . . . . .
H17A H 0.536578 0.194820 0.584630 0.048 Uiso 1 1 calc GR . . . .
H17B H 0.461636 0.183596 0.563166 0.048 Uiso 1 1 calc GR . . . .
H17C H 0.481940 0.264505 0.602576 0.048 Uiso 1 1 calc GR . . . .
C172 C 0.5419(2) 0.2160(2) 0.46752(16) 0.0337(8) Uani 1 1 d . . . . .
H17D H 0.553580 0.248898 0.432360 0.050 Uiso 1 1 calc GR . . . .
H17E H 0.508804 0.172403 0.457411 0.050 Uiso 1 1 calc GR . . . .
H17F H 0.581570 0.187861 0.483108 0.050 Uiso 1 1 calc GR . . . .
C31 C 0.42476(16) 0.7543(2) 0.27770(14) 0.0213(6) Uani 1 1 d . . . . .
C32 C 0.42888(18) 0.8458(2) 0.27070(16) 0.0280(7) Uani 1 1 d . . . . .
H32 H 0.458754 0.869919 0.243110 0.034 Uiso 1 1 calc R . . . .
C33 C 0.3879(2) 0.8999(2) 0.30533(18) 0.0352(9) Uani 1 1 d . . . . .
H33 H 0.390561 0.960397 0.300587 0.042 Uiso 1 1 calc R . . . .
C34 C 0.34343(18) 0.8652(2) 0.34663(18) 0.0339(8) Uani 1 1 d . . . . .
H34 H 0.316874 0.902131 0.369956 0.041 Uiso 1 1 calc R . . . .
C35 C 0.33858(17) 0.7753(2) 0.35312(16) 0.0280(7) Uani 1 1 d . . . . .
H35 H 0.307934 0.751726 0.380275 0.034 Uiso 1 1 calc R . . . .
C36 C 0.37933(16) 0.7198(2) 0.31921(15) 0.0233(7) Uani 1 1 d . . . . .
H36 H 0.376231 0.659425 0.324272 0.028 Uiso 1 1 calc R . . . .
C41 C 0.42425(16) 0.61477(19) 0.18917(14) 0.0200(6) Uani 1 1 d . . . . .
C42 C 0.4405(2) 0.5279(2) 0.17753(16) 0.0325(8) Uani 1 1 d . . . . .
H42 H 0.476825 0.501697 0.196979 0.039 Uiso 1 1 calc R . . . .
C43 C 0.4024(2) 0.4803(2) 0.13676(18) 0.0429(10) Uani 1 1 d . . . . .
H43 H 0.412752 0.421740 0.129386 0.051 Uiso 1 1 calc R . . . .
C44 C 0.3494(2) 0.5191(2) 0.10728(17) 0.0353(9) Uani 1 1 d . . . . .
H44 H 0.324755 0.487201 0.079311 0.042 Uiso 1 1 calc R . . . .
C45 C 0.33252(18) 0.6048(2) 0.11880(16) 0.0311(8) Uani 1 1 d . . . . .
H45 H 0.296687 0.630777 0.098525 0.037 Uiso 1 1 calc R . . . .
C46 C 0.36898(17) 0.6526(2) 0.16077(15) 0.0264(7) Uani 1 1 d . . . . .
H46 H 0.356408 0.709903 0.169830 0.032 Uiso 1 1 calc R . . . .
C51 C 0.68460(16) 0.7539(2) 0.31371(15) 0.0237(7) Uani 1 1 d . . . . .
C52 C 0.73255(17) 0.8113(2) 0.28956(16) 0.0269(7) Uani 1 1 d . . . . .
H52 H 0.736701 0.816894 0.248270 0.032 Uiso 1 1 calc R . . . .
C53 C 0.77378(17) 0.8598(2) 0.32704(17) 0.0310(8) Uani 1 1 d . . . . .
H53 H 0.804859 0.898956 0.310912 0.037 Uiso 1 1 calc R . . . .
C54 C 0.76891(18) 0.8500(2) 0.38864(18) 0.0337(8) Uani 1 1 d . . . . .
H54 H 0.797033 0.882321 0.413690 0.040 Uiso 1 1 calc R . . . .
C55 C 0.7224(2) 0.7926(2) 0.41282(17) 0.0350(8) Uani 1 1 d . . . . .
H55 H 0.719685 0.785582 0.454100 0.042 Uiso 1 1 calc R . . . .
C56 C 0.67981(17) 0.7453(2) 0.37555(15) 0.0268(7) Uani 1 1 d . . . . .
H56 H 0.647831 0.707699 0.392010 0.032 Uiso 1 1 calc R . . . .
C61 C 0.68692(17) 0.6338(2) 0.21540(16) 0.0262(7) Uani 1 1 d . . . . .
C62 C 0.6866(2) 0.6397(3) 0.15312(17) 0.0365(9) Uani 1 1 d . . . . .
H62 H 0.656028 0.676448 0.133908 0.044 Uiso 1 1 calc R . . . .
C63 C 0.7323(2) 0.5902(3) 0.11981(18) 0.0438(10) Uani 1 1 d . . . . .
H63 H 0.731534 0.593734 0.078253 0.053 Uiso 1 1 calc R . . . .
C64 C 0.7783(2) 0.5365(3) 0.1473(2) 0.0435(10) Uani 1 1 d . . . . .
H64 H 0.809254 0.504953 0.124539 0.052 Uiso 1 1 calc R . . . .
C65 C 0.77875(18) 0.5293(2) 0.2089(2) 0.0377(9) Uani 1 1 d . . . . .
H65 H 0.809514 0.492195 0.227653 0.045 Uiso 1 1 calc R . . . .
C66 C 0.73279(17) 0.5778(2) 0.24308(17) 0.0305(8) Uani 1 1 d . . . . .
H66 H 0.732898 0.572595 0.284562 0.037 Uiso 1 1 calc R . . . .
Ni1 Ni 0.54833(2) 0.60900(3) 0.29673(2) 0.01913(12) Uani 1 1 d . . . . .
O1W O 0.71623(17) 0.6068(2) 0.51781(18) 0.0616(9) Uani 1 1 d D . . . .
O15 O 0.40889(11) 0.39185(14) 0.40476(10) 0.0232(5) Uani 1 1 d . . . . .
O19 O 0.62727(12) 0.45807(15) 0.47786(10) 0.0274(5) Uani 1 1 d . . . . .
P2 P 0.47925(4) 0.67865(5) 0.23752(4) 0.02011(18) Uani 1 1 d . . . . .
S11 S 0.47423(4) 0.51235(5) 0.32911(3) 0.01998(17) Uani 1 1 d . . . . .
S13 S 0.60515(4) 0.54075(5) 0.36705(4) 0.02311(18) Uani 1 1 d . . . . .
P1 P 0.62873(4) 0.69437(5) 0.26363(4) 0.02170(18) Uani 1 1 d . . . . .
H1WA H 0.7078(18) 0.5621(19) 0.4959(14) 0.026 Uiso 1 1 d DR . . . .
H1WB H 0.6864(16) 0.613(2) 0.5451(12) 0.026 Uiso 1 1 d DR . . . .


_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
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.532(4) . ?
C3 P1 1.841(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 P2 1.838(3) . ?
C12 C14 1.386(4) . ?
C12 S11 1.739(3) . ?
C12 S13 1.736(3) . ?
C14 C15 1.469(4) . ?
C14 C19 1.473(4) . ?
C15 C16 1.515(4) . ?
C15 O15 1.232(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.526(4) . ?
C17 C18 1.530(5) . ?
C17 C171 1.535(4) . ?
C17 C172 1.529(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C19 1.512(4) . ?
C19 O19 1.228(4) . ?
C171 H17A 0.9600 . ?
C171 H17B 0.9600 . ?
C171 H17C 0.9600 . ?
C172 H17D 0.9600 . ?
C172 H17E 0.9600 . ?
C172 H17F 0.9600 . ?
C31 C32 1.405(4) . ?
C31 C36 1.394(5) . ?
C31 P2 1.816(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.391(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.380(6) . ?
C34 H34 0.9300 . ?
C34 C35 1.381(5) . ?
C35 H35 0.9300 . ?
C35 C36 1.393(5) . ?
C36 H36 0.9300 . ?
C41 C42 1.387(4) . ?
C41 C46 1.390(5) . ?
C41 P2 1.816(3) . ?
C42 H42 0.9300 . ?
C42 C43 1.388(5) . ?
C43 H43 0.9300 . ?
C43 C44 1.372(6) . ?
C44 H44 0.9300 . ?
C44 C45 1.371(5) . ?
C45 H45 0.9300 . ?
C45 C46 1.390(5) . ?
C46 H46 0.9300 . ?
C51 C52 1.399(5) . ?
C51 C56 1.391(5) . ?
C51 P1 1.816(3) . ?
C52 H52 0.9300 . ?
C52 C53 1.383(5) . ?
C53 H53 0.9300 . ?
C53 C54 1.387(5) . ?
C54 H54 0.9300 . ?
C54 C55 1.380(5) . ?
C55 H55 0.9300 . ?
C55 C56 1.387(5) . ?
C56 H56 0.9300 . ?
C61 C62 1.394(5) . ?
C61 C66 1.391(5) . ?
C61 P1 1.827(4) . ?
C62 H62 0.9300 . ?
C62 C63 1.392(6) . ?
C63 H63 0.9300 . ?
C63 C64 1.371(6) . ?
C64 H64 0.9300 . ?
C64 C65 1.380(6) . ?
C65 H65 0.9300 . ?
C65 C66 1.399(5) . ?
C66 H66 0.9300 . ?
Ni1 P2 2.1784(9) . ?
Ni1 S11 2.2007(9) . ?
Ni1 S13 2.1941(9) . ?
Ni1 P1 2.1841(9) . ?
O1W H1WA 0.855(17) . ?
O1W H1WB 0.854(17) . ?

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
H3A C3 H3B 108.2 . . ?
C2 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C2 C3 P1 109.4(2) . . ?
P1 C3 H3A 109.8 . . ?
P1 C3 H3B 109.8 . . ?
C3 C2 H2A 109.9 . . ?
C3 C2 H2B 109.9 . . ?
C3 C2 P2 109.1(2) . . ?
H2A C2 H2B 108.3 . . ?
P2 C2 H2A 109.9 . . ?
P2 C2 H2B 109.9 . . ?
C14 C12 S11 127.6(3) . . ?
C14 C12 S13 127.3(3) . . ?
S13 C12 S11 105.12(17) . . ?
C12 C14 C15 120.1(3) . . ?
C12 C14 C19 120.6(3) . . ?
C15 C14 C19 119.3(3) . . ?
C14 C15 C16 117.9(3) . . ?
O15 C15 C14 123.1(3) . . ?
O15 C15 C16 118.9(3) . . ?
C15 C16 H16A 108.5 . . ?
C15 C16 H16B 108.5 . . ?
C15 C16 C17 115.2(3) . . ?
H16A C16 H16B 107.5 . . ?
C17 C16 H16A 108.5 . . ?
C17 C16 H16B 108.5 . . ?
C16 C17 C18 107.4(3) . . ?
C16 C17 C171 108.7(3) . . ?
C16 C17 C172 111.5(3) . . ?
C18 C17 C171 110.5(3) . . ?
C172 C17 C18 109.8(3) . . ?
C172 C17 C171 109.0(3) . . ?
C17 C18 H18A 108.5 . . ?
C17 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C19 C18 C17 115.0(3) . . ?
C19 C18 H18A 108.5 . . ?
C19 C18 H18B 108.5 . . ?
C14 C19 C18 119.7(3) . . ?
O19 C19 C14 122.2(3) . . ?
O19 C19 C18 118.1(3) . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17B 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17E 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C32 C31 P2 122.7(3) . . ?
C36 C31 C32 119.1(3) . . ?
C36 C31 P2 118.1(2) . . ?
C31 C32 H32 120.2 . . ?
C33 C32 C31 119.5(3) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 H33 119.5 . . ?
C34 C33 C32 121.0(3) . . ?
C34 C33 H33 119.5 . . ?
C33 C34 H34 120.2 . . ?
C33 C34 C35 119.6(3) . . ?
C35 C34 H34 120.2 . . ?
C34 C35 H35 119.8 . . ?
C34 C35 C36 120.3(3) . . ?
C36 C35 H35 119.8 . . ?
C31 C36 H36 119.8 . . ?
C35 C36 C31 120.4(3) . . ?
C35 C36 H36 119.8 . . ?
C42 C41 C46 119.6(3) . . ?
C42 C41 P2 119.0(3) . . ?
C46 C41 P2 121.3(2) . . ?
C41 C42 H42 120.1 . . ?
C41 C42 C43 119.8(4) . . ?
C43 C42 H42 120.1 . . ?
C42 C43 H43 119.9 . . ?
C44 C43 C42 120.3(3) . . ?
C44 C43 H43 119.9 . . ?
C43 C44 H44 119.8 . . ?
C45 C44 C43 120.5(3) . . ?
C45 C44 H44 119.8 . . ?
C44 C45 H45 120.0 . . ?
C44 C45 C46 120.0(3) . . ?
C46 C45 H45 120.0 . . ?
C41 C46 C45 119.9(3) . . ?
C41 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C52 C51 P1 119.2(3) . . ?
C56 C51 C52 119.2(3) . . ?
C56 C51 P1 121.6(3) . . ?
C51 C52 H52 120.0 . . ?
C53 C52 C51 120.1(3) . . ?
C53 C52 H52 120.0 . . ?
C52 C53 H53 119.9 . . ?
C52 C53 C54 120.2(3) . . ?
C54 C53 H53 119.9 . . ?
C53 C54 H54 119.9 . . ?
C55 C54 C53 120.2(3) . . ?
C55 C54 H54 119.9 . . ?
C54 C55 H55 120.0 . . ?
C54 C55 C56 120.0(4) . . ?
C56 C55 H55 120.0 . . ?
C51 C56 H56 119.8 . . ?
C55 C56 C51 120.4(3) . . ?
C55 C56 H56 119.8 . . ?
C62 C61 P1 123.6(3) . . ?
C66 C61 C62 119.1(3) . . ?
C66 C61 P1 117.3(3) . . ?
C61 C62 H62 120.1 . . ?
C63 C62 C61 119.7(4) . . ?
C63 C62 H62 120.1 . . ?
C62 C63 H63 119.5 . . ?
C64 C63 C62 121.0(4) . . ?
C64 C63 H63 119.5 . . ?
C63 C64 H64 120.0 . . ?
C63 C64 C65 119.9(4) . . ?
C65 C64 H64 120.0 . . ?
C64 C65 H65 120.1 . . ?
C64 C65 C66 119.8(4) . . ?
C66 C65 H65 120.1 . . ?
C61 C66 C65 120.4(4) . . ?
C61 C66 H66 119.8 . . ?
C65 C66 H66 119.8 . . ?
P2 Ni1 S11 96.20(3) . . ?
P2 Ni1 S13 170.89(4) . . ?
P2 Ni1 P1 87.76(3) . . ?
S13 Ni1 S11 77.80(3) . . ?
P1 Ni1 S11 174.45(4) . . ?
P1 Ni1 S13 98.73(3) . . ?
H1WA O1W H1WB 111(3) . . ?
C2 P2 Ni1 108.95(11) . . ?
C31 P2 C2 106.05(16) . . ?
C31 P2 C41 106.19(14) . . ?
C31 P2 Ni1 112.45(10) . . ?
C41 P2 C2 103.83(14) . . ?
C41 P2 Ni1 118.40(10) . . ?
C12 S11 Ni1 88.04(11) . . ?
C12 S13 Ni1 88.33(11) . . ?
C3 P1 Ni1 109.06(11) . . ?
C51 P1 C3 103.28(15) . . ?
C51 P1 C61 103.42(15) . . ?
C51 P1 Ni1 122.17(11) . . ?
C61 P1 C3 106.82(17) . . ?
C61 P1 Ni1 110.95(11) . . ?

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
_geom_hbond_publ_flag
C3 H3B O15 0.97 2.57 3.205(4) 123.0 3_655 yes
C16 H16B S13 0.97 2.95 3.909(4) 170.0 5_666 yes
C18 H18A S11 0.97 2.92 3.877(3) 170.5 5_666 yes
C32 H32 S11 0.93 3.01 3.885(4) 156.9 3_655 yes
C36 H36 S11 0.93 2.97 3.685(3) 135.2 . yes
C42 H42 S11 0.93 2.96 3.459(4) 115.4 . yes
C56 H56 S13 0.93 2.74 3.456(3) 134.6 . yes
O1W H1WA O19 0.855(17) 2.28(3) 3.006(4) 142(3) . yes
O1W H1WB O15 0.854(17) 2.19(2) 3.020(4) 163(3) 5_666 yes

_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_1
_database_code_depnum_ccdc_archive 'CCDC 1532641'
_audit_update_record             
;
2019-12-30 deposited with the CCDC.	2020-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H34 Ni O2 P2 S2'
_chemical_formula_weight         719.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   12.6370(12)
_cell_length_b                   20.1246(14)
_cell_length_c                   14.0596(9)
_cell_angle_alpha                90
_cell_angle_beta                 109.096(8)
_cell_angle_gamma                90
_cell_volume                     3378.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    18627
_cell_measurement_theta_min      3.40
_cell_measurement_theta_max      30.00

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'

_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_T_max  1.000


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            18627
_diffrn_reflns_av_unetI/netI     0.1182
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.402
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             9487
_reflns_number_gt                6287
_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       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL, PLATON, WINGX (Ferrugia, 2012)'

_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)+(0.0345P)²] 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         9487
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0757
_refine_ls_wR_factor_ref         0.1348
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.11895(4) 0.16410(2) 0.12081(3) 0.01631(12) Uani 1 1 d . . . . .
P2 P 0.19226(8) 0.18827(5) 0.00596(6) 0.0168(2) Uani 1 1 d . . . . .
C2 C 0.0805(3) 0.21907(18) -0.1043(2) 0.0173(7) Uani 1 1 d . . . . .
H2A H 0.112038 0.241229 -0.150096 0.021 Uiso 1 1 calc R U . . .
H2B H 0.034150 0.182518 -0.139695 0.021 Uiso 1 1 calc R U . . .
C3 C 0.0106(3) 0.26798(18) -0.0661(2) 0.0177(8) Uani 1 1 d . . . . .
H3A H -0.058536 0.278361 -0.119465 0.021 Uiso 1 1 calc R U . . .
H3B H 0.051893 0.308945 -0.044398 0.021 Uiso 1 1 calc R U . . .
P1 P -0.02035(8) 0.22894(5) 0.04011(6) 0.0179(2) Uani 1 1 d . . . . .
S11 S 0.25250(8) 0.09634(5) 0.20624(6) 0.0224(2) Uani 1 1 d . . . . .
C12 C 0.1800(3) 0.08464(17) 0.2904(2) 0.0172(7) Uani 1 1 d . . . . .
S13 S 0.05939(8) 0.13187(5) 0.24350(6) 0.0221(2) Uani 1 1 d . . . . .
C14 C 0.2132(3) 0.04593(17) 0.3774(2) 0.0158(7) Uani 1 1 d . . . . .
C19 C 0.1446(3) 0.04426(18) 0.4434(3) 0.0210(8) Uani 1 1 d . . . . .
O19 O 0.0557(2) 0.07438(13) 0.42448(18) 0.0255(6) Uani 1 1 d . . . . .
C16B C 0.1866(4) 0.0044(2) 0.5397(3) 0.0438(13) Uani 0.635(11) 1 d . . P A 1
H16A H 0.229169 0.034004 0.593028 0.053 Uiso 0.635(11) 1 calc R U P A 1
H16B H 0.122110 -0.010499 0.556891 0.053 Uiso 0.635(11) 1 calc R U P A 1
C17B C 0.2563(5) -0.0535(3) 0.5392(4) 0.0180(16) Uiso 0.635(11) 1 d . . P A 1
H17B H 0.207050 -0.086585 0.495218 0.022 Uiso 0.635(11) 1 calc R U P A 1
C18B C 0.3467(3) -0.03868(19) 0.4949(2) 0.0223(8) Uani 0.635(11) 1 d . . P A 1
H18A H 0.374269 -0.080538 0.478116 0.027 Uiso 0.635(11) 1 calc R U P A 1
H18B H 0.408189 -0.017522 0.546319 0.027 Uiso 0.635(11) 1 calc R U P A 1
C16A C 0.1866(4) 0.0044(2) 0.5397(3) 0.0438(13) Uani 0.365(11) 1 d . . P A 2
H16C H 0.178461 0.032404 0.593132 0.053 Uiso 0.365(11) 1 calc R U P A 2
H16D H 0.135494 -0.032591 0.532859 0.053 Uiso 0.365(11) 1 calc R U P A 2
C17A C 0.2908(9) -0.0206(6) 0.5727(7) 0.017(3) Uiso 0.365(11) 1 d . . P A 2
H17A H 0.337851 0.013902 0.615131 0.020 Uiso 0.365(11) 1 calc R U P A 2
C18A C 0.3467(3) -0.03868(19) 0.4949(2) 0.0223(8) Uani 0.365(11) 1 d . . P A 2
H18C H 0.427204 -0.036388 0.526838 0.027 Uiso 0.365(11) 1 calc R U P A 2
H18D H 0.327855 -0.084319 0.473955 0.027 Uiso 0.365(11) 1 calc R U P A 2
C15 C 0.3141(3) 0.00521(18) 0.4017(2) 0.0178(8) Uani 1 1 d . . . . .
O15 O 0.3752(2) 0.00428(14) 0.34939(17) 0.0272(7) Uani 1 1 d . . . . .
C21 C 0.3040(4) -0.0859(2) 0.6447(3) 0.0337(11) Uani 1 1 d . . . . .
C26 C 0.4144(4) -0.1038(2) 0.6926(3) 0.0357(11) Uani 1 1 d . . . . .
H26 H 0.469872 -0.087822 0.668380 0.043 Uiso 1 1 calc R U . . .
C25 C 0.4436(3) -0.14499(19) 0.7757(3) 0.0261(9) Uani 1 1 d . . . . .
H25 H 0.517832 -0.157577 0.806121 0.031 Uiso 1 1 calc R U . . .
C24 C 0.3619(4) -0.1675(2) 0.8137(3) 0.0320(10) Uani 1 1 d . . . . .
H24 H 0.380565 -0.195459 0.869418 0.038 Uiso 1 1 calc R U . . .
C23 C 0.2529(4) -0.14793(19) 0.7681(3) 0.0286(9) Uani 1 1 d . . . . .
H23 H 0.198229 -0.161912 0.794753 0.034 Uiso 1 1 calc R U . . .
C22 C 0.2224(3) -0.10786(19) 0.6834(2) 0.0238(9) Uani 1 1 d . . . . .
H22 H 0.147951 -0.095821 0.652714 0.029 Uiso 1 1 calc R U . . .
C41 C 0.2578(3) 0.12169(19) -0.0408(2) 0.0203(8) Uani 1 1 d . . . . .
C42 C 0.3704(3) 0.1208(2) -0.0339(3) 0.0280(9) Uani 1 1 d . . . . .
H42 H 0.416763 0.156336 -0.004892 0.034 Uiso 1 1 calc R U . . .
C43 C 0.4129(4) 0.0665(2) -0.0705(3) 0.0363(11) Uani 1 1 d . . . . .
H43 H 0.488448 0.065578 -0.064438 0.044 Uiso 1 1 calc R U . . .
C44 C 0.3451(4) 0.0143(2) -0.1155(3) 0.0369(11) Uani 1 1 d . . . . .
H44 H 0.374265 -0.021113 -0.141590 0.044 Uiso 1 1 calc R U . . .
C45 C 0.2340(4) 0.0142(2) -0.1221(3) 0.0337(10) Uani 1 1 d . . . . .
H45 H 0.188201 -0.021341 -0.151951 0.040 Uiso 1 1 calc R U . . .
C46 C 0.1908(4) 0.06722(19) -0.0841(3) 0.0263(9) Uani 1 1 d . . . . .
H46 H 0.116078 0.066605 -0.087438 0.032 Uiso 1 1 calc R U . . .
C51 C 0.2921(3) 0.25633(18) 0.0419(2) 0.0193(8) Uani 1 1 d . . . . .
C52 C 0.3211(3) 0.2824(2) 0.1388(3) 0.0246(9) Uani 1 1 d . . . . .
H52 H 0.291944 0.263630 0.185289 0.029 Uiso 1 1 calc R U . . .
C53 C 0.3926(3) 0.3358(2) 0.1662(3) 0.0292(9) Uani 1 1 d . . . . .
H53 H 0.409328 0.353724 0.230383 0.035 Uiso 1 1 calc R U . . .
C54 C 0.4398(4) 0.3629(2) 0.0991(3) 0.0327(10) Uani 1 1 d . . . . .
H54 H 0.490528 0.397775 0.118928 0.039 Uiso 1 1 calc R U . . .
C55 C 0.4111(4) 0.3379(2) 0.0025(3) 0.0336(10) Uani 1 1 d . . . . .
H55 H 0.441681 0.356553 -0.043228 0.040 Uiso 1 1 calc R U . . .
C56 C 0.3375(3) 0.2857(2) -0.0264(3) 0.0275(9) Uani 1 1 d . . . . .
H56 H 0.317660 0.269647 -0.091982 0.033 Uiso 1 1 calc R U . . .
C61 C -0.0554(3) 0.29719(18) 0.1081(2) 0.0199(8) Uani 1 1 d . . . . .
C62 C 0.0142(4) 0.35329(19) 0.1319(3) 0.0267(9) Uani 1 1 d . . . . .
H62 H 0.076097 0.355604 0.110123 0.032 Uiso 1 1 calc R U . . .
C63 C -0.0076(4) 0.4054(2) 0.1874(3) 0.0340(11) Uani 1 1 d . . . . .
H63 H 0.038776 0.442465 0.202108 0.041 Uiso 1 1 calc R U . . .
C64 C -0.0991(4) 0.4016(2) 0.2208(3) 0.0365(12) Uani 1 1 d . . . . .
H64 H -0.113946 0.436194 0.258431 0.044 Uiso 1 1 calc R U . . .
C65 C -0.1683(4) 0.3468(2) 0.1986(3) 0.0343(11) Uani 1 1 d . . . . .
H65 H -0.229110 0.344372 0.221827 0.041 Uiso 1 1 calc R U . . .
C66 C -0.1474(3) 0.2952(2) 0.1416(3) 0.0255(9) Uani 1 1 d . . . . .
H66 H -0.195474 0.258881 0.125718 0.031 Uiso 1 1 calc R U . . .
C71 C -0.1494(3) 0.18427(19) -0.0227(2) 0.0208(8) Uani 1 1 d . . . . .
C72 C -0.2475(3) 0.2169(2) -0.0768(3) 0.0278(9) Uani 1 1 d . . . . .
H72 H -0.250528 0.263072 -0.074515 0.033 Uiso 1 1 calc R U . . .
C73 C -0.3408(4) 0.1819(2) -0.1340(3) 0.0342(10) Uani 1 1 d . . . . .
H73 H -0.406412 0.204251 -0.169066 0.041 Uiso 1 1 calc R U . . .
C74 C -0.3357(4) 0.1134(2) -0.1387(3) 0.0367(11) Uani 1 1 d . . . . .
H74 H -0.397593 0.089732 -0.178335 0.044 Uiso 1 1 calc R U . . .
C75 C -0.2401(4) 0.0801(2) -0.0853(3) 0.0333(10) Uani 1 1 d . . . . .
H75 H -0.237418 0.034030 -0.088608 0.040 Uiso 1 1 calc R U . . .
C76 C -0.1472(4) 0.1153(2) -0.0263(3) 0.0268(9) Uani 1 1 d . . . . .
H76 H -0.083024 0.092517 0.011143 0.032 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 P2 2.1636(9) . ?
Ni1 P1 2.1867(11) . ?
Ni1 S13 2.1937(9) . ?
Ni1 S11 2.1963(11) . ?
P2 C41 1.808(4) . ?
P2 C51 1.818(4) . ?
P2 C2 1.830(3) . ?
C2 C3 1.532(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 P1 1.839(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
P1 C61 1.810(4) . ?
P1 C71 1.818(4) . ?
S11 C12 1.734(3) . ?
C12 C14 1.394(4) . ?
C12 S13 1.733(4) . ?
C14 C15 1.459(5) . ?
C14 C19 1.462(4) . ?
C19 O19 1.228(4) . ?
C19 C16A 1.512(5) . ?
C19 C16B 1.512(5) . ?
C16B C17B 1.463(7) . ?
C16B H16A 0.9700 . ?
C16B H16B 0.9700 . ?
C17B C18B 1.499(6) . ?
C17B C21 1.550(6) . ?
C17B H17B 0.9800 . ?
C18B C15 1.521(4) . ?
C18B H18A 0.9700 . ?
C18B H18B 0.9700 . ?
C16A C17A 1.344(10) . ?
C16A H16C 0.9700 . ?
C16A H16D 0.9700 . ?
C17A C18A 1.527(9) . ?
C17A C21 1.632(10) . ?
C17A H17A 0.9800 . ?
C18A C15 1.521(4) . ?
C18A H18C 0.9700 . ?
C18A H18D 0.9700 . ?
C15 O15 1.228(4) . ?
C21 C26 1.384(6) . ?
C21 C22 1.387(5) . ?
C26 C25 1.382(5) . ?
C26 H26 0.9300 . ?
C25 C24 1.385(5) . ?
C25 H25 0.9300 . ?
C24 C23 1.373(6) . ?
C24 H24 0.9300 . ?
C23 C22 1.385(5) . ?
C23 H23 0.9300 . ?
C22 H22 0.9300 . ?
C41 C42 1.394(5) . ?
C41 C46 1.397(5) . ?
C42 C43 1.388(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.374(6) . ?
C43 H43 0.9300 . ?
C44 C45 1.376(6) . ?
C44 H44 0.9300 . ?
C45 C46 1.383(5) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C51 C52 1.393(5) . ?
C51 C56 1.400(5) . ?
C52 C53 1.374(5) . ?
C52 H52 0.9300 . ?
C53 C54 1.383(5) . ?
C53 H53 0.9300 . ?
C54 C55 1.381(5) . ?
C54 H54 0.9300 . ?
C55 C56 1.374(6) . ?
C55 H55 0.9300 . ?
C56 H56 0.9300 . ?
C61 C66 1.390(5) . ?
C61 C62 1.403(5) . ?
C62 C63 1.387(5) . ?
C62 H62 0.9300 . ?
C63 C64 1.385(6) . ?
C63 H63 0.9300 . ?
C64 C65 1.378(6) . ?
C64 H64 0.9300 . ?
C65 C66 1.388(5) . ?
C65 H65 0.9300 . ?
C66 H66 0.9300 . ?
C71 C76 1.389(5) . ?
C71 C72 1.390(5) . ?
C72 C73 1.383(6) . ?
C72 H72 0.9300 . ?
C73 C74 1.383(6) . ?
C73 H73 0.9300 . ?
C74 C75 1.370(6) . ?
C74 H74 0.9300 . ?
C75 C76 1.390(5) . ?
C75 H75 0.9300 . ?
C76 H76 0.9300 . ?

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
P2 Ni1 P1 86.97(4) . . ?
P2 Ni1 S13 173.82(4) . . ?
P1 Ni1 S13 99.17(4) . . ?
P2 Ni1 S11 96.18(4) . . ?
P1 Ni1 S11 176.67(4) . . ?
S13 Ni1 S11 77.66(4) . . ?
C41 P2 C51 107.49(17) . . ?
C41 P2 C2 105.17(15) . . ?
C51 P2 C2 104.67(17) . . ?
C41 P2 Ni1 117.61(11) . . ?
C51 P2 Ni1 112.94(10) . . ?
C2 P2 Ni1 107.93(11) . . ?
C3 C2 P2 107.1(2) . . ?
C3 C2 H2A 110.3 . . ?
P2 C2 H2A 110.3 . . ?
C3 C2 H2B 110.3 . . ?
P2 C2 H2B 110.3 . . ?
H2A C2 H2B 108.5 . . ?
C2 C3 P1 108.1(2) . . ?
C2 C3 H3A 110.1 . . ?
P1 C3 H3A 110.1 . . ?
C2 C3 H3B 110.1 . . ?
P1 C3 H3B 110.1 . . ?
H3A C3 H3B 108.4 . . ?
C61 P1 C71 107.22(17) . . ?
C61 P1 C3 104.98(15) . . ?
C71 P1 C3 102.25(16) . . ?
C61 P1 Ni1 118.26(12) . . ?
C71 P1 Ni1 113.52(13) . . ?
C3 P1 Ni1 109.11(12) . . ?
C12 S11 Ni1 88.53(12) . . ?
C14 C12 S13 128.0(3) . . ?
C14 C12 S11 126.9(3) . . ?
S13 C12 S11 105.13(17) . . ?
C12 S13 Ni1 88.65(11) . . ?
C12 C14 C15 120.6(3) . . ?
C12 C14 C19 119.9(3) . . ?
C15 C14 C19 119.5(3) . . ?
O19 C19 C14 122.8(3) . . ?
O19 C19 C16A 118.9(3) . . ?
C14 C19 C16A 118.3(3) . . ?
O19 C19 C16B 118.9(3) . . ?
C14 C19 C16B 118.3(3) . . ?
C17B C16B C19 116.9(3) . . ?
C17B C16B H16A 108.1 . . ?
C19 C16B H16A 108.1 . . ?
C17B C16B H16B 108.1 . . ?
C19 C16B H16B 108.1 . . ?
H16A C16B H16B 107.3 . . ?
C16B C17B C18B 112.7(5) . . ?
C16B C17B C21 112.1(4) . . ?
C18B C17B C21 111.7(4) . . ?
C16B C17B H17B 106.6 . . ?
C18B C17B H17B 106.6 . . ?
C21 C17B H17B 106.6 . . ?
C17B C18B C15 116.5(4) . . ?
C17B C18B H18A 108.2 . . ?
C15 C18B H18A 108.2 . . ?
C17B C18B H18B 108.2 . . ?
C15 C18B H18B 108.2 . . ?
H18A C18B H18B 107.3 . . ?
C17A C16A C19 121.6(5) . . ?
C17A C16A H16C 106.9 . . ?
C19 C16A H16C 106.9 . . ?
C17A C16A H16D 106.9 . . ?
C19 C16A H16D 106.9 . . ?
H16C C16A H16D 106.7 . . ?
C16A C17A C18A 118.2(7) . . ?
C16A C17A C21 113.9(7) . . ?
C18A C17A C21 106.0(6) . . ?
C16A C17A H17A 105.9 . . ?
C18A C17A H17A 105.9 . . ?
C21 C17A H17A 105.9 . . ?
C15 C18A C17A 114.9(4) . . ?
C15 C18A H18C 108.5 . . ?
C17A C18A H18C 108.5 . . ?
C15 C18A H18D 108.5 . . ?
C17A C18A H18D 108.5 . . ?
H18C C18A H18D 107.5 . . ?
O15 C15 C14 122.8(3) . . ?
O15 C15 C18B 117.5(3) . . ?
C14 C15 C18B 119.8(3) . . ?
O15 C15 C18A 117.5(3) . . ?
C14 C15 C18A 119.8(3) . . ?
C26 C21 C22 119.1(3) . . ?
C26 C21 C17B 126.1(4) . . ?
C22 C21 C17B 113.8(4) . . ?
C26 C21 C17A 113.2(5) . . ?
C22 C21 C17A 124.2(5) . . ?
C25 C26 C21 121.0(4) . . ?
C25 C26 H26 119.5 . . ?
C21 C26 H26 119.5 . . ?
C26 C25 C24 119.8(4) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C23 C24 C25 119.1(3) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C24 C23 C22 121.5(4) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C22 C21 119.4(4) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C42 C41 C46 118.6(3) . . ?
C42 C41 P2 124.2(3) . . ?
C46 C41 P2 117.1(3) . . ?
C43 C42 C41 119.7(4) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C44 C43 C42 121.0(4) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C43 C44 C45 120.0(4) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C46 119.8(4) . . ?
C44 C45 H45 120.1 . . ?
C46 C45 H45 120.1 . . ?
C45 C46 C41 120.9(4) . . ?
C45 C46 H46 119.5 . . ?
C41 C46 H46 119.5 . . ?
C52 C51 C56 118.4(3) . . ?
C52 C51 P2 119.5(3) . . ?
C56 C51 P2 122.0(3) . . ?
C53 C52 C51 120.5(3) . . ?
C53 C52 H52 119.7 . . ?
C51 C52 H52 119.7 . . ?
C52 C53 C54 120.5(4) . . ?
C52 C53 H53 119.8 . . ?
C54 C53 H53 119.8 . . ?
C55 C54 C53 119.6(4) . . ?
C55 C54 H54 120.2 . . ?
C53 C54 H54 120.2 . . ?
C56 C55 C54 120.2(4) . . ?
C56 C55 H55 119.9 . . ?
C54 C55 H55 119.9 . . ?
C55 C56 C51 120.6(3) . . ?
C55 C56 H56 119.7 . . ?
C51 C56 H56 119.7 . . ?
C66 C61 C62 118.1(3) . . ?
C66 C61 P1 122.3(3) . . ?
C62 C61 P1 119.6(3) . . ?
C63 C62 C61 121.2(4) . . ?
C63 C62 H62 119.4 . . ?
C61 C62 H62 119.4 . . ?
C64 C63 C62 119.4(4) . . ?
C64 C63 H63 120.3 . . ?
C62 C63 H63 120.3 . . ?
C65 C64 C63 120.3(4) . . ?
C65 C64 H64 119.8 . . ?
C63 C64 H64 119.8 . . ?
C64 C65 C66 120.2(4) . . ?
C64 C65 H65 119.9 . . ?
C66 C65 H65 119.9 . . ?
C65 C66 C61 120.8(4) . . ?
C65 C66 H66 119.6 . . ?
C61 C66 H66 119.6 . . ?
C76 C71 C72 118.6(4) . . ?
C76 C71 P1 119.0(3) . . ?
C72 C71 P1 122.0(3) . . ?
C73 C72 C71 121.0(4) . . ?
C73 C72 H72 119.5 . . ?
C71 C72 H72 119.5 . . ?
C74 C73 C72 119.4(4) . . ?
C74 C73 H73 120.3 . . ?
C72 C73 H73 120.3 . . ?
C75 C74 C73 120.5(4) . . ?
C75 C74 H74 119.7 . . ?
C73 C74 H74 119.7 . . ?
C74 C75 C76 120.0(4) . . ?
C74 C75 H75 120.0 . . ?
C76 C75 H75 120.0 . . ?
C71 C76 C75 120.5(4) . . ?
C71 C76 H76 119.8 . . ?
C75 C76 H76 119.8 . . ?

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
C2 H2A S13 0.97 2.92 3.644(3) 131.8 4_565
C26 H26 O15 0.93 2.65 3.528(5) 156.9 3_656
C18A H18C O15 0.97 2.61 3.548(5) 161.6 3_656
C3 H3B O19 0.97 2.39 3.233(4) 144.9 4_565
C22 H22 O19 0.93 2.48 3.408(5) 174.5 3_556
C16B H16B O19 0.97 2.67 3.626(5) 166.9 3_556
C2 H2A S13 0.97 2.92 3.644(3) 131.8 4_565
C3 H3B O19 0.97 2.39 3.233(4) 144.9 4_565
C18A H18C O15 0.97 2.61 3.548(5) 161.6 3_656

_refine_diff_density_max         0.687
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.098

