# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_6a
_audit_block_doi                 10.5517/cc7q9cl
_database_code_depnum_ccdc_archive 'CCDC 229969'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/b401245c 2004
_audit_update_record             
;
2004-01-29 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H19 Cl4 F2 N O5 Sn'
_chemical_formula_weight         579.79

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   10.4879(11)
_cell_length_b                   18.8071(19)
_cell_length_c                   10.7203(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.993(2)
_cell_angle_gamma                90.00
_cell_volume                     2060.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7168
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      28.39

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    1.802
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_process_details   
;
absorption correction based on 5879 reflections (SADABS); Rint 0.034 before
correction and 0.014 after.
;

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10971
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         26.00
_reflns_number_total             4033
_reflns_number_gt                3761
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0328P)²+1.0826P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4033
_refine_ls_number_parameters     247
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0639
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.732849(17) 0.482949(9) 0.775439(15) 0.02270(7) Uani 1 1 d . . .
Cl1 Cl 0.50709(7) 0.50333(4) 0.70984(8) 0.04142(18) Uani 1 1 d . . .
Cl2 Cl 0.74585(7) 0.52387(3) 0.98742(6) 0.02899(15) Uani 1 1 d . . .
Cl3 Cl 0.74903(7) 0.42475(4) 0.58570(6) 0.03208(16) Uani 1 1 d . . .
Cl4 Cl 0.82018(9) 0.58959(4) 0.71858(7) 0.0439(2) Uani 1 1 d . . .
F1 F 0.78495(15) 0.23688(8) 0.87737(14) 0.0310(3) Uani 1 1 d . . .
F2 F 0.88786(17) 0.25825(9) 0.72809(14) 0.0376(4) Uani 1 1 d . . .
N1 N 0.6762(2) 0.34931(11) 1.04422(19) 0.0230(4) Uani 1 1 d . . .
O1 O 1.12119(18) 0.24508(10) 0.92390(18) 0.0307(4) Uani 1 1 d . . .
O2 O 0.93782(17) 0.44521(9) 0.84473(16) 0.0230(4) Uani 1 1 d . . .
O3 O 1.06855(18) 0.36946(9) 0.77628(17) 0.0286(4) Uani 1 1 d . . .
O4 O 0.87694(16) 0.34858(9) 1.00860(15) 0.0189(3) Uani 1 1 d . . .
O5 O 0.70338(16) 0.37991(9) 0.84833(15) 0.0212(4) Uani 1 1 d . . .
C1 C 1.0874(2) 0.29510(14) 1.0102(2) 0.0244(5) Uani 1 1 d . . .
H1 H 1.1558 0.3319 1.0421 0.029 Uiso 1 1 calc R . .
C2 C 0.9553(2) 0.32511(13) 0.9250(2) 0.0187(5) Uani 1 1 d . . .
C3 C 0.9025(3) 0.25417(14) 0.8545(2) 0.0259(5) Uani 1 1 d . . .
C4 C 1.0109(3) 0.20043(14) 0.9156(3) 0.0288(6) Uani 1 1 d . . .
H4 H 1.0124 0.1555 0.8661 0.035 Uiso 1 1 calc R . .
C5 C 1.0033(3) 0.19049(15) 1.0527(3) 0.0327(6) Uani 1 1 d . . .
H5 H 0.9709 0.1503 1.0895 0.039 Uiso 1 1 calc R . .
C6 C 1.0520(2) 0.25047(15) 1.1120(2) 0.0274(6) Uani 1 1 d . . .
H6 H 1.0618 0.2621 1.1999 0.033 Uiso 1 1 calc R . .
C7 C 0.9840(2) 0.38575(13) 0.8422(2) 0.0211(5) Uani 1 1 d . . .
C8 C 1.1058(3) 0.42550(16) 0.6945(3) 0.0352(7) Uani 1 1 d . . .
H8A H 1.0274 0.4431 0.6326 0.042 Uiso 1 1 calc R . .
H8B H 1.1469 0.4660 0.7477 0.042 Uiso 1 1 calc R . .
C9 C 1.1970(5) 0.3944(2) 0.6277(4) 0.0737(13) Uani 1 1 d . . .
H9A H 1.2719 0.3749 0.6899 0.111 Uiso 1 1 calc R . .
H9B H 1.2275 0.4310 0.5761 0.111 Uiso 1 1 calc R . .
H9C H 1.1536 0.3563 0.5716 0.111 Uiso 1 1 calc R . .
C10 C 0.7476(2) 0.36033(12) 0.9620(2) 0.0200(5) Uani 1 1 d . . .
C11 C 0.5366(3) 0.36802(15) 1.0106(3) 0.0313(6) Uani 1 1 d . . .
H11A H 0.5235 0.4087 0.9506 0.038 Uiso 1 1 calc R . .
H11B H 0.5085 0.3829 1.0889 0.038 Uiso 1 1 calc R . .
C12 C 0.4536(3) 0.30654(18) 0.9499(3) 0.0426(7) Uani 1 1 d . . .
H12A H 0.4763 0.2943 0.8687 0.064 Uiso 1 1 calc R . .
H12B H 0.3610 0.3199 0.9338 0.064 Uiso 1 1 calc R . .
H12C H 0.4695 0.2655 1.0075 0.064 Uiso 1 1 calc R . .
C13 C 0.7291(3) 0.31724(14) 1.1705(2) 0.0275(6) Uani 1 1 d . . .
H13A H 0.7965 0.2817 1.1627 0.033 Uiso 1 1 calc R . .
H13B H 0.6580 0.2922 1.1994 0.033 Uiso 1 1 calc R . .
C14 C 0.7889(3) 0.37190(16) 1.2694(3) 0.0362(7) Uani 1 1 d . . .
H14A H 0.8641 0.3941 1.2447 0.054 Uiso 1 1 calc R . .
H14B H 0.8178 0.3488 1.3528 0.054 Uiso 1 1 calc R . .
H14C H 0.7236 0.4084 1.2748 0.054 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 O5 2.1378(16) . ?
Sn1 O2 2.2268(17) . ?
Sn1 Cl4 2.3418(7) . ?
Sn1 Cl1 2.3450(8) . ?
Sn1 Cl3 2.3494(7) . ?
Sn1 Cl2 2.3740(7) . ?
F1 C3 1.350(3) . ?
F2 C3 1.332(3) . ?
N1 C10 1.295(3) . ?
N1 C11 1.469(3) . ?
N1 C13 1.472(3) . ?
O1 C4 1.416(3) . ?
O1 C1 1.419(3) . ?
O2 C7 1.221(3) . ?
O3 C7 1.289(3) . ?
O3 C8 1.478(3) . ?
O4 C10 1.354(3) . ?
O4 C2 1.416(3) . ?
O5 C10 1.258(3) . ?
C1 C6 1.488(4) . ?
C1 C2 1.582(3) . ?
C2 C7 1.517(3) . ?
C2 C3 1.571(3) . ?
C3 C4 1.551(4) . ?
C4 C5 1.502(4) . ?
C5 C6 1.338(4) . ?
C8 C9 1.442(5) . ?
C11 C12 1.505(4) . ?
C13 C14 1.508(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
O5 Sn1 O2 78.30(6) . . ?
O5 Sn1 Cl4 165.61(5) . . ?
O2 Sn1 Cl4 87.43(5) . . ?
O5 Sn1 Cl1 92.21(5) . . ?
O2 Sn1 Cl1 170.42(5) . . ?
Cl4 Sn1 Cl1 102.10(3) . . ?
O5 Sn1 Cl3 86.48(5) . . ?
O2 Sn1 Cl3 83.57(5) . . ?
Cl4 Sn1 Cl3 93.73(3) . . ?
Cl1 Sn1 Cl3 94.65(3) . . ?
O5 Sn1 Cl2 85.75(5) . . ?
O2 Sn1 Cl2 86.60(5) . . ?
Cl4 Sn1 Cl2 91.71(3) . . ?
Cl1 Sn1 Cl2 94.07(3) . . ?
Cl3 Sn1 Cl2 168.53(2) . . ?
C10 N1 C11 119.4(2) . . ?
C10 N1 C13 122.4(2) . . ?
C11 N1 C13 118.2(2) . . ?
C4 O1 C1 96.54(19) . . ?
C7 O2 Sn1 129.98(16) . . ?
C7 O3 C8 117.5(2) . . ?
C10 O4 C2 119.57(18) . . ?
C10 O5 Sn1 124.58(15) . . ?
O1 C1 C6 104.1(2) . . ?
O1 C1 C2 100.06(19) . . ?
C6 C1 C2 107.1(2) . . ?
O4 C2 C7 110.85(19) . . ?
O4 C2 C3 112.16(19) . . ?
C7 C2 C3 116.86(19) . . ?
O4 C2 C1 107.68(17) . . ?
C7 C2 C1 110.0(2) . . ?
C3 C2 C1 98.21(19) . . ?
F2 C3 F1 107.3(2) . . ?
F2 C3 C4 111.9(2) . . ?
F1 C3 C4 112.3(2) . . ?
F2 C3 C2 112.8(2) . . ?
F1 C3 C2 110.78(19) . . ?
C4 C3 C2 101.8(2) . . ?
O1 C4 C5 103.6(2) . . ?
O1 C4 C3 98.7(2) . . ?
C5 C4 C3 107.4(2) . . ?
C6 C5 C4 105.1(2) . . ?
C5 C6 C1 105.0(2) . . ?
O2 C7 O3 123.7(2) . . ?
O2 C7 C2 122.9(2) . . ?
O3 C7 C2 113.2(2) . . ?
C9 C8 O3 107.4(3) . . ?
O5 C10 N1 124.3(2) . . ?
O5 C10 O4 121.7(2) . . ?
N1 C10 O4 114.0(2) . . ?
N1 C11 C12 111.7(2) . . ?
N1 C13 C14 112.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_mv40a
_database_code_depnum_ccdc_archive 'CCDC 2299001'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2016-10-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H24 N2 Ni O2 P S2, Cl O4'
_chemical_formula_sum            'C20 H24 Cl N2 Ni O6 P S2'
_chemical_formula_weight         577.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C40 H48 N4 O8 P2 S4 Cl2 Ni2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   7.2158(3)
_cell_length_b                   10.0031(8)
_cell_length_c                   18.9825(10)
_cell_angle_alpha                99.859(5)
_cell_angle_beta                 97.908(4)
_cell_angle_gamma                105.106(5)
_cell_volume                     1279.16(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3689
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.7383
_cell_measurement_theta_min      2.1557
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.2747
_exptl_crystal_size_min          0.0631
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9842
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.804
_diffrn_reflns_theta_min         2.160
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.816
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -58.00   35.00   1.0000   47.5900
omega____ theta____ kappa____ phi______ frames
    -       11.7464  -57.0000   60.0000 93

#__ type_ start__ end____ width___ exp.time_
  2 omega  -12.00   68.00   1.0000   47.5900
omega____ theta____ kappa____ phi______ frames
    -       11.7464   72.0000  -26.0000 80

#__ type_ start__ end____ width___ exp.time_
  3 omega  -13.00   82.00   1.0000   47.5900
omega____ theta____ kappa____ phi______ frames
    -       11.7464   57.0000 -150.0000 95
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0608961000
_diffrn_orient_matrix_UB_12      0.0453127000
_diffrn_orient_matrix_UB_13      -0.0008070000
_diffrn_orient_matrix_UB_21      0.0345658000
_diffrn_orient_matrix_UB_22      0.0209515000
_diffrn_orient_matrix_UB_23      -0.0308120000
_diffrn_orient_matrix_UB_31      -0.0765390000
_diffrn_orient_matrix_UB_32      -0.0562802000
_diffrn_orient_matrix_UB_33      -0.0233054000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3907
_reflns_number_total             5964
_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, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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         0.905
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0589
_refine_ls_restrained_S_all      1.034
_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)+(0.0819P)²+0.8576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1815
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   geom
_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 0.43937(8) 0.72830(5) 0.67274(2) 0.0515(2) Uani 1 1 d . . . . .
S1 S 0.4731(2) 0.90037(13) 0.61091(6) 0.0766(4) Uani 1 1 d . . . . .
S2 S 0.2671(2) 0.57491(13) 0.57162(6) 0.0793(4) Uani 1 1 d . . . . .
P1 P 0.2958(2) 0.74855(14) 0.53089(6) 0.0702(4) Uani 1 1 d . . . . .
O1 O 0.0980(6) 0.7738(4) 0.50590(18) 0.0862(11) Uani 1 1 d . . . . .
O2 O 0.3833(6) 0.7418(4) 0.45985(18) 0.0908(11) Uani 1 1 d . . . . .
N6 N 0.6460(4) 0.9530(3) 0.80508(17) 0.0484(7) Uani 1 1 d . . . . .
N7 N 0.3874(5) 0.4800(4) 0.74300(18) 0.0516(8) Uani 1 1 d . . . . .
C1 C 0.5697(6) 0.8636(4) 0.7557(2) 0.0483(9) Uani 1 1 d . . . . .
C2 C 0.4121(6) 0.5777(4) 0.7184(2) 0.0507(9) Uani 1 1 d . . . . .
C3 C 0.2903(9) 0.6312(8) 0.3971(3) 0.104(2) Uani 1 1 d . . . . .
H3A H 0.3330 0.6596 0.3548 0.156 Uiso 1 1 calc GR . . . .
H3B H 0.1511 0.6129 0.3911 0.156 Uiso 1 1 calc GR . . . .
H3C H 0.3243 0.5467 0.4032 0.156 Uiso 1 1 calc GR . . . .
C4 C -0.0407(9) 0.7830(7) 0.5529(3) 0.105(2) Uani 1 1 d . . . . .
H4A H -0.1655 0.7737 0.5242 0.158 Uiso 1 1 calc GR . . . .
H4B H 0.0041 0.8731 0.5867 0.158 Uiso 1 1 calc GR . . . .
H4C H -0.0530 0.7083 0.5793 0.158 Uiso 1 1 calc GR . . . .
C11 C 0.7417(5) 1.0677(4) 0.8629(2) 0.0487(9) Uani 1 1 d . . . . .
C12 C 0.8146(6) 1.1982(4) 0.8458(2) 0.0571(10) Uani 1 1 d . . . . .
C13 C 0.9103(7) 1.3104(5) 0.9044(3) 0.0831(16) Uani 1 1 d . . . . .
H13 H 0.9636 1.3999 0.8957 0.100 Uiso 1 1 calc R . . . .
C14 C 0.9280(8) 1.2924(6) 0.9743(3) 0.0902(17) Uani 1 1 d . . . . .
H14 H 0.9935 1.3692 1.0125 0.108 Uiso 1 1 calc R . . . .
C15 C 0.8496(8) 1.1612(6) 0.9888(3) 0.0804(15) Uani 1 1 d . . . . .
H15 H 0.8621 1.1510 1.0369 0.096 Uiso 1 1 calc R . . . .
C16 C 0.7530(6) 1.0448(5) 0.9337(2) 0.0602(11) Uani 1 1 d . . . . .
C17 C 0.6659(9) 0.9018(6) 0.9477(3) 0.0833(15) Uani 1 1 d . . . . .
H17A H 0.5289 0.8693 0.9266 0.125 Uiso 1 1 calc GR . . . .
H17B H 0.6828 0.9074 0.9993 0.125 Uiso 1 1 calc GR . . . .
H17C H 0.7299 0.8367 0.9262 0.125 Uiso 1 1 calc GR . . . .
C18 C 0.7882(7) 1.2159(6) 0.7693(3) 0.0736(13) Uani 1 1 d . . . . .
H18A H 0.8421 1.1522 0.7406 0.110 Uiso 1 1 calc GR . . . .
H18B H 0.8541 1.3118 0.7679 0.110 Uiso 1 1 calc GR . . . .
H18C H 0.6513 1.1950 0.7498 0.110 Uiso 1 1 calc GR . . . .
C21 C 0.3504(6) 0.3593(4) 0.7727(2) 0.0506(9) Uani 1 1 d . . . . .
C22 C 0.4114(6) 0.3784(5) 0.8480(2) 0.0584(10) Uani 1 1 d . . . . .
C23 C 0.3749(7) 0.2584(5) 0.8759(3) 0.0697(12) Uani 1 1 d . . . . .
H23 H 0.4137 0.2664 0.9256 0.084 Uiso 1 1 calc R . . . .
C24 C 0.2820(7) 0.1260(5) 0.8319(3) 0.0718(13) Uani 1 1 d . . . . .
H24 H 0.2572 0.0463 0.8521 0.086 Uiso 1 1 calc R . . . .
C25 C 0.2261(7) 0.1119(5) 0.7581(3) 0.0657(12) Uani 1 1 d . . . . .
H25 H 0.1660 0.0221 0.7287 0.079 Uiso 1 1 calc R . . . .
C26 C 0.2577(6) 0.2292(5) 0.7268(2) 0.0559(10) Uani 1 1 d . . . . .
C27 C 0.1940(8) 0.2135(6) 0.6464(3) 0.0823(15) Uani 1 1 d . . . . .
H27A H 0.1584 0.2960 0.6375 0.123 Uiso 1 1 calc GR . . . .
H27B H 0.0833 0.1309 0.6281 0.123 Uiso 1 1 calc GR . . . .
H27C H 0.2994 0.2035 0.6221 0.123 Uiso 1 1 calc GR . . . .
C28 C 0.5110(9) 0.5235(6) 0.8948(3) 0.0885(17) Uani 1 1 d . . . . .
H28A H 0.6198 0.5696 0.8750 0.133 Uiso 1 1 calc GR . . . .
H28B H 0.5570 0.5153 0.9433 0.133 Uiso 1 1 calc GR . . . .
H28C H 0.4200 0.5784 0.8961 0.133 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.00075(17) 0.68647(12) 0.78212(6) 0.0647(3) Uani 1 1 d . . . . .
O3 O -0.0573(15) 0.5548(6) 0.7560(6) 0.289(6) Uani 1 1 d . . . . .
O4 O 0.021(2) 0.7430(10) 0.7261(5) 0.305(6) Uani 1 1 d . . . . .
O5 O -0.1044(9) 0.7432(9) 0.8259(3) 0.193(3) Uani 1 1 d . . . . .
O6 O 0.1823(10) 0.7222(13) 0.8204(4) 0.282(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 2.2251(13) . ?
Ni1 S2 2.2191(12) . ?
Ni1 C1 1.843(4) . ?
Ni1 C2 1.844(4) . ?
S1 P1 1.9782(17) . ?
S2 P1 1.9934(17) . ?
P1 O1 1.540(4) . ?
P1 O2 1.564(4) . ?
O1 C4 1.439(7) . ?
O2 C3 1.426(7) . ?
N6 C1 1.138(5) . ?
N6 C11 1.394(5) . ?
N7 C2 1.138(5) . ?
N7 C21 1.397(5) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C11 C12 1.386(6) . ?
C11 C16 1.396(6) . ?
C12 C13 1.390(7) . ?
C12 C18 1.485(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.364(8) . ?
C14 H14 0.9300 . ?
C14 C15 1.377(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.377(6) . ?
C16 C17 1.490(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.400(6) . ?
C21 C26 1.379(6) . ?
C22 C23 1.372(6) . ?
C22 C28 1.501(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.380(7) . ?
C24 H24 0.9300 . ?
C24 C25 1.376(7) . ?
C25 H25 0.9300 . ?
C25 C26 1.384(6) . ?
C26 C27 1.500(6) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Cl1 O3 1.260(6) . ?
Cl1 O4 1.296(7) . ?
Cl1 O5 1.350(5) . ?
Cl1 O6 1.333(6) . ?

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
S2 Ni1 S1 89.01(5) . . ?
C1 Ni1 S1 88.49(12) . . ?
C1 Ni1 S2 175.75(13) . . ?
C1 Ni1 C2 94.79(16) . . ?
C2 Ni1 S1 176.18(12) . . ?
C2 Ni1 S2 87.83(12) . . ?
P1 S1 Ni1 83.66(6) . . ?
P1 S2 Ni1 83.47(5) . . ?
S1 P1 Ni1 51.92(4) . . ?
S1 P1 S2 103.33(7) . . ?
S2 P1 Ni1 51.70(4) . . ?
O1 P1 Ni1 125.11(15) . . ?
O1 P1 S1 114.09(16) . . ?
O1 P1 S2 112.59(17) . . ?
O1 P1 O2 102.4(2) . . ?
O2 P1 Ni1 132.51(17) . . ?
O2 P1 S1 110.78(17) . . ?
O2 P1 S2 114.06(18) . . ?
C4 O1 P1 123.0(4) . . ?
C3 O2 P1 120.7(4) . . ?
C1 N6 C11 176.8(4) . . ?
C2 N7 C21 178.1(4) . . ?
N6 C1 Ni1 175.8(3) . . ?
N7 C2 Ni1 175.9(4) . . ?
O2 C3 H3A 109.5 . . ?
O2 C3 H3B 109.5 . . ?
O2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1 C4 H4A 109.5 . . ?
O1 C4 H4B 109.5 . . ?
O1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N6 C11 C16 118.3(4) . . ?
C12 C11 N6 117.2(4) . . ?
C12 C11 C16 124.5(4) . . ?
C11 C12 C13 116.0(4) . . ?
C11 C12 C18 121.4(4) . . ?
C13 C12 C18 122.6(4) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 C12 121.5(5) . . ?
C14 C13 H13 119.2 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.5(5) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.4(5) . . ?
C16 C15 H15 119.3 . . ?
C11 C16 C17 121.2(4) . . ?
C15 C16 C11 116.1(4) . . ?
C15 C16 C17 122.6(5) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C18 H18A 109.5 . . ?
C12 C18 H18B 109.5 . . ?
C12 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N7 C21 C22 117.5(4) . . ?
C26 C21 N7 118.6(4) . . ?
C26 C21 C22 123.8(4) . . ?
C21 C22 C28 121.0(4) . . ?
C23 C22 C21 116.5(4) . . ?
C23 C22 C28 122.5(4) . . ?
C22 C23 H23 119.2 . . ?
C22 C23 C24 121.5(5) . . ?
C24 C23 H23 119.2 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.0(4) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121.1(4) . . ?
C26 C25 H25 119.4 . . ?
C21 C26 C25 116.9(4) . . ?
C21 C26 C27 122.1(4) . . ?
C25 C26 C27 120.9(4) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C22 C28 H28A 109.5 . . ?
C22 C28 H28B 109.5 . . ?
C22 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O3 Cl1 O4 104.6(7) . . ?
O3 Cl1 O5 118.3(6) . . ?
O3 Cl1 O6 109.7(7) . . ?
O4 Cl1 O5 113.3(6) . . ?
O4 Cl1 O6 103.8(8) . . ?
O6 Cl1 O5 106.3(4) . . ?

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 P1 O1 C4 -3.1(5) . . . . ?
Ni1 P1 O2 C3 116.8(4) . . . . ?
S1 P1 O1 C4 -62.4(5) . . . . ?
S1 P1 O2 C3 173.7(4) . . . . ?
S2 P1 O1 C4 55.0(5) . . . . ?
S2 P1 O2 C3 57.6(5) . . . . ?
O1 P1 O2 C3 -64.3(5) . . . . ?
O2 P1 O1 C4 177.9(4) . . . . ?
N6 C11 C12 C13 -179.6(4) . . . . ?
N6 C11 C12 C18 1.3(6) . . . . ?
N6 C11 C16 C15 179.7(4) . . . . ?
N6 C11 C16 C17 0.1(6) . . . . ?
N7 C21 C22 C23 -179.5(4) . . . . ?
N7 C21 C22 C28 0.6(6) . . . . ?
N7 C21 C26 C25 179.1(4) . . . . ?
N7 C21 C26 C27 -0.6(6) . . . . ?
C11 C12 C13 C14 -0.9(7) . . . . ?
C12 C11 C16 C15 -2.1(7) . . . . ?
C12 C11 C16 C17 178.3(4) . . . . ?
C12 C13 C14 C15 -0.4(9) . . . . ?
C13 C14 C15 C16 0.5(9) . . . . ?
C14 C15 C16 C11 0.7(8) . . . . ?
C14 C15 C16 C17 -179.7(5) . . . . ?
C16 C11 C12 C13 2.3(6) . . . . ?
C16 C11 C12 C18 -176.8(4) . . . . ?
C18 C12 C13 C14 178.1(5) . . . . ?
C21 C22 C23 C24 -0.3(7) . . . . ?
C22 C21 C26 C25 -0.5(6) . . . . ?
C22 C21 C26 C27 179.8(4) . . . . ?
C22 C23 C24 C25 0.9(8) . . . . ?
C23 C24 C25 C26 -1.3(7) . . . . ?
C24 C25 C26 C21 1.1(7) . . . . ?
C24 C25 C26 C27 -179.2(4) . . . . ?
C26 C21 C22 C23 0.1(7) . . . . ?
C26 C21 C22 C28 -179.8(4) . . . . ?
C28 C22 C23 C24 179.6(5) . . . . ?

_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
-9 9 0 0.1423 -9.0000 9.0000 -0.0000 0.9552 -0.1239 0.1811
0 -12 -9 0.1078 0.0000 -12.0000 -9.0000 -0.5352 0.0234 0.8849
0 12 9 0.1258 0.0000 12.0000 9.0000 0.5352 -0.0234 -0.8849
9 -6 6 0.1028 9.0000 -6.0000 6.0000 -0.8245 0.0029 -0.4901
1 1 -26 0.0261 1.0000 1.0000 -26.0000 0.0063 0.8544 0.4762
-1 -1 26 0.0371 -1.0000 -1.0000 26.0000 -0.0063 -0.8544 -0.4762
-1 1 26 0.0389 -1.0000 1.0000 26.0000 0.0842 -0.8122 -0.5885
0 -1 -25 0.0315 0.0000 -1.0000 -25.0000 -0.0241 0.7467 0.6414

_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_mv62a
_database_code_depnum_ccdc_archive 'CCDC 2298997'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2022-06-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C19 H21 N2 Ni O2 P S2'
_chemical_formula_sum            'C19 H21 N2 Ni O2 P S2'
_chemical_formula_weight         463.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C19  H21  N2  O2  P1  S2  Ni1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   9.6257(4)
_cell_length_b                   22.5461(9)
_cell_length_c                   9.8951(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.047(3)
_cell_angle_gamma                90
_cell_volume                     2139.14(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4888
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.4992
_cell_measurement_theta_min      2.0620
_shelx_estimated_absorpt_T_max   0.833
_shelx_estimated_absorpt_T_min   0.718
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.2973
_exptl_crystal_size_mid          0.1851
_exptl_crystal_size_min          0.1595
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11284
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.565
_diffrn_reflns_theta_min         2.255
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -19.00   25.00   1.0000   10.3200
omega____ theta____ kappa____ phi______ frames
    -      -10.0277  -99.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
  2 omega  -43.00   62.00   1.0000   10.3200
omega____ theta____ kappa____ phi______ frames
    -      -10.0277   77.0000  -60.0000 105

#__ type_ start__ end____ width___ exp.time_
  3 omega   40.00   84.00   1.0000   10.3200
omega____ theta____ kappa____ phi______ frames
    -       11.8245   57.0000   90.0000 44
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0319891000
_diffrn_orient_matrix_UB_12      -0.0267205000
_diffrn_orient_matrix_UB_13      -0.0247027000
_diffrn_orient_matrix_UB_21      0.0046837000
_diffrn_orient_matrix_UB_22      0.0097219000
_diffrn_orient_matrix_UB_23      -0.0675761000
_diffrn_orient_matrix_UB_31      0.0664583000
_diffrn_orient_matrix_UB_32      -0.0135567000
_diffrn_orient_matrix_UB_33      0.0000806000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3903
_reflns_number_total             5057
_reflns_odcompleteness_completeness 99.91
_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, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.0303(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+0.4380P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0946
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   geom
_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 0.13970(3) 0.54071(2) 0.93094(3) 0.04184(12) Uani 1 1 d . . . . .
S1 S 0.04418(7) 0.62684(3) 0.87458(6) 0.06011(18) Uani 1 1 d . . . . .
S2 S 0.00882(8) 0.50169(3) 0.76055(6) 0.0638(2) Uani 1 1 d . . . . .
P1 P -0.06411(6) 0.58471(3) 0.71614(6) 0.05818(19) Uani 1 1 d . . . . .
O1 O -0.21503(19) 0.59329(13) 0.7016(2) 0.1034(8) Uani 1 1 d . . . . .
O2 O -0.00779(19) 0.60542(9) 0.57802(17) 0.0705(5) Uani 1 1 d . . . . .
N1 N 0.2964(2) 0.60109(9) 1.16609(18) 0.0498(5) Uani 1 1 d . . . . .
N2 N 0.2801(2) 0.42277(9) 0.95858(19) 0.0507(5) Uani 1 1 d . . . . .
C1 C 0.2379(2) 0.57729(10) 1.0759(2) 0.0453(5) Uani 1 1 d . . . . .
C2 C 0.2251(2) 0.46807(11) 0.9549(2) 0.0471(5) Uani 1 1 d . . . . .
C11 C 0.3657(2) 0.62922(11) 1.2787(2) 0.0478(5) Uani 1 1 d . . . . .
C12 C 0.3296(3) 0.68696(13) 1.3071(3) 0.0625(7) Uani 1 1 d . . . . .
C13 C 0.4003(4) 0.71268(16) 1.4202(3) 0.0915(11) Uani 1 1 d . . . . .
H13 H 0.3796 0.7514 1.4437 0.110 Uiso 1 1 calc R U . . .
C14 C 0.4989(5) 0.6821(2) 1.4970(3) 0.1127(16) Uani 1 1 d . . . . .
H14 H 0.5449 0.7004 1.5724 0.135 Uiso 1 1 calc R U . . .
C15 C 0.5332(4) 0.6247(2) 1.4667(3) 0.0936(11) Uani 1 1 d . . . . .
H15 H 0.6014 0.6048 1.5216 0.112 Uiso 1 1 calc R U . . .
C16 C 0.4665(3) 0.59653(14) 1.3552(2) 0.0630(7) Uani 1 1 d . . . . .
C17 C 0.2201(3) 0.72008(15) 1.2210(4) 0.0908(10) Uani 1 1 d . . . . .
H17A H 0.2348 0.7148 1.1270 0.136 Uiso 1 1 calc R U . . .
H17B H 0.2256 0.7615 1.2432 0.136 Uiso 1 1 calc R U . . .
H17C H 0.1297 0.7052 1.2374 0.136 Uiso 1 1 calc R U . . .
C18 C 0.5004(4) 0.53447(15) 1.3184(3) 0.0913(10) Uani 1 1 d . . . . .
H18A H 0.4191 0.5101 1.3219 0.137 Uiso 1 1 calc R U . . .
H18B H 0.5739 0.5196 1.3812 0.137 Uiso 1 1 calc R U . . .
H18C H 0.5300 0.5337 1.2283 0.137 Uiso 1 1 calc R U . . .
C20 C 0.1334(3) 0.59774(16) 0.5493(3) 0.0869(10) Uani 1 1 d . . . . .
H20A H 0.1441 0.6107 0.4584 0.130 Uiso 1 1 calc R U . . .
H20B H 0.1582 0.5566 0.5583 0.130 Uiso 1 1 calc R U . . .
H20C H 0.1931 0.6208 0.6120 0.130 Uiso 1 1 calc R U . . .
C21 C 0.3419(3) 0.36652(10) 0.9519(3) 0.0539(6) Uani 1 1 d . . . . .
C22 C 0.2895(3) 0.32870(12) 0.8498(3) 0.0727(8) Uani 1 1 d . . . . .
C23 C 0.3548(4) 0.27406(14) 0.8439(4) 0.0953(12) Uani 1 1 d . . . . .
H23 H 0.3235 0.2472 0.7766 0.114 Uiso 1 1 calc R U . . .
C24 C 0.4639(5) 0.25889(15) 0.9345(5) 0.1058(14) Uani 1 1 d . . . . .
H24 H 0.5053 0.2218 0.9289 0.127 Uiso 1 1 calc R U . . .
C25 C 0.5131(4) 0.29778(15) 1.0339(4) 0.0879(11) Uani 1 1 d . . . . .
H25 H 0.5880 0.2867 1.0944 0.105 Uiso 1 1 calc R U . . .
C26 C 0.4534(3) 0.35325(12) 1.0462(3) 0.0610(7) Uani 1 1 d . . . . .
C27 C 0.1702(4) 0.34648(18) 0.7498(4) 0.1062(12) Uani 1 1 d . . . . .
H27A H 0.0930 0.3592 0.7979 0.159 Uiso 1 1 calc R U . . .
H27B H 0.1422 0.3132 0.6933 0.159 Uiso 1 1 calc R U . . .
H27C H 0.1989 0.3784 0.6944 0.159 Uiso 1 1 calc R U . . .
C28 C 0.5054(3) 0.39694(16) 1.1518(3) 0.0796(9) Uani 1 1 d . . . . .
H28A H 0.5374 0.4319 1.1088 0.119 Uiso 1 1 calc R U . . .
H28B H 0.5811 0.3798 1.2084 0.119 Uiso 1 1 calc R U . . .
H28C H 0.4313 0.4072 1.2063 0.119 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 S1 2.1993(7) . ?
Ni1 S2 2.1977(7) . ?
Ni1 C1 1.842(2) . ?
Ni1 C2 1.838(2) . ?
S1 P1 2.0394(9) . ?
S2 P1 2.0336(10) . ?
P1 O1 1.460(2) . ?
P1 O2 1.5843(17) . ?
O2 C20 1.423(3) . ?
N1 C1 1.146(3) . ?
N1 C11 1.400(3) . ?
N2 C2 1.150(3) . ?
N2 C21 1.405(3) . ?
C11 C12 1.383(4) . ?
C11 C16 1.389(4) . ?
C12 C13 1.385(4) . ?
C12 C17 1.495(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.351(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.375(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.381(4) . ?
C16 C18 1.489(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.383(4) . ?
C21 C26 1.391(4) . ?
C22 C23 1.386(4) . ?
C22 C27 1.503(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.363(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.371(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.386(4) . ?
C26 C28 1.490(4) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 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
S2 Ni1 S1 87.72(3) . . ?
C1 Ni1 S1 88.66(7) . . ?
C1 Ni1 S2 175.53(7) . . ?
C2 Ni1 S1 172.51(7) . . ?
C2 Ni1 S2 87.82(7) . . ?
C2 Ni1 C1 96.05(10) . . ?
P1 S1 Ni1 87.58(3) . . ?
P1 S2 Ni1 87.77(3) . . ?
S2 P1 S1 96.84(4) . . ?
O1 P1 S1 116.80(11) . . ?
O1 P1 S2 117.70(12) . . ?
O1 P1 O2 106.79(11) . . ?
O2 P1 S1 109.60(8) . . ?
O2 P1 S2 108.66(8) . . ?
C20 O2 P1 122.78(18) . . ?
C1 N1 C11 178.4(2) . . ?
C2 N2 C21 175.1(2) . . ?
N1 C1 Ni1 178.2(2) . . ?
N2 C2 Ni1 174.3(2) . . ?
C12 C11 N1 118.5(2) . . ?
C12 C11 C16 124.4(2) . . ?
C16 C11 N1 117.1(2) . . ?
C11 C12 C13 116.3(3) . . ?
C11 C12 C17 122.1(3) . . ?
C13 C12 C17 121.5(3) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 C12 120.8(3) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 H14 119.1 . . ?
C13 C14 C15 121.9(3) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.2(3) . . ?
C16 C15 H15 119.9 . . ?
C11 C16 C18 121.5(3) . . ?
C15 C16 C11 116.4(3) . . ?
C15 C16 C18 122.1(3) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N2 117.5(3) . . ?
C22 C21 C26 124.6(2) . . ?
C26 C21 N2 117.8(2) . . ?
C21 C22 C23 116.2(3) . . ?
C21 C22 C27 121.7(3) . . ?
C23 C22 C27 122.2(3) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.4(4) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 119.7 . . ?
C23 C24 C25 120.6(3) . . ?
C25 C24 H24 119.7 . . ?
C24 C25 H25 119.3 . . ?
C24 C25 C26 121.3(3) . . ?
C26 C25 H25 119.3 . . ?
C21 C26 C28 121.3(2) . . ?
C25 C26 C21 115.9(3) . . ?
C25 C26 C28 122.8(3) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 P1 O2 C20 59.3(2) . . . . ?
S2 P1 O2 C20 -45.4(2) . . . . ?
O1 P1 O2 C20 -173.3(2) . . . . ?
N1 C11 C12 C13 179.5(2) . . . . ?
N1 C11 C12 C17 -0.4(3) . . . . ?
N1 C11 C16 C15 -179.4(2) . . . . ?
N1 C11 C16 C18 0.5(3) . . . . ?
N2 C21 C22 C23 178.5(2) . . . . ?
N2 C21 C22 C27 -0.5(4) . . . . ?
N2 C21 C26 C25 -178.7(2) . . . . ?
N2 C21 C26 C28 0.4(3) . . . . ?
C11 C12 C13 C14 0.1(4) . . . . ?
C12 C11 C16 C15 0.2(4) . . . . ?
C12 C11 C16 C18 -179.8(2) . . . . ?
C12 C13 C14 C15 -0.1(6) . . . . ?
C13 C14 C15 C16 0.1(6) . . . . ?
C14 C15 C16 C11 -0.1(4) . . . . ?
C14 C15 C16 C18 179.9(3) . . . . ?
C16 C11 C12 C13 -0.2(4) . . . . ?
C16 C11 C12 C17 179.9(2) . . . . ?
C17 C12 C13 C14 180.0(3) . . . . ?
C21 C22 C23 C24 0.3(4) . . . . ?
C22 C21 C26 C25 -0.2(4) . . . . ?
C22 C21 C26 C28 178.9(2) . . . . ?
C22 C23 C24 C25 -0.6(5) . . . . ?
C23 C24 C25 C26 0.5(5) . . . . ?
C24 C25 C26 C21 -0.1(4) . . . . ?
C24 C25 C26 C28 -179.2(3) . . . . ?
C26 C21 C22 C23 0.1(4) . . . . ?
C26 C21 C22 C27 -178.9(3) . . . . ?
C27 C22 C23 C24 179.3(3) . . . . ?

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 32 0 0.1659 1.0000 32.0000 -0.0000 -0.8873 0.3143 -0.3696
-1 -32 0 0.1659 -1.0000 -32.0000 0.0000 0.8873 -0.3143 0.3696
12 13 -1 0.4636 12.0000 13.0000 -1.0000 -0.7065 0.2534 0.6206
12 -14 -1 0.4643 12.0000 -14.0000 -1.0000 0.0152 -0.0075 0.9886
0 14 12 0.1578 0.0000 14.0000 12.0000 -0.6702 -0.6762 -0.1876
0 7 -14 0.1320 -0.0000 7.0000 -14.0000 0.1581 1.0144 -0.0992
-11 -12 8 0.4891 -11.0000 -12.0000 8.0000 0.4752 -0.7122 -0.5659
11 -5 -9 0.4124 11.0000 -5.0000 -9.0000 0.0039 0.6155 0.7973
0 -25 9 0.1528 -0.0000 -25.0000 9.0000 0.4463 -0.8503 0.3432
0 -32 -1 0.1535 -0.0000 -32.0000 -1.0000 0.8800 -0.2417 0.4359
0 -14 -13 0.1403 -0.0000 -14.0000 -13.0000 0.6948 0.7438 0.1873
0 0 14 0.1622 0.0000 -0.0000 14.0000 -0.3453 -0.9468 0.0037
-11 12 7 0.4789 -11.0000 12.0000 7.0000 -0.1417 -0.4126 -0.8933

_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_mv63f
_database_code_depnum_ccdc_archive 'CCDC 2298999'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2022-06-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H37 N2 Ni O2 P S2'
_chemical_formula_sum            'C27 H37 N2 Ni O2 P S2'
_chemical_formula_weight         575.38
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C27 H29 N2 O2 P1 S2 Ni1'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   13.8109(4)
_cell_length_b                   10.3758(3)
_cell_length_c                   21.4053(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.863(2)
_cell_angle_gamma                90
_cell_volume                     3065.74(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5951
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.7269
_cell_measurement_theta_min      2.1771
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
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)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.5581
_exptl_crystal_size_mid          0.2318
_exptl_crystal_size_min          0.1449
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14802
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.793
_diffrn_reflns_theta_min         2.181
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 10.4757
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -61.00   28.00   1.0000   53.4950
omega____ theta____ kappa____ phi______ frames
    -       11.7464  -57.0000   30.0000 89

#__ type_ start__ end____ width___ exp.time_
  2 omega  -43.00   44.00   1.0000   53.4950
omega____ theta____ kappa____ phi______ frames
    -       11.7464  -77.0000  150.0000 87
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0371248000
_diffrn_orient_matrix_UB_12      0.0459315000
_diffrn_orient_matrix_UB_13      0.0046251000
_diffrn_orient_matrix_UB_21      -0.0011287000
_diffrn_orient_matrix_UB_22      -0.0176562000
_diffrn_orient_matrix_UB_23      0.0319787000
_diffrn_orient_matrix_UB_31      0.0354962000
_diffrn_orient_matrix_UB_32      0.0474614000
_diffrn_orient_matrix_UB_33      0.0074437000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4955
_reflns_number_total             7266
_reflns_odcompleteness_completeness 99.88
_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, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)²+1.1091P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1101
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C27(H27), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_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 0.49653(2) 0.16313(3) 0.51347(2) 0.04355(11) Uani 1 1 d . . . . .
S1 S 0.58411(5) 0.19052(8) 0.60029(3) 0.0606(2) Uani 1 1 d . . . . .
S2 S 0.37787(5) 0.10017(8) 0.57194(3) 0.0585(2) Uani 1 1 d . . . . .
P1 P 0.46378(5) 0.14465(7) 0.64815(3) 0.05377(19) Uani 1 1 d . . . . .
O1 O 0.47379(16) 0.0496(2) 0.69833(9) 0.0809(6) Uani 1 1 d . . . . .
O2 O 0.42257(15) 0.2717(2) 0.67909(8) 0.0707(6) Uani 1 1 d . . . . .
N1 N 0.35196(16) 0.1630(2) 0.40699(9) 0.0506(5) Uani 1 1 d . . . . .
N2 N 0.66491(15) 0.2616(2) 0.44464(9) 0.0495(5) Uani 1 1 d . . . . .
C1 C 0.41143(18) 0.1558(2) 0.44535(11) 0.0457(6) Uani 1 1 d . . . . .
C2 C 0.59978(18) 0.2206(3) 0.46955(10) 0.0474(6) Uani 1 1 d . . . . .
C11 C 0.2693(2) 0.1792(3) 0.36841(12) 0.0579(7) Uani 1 1 d . . . . .
C12 C 0.1811(2) 0.1447(4) 0.39278(15) 0.0782(9) Uani 1 1 d . . . . .
C13 C 0.0993(3) 0.1716(5) 0.35654(19) 0.1058(14) Uani 1 1 d . . . . .
H13 H 0.0388 0.1491 0.3710 0.127 Uiso 1 1 calc R . . . .
C14 C 0.1053(3) 0.2302(5) 0.3002(2) 0.1139(15) Uani 1 1 d . . . . .
H14 H 0.0489 0.2501 0.2773 0.137 Uiso 1 1 calc R . . . .
C15 C 0.1929(3) 0.2601(4) 0.27699(17) 0.1037(13) Uani 1 1 d . . . . .
H15 H 0.1952 0.2985 0.2378 0.124 Uiso 1 1 calc R . . . .
C16 C 0.2794(2) 0.2349(3) 0.31000(13) 0.0753(9) Uani 1 1 d . . . . .
C17 C 0.1741(3) 0.0778(6) 0.45520(18) 0.1148(17) Uani 1 1 d . . . . .
H17 H 0.2375 0.0855 0.4768 0.138 Uiso 1 1 calc R . . . .
C18 C 0.3769(3) 0.2654(4) 0.28436(15) 0.0972(12) Uani 1 1 d . . . . .
H18 H 0.4269 0.2350 0.3144 0.117 Uiso 1 1 calc R . . . .
C20 C 0.3985(3) 0.3839(4) 0.64351(17) 0.0996(12) Uani 1 1 d . . . . .
H20A H 0.4508 0.4044 0.6168 0.149 Uiso 1 1 calc GR . . . .
H20B H 0.3878 0.4547 0.6713 0.149 Uiso 1 1 calc GR . . . .
H20C H 0.3408 0.3680 0.6185 0.149 Uiso 1 1 calc GR . . . .
C21 C 0.74526(17) 0.3219(2) 0.41868(11) 0.0475(6) Uani 1 1 d . . . . .
C22 C 0.7959(2) 0.4098(3) 0.45654(12) 0.0567(7) Uani 1 1 d . . . . .
C23 C 0.8724(2) 0.4720(3) 0.42936(15) 0.0728(9) Uani 1 1 d . . . . .
H23 H 0.9086 0.5318 0.4526 0.087 Uiso 1 1 calc R . . . .
C24 C 0.8960(2) 0.4471(3) 0.36824(15) 0.0746(9) Uani 1 1 d . . . . .
H24 H 0.9465 0.4920 0.3505 0.089 Uiso 1 1 calc R . . . .
C25 C 0.8458(2) 0.3570(3) 0.33356(14) 0.0644(8) Uani 1 1 d . . . . .
H25 H 0.8639 0.3399 0.2929 0.077 Uiso 1 1 calc R . . . .
C26 C 0.76874(18) 0.2909(3) 0.35786(12) 0.0519(6) Uani 1 1 d . . . . .
C27 C 0.7669(2) 0.4340(3) 0.52346(13) 0.0677(8) Uani 1 1 d . . . . .
H27 H 0.7415 0.3527 0.5395 0.081 Uiso 1 1 calc R . . . .
C28 C 0.7163(2) 0.1860(3) 0.32117(13) 0.0655(8) Uani 1 1 d . . . . .
H28 H 0.6608 0.1583 0.3452 0.079 Uiso 1 1 calc R . . . .
C31 C 0.1014(5) 0.1382(5) 0.4962(2) 0.166(3) Uani 1 1 d . . . . .
H31A H 0.1231 0.2227 0.5084 0.249 Uiso 1 1 calc GR . . . .
H31B H 0.0941 0.0860 0.5328 0.249 Uiso 1 1 calc GR . . . .
H31C H 0.0402 0.1447 0.4738 0.249 Uiso 1 1 calc GR . . . .
C32 C 0.1533(4) -0.0637(6) 0.4473(3) 0.163(3) Uani 1 1 d . . . . .
H32A H 0.0915 -0.0748 0.4262 0.245 Uiso 1 1 calc GR . . . .
H32B H 0.1524 -0.1040 0.4877 0.245 Uiso 1 1 calc GR . . . .
H32C H 0.2028 -0.1025 0.4231 0.245 Uiso 1 1 calc GR . . . .
C33 C 0.3879(5) 0.4104(6) 0.2774(3) 0.208(3) Uani 1 1 d . . . . .
H33A H 0.3312 0.4449 0.2563 0.312 Uiso 1 1 calc GR . . . .
H33B H 0.4438 0.4287 0.2534 0.312 Uiso 1 1 calc GR . . . .
H33C H 0.3956 0.4491 0.3180 0.312 Uiso 1 1 calc GR . . . .
C34 C 0.3923(4) 0.1996(6) 0.2227(2) 0.1425(19) Uani 1 1 d . . . . .
H34A H 0.3875 0.1079 0.2280 0.214 Uiso 1 1 calc GR . . . .
H34B H 0.4554 0.2208 0.2083 0.214 Uiso 1 1 calc GR . . . .
H34C H 0.3439 0.2280 0.1926 0.214 Uiso 1 1 calc GR . . . .
C41 C 0.8514(3) 0.4741(4) 0.56685(16) 0.1092(14) Uani 1 1 d . . . . .
H41A H 0.9015 0.4103 0.5656 0.164 Uiso 1 1 calc GR . . . .
H41B H 0.8294 0.4819 0.6088 0.164 Uiso 1 1 calc GR . . . .
H41C H 0.8763 0.5556 0.5534 0.164 Uiso 1 1 calc GR . . . .
C42 C 0.6857(3) 0.5316(4) 0.52448(16) 0.0987(12) Uani 1 1 d . . . . .
H42A H 0.7078 0.6122 0.5082 0.148 Uiso 1 1 calc GR . . . .
H42B H 0.6660 0.5436 0.5667 0.148 Uiso 1 1 calc GR . . . .
H42C H 0.6317 0.5011 0.4993 0.148 Uiso 1 1 calc GR . . . .
C43 C 0.7818(3) 0.0711(3) 0.31346(18) 0.1021(13) Uani 1 1 d . . . . .
H43A H 0.8382 0.0968 0.2916 0.153 Uiso 1 1 calc GR . . . .
H43B H 0.7478 0.0055 0.2900 0.153 Uiso 1 1 calc GR . . . .
H43C H 0.8010 0.0380 0.3539 0.153 Uiso 1 1 calc GR . . . .
C44 C 0.6784(3) 0.2328(4) 0.25804(17) 0.1056(13) Uani 1 1 d . . . . .
H44A H 0.6343 0.3030 0.2637 0.158 Uiso 1 1 calc GR . . . .
H44B H 0.6453 0.1637 0.2366 0.158 Uiso 1 1 calc GR . . . .
H44C H 0.7316 0.2614 0.2338 0.158 Uiso 1 1 calc GR . . . .


_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 2.2026(7) . ?
Ni1 S2 2.1936(7) . ?
Ni1 C1 1.844(3) . ?
Ni1 C2 1.833(2) . ?
S1 P1 2.0369(9) . ?
S2 P1 2.0387(10) . ?
P1 O1 1.461(2) . ?
P1 O2 1.589(2) . ?
O2 C20 1.424(4) . ?
N1 C1 1.145(3) . ?
N1 C11 1.398(3) . ?
N2 C2 1.143(3) . ?
N2 C21 1.404(3) . ?
C11 C12 1.387(4) . ?
C11 C16 1.389(4) . ?
C12 C13 1.378(5) . ?
C12 C17 1.511(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.355(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.359(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.393(5) . ?
C16 C18 1.505(5) . ?
C17 H17 0.9800 . ?
C17 C31 1.493(6) . ?
C17 C32 1.504(7) . ?
C18 H18 0.9800 . ?
C18 C33 1.519(7) . ?
C18 C34 1.507(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.394(4) . ?
C21 C26 1.389(3) . ?
C22 C23 1.382(4) . ?
C22 C27 1.521(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.383(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.368(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.382(3) . ?
C26 C28 1.513(4) . ?
C27 H27 0.9800 . ?
C27 C41 1.526(5) . ?
C27 C42 1.512(5) . ?
C28 H28 0.9800 . ?
C28 C43 1.508(5) . ?
C28 C44 1.513(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 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
S2 Ni1 S1 87.54(3) . . ?
C1 Ni1 S1 172.18(8) . . ?
C1 Ni1 S2 88.29(7) . . ?
C2 Ni1 S1 88.61(8) . . ?
C2 Ni1 S2 175.99(8) . . ?
C2 Ni1 C1 95.40(10) . . ?
P1 S1 Ni1 87.68(3) . . ?
P1 S2 Ni1 87.88(3) . . ?
S1 P1 S2 96.52(4) . . ?
O1 P1 S1 117.91(10) . . ?
O1 P1 S2 118.29(10) . . ?
O1 P1 O2 106.27(12) . . ?
O2 P1 S1 108.97(9) . . ?
O2 P1 S2 108.32(9) . . ?
C20 O2 P1 122.37(19) . . ?
C1 N1 C11 170.1(2) . . ?
C2 N2 C21 174.2(2) . . ?
N1 C1 Ni1 171.2(2) . . ?
N2 C2 Ni1 176.2(2) . . ?
C12 C11 N1 117.2(3) . . ?
C12 C11 C16 124.2(3) . . ?
C16 C11 N1 118.5(3) . . ?
C11 C12 C17 122.2(3) . . ?
C13 C12 C11 116.7(3) . . ?
C13 C12 C17 121.0(3) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.3(4) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.6(4) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 119.0 . . ?
C14 C15 C16 122.1(4) . . ?
C16 C15 H15 119.0 . . ?
C11 C16 C15 115.1(3) . . ?
C11 C16 C18 122.2(3) . . ?
C15 C16 C18 122.6(3) . . ?
C12 C17 H17 107.3 . . ?
C31 C17 C12 113.0(4) . . ?
C31 C17 H17 107.3 . . ?
C31 C17 C32 110.2(4) . . ?
C32 C17 C12 111.5(4) . . ?
C32 C17 H17 107.3 . . ?
C16 C18 H18 108.2 . . ?
C16 C18 C33 109.7(4) . . ?
C16 C18 C34 112.2(4) . . ?
C33 C18 H18 108.2 . . ?
C34 C18 H18 108.2 . . ?
C34 C18 C33 110.2(4) . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N2 116.7(2) . . ?
C26 C21 N2 118.6(2) . . ?
C26 C21 C22 124.6(2) . . ?
C21 C22 C27 120.8(2) . . ?
C23 C22 C21 115.9(2) . . ?
C23 C22 C27 123.2(3) . . ?
C22 C23 H23 119.4 . . ?
C22 C23 C24 121.2(3) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 H24 119.7 . . ?
C25 C24 C23 120.7(3) . . ?
C25 C24 H24 119.7 . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121.2(3) . . ?
C26 C25 H25 119.4 . . ?
C21 C26 C28 122.1(2) . . ?
C25 C26 C21 116.3(2) . . ?
C25 C26 C28 121.5(2) . . ?
C22 C27 H27 107.3 . . ?
C22 C27 C41 113.5(3) . . ?
C41 C27 H27 107.3 . . ?
C42 C27 C22 110.0(3) . . ?
C42 C27 H27 107.3 . . ?
C42 C27 C41 111.2(3) . . ?
C26 C28 H28 107.9 . . ?
C26 C28 C44 112.2(3) . . ?
C43 C28 C26 110.3(3) . . ?
C43 C28 H28 107.9 . . ?
C43 C28 C44 110.3(3) . . ?
C44 C28 H28 107.9 . . ?
C17 C31 H31A 109.5 . . ?
C17 C31 H31B 109.5 . . ?
C17 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C17 C32 H32A 109.5 . . ?
C17 C32 H32B 109.5 . . ?
C17 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C18 C33 H33A 109.5 . . ?
C18 C33 H33B 109.5 . . ?
C18 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C18 C34 H34A 109.5 . . ?
C18 C34 H34B 109.5 . . ?
C18 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C27 C41 H41A 109.5 . . ?
C27 C41 H41B 109.5 . . ?
C27 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C27 C42 H42A 109.5 . . ?
C27 C42 H42B 109.5 . . ?
C27 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C28 C43 H43A 109.5 . . ?
C28 C43 H43B 109.5 . . ?
C28 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C28 C44 H44A 109.5 . . ?
C28 C44 H44B 109.5 . . ?
C28 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 P1 O2 C20 55.3(3) . . . . ?
S2 P1 O2 C20 -48.6(3) . . . . ?
O1 P1 O2 C20 -176.6(3) . . . . ?
N1 C11 C12 C13 174.4(3) . . . . ?
N1 C11 C12 C17 -7.1(5) . . . . ?
N1 C11 C16 C15 -173.6(3) . . . . ?
N1 C11 C16 C18 6.5(5) . . . . ?
N2 C21 C22 C23 -177.5(3) . . . . ?
N2 C21 C22 C27 2.3(4) . . . . ?
N2 C21 C26 C25 177.3(2) . . . . ?
N2 C21 C26 C28 -5.7(4) . . . . ?
C11 C12 C13 C14 -0.7(6) . . . . ?
C11 C12 C17 C31 131.9(4) . . . . ?
C11 C12 C17 C32 -103.3(4) . . . . ?
C11 C16 C18 C33 -114.8(4) . . . . ?
C11 C16 C18 C34 122.4(4) . . . . ?
C12 C11 C16 C15 2.6(5) . . . . ?
C12 C11 C16 C18 -177.3(3) . . . . ?
C12 C13 C14 C15 2.3(8) . . . . ?
C13 C12 C17 C31 -49.7(6) . . . . ?
C13 C12 C17 C32 75.2(6) . . . . ?
C13 C14 C15 C16 -1.4(8) . . . . ?
C14 C15 C16 C11 -0.9(6) . . . . ?
C14 C15 C16 C18 178.9(4) . . . . ?
C15 C16 C18 C33 65.4(5) . . . . ?
C15 C16 C18 C34 -57.5(6) . . . . ?
C16 C11 C12 C13 -1.8(5) . . . . ?
C16 C11 C12 C17 176.7(4) . . . . ?
C17 C12 C13 C14 -179.2(5) . . . . ?
C21 C22 C23 C24 -0.1(5) . . . . ?
C21 C22 C27 C41 151.0(3) . . . . ?
C21 C22 C27 C42 -83.8(4) . . . . ?
C21 C26 C28 C43 -109.1(3) . . . . ?
C21 C26 C28 C44 127.5(3) . . . . ?
C22 C21 C26 C25 -2.6(4) . . . . ?
C22 C21 C26 C28 174.4(3) . . . . ?
C22 C23 C24 C25 -1.9(5) . . . . ?
C23 C22 C27 C41 -29.3(4) . . . . ?
C23 C22 C27 C42 96.0(4) . . . . ?
C23 C24 C25 C26 1.7(5) . . . . ?
C24 C25 C26 C21 0.5(4) . . . . ?
C24 C25 C26 C28 -176.6(3) . . . . ?
C25 C26 C28 C43 67.8(4) . . . . ?
C25 C26 C28 C44 -55.7(4) . . . . ?
C26 C21 C22 C23 2.4(4) . . . . ?
C26 C21 C22 C27 -177.8(3) . . . . ?
C27 C22 C23 C24 -179.9(3) . . . . ?

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
15 0 18 0.0725 15.0000 0.0000 18.0000 -0.4735 0.5591 0.6657
-15 0 -18 0.0725 -15.0000 -0.0000 -18.0000 0.4735 -0.5591 -0.6657
12 -1 -24 0.1084 12.0000 -1.0000 -24.0000 -0.6001 -0.7648 0.2033
-12 1 24 0.1234 -12.0000 1.0000 24.0000 0.6001 0.7648 -0.2033
10 11 13 0.1501 10.0000 11.0000 13.0000 0.1954 0.2115 0.9727
-3 2 30 0.1246 -3.0000 2.0000 30.0000 0.3402 0.9290 0.2083
-16 1 -17 0.0885 -16.0000 1.0000 -17.0000 0.5611 -0.5435 -0.6466
-12 -12 2 0.1949 -12.0000 -12.0000 2.0000 -0.0989 0.2887 -0.9811
0 2 -30 0.1349 0.0000 2.0000 -30.0000 -0.0449 -0.9958 -0.1254
3 12 -15 0.2151 3.0000 12.0000 -15.0000 0.3729 -0.6945 0.5656
-18 2 -10 0.0611 -18.0000 2.0000 -10.0000 0.7132 -0.3345 -0.6189

_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_dm491a
_database_code_depnum_ccdc_archive 'CCDC 2299006'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-03 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2023-10-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C22 H28 N2 Ni O2 P S2, Cl O4'
_chemical_formula_sum            'C22 H28 Cl N2 Ni O6 P S2'
_chemical_formula_weight         605.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22  H28  N2  O6  P1  S2 Cl1 Ni1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   7.7849(4)
_cell_length_b                   9.6864(4)
_cell_length_c                   19.6397(10)
_cell_angle_alpha                100.452(4)
_cell_angle_beta                 100.473(4)
_cell_angle_gamma                100.035(4)
_cell_volume                     1398.88(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4884
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.8950
_cell_measurement_theta_min      2.7020
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.071
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11919
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.774
_diffrn_reflns_theta_min         2.162
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -16.00   74.00   1.0000   11.9650
omega____ theta____ kappa____ phi______ frames
    -       11.9027   57.0000  -90.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega  -37.00   62.00   1.0000   11.9650
omega____ theta____ kappa____ phi______ frames
    -      -10.1058   57.0000  120.0000 99

#__ type_ start__ end____ width___ exp.time_
  3 omega  -18.00    8.00   1.0000   11.9650
omega____ theta____ kappa____ phi______ frames
    -      -10.1058  -99.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega  -77.00   11.00   1.0000   11.9650
omega____ theta____ kappa____ phi______ frames
    -      -10.1058  -57.0000  -30.0000 88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0676868000
_diffrn_orient_matrix_UB_12      0.0072122000
_diffrn_orient_matrix_UB_13      -0.0196885000
_diffrn_orient_matrix_UB_21      -0.0629191000
_diffrn_orient_matrix_UB_22      -0.0390094000
_diffrn_orient_matrix_UB_23      -0.0313424000
_diffrn_orient_matrix_UB_31      -0.0213987000
_diffrn_orient_matrix_UB_32      0.0650978000
_diffrn_orient_matrix_UB_33      -0.0068974000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4470
_reflns_number_total             6565
_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 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0718
_refine_ls_restrained_S_all      1.035
_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)+(0.1336P)²+0.9539P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2105
_refine_ls_wR_factor_ref         0.2432
_refine_special_details          ?
_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
 C32-C33 = C42-C43
 1.498 with sigma of 0.004
 O31-C32 = O41-C42
 1.442 with sigma of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C42(H42A,H42B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C33(H33A,H33B,H33C), C43(H43A,H43B,H43C)
;
_atom_sites_solution_hydrogens   geom
_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 0.38938(8) 0.23999(5) 0.68990(3) 0.0635(3) Uani 1 1 d . . . . .
S1 S 0.3786(2) 0.41363(14) 0.63042(7) 0.0912(5) Uani 1 1 d . . . . .
S2 S 0.2273(3) 0.08355(14) 0.59283(7) 0.0963(5) Uani 1 1 d . . . . .
P1 P 0.2328(2) 0.25691(16) 0.55111(7) 0.0859(4) Uani 1 1 d . . . . .
O31 O 0.0473(7) 0.2797(5) 0.5214(2) 0.1093(13) Uani 1 1 d D . . . .
O41 O 0.3259(8) 0.2556(5) 0.4866(2) 0.1257(16) Uani 1 1 d D . . . .
N1 N 0.3743(5) -0.0038(4) 0.76349(19) 0.0629(8) Uani 1 1 d . . . . .
N2 N 0.6197(5) 0.4615(4) 0.81310(19) 0.0634(8) Uani 1 1 d . . . . .
C1 C 0.3864(6) 0.0914(5) 0.7365(2) 0.0606(9) Uani 1 1 d . . . . .
C2 C 0.5313(6) 0.3752(4) 0.7674(2) 0.0601(9) Uani 1 1 d . . . . .
C11 C 0.3428(6) -0.1260(4) 0.7922(2) 0.0603(10) Uani 1 1 d . . . . .
C12 C 0.2313(6) -0.2486(5) 0.7491(2) 0.0653(10) Uani 1 1 d . . . . .
C13 C 0.2043(7) -0.3680(5) 0.7787(3) 0.0761(13) Uani 1 1 d . . . . .
H13 H 0.1291 -0.4531 0.7515 0.091 Uiso 1 1 calc R U . . .
C14 C 0.2858(7) -0.3627(5) 0.8464(3) 0.0780(13) Uani 1 1 d . . . . .
H14 H 0.2661 -0.4444 0.8649 0.094 Uiso 1 1 calc R U . . .
C15 C 0.3987(7) -0.2370(5) 0.8888(3) 0.0776(13) Uani 1 1 d . . . . .
H15 H 0.4529 -0.2355 0.9353 0.093 Uiso 1 1 calc R U . . .
C16 C 0.4301(7) -0.1154(5) 0.8623(2) 0.0684(11) Uani 1 1 d . . . . .
C17 C 0.1411(8) -0.2505(6) 0.6748(3) 0.0937(16) Uani 1 1 d . . . . .
H17A H 0.0799 -0.1726 0.6751 0.141 Uiso 1 1 calc R U . . .
H17B H 0.0565 -0.3400 0.6552 0.141 Uiso 1 1 calc R U . . .
H17C H 0.2290 -0.2402 0.6465 0.141 Uiso 1 1 calc R U . . .
C18 C 0.5518(10) 0.0206(6) 0.9049(3) 0.1009(19) Uani 1 1 d . . . . .
H18A H 0.6416 0.0506 0.8799 0.151 Uiso 1 1 calc R U . . .
H18B H 0.6082 0.0052 0.9498 0.151 Uiso 1 1 calc R U . . .
H18C H 0.4842 0.0937 0.9127 0.151 Uiso 1 1 calc R U . . .
C21 C 0.7304(6) 0.5706(4) 0.8677(3) 0.0663(11) Uani 1 1 d . . . . .
C22 C 0.7569(8) 0.5482(5) 0.9364(3) 0.0834(14) Uani 1 1 d . . . . .
C23 C 0.8662(10) 0.6592(7) 0.9884(4) 0.110(2) Uani 1 1 d . . . . .
H23 H 0.8901 0.6471 1.0349 0.132 Uiso 1 1 calc R U . . .
C24 C 0.9401(10) 0.7855(7) 0.9747(4) 0.118(2) Uani 1 1 d . . . . .
H24 H 1.0095 0.8596 1.0115 0.142 Uiso 1 1 calc R U . . .
C25 C 0.9118(8) 0.8039(6) 0.9049(5) 0.104(2) Uani 1 1 d . . . . .
H25 H 0.9675 0.8893 0.8956 0.125 Uiso 1 1 calc R U . . .
C26 C 0.8024(7) 0.6979(5) 0.8492(3) 0.0776(13) Uani 1 1 d . . . . .
C27 C 0.6735(11) 0.4081(6) 0.9518(3) 0.109(2) Uani 1 1 d . . . . .
H27A H 0.5463 0.3884 0.9343 0.164 Uiso 1 1 calc R U . . .
H27B H 0.6997 0.4146 1.0021 0.164 Uiso 1 1 calc R U . . .
H27C H 0.7213 0.3320 0.9288 0.164 Uiso 1 1 calc R U . . .
C28 C 0.7622(9) 0.7174(6) 0.7757(3) 0.0957(17) Uani 1 1 d . . . . .
H28A H 0.7896 0.6397 0.7446 0.143 Uiso 1 1 calc R U . . .
H28B H 0.8332 0.8068 0.7729 0.143 Uiso 1 1 calc R U . . .
H28C H 0.6377 0.7182 0.7619 0.143 Uiso 1 1 calc R U . . .
C33 C -0.1912(13) 0.3965(12) 0.5472(7) 0.209(6) Uani 1 1 d D . . . .
H33A H -0.2586 0.3655 0.4990 0.314 Uiso 1 1 calc R U . . .
H33B H -0.1124 0.4879 0.5529 0.314 Uiso 1 1 calc R U . . .
H33C H -0.2715 0.4054 0.5787 0.314 Uiso 1 1 calc R U . . .
C32 C -0.0838(11) 0.2889(10) 0.5641(5) 0.148(3) Uani 1 1 d D . . . .
H32A H -0.0240 0.3159 0.6139 0.177 Uiso 1 1 calc R U . . .
H32B H -0.1630 0.1954 0.5558 0.177 Uiso 1 1 calc R U . . .
C43 C 0.4030(12) 0.1506(12) 0.3804(5) 0.179(5) Uani 1 1 d D . . . .
H43A H 0.3416 0.1452 0.3326 0.269 Uiso 1 1 calc R U . . .
H43B H 0.4659 0.0738 0.3811 0.269 Uiso 1 1 calc R U . . .
H43C H 0.4867 0.2412 0.3979 0.269 Uiso 1 1 calc R U . . .
Cl1 Cl -0.0295(2) 0.19179(15) 0.78405(9) 0.0982(5) Uani 1 1 d . . . . .
O1 O -0.1437(13) 0.2043(14) 0.8245(5) 0.276(6) Uani 1 1 d . . . . .
O2 O -0.073(3) 0.247(2) 0.7309(6) 0.431(13) Uani 1 1 d . . . . .
O3 O 0.1317(14) 0.2701(9) 0.8014(11) 0.353(11) Uani 1 1 d . . . . .
O4 O -0.0229(12) 0.0583(7) 0.7552(8) 0.287(7) Uani 1 1 d . . . . .
C42 C 0.2716(11) 0.1379(9) 0.4260(4) 0.151(3) Uani 1 1 d D . . . .
H42A H 0.1541 0.1391 0.3994 0.181 Uiso 1 1 calc R U . . .
H42B H 0.2647 0.0477 0.4413 0.181 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 S1 2.2196(13) . ?
Ni1 S2 2.2212(14) . ?
Ni1 P1 2.8223(14) . ?
Ni1 C1 1.840(4) . ?
Ni1 C2 1.847(5) . ?
S1 P1 1.979(2) . ?
S2 P1 1.995(2) . ?
P1 O31 1.526(5) . ?
P1 O41 1.568(5) . ?
O31 C32 1.439(4) . ?
O41 C42 1.433(4) . ?
N1 C1 1.143(5) . ?
N1 C11 1.403(5) . ?
N2 C2 1.132(5) . ?
N2 C21 1.395(6) . ?
C11 C12 1.374(6) . ?
C11 C16 1.397(6) . ?
C12 C13 1.386(7) . ?
C12 C17 1.495(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.352(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.394(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.375(6) . ?
C16 C18 1.487(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.390(7) . ?
C21 C26 1.400(7) . ?
C22 C23 1.375(8) . ?
C22 C27 1.506(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.353(10) . ?
C24 H24 0.9300 . ?
C24 C25 1.397(10) . ?
C25 H25 0.9300 . ?
C25 C26 1.388(8) . ?
C26 C28 1.474(8) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C33 C32 1.491(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C43 C42 1.481(4) . ?
Cl1 O1 1.303(7) . ?
Cl1 O2 1.275(15) . ?
Cl1 O3 1.298(9) . ?
Cl1 O4 1.328(7) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?

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 S2 88.89(6) . . ?
S1 Ni1 P1 44.25(5) . . ?
S2 Ni1 P1 44.65(5) . . ?
C1 Ni1 S1 176.99(14) . . ?
C1 Ni1 S2 88.63(13) . . ?
C1 Ni1 P1 133.22(13) . . ?
C1 Ni1 C2 93.93(18) . . ?
C2 Ni1 S1 88.61(13) . . ?
C2 Ni1 S2 176.74(13) . . ?
C2 Ni1 P1 132.84(12) . . ?
P1 S1 Ni1 84.26(6) . . ?
P1 S2 Ni1 83.86(6) . . ?
S1 P1 Ni1 51.49(5) . . ?
S1 P1 S2 102.97(8) . . ?
S2 P1 Ni1 51.49(5) . . ?
O31 P1 Ni1 129.81(18) . . ?
O31 P1 S1 114.40(19) . . ?
O31 P1 S2 113.4(2) . . ?
O31 P1 O41 103.2(3) . . ?
O41 P1 Ni1 126.8(2) . . ?
O41 P1 S1 107.8(2) . . ?
O41 P1 S2 115.3(2) . . ?
C32 O31 P1 121.7(5) . . ?
C42 O41 P1 120.9(4) . . ?
C1 N1 C11 174.4(5) . . ?
C2 N2 C21 177.9(4) . . ?
N1 C1 Ni1 176.0(4) . . ?
N2 C2 Ni1 177.3(4) . . ?
C12 C11 N1 118.0(4) . . ?
C12 C11 C16 124.4(4) . . ?
C16 C11 N1 117.6(4) . . ?
C11 C12 C13 116.6(4) . . ?
C11 C12 C17 121.1(4) . . ?
C13 C12 C17 122.2(4) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.0(4) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.2(4) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 H15 119.9 . . ?
C16 C15 C14 120.2(5) . . ?
C16 C15 H15 119.9 . . ?
C11 C16 C18 121.2(4) . . ?
C15 C16 C11 116.5(4) . . ?
C15 C16 C18 122.3(5) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C21 C26 117.0(4) . . ?
C22 C21 N2 118.4(4) . . ?
C22 C21 C26 124.6(4) . . ?
C21 C22 C27 121.2(5) . . ?
C23 C22 C21 116.2(5) . . ?
C23 C22 C27 122.5(6) . . ?
C22 C23 H23 118.7 . . ?
C24 C23 C22 122.5(7) . . ?
C24 C23 H23 118.7 . . ?
C23 C24 H24 120.1 . . ?
C23 C24 C25 119.7(6) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 119.2 . . ?
C26 C25 C24 121.5(6) . . ?
C26 C25 H25 119.2 . . ?
C21 C26 C28 121.9(5) . . ?
C25 C26 C21 115.3(6) . . ?
C25 C26 C28 122.7(5) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
O31 C32 C33 111.2(8) . . ?
O31 C32 H32A 109.4 . . ?
O31 C32 H32B 109.4 . . ?
C33 C32 H32A 109.4 . . ?
C33 C32 H32B 109.4 . . ?
H32A C32 H32B 108.0 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
O1 Cl1 O4 115.9(8) . . ?
O2 Cl1 O1 109.1(12) . . ?
O2 Cl1 O3 92.9(11) . . ?
O2 Cl1 O4 104.1(11) . . ?
O3 Cl1 O1 122.3(9) . . ?
O3 Cl1 O4 108.6(6) . . ?
O41 C42 C43 109.2(6) . . ?
O41 C42 H42A 109.8 . . ?
O41 C42 H42B 109.8 . . ?
C43 C42 H42A 109.8 . . ?
C43 C42 H42B 109.8 . . ?
H42A C42 H42B 108.3 . . ?

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 P1 O31 C32 -3.4(7) . . . . ?
Ni1 P1 O41 C42 113.3(6) . . . . ?
S1 P1 O31 C32 -62.6(6) . . . . ?
S1 P1 O41 C42 168.1(6) . . . . ?
S2 P1 O31 C32 55.1(6) . . . . ?
S2 P1 O41 C42 53.7(7) . . . . ?
P1 O31 C32 C33 143.0(7) . . . . ?
P1 O41 C42 C43 -169.0(7) . . . . ?
O31 P1 O41 C42 -70.5(7) . . . . ?
O41 P1 O31 C32 -179.5(6) . . . . ?
N1 C11 C12 C13 179.3(4) . . . . ?
N1 C11 C12 C17 -2.1(7) . . . . ?
N1 C11 C16 C15 -179.2(4) . . . . ?
N1 C11 C16 C18 0.1(7) . . . . ?
N2 C21 C22 C23 -179.6(5) . . . . ?
N2 C21 C22 C27 1.9(8) . . . . ?
N2 C21 C26 C25 180.0(4) . . . . ?
N2 C21 C26 C28 0.7(7) . . . . ?
C11 C12 C13 C14 -0.5(7) . . . . ?
C12 C11 C16 C15 -0.7(7) . . . . ?
C12 C11 C16 C18 178.7(5) . . . . ?
C12 C13 C14 C15 0.4(8) . . . . ?
C13 C14 C15 C16 -0.3(8) . . . . ?
C14 C15 C16 C11 0.5(7) . . . . ?
C14 C15 C16 C18 -178.9(5) . . . . ?
C16 C11 C12 C13 0.7(7) . . . . ?
C16 C11 C12 C17 179.3(5) . . . . ?
C17 C12 C13 C14 -179.1(5) . . . . ?
C21 C22 C23 C24 2.0(10) . . . . ?
C22 C21 C26 C25 2.3(8) . . . . ?
C22 C21 C26 C28 -177.0(5) . . . . ?
C22 C23 C24 C25 -2.6(12) . . . . ?
C23 C24 C25 C26 3.0(11) . . . . ?
C24 C25 C26 C21 -2.7(9) . . . . ?
C24 C25 C26 C28 176.6(6) . . . . ?
C26 C21 C22 C23 -1.9(8) . . . . ?
C26 C21 C22 C27 179.6(6) . . . . ?
C27 C22 C23 C24 -179.5(7) . . . . ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
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
0 0 -26 0.1125 -0.0000 0.0000 -26.0000 0.5119 0.8149 0.1793
0 0 26 0.1045 0.0000 -0.0000 26.0000 -0.5119 -0.8149 -0.1793
-10 0 0 0.1798 -10.0000 0.0000 0.0000 -0.6769 0.6292 0.2140
0 13 -12 0.2504 0.0000 13.0000 -12.0000 0.3300 -0.1310 0.9290
8 -5 -19 0.1946 8.0000 -5.0000 -19.0000 0.8795 0.2872 -0.3656
-11 4 5 0.1993 -11.0000 4.0000 5.0000 -0.8141 0.3794 0.4613
-1 -13 9 0.2710 -1.0000 -13.0000 9.0000 -0.3386 0.2880 -0.8869
9 5 -9 0.3231 9.0000 5.0000 -9.0000 0.8224 -0.4792 0.1950
3 -10 21 0.2211 3.0000 -10.0000 21.0000 -0.2825 -0.4569 -0.8600

_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_m078a
_database_code_depnum_ccdc_archive 'CCDC 2299268'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2024-04-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2024-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H32 N2 Ni O2 P S2, Cl O4'
_chemical_formula_sum            'C24 H32 Cl N2 Ni O6 P S2'
_chemical_formula_weight         633.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C24 H32 Cl1 N2 O6 P1 S2 Ni1'
_chemical_oxdiff_usercomment     'orange prism'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   8.6853(3)
_cell_length_b                   11.9625(5)
_cell_length_c                   16.6919(6)
_cell_angle_alpha                93.616(3)
_cell_angle_beta                 98.940(3)
_cell_angle_gamma                103.585(3)
_cell_volume                     1656.28(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4696
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7460
_cell_measurement_theta_min      2.6180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             660
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 16 0 0.0537
-5 -5 21 0.0900
1 -16 10 0.0995
-11 -1 0 0.0883
11 1 0 0.0883
0 -16 0 0.0747
6 -2 -22 0.0910

_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.129
loop_
_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
-0.1397 16.3496 0.0359 -0.7972 -0.5474 0.2545
-5.0005 -5.0017 21.0046 0.4058 0.3646 0.8216
1.2746 -15.6590 10.0092 0.6060 0.7892 0.0997
-11.4166 -1.3864 -0.1489 0.8251 -0.5061 0.2511
11.4166 1.3864 0.1489 -0.8251 0.5061 -0.2511
0.1397 -16.3496 -0.0359 0.7972 0.5474 -0.2545
6.2029 -2.3441 -21.7328 -0.1172 -0.0788 -0.9900

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14723
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.512
_diffrn_reflns_theta_min         2.258
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  20.00   1.00    9.16    --  -10.48 -99.00-180.00   32
  2  ω    -29.00  63.00   1.00    9.16    --  -10.48  57.00-180.00   92
  3  ω    -85.00  13.00   1.00    9.16    --  -10.48 -37.00  30.00   98
  4  ω    -12.00  52.00   1.00    9.16    --   12.36 -99.00 -30.00   64
  5  ω    -19.00  18.00   1.00    9.16    --   12.36  77.00  90.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0661756000
_diffrn_orient_matrix_UB_12      -0.0493096000
_diffrn_orient_matrix_UB_13      -0.0081758000
_diffrn_orient_matrix_UB_21      0.0480821000
_diffrn_orient_matrix_UB_22      -0.0331146000
_diffrn_orient_matrix_UB_23      0.0209212000
_diffrn_orient_matrix_UB_31      -0.0243337000
_diffrn_orient_matrix_UB_32      0.0152789000
_diffrn_orient_matrix_UB_33      0.0369589000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4557
_reflns_number_total             7756
_reflns_odcompleteness_completeness 99.96
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         7756
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0654
_refine_ls_restrained_S_all      1.052
_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)+(0.0868P)²+1.0698P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1977
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C41 \\sim C43 \\sim C42: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C41 \\sim O41: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C43 \\sim C41 \\sim C42: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
3. Rigid body (RIGU) restrains
 C43, C41, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Ternary CH refined with riding coordinates:
 C31(H31), C41(H41)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C)
;
_atom_sites_solution_hydrogens   geom
_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 0.36656(7) 0.67365(4) 0.75433(3) 0.0540(2) Uani 1 1 d . . . . .
S1 S 0.41893(19) 0.52310(11) 0.69008(8) 0.0791(4) Uani 1 1 d . . . . .
S2 S 0.36038(16) 0.57823(9) 0.86393(7) 0.0653(3) Uani 1 1 d . . . . .
P1 P 0.42042(15) 0.45660(9) 0.79664(8) 0.0603(3) Uani 1 1 d . . . . .
O31 O 0.3125(4) 0.3324(2) 0.7927(2) 0.0786(10) Uani 1 1 d . . . . .
O41 O 0.5812(4) 0.4295(2) 0.8335(2) 0.0780(10) Uani 1 1 d . U . . .
N1 N 0.3301(4) 0.8780(3) 0.85371(19) 0.0525(8) Uani 1 1 d . . . . .
N2 N 0.3737(5) 0.7860(3) 0.6030(2) 0.0699(11) Uani 1 1 d . . . . .
C1 C 0.3377(5) 0.7996(3) 0.8139(2) 0.0535(10) Uani 1 1 d . . . . .
C2 C 0.3613(7) 0.7429(4) 0.6588(3) 0.0752(15) Uani 1 1 d . . . . .
C11 C 0.3249(5) 0.9705(3) 0.9085(2) 0.0481(9) Uani 1 1 d . . . . .
C12 C 0.2353(5) 0.9451(4) 0.9699(3) 0.0583(11) Uani 1 1 d . . . . .
C13 C 0.2351(6) 1.0382(4) 1.0241(3) 0.0699(13) Uani 1 1 d . . . . .
H13 H 0.1768 1.0257 1.0663 0.084 Uiso 1 1 calc R U . . .
C14 C 0.3189(7) 1.1474(4) 1.0164(3) 0.0742(14) Uani 1 1 d . . . . .
H14 H 0.3174 1.2081 1.0537 0.089 Uiso 1 1 calc R U . . .
C15 C 0.4053(6) 1.1692(4) 0.9547(3) 0.0698(13) Uani 1 1 d . . . . .
H15 H 0.4618 1.2444 0.9508 0.084 Uiso 1 1 calc R U . . .
C16 C 0.4098(5) 1.0807(3) 0.8981(3) 0.0569(10) Uani 1 1 d . . . . .
C17 C 0.1438(7) 0.8240(5) 0.9762(3) 0.0858(16) Uani 1 1 d . . . . .
H17A H 0.0614 0.7979 0.9289 0.129 Uiso 1 1 calc R U . . .
H17B H 0.0954 0.8224 1.0242 0.129 Uiso 1 1 calc R U . . .
H17C H 0.2161 0.7742 0.9796 0.129 Uiso 1 1 calc R U . . .
C18 C 0.5033(7) 1.1024(4) 0.8298(3) 0.0857(16) Uani 1 1 d . . . . .
H18A H 0.5848 1.0600 0.8347 0.129 Uiso 1 1 calc R U . . .
H18B H 0.5531 1.1835 0.8325 0.129 Uiso 1 1 calc R U . . .
H18C H 0.4319 1.0776 0.7786 0.129 Uiso 1 1 calc R U . . .
C21 C 0.3620(6) 0.8257(4) 0.5251(3) 0.0630(11) Uani 1 1 d . . . . .
C22 C 0.2804(6) 0.9113(4) 0.5104(3) 0.0687(12) Uani 1 1 d . . . . .
C23 C 0.2732(7) 0.9483(5) 0.4332(3) 0.0885(16) Uani 1 1 d . . . . .
H23 H 0.2205 1.0059 0.4206 0.106 Uiso 1 1 calc R U . . .
C24 C 0.3411(8) 0.9025(6) 0.3755(4) 0.100(2) Uani 1 1 d . . . . .
H24 H 0.3355 0.9293 0.3243 0.120 Uiso 1 1 calc R U . . .
C25 C 0.4179(8) 0.8168(6) 0.3923(3) 0.0977(19) Uani 1 1 d . . . . .
H25 H 0.4613 0.7848 0.3517 0.117 Uiso 1 1 calc R U . . .
C26 C 0.4325(7) 0.7767(5) 0.4684(3) 0.0762(14) Uani 1 1 d . . . . .
C27 C 0.2039(8) 0.9609(5) 0.5742(4) 0.0974(18) Uani 1 1 d . . . . .
H27A H 0.1116 0.9040 0.5831 0.146 Uiso 1 1 calc R U . . .
H27B H 0.1712 1.0277 0.5562 0.146 Uiso 1 1 calc R U . . .
H27C H 0.2801 0.9827 0.6242 0.146 Uiso 1 1 calc R U . . .
C28 C 0.5223(9) 0.6864(6) 0.4882(4) 0.118(2) Uani 1 1 d . . . . .
H28A H 0.5989 0.7126 0.5377 0.177 Uiso 1 1 calc R U . . .
H28B H 0.5777 0.6728 0.4445 0.177 Uiso 1 1 calc R U . . .
H28C H 0.4478 0.6159 0.4951 0.177 Uiso 1 1 calc R U . . .
C31 C 0.1394(6) 0.3007(5) 0.7587(4) 0.0817(15) Uani 1 1 d . . . . .
H31 H 0.1029 0.3710 0.7489 0.098 Uiso 1 1 calc R U . . .
C32 C 0.0548(8) 0.2401(6) 0.8213(5) 0.116(2) Uani 1 1 d . . . . .
H32A H 0.0849 0.1686 0.8283 0.174 Uiso 1 1 calc R U . . .
H32B H -0.0595 0.2245 0.8036 0.174 Uiso 1 1 calc R U . . .
H32C H 0.0847 0.2883 0.8722 0.174 Uiso 1 1 calc R U . . .
C33 C 0.1195(9) 0.2291(8) 0.6789(5) 0.167(4) Uani 1 1 d . . . . .
H33A H 0.1357 0.1542 0.6889 0.250 Uiso 1 1 calc R U . . .
H33B H 0.1971 0.2666 0.6477 0.250 Uiso 1 1 calc R U . . .
H33C H 0.0130 0.2207 0.6489 0.250 Uiso 1 1 calc R U . . .
C41 C 0.7323(7) 0.5201(5) 0.8536(5) 0.1037(17) Uani 1 1 d . U . . .
H41 H 0.7145 0.5932 0.8357 0.124 Uiso 1 1 calc R U . . .
C42 C 0.7853(10) 0.5335(7) 0.9450(5) 0.149(3) Uani 1 1 d . U . . .
H42A H 0.7085 0.5616 0.9708 0.223 Uiso 1 1 calc R U . . .
H42B H 0.8888 0.5874 0.9593 0.223 Uiso 1 1 calc R U . . .
H42C H 0.7924 0.4599 0.9629 0.223 Uiso 1 1 calc R U . . .
C43 C 0.8457(10) 0.4817(9) 0.8080(6) 0.173(3) Uani 1 1 d . U . . .
H43A H 0.8674 0.4124 0.8278 0.259 Uiso 1 1 calc R U . . .
H43B H 0.9442 0.5411 0.8154 0.259 Uiso 1 1 calc R U . . .
H43C H 0.7996 0.4667 0.7511 0.259 Uiso 1 1 calc R U . . .
Cl1 Cl 0.8476(2) 0.85090(13) 0.74848(9) 0.0859(4) Uani 1 1 d . . . . .
O11 O 0.8692(16) 0.7754(6) 0.7947(6) 0.312(7) Uani 1 1 d . . . . .
O12 O 0.7947(12) 0.8184(7) 0.6685(3) 0.218(4) Uani 1 1 d . . . . .
O13 O 0.7280(14) 0.8874(18) 0.7679(6) 0.427(12) Uani 1 1 d . . . . .
O14 O 0.9655(15) 0.9377(8) 0.7641(8) 0.343(7) 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 2.2120(11) . ?
Ni1 S2 2.2176(12) . ?
Ni1 C1 1.841(4) . ?
Ni1 C2 1.842(5) . ?
S1 P1 1.9932(18) . ?
S2 P1 1.9957(15) . ?
P1 O31 1.550(3) . ?
P1 O41 1.551(3) . ?
O31 C31 1.473(6) . ?
O41 C41 1.470(6) . ?
N1 C1 1.135(5) . ?
N1 C11 1.405(4) . ?
N2 C2 1.100(6) . ?
N2 C21 1.409(6) . ?
C11 C12 1.387(5) . ?
C11 C16 1.386(6) . ?
C12 C13 1.391(6) . ?
C12 C17 1.498(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.363(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.368(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.385(6) . ?
C16 C18 1.501(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.389(7) . ?
C21 C26 1.375(6) . ?
C22 C23 1.386(7) . ?
C22 C27 1.502(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.356(8) . ?
C24 H24 0.9300 . ?
C24 C25 1.368(9) . ?
C25 H25 0.9300 . ?
C25 C26 1.384(8) . ?
C26 C28 1.499(8) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C31 H31 0.9800 . ?
C31 C32 1.498(8) . ?
C31 C33 1.501(8) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C41 H41 0.9800 . ?
C41 C42 1.511(10) . ?
C41 C43 1.470(10) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
Cl1 O11 1.252(6) . ?
Cl1 O12 1.343(6) . ?
Cl1 O13 1.295(9) . ?
Cl1 O14 1.256(8) . ?

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 S2 88.12(5) . . ?
C1 Ni1 S1 175.37(14) . . ?
C1 Ni1 S2 89.43(12) . . ?
C1 Ni1 C2 93.63(17) . . ?
C2 Ni1 S1 89.04(13) . . ?
C2 Ni1 S2 175.64(17) . . ?
P1 S1 Ni1 85.40(5) . . ?
P1 S2 Ni1 85.19(5) . . ?
S1 P1 S2 101.11(6) . . ?
O31 P1 S1 114.98(16) . . ?
O31 P1 S2 115.64(15) . . ?
O31 P1 O41 96.94(17) . . ?
O41 P1 S1 115.13(16) . . ?
O41 P1 S2 113.90(15) . . ?
C31 O31 P1 123.2(3) . . ?
C41 O41 P1 121.7(3) . . ?
C1 N1 C11 175.4(4) . . ?
C2 N2 C21 169.1(6) . . ?
N1 C1 Ni1 175.3(4) . . ?
N2 C2 Ni1 173.2(5) . . ?
C12 C11 N1 117.4(4) . . ?
C16 C11 N1 118.2(3) . . ?
C16 C11 C12 124.4(3) . . ?
C11 C12 C13 116.1(4) . . ?
C11 C12 C17 121.4(4) . . ?
C13 C12 C17 122.6(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.1(4) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 H14 119.5 . . ?
C13 C14 C15 121.1(4) . . ?
C15 C14 H14 119.5 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.9(4) . . ?
C16 C15 H15 119.6 . . ?
C11 C16 C18 121.7(4) . . ?
C15 C16 C11 116.4(4) . . ?
C15 C16 C18 121.9(4) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C21 N2 118.2(4) . . ?
C26 C21 N2 117.6(5) . . ?
C26 C21 C22 124.2(4) . . ?
C21 C22 C27 122.1(4) . . ?
C23 C22 C21 116.2(5) . . ?
C23 C22 C27 121.7(5) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 C22 121.5(6) . . ?
C24 C23 H23 119.2 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.2(6) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 119.2 . . ?
C24 C25 C26 121.6(5) . . ?
C26 C25 H25 119.2 . . ?
C21 C26 C25 116.2(5) . . ?
C21 C26 C28 122.0(5) . . ?
C25 C26 C28 121.8(5) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O31 C31 H31 109.4 . . ?
O31 C31 C32 106.9(5) . . ?
O31 C31 C33 106.7(5) . . ?
C32 C31 H31 109.4 . . ?
C33 C31 H31 109.4 . . ?
C33 C31 C32 115.0(6) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O41 C41 H41 109.7 . . ?
O41 C41 C42 107.8(5) . . ?
C42 C41 H41 109.7 . . ?
C43 C41 O41 106.0(6) . . ?
C43 C41 H41 109.7 . . ?
C43 C41 C42 113.8(7) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O11 Cl1 O12 118.7(6) . . ?
O11 Cl1 O13 106.7(9) . . ?
O11 Cl1 O14 110.0(7) . . ?
O13 Cl1 O12 100.6(6) . . ?
O14 Cl1 O12 114.3(7) . . ?
O14 Cl1 O13 104.8(10) . . ?

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
S1 P1 O31 C31 -55.7(4) . . . . ?
S1 P1 O41 C41 59.9(5) . . . . ?
S2 P1 O31 C31 61.7(4) . . . . ?
S2 P1 O41 C41 -56.2(5) . . . . ?
P1 O31 C31 C32 -128.2(4) . . . . ?
P1 O31 C31 C33 108.2(6) . . . . ?
P1 O41 C41 C42 114.5(5) . . . . ?
P1 O41 C41 C43 -123.4(6) . . . . ?
O31 P1 O41 C41 -178.3(5) . . . . ?
O41 P1 O31 C31 -177.6(4) . . . . ?
N1 C11 C12 C13 178.7(4) . . . . ?
N1 C11 C12 C17 -1.6(6) . . . . ?
N1 C11 C16 C15 -178.2(4) . . . . ?
N1 C11 C16 C18 0.9(6) . . . . ?
N2 C21 C22 C23 179.5(4) . . . . ?
N2 C21 C22 C27 -0.7(7) . . . . ?
N2 C21 C26 C25 179.5(5) . . . . ?
N2 C21 C26 C28 -1.4(8) . . . . ?
C2 N2 C21 C22 90(2) . . . . ?
C2 N2 C21 C26 -90(3) . . . . ?
C11 C12 C13 C14 0.0(7) . . . . ?
C12 C11 C16 C15 1.4(6) . . . . ?
C12 C11 C16 C18 -179.4(5) . . . . ?
C12 C13 C14 C15 0.4(8) . . . . ?
C13 C14 C15 C16 0.1(8) . . . . ?
C14 C15 C16 C11 -1.0(7) . . . . ?
C14 C15 C16 C18 179.9(5) . . . . ?
C16 C11 C12 C13 -0.9(6) . . . . ?
C16 C11 C12 C17 178.7(5) . . . . ?
C17 C12 C13 C14 -179.7(5) . . . . ?
C21 C22 C23 C24 0.5(8) . . . . ?
C22 C21 C26 C25 -0.4(8) . . . . ?
C22 C21 C26 C28 178.6(5) . . . . ?
C22 C23 C24 C25 0.6(9) . . . . ?
C23 C24 C25 C26 -1.8(10) . . . . ?
C24 C25 C26 C21 1.6(9) . . . . ?
C24 C25 C26 C28 -177.5(6) . . . . ?
C26 C21 C22 C23 -0.6(7) . . . . ?
C26 C21 C22 C27 179.3(5) . . . . ?
C27 C22 C23 C24 -179.4(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.500 211.7 41.7 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.782
####################################################################### 
# 
# 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_mv57e
_database_code_depnum_ccdc_archive 'CCDC 2299270'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2023-09-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C23 H32 N3 Ni O2 P S2'
_chemical_formula_sum            'C23 H32 N3 Ni O2 P S2'
_chemical_formula_weight         536.31
_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   14.1712(3)
_cell_length_b                   14.4321(4)
_cell_length_c                   14.8981(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.956(2)
_cell_angle_gamma                90
_cell_volume                     2991.42(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7171
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.2750
_cell_measurement_theta_min      2.7850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.1842
_exptl_crystal_size_min          0.1639
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16554
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.755
_diffrn_reflns_theta_min         2.033
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   34.00   92.00   1.0000   49.3750
omega____ theta____ kappa____ phi______ frames
    -       11.7464 -179.0000   60.0000 58

#__ type_ start__ end____ width___ exp.time_
  2 omega  -14.00   30.00   1.0000   49.3750
omega____ theta____ kappa____ phi______ frames
    -       11.7464  -37.0000   30.0000 44

#__ type_ start__ end____ width___ exp.time_
  3 omega  -23.00   76.00   1.0000   49.3750
omega____ theta____ kappa____ phi______ frames
    -       11.7464   19.0000  -90.0000 99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_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                5301
_reflns_number_total             7189
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         7189
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0367
_refine_ls_restrained_S_all      1.022
_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)+(0.0414P)²+0.5303P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0954
_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 Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C),
 C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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 0.36065(2) 0.73809(2) 0.04718(2) 0.03898(9) Uani 1 1 d . . . . .
S1 S 0.31487(4) 0.80166(5) 0.16678(3) 0.05383(16) Uani 1 1 d . . . . .
S2 S 0.50732(4) 0.79572(5) 0.09831(4) 0.05700(16) Uani 1 1 d . . . . .
P1 P 0.45340(4) 0.84350(4) 0.20574(4) 0.04991(15) Uani 1 1 d . . . . .
O1 O 0.50221(11) 0.81348(13) 0.29795(10) 0.0695(5) Uani 1 1 d . . . . .
O2 O 0.45877(12) 0.95336(12) 0.20665(11) 0.0660(4) Uani 1 1 d . . . . .
N1 N 0.44229(12) 0.63557(14) -0.09150(12) 0.0524(4) Uani 1 1 d . . . . .
N2 N 0.18254(11) 0.73532(12) -0.07422(11) 0.0448(4) Uani 1 1 d . . . . .
H2 H 0.1263 0.7150 -0.0982 0.054 Uiso 1 1 calc R U . . .
N3 N 0.19929(11) 0.61643(12) 0.02916(10) 0.0443(4) Uani 1 1 d . . . . .
C1 C 0.40873(13) 0.67684(15) -0.03937(13) 0.0437(5) Uani 1 1 d . . . . .
C2 C 0.23446(12) 0.69165(14) -0.00189(11) 0.0389(4) Uani 1 1 d . . . . .
C3 C 0.10672(14) 0.57428(17) -0.01352(14) 0.0524(5) Uani 1 1 d . . . . .
H3A H 0.0616 0.6230 -0.0372 0.063 Uiso 1 1 calc R U . . .
H3B H 0.0806 0.5406 0.0326 0.063 Uiso 1 1 calc R U . . .
C4 C 0.11683(17) 0.50946(18) -0.08969(16) 0.0652(6) Uani 1 1 d . . . . .
H4A H 0.1436 0.5422 -0.1351 0.098 Uiso 1 1 calc R U . . .
H4B H 0.0548 0.4854 -0.1169 0.098 Uiso 1 1 calc R U . . .
H4C H 0.1586 0.4592 -0.0659 0.098 Uiso 1 1 calc R U . . .
C5 C 0.25515(15) 0.56308(17) 0.10509(13) 0.0538(5) Uani 1 1 d . . . . .
H5A H 0.3199 0.5878 0.1194 0.065 Uiso 1 1 calc R U . . .
H5B H 0.2593 0.4992 0.0860 0.065 Uiso 1 1 calc R U . . .
C6 C 0.2119(2) 0.5655(2) 0.18995(16) 0.0829(9) Uani 1 1 d . . . . .
H6A H 0.1483 0.5397 0.1767 0.124 Uiso 1 1 calc R U . . .
H6B H 0.2086 0.6285 0.2099 0.124 Uiso 1 1 calc R U . . .
H6C H 0.2511 0.5300 0.2373 0.124 Uiso 1 1 calc R U . . .
C7 C 0.4215(2) 1.0067(2) 0.1268(2) 0.0865(9) Uani 1 1 d . . . . .
H7A H 0.4304 1.0714 0.1406 0.130 Uiso 1 1 calc R U . . .
H7B H 0.3542 0.9939 0.1076 0.130 Uiso 1 1 calc R U . . .
H7C H 0.4549 0.9905 0.0787 0.130 Uiso 1 1 calc R U . . .
C11 C 0.47619(14) 0.58268(17) -0.15744(13) 0.0512(5) Uani 1 1 d . . . . .
C12 C 0.53277(19) 0.6264(2) -0.21115(18) 0.0741(7) Uani 1 1 d . . . . .
C13 C 0.5624(2) 0.5715(3) -0.2770(2) 0.0942(10) Uani 1 1 d . . . . .
H13 H 0.6009 0.5971 -0.3147 0.113 Uiso 1 1 calc R U . . .
C14 C 0.5361(2) 0.4813(3) -0.28737(19) 0.0927(11) Uani 1 1 d . . . . .
H14 H 0.5563 0.4465 -0.3327 0.111 Uiso 1 1 calc R U . . .
C15 C 0.48081(18) 0.4401(2) -0.23325(18) 0.0756(8) Uani 1 1 d . . . . .
H15 H 0.4646 0.3778 -0.2417 0.091 Uiso 1 1 calc R U . . .
C16 C 0.44864(14) 0.49048(17) -0.16554(14) 0.0549(6) Uani 1 1 d . . . . .
C17 C 0.5591(3) 0.7268(3) -0.1986(3) 0.1269(15) Uani 1 1 d . . . . .
H17A H 0.5017 0.7638 -0.2104 0.190 Uiso 1 1 calc R U . . .
H17B H 0.6000 0.7439 -0.2404 0.190 Uiso 1 1 calc R U . . .
H17C H 0.5923 0.7371 -0.1370 0.190 Uiso 1 1 calc R U . . .
C18 C 0.38685(17) 0.4487(2) -0.10552(18) 0.0731(7) Uani 1 1 d . . . . .
H18A H 0.4152 0.4597 -0.0426 0.110 Uiso 1 1 calc R U . . .
H18B H 0.3815 0.3832 -0.1164 0.110 Uiso 1 1 calc R U . . .
H18C H 0.3241 0.4763 -0.1189 0.110 Uiso 1 1 calc R U . . .
C21 C 0.22014(14) 0.81587(15) -0.11198(13) 0.0460(5) Uani 1 1 d . . . . .
C22 C 0.21039(16) 0.90241(17) -0.07468(14) 0.0561(6) Uani 1 1 d . . . . .
C23 C 0.2567(2) 0.97680(19) -0.10817(18) 0.0741(7) Uani 1 1 d . . . . .
H23 H 0.2528 1.0355 -0.0834 0.089 Uiso 1 1 calc R U . . .
C24 C 0.3072(2) 0.9650(2) -0.1761(2) 0.0799(8) Uani 1 1 d . . . . .
H24 H 0.3401 1.0147 -0.1952 0.096 Uiso 1 1 calc R U . . .
C25 C 0.30977(18) 0.8802(2) -0.21649(17) 0.0714(7) Uani 1 1 d . . . . .
H25 H 0.3422 0.8737 -0.2649 0.086 Uiso 1 1 calc R U . . .
C26 C 0.26518(15) 0.80384(17) -0.18687(14) 0.0531(5) Uani 1 1 d . . . . .
C27 C 0.15002(19) 0.9184(2) -0.00413(17) 0.0748(7) Uani 1 1 d . . . . .
H27A H 0.1044 0.8688 -0.0063 0.112 Uiso 1 1 calc R U . . .
H27B H 0.1164 0.9761 -0.0161 0.112 Uiso 1 1 calc R U . . .
H27C H 0.1904 0.9204 0.0554 0.112 Uiso 1 1 calc R U . . .
C28 C 0.26057(18) 0.7137(2) -0.23733(15) 0.0677(7) Uani 1 1 d . . . . .
H28A H 0.2630 0.6634 -0.1948 0.101 Uiso 1 1 calc R U . . .
H28B H 0.3141 0.7094 -0.2681 0.101 Uiso 1 1 calc R U . . .
H28C H 0.2017 0.7106 -0.2814 0.101 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 S1 2.2083(6) . ?
Ni1 S2 2.2338(5) . ?
Ni1 C1 1.801(2) . ?
Ni1 C2 1.9196(18) . ?
S1 P1 2.0303(7) . ?
S2 P1 2.0213(8) . ?
P1 O1 1.4806(16) . ?
P1 O2 1.5872(18) . ?
O2 C7 1.431(3) . ?
N1 C1 1.151(2) . ?
N1 C11 1.399(3) . ?
N2 H2 0.8600 . ?
N2 C2 1.341(2) . ?
N2 C21 1.437(3) . ?
N3 C2 1.315(2) . ?
N3 C3 1.476(2) . ?
N3 C5 1.469(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.498(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.507(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C11 C12 1.387(3) . ?
C11 C16 1.386(3) . ?
C12 C13 1.386(4) . ?
C12 C17 1.500(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.355(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.363(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.389(3) . ?
C16 C18 1.492(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.385(3) . ?
C21 C26 1.398(3) . ?
C22 C23 1.399(3) . ?
C22 C27 1.494(3) . ?
C23 H23 0.9300 . ?
C23 C24 1.356(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.367(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.383(3) . ?
C26 C28 1.498(3) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 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
S1 Ni1 S2 88.12(2) . . ?
C1 Ni1 S1 172.27(6) . . ?
C1 Ni1 S2 88.44(6) . . ?
C1 Ni1 C2 90.44(8) . . ?
C2 Ni1 S1 93.27(6) . . ?
C2 Ni1 S2 177.37(6) . . ?
P1 S1 Ni1 86.44(3) . . ?
P1 S2 Ni1 85.97(3) . . ?
S2 P1 S1 99.36(3) . . ?
O1 P1 S1 115.73(8) . . ?
O1 P1 S2 117.03(8) . . ?
O1 P1 O2 105.73(9) . . ?
O2 P1 S1 109.99(7) . . ?
O2 P1 S2 108.83(7) . . ?
C7 O2 P1 121.38(15) . . ?
C1 N1 C11 175.7(2) . . ?
C2 N2 H2 119.8 . . ?
C2 N2 C21 120.47(15) . . ?
C21 N2 H2 119.8 . . ?
C2 N3 C3 123.65(16) . . ?
C2 N3 C5 121.25(15) . . ?
C5 N3 C3 114.87(17) . . ?
N1 C1 Ni1 176.82(18) . . ?
N2 C2 Ni1 118.11(14) . . ?
N3 C2 Ni1 122.85(13) . . ?
N3 C2 N2 118.94(16) . . ?
N3 C3 H3A 109.2 . . ?
N3 C3 H3B 109.2 . . ?
N3 C3 C4 112.25(18) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.0 . . ?
N3 C5 H5B 109.0 . . ?
N3 C5 C6 112.83(19) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C12 C11 N1 118.0(2) . . ?
C16 C11 N1 117.1(2) . . ?
C16 C11 C12 124.8(2) . . ?
C11 C12 C17 121.6(3) . . ?
C13 C12 C11 115.8(3) . . ?
C13 C12 C17 122.6(3) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.0(3) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.0 . . ?
C13 C14 C15 121.9(3) . . ?
C15 C14 H14 119.0 . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C16 120.4(3) . . ?
C16 C15 H15 119.8 . . ?
C11 C16 C15 116.1(2) . . ?
C11 C16 C18 121.6(2) . . ?
C15 C16 C18 122.3(2) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C21 N2 119.99(19) . . ?
C22 C21 C26 121.9(2) . . ?
C26 C21 N2 118.1(2) . . ?
C21 C22 C23 117.4(2) . . ?
C21 C22 C27 122.4(2) . . ?
C23 C22 C27 120.2(2) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 C22 121.3(3) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 H24 119.9 . . ?
C23 C24 C25 120.2(3) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 119.3 . . ?
C24 C25 C26 121.3(3) . . ?
C26 C25 H25 119.3 . . ?
C21 C26 C28 121.7(2) . . ?
C25 C26 C21 117.5(2) . . ?
C25 C26 C28 120.7(2) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 P1 O2 C7 -56.8(2) . . . . ?
S2 P1 O2 C7 51.1(2) . . . . ?
O1 P1 O2 C7 177.6(2) . . . . ?
N1 C11 C12 C13 -178.3(2) . . . . ?
N1 C11 C12 C17 1.2(4) . . . . ?
N1 C11 C16 C15 178.16(18) . . . . ?
N1 C11 C16 C18 -1.0(3) . . . . ?
N2 C21 C22 C23 173.71(18) . . . . ?
N2 C21 C22 C27 -8.7(3) . . . . ?
N2 C21 C26 C25 -173.42(18) . . . . ?
N2 C21 C26 C28 10.3(3) . . . . ?
C2 N2 C21 C22 -84.6(2) . . . . ?
C2 N2 C21 C26 96.0(2) . . . . ?
C2 N3 C3 C4 85.7(3) . . . . ?
C2 N3 C5 C6 113.7(2) . . . . ?
C3 N3 C2 Ni1 -173.53(15) . . . . ?
C3 N3 C2 N2 2.7(3) . . . . ?
C3 N3 C5 C6 -71.7(3) . . . . ?
C5 N3 C2 Ni1 0.6(3) . . . . ?
C5 N3 C2 N2 176.75(18) . . . . ?
C5 N3 C3 C4 -88.7(2) . . . . ?
C11 C12 C13 C14 0.5(4) . . . . ?
C12 C11 C16 C15 -0.3(3) . . . . ?
C12 C11 C16 C18 -179.5(2) . . . . ?
C12 C13 C14 C15 -0.9(5) . . . . ?
C13 C14 C15 C16 0.7(4) . . . . ?
C14 C15 C16 C11 -0.1(3) . . . . ?
C14 C15 C16 C18 179.1(2) . . . . ?
C16 C11 C12 C13 0.1(4) . . . . ?
C16 C11 C12 C17 179.6(3) . . . . ?
C17 C12 C13 C14 -179.0(3) . . . . ?
C21 N2 C2 Ni1 -1.5(2) . . . . ?
C21 N2 C2 N3 -177.82(18) . . . . ?
C21 C22 C23 C24 1.6(3) . . . . ?
C22 C21 C26 C25 7.2(3) . . . . ?
C22 C21 C26 C28 -169.05(19) . . . . ?
C22 C23 C24 C25 3.2(4) . . . . ?
C23 C24 C25 C26 -3.0(4) . . . . ?
C24 C25 C26 C21 -2.2(3) . . . . ?
C24 C25 C26 C28 174.1(2) . . . . ?
C26 C21 C22 C23 -6.9(3) . . . . ?
C26 C21 C22 C27 170.65(19) . . . . ?
C27 C22 C23 C24 -176.0(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.152 0.241 0.009 158.1 27.1 ?
2 -0.152 0.759 -0.009 158.1 27.1 ?
3 0.348 0.741 0.491 158.1 27.1 ?
4 0.652 0.259 0.509 158.1 27.1 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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_m246a
_database_code_depnum_ccdc_archive 'CCDC 2299274'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2023-10-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C31 H47 N4 Ni O2 P S2'
_chemical_formula_sum            'C31 H47 N4 Ni O2 P S2'
_chemical_formula_weight         661.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C300  H300  N20  O20  P10  S20  Ni10  '
_chemical_oxdiff_usercomment     'yellow needle'
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      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                   17.6491(10)
_cell_length_b                   21.2342(13)
_cell_length_c                   17.9976(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6744.8(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4410
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.2910
_cell_measurement_theta_min      2.6850
_shelx_estimated_absorpt_T_max   0.958
_shelx_estimated_absorpt_T_min   0.805
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2816
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -29 2 0.0164
-4 29 -1 0.0377
-3 0 -25 0.1515
3 0 25 0.1355
24 5 -3 0.0426
-24 -5 3 0.0426

_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.056
loop_
_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
4.4009 -29.3622 2.2000 -0.1031 -0.7879 -0.6072
-4.2934 29.4716 -1.1074 0.1065 0.8132 0.5721
-2.7692 -0.4793 -25.2019 -0.0706 -0.5278 0.8464
2.7692 0.4793 25.2019 0.0706 0.5278 -0.8464
24.4171 4.8174 -2.6787 -0.9914 0.1306 -0.0089
-24.4171 -4.8174 2.6787 0.9914 -0.1306 0.0089

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_unetI/netI     0.1379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25073
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.739
_diffrn_reflns_theta_min         2.263
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -81.00  -4.00   1.00   90.89    --  -10.64 -37.00-180.00   77
  2  ω     35.00  78.00   1.00   90.89    --   12.51 178.00 120.00   43
  3  ω     70.00  98.00   1.00   90.89    --   12.51-178.00-120.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0394478000
_diffrn_orient_matrix_UB_12      -0.0018639000
_diffrn_orient_matrix_UB_13      0.0071707000
_diffrn_orient_matrix_UB_21      0.0019164000
_diffrn_orient_matrix_UB_22      0.0286321000
_diffrn_orient_matrix_UB_23      0.0201889000
_diffrn_orient_matrix_UB_31      -0.0073670000
_diffrn_orient_matrix_UB_32      0.0170945000
_diffrn_orient_matrix_UB_33      -0.0331008000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3878
_reflns_number_total             8204
_reflns_odcompleteness_completeness 99.74
_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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         8204
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1475
_refine_ls_R_factor_gt           0.0654
_refine_ls_restrained_S_all      1.030
_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)+(0.0310P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1494
_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 Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C27(H27), C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.31836(3) 0.43968(2) 0.46955(3) 0.03270(16) Uani 1 1 d . . . . .
S1 S 0.27048(7) 0.51012(5) 0.54619(6) 0.0446(3) Uani 1 1 d . . . . .
S2 S 0.31501(7) 0.37156(6) 0.56366(6) 0.0531(4) Uani 1 1 d . . . . .
P1 P 0.25940(7) 0.43916(6) 0.62142(6) 0.0420(3) Uani 1 1 d . . . . .
O1 O 0.17240(17) 0.41960(16) 0.62691(17) 0.0565(9) Uani 1 1 d . . . . .
O2 O 0.28221(18) 0.45151(16) 0.69856(16) 0.0598(9) Uani 1 1 d . . . . .
N1 N 0.25992(19) 0.50672(15) 0.34522(18) 0.0344(8) Uani 1 1 d . . . . .
H1 H 0.256(2) 0.5293(17) 0.302(2) 0.041 Uiso 1 1 d . U . . .
N2 N 0.4105(2) 0.34790(16) 0.38576(19) 0.0427(9) Uani 1 1 d . . . . .
N3 N 0.38546(19) 0.52238(16) 0.36453(18) 0.0391(9) Uani 1 1 d . . . . .
N4 N 0.5287(2) 0.5556(2) 0.3080(3) 0.0737(15) Uani 1 1 d . . . . .
H4 H 0.576(3) 0.554(2) 0.284(3) 0.088 Uiso 1 1 d . U . . .
C1 C 0.3209(2) 0.49622(19) 0.3871(2) 0.0328(9) Uani 1 1 d . . . . .
C2 C 0.3707(2) 0.38197(19) 0.4158(2) 0.0377(10) Uani 1 1 d . . . . .
C10 C 0.1300(3) 0.4048(2) 0.5613(3) 0.0678(15) Uani 1 1 d . . . . .
H10A H 0.1579 0.3751 0.5317 0.102 Uiso 1 1 calc R U . . .
H10B H 0.1216 0.4425 0.5331 0.102 Uiso 1 1 calc R U . . .
H10C H 0.0821 0.3867 0.5751 0.102 Uiso 1 1 calc R U . . .
C11 C 0.1825(2) 0.4928(2) 0.3690(2) 0.0373(10) Uani 1 1 d . . . . .
C12 C 0.1419(3) 0.5422(2) 0.4015(2) 0.0433(11) Uani 1 1 d . . . . .
C13 C 0.0671(3) 0.5310(3) 0.4193(3) 0.0577(14) Uani 1 1 d . . . . .
H13 H 0.0386 0.5627 0.4416 0.069 Uiso 1 1 calc R U . . .
C14 C 0.0337(3) 0.4734(3) 0.4047(3) 0.0672(16) Uani 1 1 d . . . . .
H14 H -0.0171 0.4671 0.4165 0.081 Uiso 1 1 calc R U . . .
C15 C 0.0743(3) 0.4260(3) 0.3733(3) 0.0590(14) Uani 1 1 d . . . . .
H15 H 0.0512 0.3874 0.3643 0.071 Uiso 1 1 calc R U . . .
C16 C 0.1505(2) 0.4347(2) 0.3544(2) 0.0437(11) Uani 1 1 d . . . . .
C17 C 0.1768(3) 0.6066(2) 0.4153(3) 0.0551(13) Uani 1 1 d . . . . .
H17 H 0.2314 0.6006 0.4224 0.066 Uiso 1 1 calc R U . . .
C18 C 0.1929(3) 0.3831(2) 0.3136(3) 0.0502(12) Uani 1 1 d . . . . .
H18 H 0.2468 0.3941 0.3136 0.060 Uiso 1 1 calc R U . . .
C21 C 0.4622(3) 0.30614(18) 0.3512(2) 0.0442(12) Uani 1 1 d . . . . .
C22 C 0.4439(3) 0.2837(2) 0.2808(3) 0.0512(13) Uani 1 1 d . . . . .
C23 C 0.4966(4) 0.2406(2) 0.2501(3) 0.0707(17) Uani 1 1 d . . . . .
H23 H 0.4879 0.2238 0.2032 0.085 Uiso 1 1 calc R U . . .
C24 C 0.5601(4) 0.2233(2) 0.2886(4) 0.0770(18) Uani 1 1 d . . . . .
H24 H 0.5928 0.1939 0.2679 0.092 Uiso 1 1 calc R U . . .
C25 C 0.5765(3) 0.2481(2) 0.3564(3) 0.0617(14) Uani 1 1 d . . . . .
H25 H 0.6213 0.2368 0.3801 0.074 Uiso 1 1 calc R U . . .
C26 C 0.5270(3) 0.2902(2) 0.3910(3) 0.0497(12) Uani 1 1 d . . . . .
C27 C 0.3733(3) 0.3052(2) 0.2415(3) 0.0568(13) Uani 1 1 d . . . . .
H27 H 0.3334 0.3089 0.2791 0.068 Uiso 1 1 calc R U . . .
C28 C 0.5439(3) 0.3175(2) 0.4666(3) 0.0573(13) Uani 1 1 d . . . . .
H28 H 0.5197 0.3590 0.4692 0.069 Uiso 1 1 calc R U . . .
C31 C 0.3935(3) 0.5659(2) 0.3011(2) 0.0497(12) Uani 1 1 d . . . . .
H31A H 0.3943 0.6090 0.3192 0.060 Uiso 1 1 calc R U . . .
H31B H 0.3503 0.5613 0.2682 0.060 Uiso 1 1 calc R U . . .
C32 C 0.4649(3) 0.5528(2) 0.2589(3) 0.0542(13) Uani 1 1 d . . . . .
H32A H 0.4620 0.5114 0.2364 0.065 Uiso 1 1 calc R U . . .
H32B H 0.4709 0.5837 0.2196 0.065 Uiso 1 1 calc R U . . .
C33 C 0.5228(3) 0.5061(3) 0.3650(3) 0.0662(15) Uani 1 1 d . . . . .
H33A H 0.5676 0.5061 0.3961 0.079 Uiso 1 1 calc R U . . .
H33B H 0.5184 0.4651 0.3416 0.079 Uiso 1 1 calc R U . . .
C34 C 0.4536(2) 0.5195(2) 0.4109(2) 0.0457(11) Uani 1 1 d . . . . .
H34A H 0.4476 0.4867 0.4480 0.055 Uiso 1 1 calc R U . . .
H34B H 0.4601 0.5593 0.4366 0.055 Uiso 1 1 calc R U . . .
C41 C 0.1463(3) 0.6397(3) 0.4835(3) 0.0840(19) Uani 1 1 d . . . . .
H41A H 0.1729 0.6787 0.4905 0.126 Uiso 1 1 calc R U . . .
H41B H 0.1534 0.6134 0.5263 0.126 Uiso 1 1 calc R U . . .
H41C H 0.0932 0.6481 0.4769 0.126 Uiso 1 1 calc R U . . .
C42 C 0.1660(4) 0.6475(3) 0.3462(3) 0.093(2) Uani 1 1 d . . . . .
H42A H 0.1130 0.6556 0.3389 0.139 Uiso 1 1 calc R U . . .
H42B H 0.1859 0.6259 0.3035 0.139 Uiso 1 1 calc R U . . .
H42C H 0.1924 0.6866 0.3526 0.139 Uiso 1 1 calc R U . . .
C43 C 0.1845(3) 0.3186(2) 0.3519(3) 0.0739(17) Uani 1 1 d . . . . .
H43A H 0.2055 0.3208 0.4010 0.111 Uiso 1 1 calc R U . . .
H43B H 0.2110 0.2873 0.3236 0.111 Uiso 1 1 calc R U . . .
H43C H 0.1318 0.3077 0.3549 0.111 Uiso 1 1 calc R U . . .
C44 C 0.1662(3) 0.3808(2) 0.2329(3) 0.0736(17) Uani 1 1 d . . . . .
H44A H 0.1757 0.4206 0.2095 0.110 Uiso 1 1 calc R U . . .
H44B H 0.1129 0.3719 0.2314 0.110 Uiso 1 1 calc R U . . .
H44C H 0.1933 0.3483 0.2069 0.110 Uiso 1 1 calc R U . . .
C45 C 0.3844(3) 0.3710(3) 0.2073(3) 0.0834(18) Uani 1 1 d . . . . .
H45A H 0.4033 0.3993 0.2446 0.125 Uiso 1 1 calc R U . . .
H45B H 0.3367 0.3863 0.1890 0.125 Uiso 1 1 calc R U . . .
H45C H 0.4200 0.3685 0.1671 0.125 Uiso 1 1 calc R U . . .
C46 C 0.3445(4) 0.2603(3) 0.1824(3) 0.094(2) Uani 1 1 d . . . . .
H46A H 0.3779 0.2614 0.1402 0.141 Uiso 1 1 calc R U . . .
H46B H 0.2945 0.2727 0.1673 0.141 Uiso 1 1 calc R U . . .
H46C H 0.3430 0.2183 0.2021 0.141 Uiso 1 1 calc R U . . .
C47 C 0.5091(4) 0.2771(3) 0.5261(3) 0.107(2) Uani 1 1 d . . . . .
H47A H 0.4582 0.2664 0.5123 0.160 Uiso 1 1 calc R U . . .
H47B H 0.5085 0.2999 0.5722 0.160 Uiso 1 1 calc R U . . .
H47C H 0.5384 0.2394 0.5319 0.160 Uiso 1 1 calc R U . . .
C48 C 0.6276(3) 0.3266(3) 0.4825(3) 0.095(2) Uani 1 1 d . . . . .
H48A H 0.6523 0.2863 0.4841 0.142 Uiso 1 1 calc R U . . .
H48B H 0.6337 0.3474 0.5295 0.142 Uiso 1 1 calc R U . . .
H48C H 0.6498 0.3519 0.4440 0.142 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 S1 2.2032(12) . ?
Ni1 S2 2.2280(12) . ?
Ni1 C1 1.909(4) . ?
Ni1 C2 1.814(4) . ?
S1 P1 2.0351(16) . ?
S2 P1 2.0259(16) . ?
P1 O1 1.594(3) . ?
P1 O2 1.469(3) . ?
O1 C10 1.433(5) . ?
N1 H1 0.91(4) . ?
N1 C1 1.332(5) . ?
N1 C11 1.462(5) . ?
N2 C2 1.144(5) . ?
N2 C21 1.417(5) . ?
N3 C1 1.332(5) . ?
N3 C31 1.476(5) . ?
N3 C34 1.465(5) . ?
N4 H4 0.93(5) . ?
N4 C32 1.432(6) . ?
N4 C33 1.471(6) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.398(6) . ?
C11 C16 1.383(6) . ?
C12 C13 1.380(6) . ?
C12 C17 1.520(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.382(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.359(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.400(6) . ?
C16 C18 1.516(6) . ?
C17 H17 0.9800 . ?
C17 C41 1.515(6) . ?
C17 C42 1.529(7) . ?
C18 H18 0.9800 . ?
C18 C43 1.539(6) . ?
C18 C44 1.529(6) . ?
C21 C22 1.392(6) . ?
C21 C26 1.391(6) . ?
C22 C23 1.417(6) . ?
C22 C27 1.504(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.367(7) . ?
C24 H24 0.9300 . ?
C24 C25 1.360(7) . ?
C25 H25 0.9300 . ?
C25 C26 1.398(6) . ?
C26 C28 1.509(6) . ?
C27 H27 0.9800 . ?
C27 C45 1.540(6) . ?
C27 C46 1.515(6) . ?
C28 H28 0.9800 . ?
C28 C47 1.503(7) . ?
C28 C48 1.517(7) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.497(6) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.502(6) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 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
S1 Ni1 S2 87.40(5) . . ?
C1 Ni1 S1 93.92(12) . . ?
C1 Ni1 S2 178.48(12) . . ?
C2 Ni1 S1 171.02(14) . . ?
C2 Ni1 S2 88.87(13) . . ?
C2 Ni1 C1 89.94(17) . . ?
P1 S1 Ni1 87.18(5) . . ?
P1 S2 Ni1 86.73(5) . . ?
S2 P1 S1 97.85(6) . . ?
O1 P1 S1 109.07(13) . . ?
O1 P1 S2 108.30(14) . . ?
O2 P1 S1 118.05(16) . . ?
O2 P1 S2 118.60(15) . . ?
O2 P1 O1 104.59(18) . . ?
C10 O1 P1 120.6(3) . . ?
C1 N1 H1 129(3) . . ?
C1 N1 C11 123.7(3) . . ?
C11 N1 H1 106(2) . . ?
C2 N2 C21 177.3(5) . . ?
C1 N3 C31 125.5(3) . . ?
C1 N3 C34 120.7(3) . . ?
C34 N3 C31 112.8(3) . . ?
C32 N4 H4 114(4) . . ?
C32 N4 C33 110.2(4) . . ?
C33 N4 H4 111(3) . . ?
N1 C1 Ni1 121.8(3) . . ?
N3 C1 Ni1 121.3(3) . . ?
N3 C1 N1 116.6(4) . . ?
N2 C2 Ni1 172.7(4) . . ?
O1 C10 H10A 109.5 . . ?
O1 C10 H10B 109.5 . . ?
O1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 N1 116.8(4) . . ?
C16 C11 N1 120.4(4) . . ?
C16 C11 C12 122.7(4) . . ?
C11 C12 C17 122.3(4) . . ?
C13 C12 C11 117.3(5) . . ?
C13 C12 C17 120.4(4) . . ?
C12 C13 H13 119.4 . . ?
C12 C13 C14 121.1(5) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.7(5) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.7(5) . . ?
C16 C15 H15 119.7 . . ?
C11 C16 C15 117.6(4) . . ?
C11 C16 C18 122.4(4) . . ?
C15 C16 C18 119.8(4) . . ?
C12 C17 H17 107.7 . . ?
C12 C17 C42 109.1(4) . . ?
C41 C17 C12 114.0(4) . . ?
C41 C17 H17 107.7 . . ?
C41 C17 C42 110.6(4) . . ?
C42 C17 H17 107.7 . . ?
C16 C18 H18 107.8 . . ?
C16 C18 C43 112.2(4) . . ?
C16 C18 C44 109.4(4) . . ?
C43 C18 H18 107.8 . . ?
C44 C18 H18 107.8 . . ?
C44 C18 C43 111.6(4) . . ?
C22 C21 N2 117.7(4) . . ?
C26 C21 N2 117.1(4) . . ?
C26 C21 C22 125.2(4) . . ?
C21 C22 C23 115.0(5) . . ?
C21 C22 C27 121.1(4) . . ?
C23 C22 C27 123.8(5) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 C22 120.9(5) . . ?
C24 C23 H23 119.5 . . ?
C23 C24 H24 119.1 . . ?
C25 C24 C23 121.7(5) . . ?
C25 C24 H24 119.1 . . ?
C24 C25 H25 119.5 . . ?
C24 C25 C26 120.9(5) . . ?
C26 C25 H25 119.5 . . ?
C21 C26 C25 116.1(5) . . ?
C21 C26 C28 122.3(4) . . ?
C25 C26 C28 121.6(5) . . ?
C22 C27 H27 107.1 . . ?
C22 C27 C45 111.0(4) . . ?
C22 C27 C46 114.6(4) . . ?
C45 C27 H27 107.1 . . ?
C46 C27 H27 107.1 . . ?
C46 C27 C45 109.5(5) . . ?
C26 C28 H28 107.5 . . ?
C26 C28 C48 114.3(4) . . ?
C47 C28 C26 110.1(4) . . ?
C47 C28 H28 107.5 . . ?
C47 C28 C48 109.6(5) . . ?
C48 C28 H28 107.5 . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
N3 C31 C32 110.9(4) . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
N4 C32 C31 109.9(4) . . ?
N4 C32 H32A 109.7 . . ?
N4 C32 H32B 109.7 . . ?
C31 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
N4 C33 H33A 110.1 . . ?
N4 C33 H33B 110.1 . . ?
N4 C33 C34 107.8(4) . . ?
H33A C33 H33B 108.5 . . ?
C34 C33 H33A 110.1 . . ?
C34 C33 H33B 110.1 . . ?
N3 C34 C33 111.2(4) . . ?
N3 C34 H34A 109.4 . . ?
N3 C34 H34B 109.4 . . ?
C33 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C17 C41 H41A 109.5 . . ?
C17 C41 H41B 109.5 . . ?
C17 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C17 C42 H42A 109.5 . . ?
C17 C42 H42B 109.5 . . ?
C17 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C18 C43 H43A 109.5 . . ?
C18 C43 H43B 109.5 . . ?
C18 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C18 C44 H44A 109.5 . . ?
C18 C44 H44B 109.5 . . ?
C18 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C27 C45 H45A 109.5 . . ?
C27 C45 H45B 109.5 . . ?
C27 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C27 C46 H46A 109.5 . . ?
C27 C46 H46B 109.5 . . ?
C27 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C28 C47 H47A 109.5 . . ?
C28 C47 H47B 109.5 . . ?
C28 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C28 C48 H48A 109.5 . . ?
C28 C48 H48B 109.5 . . ?
C28 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 P1 O1 C10 51.9(4) . . . . ?
S2 P1 O1 C10 -53.5(4) . . . . ?
O2 P1 O1 C10 179.1(3) . . . . ?
N1 C11 C12 C13 175.6(4) . . . . ?
N1 C11 C12 C17 -2.9(6) . . . . ?
N1 C11 C16 C15 -175.1(4) . . . . ?
N1 C11 C16 C18 -0.3(6) . . . . ?
N2 C21 C22 C23 -178.1(4) . . . . ?
N2 C21 C22 C27 2.6(6) . . . . ?
N2 C21 C26 C25 178.9(4) . . . . ?
N2 C21 C26 C28 -2.1(6) . . . . ?
N3 C31 C32 N4 -55.5(5) . . . . ?
N4 C33 C34 N3 57.4(5) . . . . ?
C1 N1 C11 C12 94.0(5) . . . . ?
C1 N1 C11 C16 -90.5(5) . . . . ?
C1 N3 C31 C32 -140.9(4) . . . . ?
C1 N3 C34 C33 138.5(4) . . . . ?
C11 N1 C1 Ni1 19.1(5) . . . . ?
C11 N1 C1 N3 -167.1(4) . . . . ?
C11 C12 C13 C14 -0.8(7) . . . . ?
C11 C12 C17 C41 -147.7(4) . . . . ?
C11 C12 C17 C42 88.2(5) . . . . ?
C11 C16 C18 C43 134.3(4) . . . . ?
C11 C16 C18 C44 -101.3(5) . . . . ?
C12 C11 C16 C15 0.2(6) . . . . ?
C12 C11 C16 C18 175.0(4) . . . . ?
C12 C13 C14 C15 1.1(8) . . . . ?
C13 C12 C17 C41 33.9(6) . . . . ?
C13 C12 C17 C42 -90.2(5) . . . . ?
C13 C14 C15 C16 -0.7(8) . . . . ?
C14 C15 C16 C11 0.1(7) . . . . ?
C14 C15 C16 C18 -174.9(5) . . . . ?
C15 C16 C18 C43 -51.0(6) . . . . ?
C15 C16 C18 C44 73.4(5) . . . . ?
C16 C11 C12 C13 0.2(6) . . . . ?
C16 C11 C12 C17 -178.2(4) . . . . ?
C17 C12 C13 C14 177.7(4) . . . . ?
C21 C22 C23 C24 0.2(7) . . . . ?
C21 C22 C27 C45 78.2(6) . . . . ?
C21 C22 C27 C46 -157.1(4) . . . . ?
C21 C26 C28 C47 89.0(6) . . . . ?
C21 C26 C28 C48 -147.1(5) . . . . ?
C22 C21 C26 C25 -0.2(7) . . . . ?
C22 C21 C26 C28 178.8(4) . . . . ?
C22 C23 C24 C25 -2.2(9) . . . . ?
C23 C22 C27 C45 -101.0(5) . . . . ?
C23 C22 C27 C46 23.7(7) . . . . ?
C23 C24 C25 C26 3.0(9) . . . . ?
C24 C25 C26 C21 -1.8(7) . . . . ?
C24 C25 C26 C28 179.2(5) . . . . ?
C25 C26 C28 C47 -92.0(6) . . . . ?
C25 C26 C28 C48 31.9(7) . . . . ?
C26 C21 C22 C23 1.0(7) . . . . ?
C26 C21 C22 C27 -178.3(4) . . . . ?
C27 C22 C23 C24 179.5(5) . . . . ?
C31 N3 C1 Ni1 179.2(3) . . . . ?
C31 N3 C1 N1 5.5(6) . . . . ?
C31 N3 C34 C33 -52.3(5) . . . . ?
C32 N4 C33 C34 -63.7(6) . . . . ?
C33 N4 C32 C31 63.2(5) . . . . ?
C34 N3 C1 Ni1 -13.0(5) . . . . ?
C34 N3 C1 N1 173.2(4) . . . . ?
C34 N3 C31 C32 50.5(5) . . . . ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.241
_oxdiff_exptl_absorpt_empirical_full_min 0.283
####################################################################### 
# 
# 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_m144b
_database_code_depnum_ccdc_archive 'CCDC 2299273'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2023-10-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H33 N4 Ni O2 P S2'
_chemical_formula_sum            'C25 H32 N4 Ni O2 P S2'
_chemical_formula_weight         574.34
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C25  H32  N4  O2  P1  S2  Ni1  '
_chemical_oxdiff_usercomment     'yellow plate'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   14.3103(5)
_cell_length_b                   15.1738(5)
_cell_length_c                   14.3126(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.034(3)
_cell_angle_gamma                90
_cell_volume                     3060.32(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6457
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9660
_cell_measurement_theta_min      2.8610
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1204
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-16 1 15 0.0270
-2 21 1 0.0935
9 3 16 0.0751
-5 1 -18 0.1550
0 -21 1 0.1195
3 19 7 0.0705
16 0 -15 0.0652

_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.095
loop_
_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
-16.2850 0.8706 14.5232 0.0602 -0.7537 0.6545
-2.1908 21.2426 1.3130 -0.1019 -0.7661 -0.6346
8.7347 3.0738 16.1709 -0.9711 -0.1801 0.1567
-5.4927 1.2945 -18.1349 0.8947 0.1663 -0.4145
0.1151 -21.3581 1.1176 0.0889 0.6659 0.7407
3.0785 19.3250 7.4319 -0.5247 -0.6823 -0.5090
16.2529 -0.4824 -14.5803 -0.0593 0.7415 -0.6683

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23465
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.859
_diffrn_reflns_theta_min         2.215
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.866
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00  38.00   1.00   34.87    --   12.51 -57.00-120.00   93
  2  ω    -14.00  74.00   1.00   34.87    --   12.51  77.00 150.00   88
  3  ω    -12.00  85.00   1.00   34.87    --   12.51  57.00  30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0381402000
_diffrn_orient_matrix_UB_12      -0.0063683000
_diffrn_orient_matrix_UB_13      -0.0382400000
_diffrn_orient_matrix_UB_21      0.0270436000
_diffrn_orient_matrix_UB_22      -0.0320605000
_diffrn_orient_matrix_UB_23      -0.0196486000
_diffrn_orient_matrix_UB_31      -0.0186745000
_diffrn_orient_matrix_UB_32      -0.0334144000
_diffrn_orient_matrix_UB_33      0.0261279000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4983
_reflns_number_total             7625
_reflns_odcompleteness_completeness 99.91
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         7625
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0384
_refine_ls_restrained_S_all      1.013
_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)+(0.0439P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0976
_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 Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.62331(2) 0.23631(2) 0.47325(2) 0.04137(9) Uani 1 1 d . . . . .
S1 S 0.47853(4) 0.28845(4) 0.41791(4) 0.05627(16) Uani 1 1 d . . . . .
S2 S 0.66860(4) 0.28843(4) 0.34414(4) 0.05430(16) Uani 1 1 d . . . . .
P1 P 0.53290(4) 0.33145(4) 0.30441(4) 0.04692(15) Uani 1 1 d . . . . .
O1 O 0.48325(11) 0.30361(11) 0.20983(10) 0.0641(4) Uani 1 1 d . . . . .
O2 O 0.53310(12) 0.43650(10) 0.30308(10) 0.0605(4) Uani 1 1 d . . . . .
N1 N 0.80074(13) 0.24303(12) 0.59382(12) 0.0490(5) Uani 1 1 d . . . . .
H1 H 0.8497(17) 0.2248(15) 0.6199(16) 0.059 Uiso 1 1 d . U . . .
N2 N 0.54608(13) 0.13389(12) 0.61807(12) 0.0540(5) Uani 1 1 d . . . . .
N3 N 0.78979(13) 0.13155(12) 0.48553(12) 0.0557(5) Uani 1 1 d . . . . .
N4 N 0.87546(17) 0.01192(15) 0.37497(15) 0.0731(6) Uani 1 1 d . . . . .
H4 H 0.902(2) -0.007(2) 0.326(2) 0.103(10) Uiso 1 1 d . . . . .
C1 C 0.75017(14) 0.19881(13) 0.52198(13) 0.0425(5) Uani 1 1 d . . . . .
C2 C 0.57702(15) 0.17741(14) 0.56463(14) 0.0471(5) Uani 1 1 d . . . . .
C8 C 0.5627(3) 0.48639(18) 0.38928(19) 0.0908(9) Uani 1 1 d . . . . .
H8A H 0.5113 0.4879 0.4254 0.109 Uiso 1 1 calc R U . . .
H8B H 0.6164 0.4573 0.4277 0.109 Uiso 1 1 calc R U . . .
C9 C 0.5885(3) 0.5740(2) 0.3699(2) 0.1312(15) Uani 1 1 d . . . . .
H9A H 0.5894 0.6097 0.4253 0.197 Uiso 1 1 calc R U . . .
H9B H 0.5432 0.5975 0.3185 0.197 Uiso 1 1 calc R U . . .
H9C H 0.6504 0.5739 0.3526 0.197 Uiso 1 1 calc R U . . .
C11 C 0.76137(14) 0.31552(14) 0.63876(14) 0.0491(5) Uani 1 1 d . . . . .
C12 C 0.76680(17) 0.39967(16) 0.60230(16) 0.0612(6) Uani 1 1 d . . . . .
C13 C 0.7243(2) 0.46749(18) 0.6444(2) 0.0827(9) Uani 1 1 d . . . . .
H13 H 0.7253 0.5243 0.6204 0.099 Uiso 1 1 calc R U . . .
C14 C 0.6810(2) 0.4522(2) 0.7210(2) 0.0942(10) Uani 1 1 d . . . . .
H14 H 0.6507 0.4981 0.7468 0.113 Uiso 1 1 calc R U . . .
C15 C 0.68201(19) 0.3694(2) 0.75981(19) 0.0807(8) Uani 1 1 d . . . . .
H15 H 0.6549 0.3604 0.8136 0.097 Uiso 1 1 calc R U . . .
C16 C 0.72276(16) 0.29905(17) 0.72015(15) 0.0577(6) Uani 1 1 d . . . . .
C17 C 0.8199(2) 0.41908(19) 0.52300(18) 0.0805(8) Uani 1 1 d . . . . .
H17A H 0.8826 0.3948 0.5379 0.121 Uiso 1 1 calc R U . . .
H17B H 0.8239 0.4817 0.5150 0.121 Uiso 1 1 calc R U . . .
H17C H 0.7870 0.3932 0.4653 0.121 Uiso 1 1 calc R U . . .
C18 C 0.73003(19) 0.21003(19) 0.76695(17) 0.0740(7) Uani 1 1 d . . . . .
H18A H 0.7293 0.1650 0.7197 0.111 Uiso 1 1 calc R U . . .
H18B H 0.6773 0.2017 0.7993 0.111 Uiso 1 1 calc R U . . .
H18C H 0.7882 0.2065 0.8118 0.111 Uiso 1 1 calc R U . . .
C21 C 0.51570(17) 0.07501(15) 0.68153(15) 0.0546(6) Uani 1 1 d . . . . .
C22 C 0.54334(18) -0.01220(16) 0.67595(18) 0.0664(7) Uani 1 1 d . . . . .
C23 C 0.5142(3) -0.0698(2) 0.7393(3) 0.0967(11) Uani 1 1 d . . . . .
H23 H 0.5308 -0.1290 0.7379 0.116 Uiso 1 1 calc R U . . .
C24 C 0.4617(3) -0.0419(3) 0.8038(3) 0.1170(15) Uani 1 1 d . . . . .
H24 H 0.4429 -0.0824 0.8458 0.140 Uiso 1 1 calc R U . . .
C25 C 0.4354(3) 0.0454(3) 0.8086(2) 0.1096(12) Uani 1 1 d . . . . .
H25 H 0.3997 0.0630 0.8538 0.131 Uiso 1 1 calc R U . . .
C26 C 0.4621(2) 0.10733(19) 0.74605(19) 0.0777(8) Uani 1 1 d . . . . .
C27 C 0.6028(2) -0.04196(19) 0.6060(2) 0.0910(9) Uani 1 1 d . . . . .
H27A H 0.5703 -0.0296 0.5428 0.136 Uiso 1 1 calc R U . . .
H27B H 0.6140 -0.1042 0.6128 0.136 Uiso 1 1 calc R U . . .
H27C H 0.6623 -0.0112 0.6172 0.136 Uiso 1 1 calc R U . . .
C28 C 0.4354(3) 0.2023(2) 0.7474(3) 0.1214(13) Uani 1 1 d . . . . .
H28A H 0.4904 0.2365 0.7731 0.182 Uiso 1 1 calc R U . . .
H28B H 0.3875 0.2099 0.7861 0.182 Uiso 1 1 calc R U . . .
H28C H 0.4113 0.2216 0.6839 0.182 Uiso 1 1 calc R U . . .
C31 C 0.73298(18) 0.06853(16) 0.42109(17) 0.0644(6) Uani 1 1 d . . . . .
H31A H 0.6713 0.0941 0.3972 0.077 Uiso 1 1 calc R U . . .
H31B H 0.7231 0.0155 0.4560 0.077 Uiso 1 1 calc R U . . .
C32 C 0.7802(2) 0.04492(19) 0.33969(17) 0.0774(8) Uani 1 1 d . . . . .
H32A H 0.7435 0.0001 0.3012 0.093 Uiso 1 1 calc R U . . .
H32B H 0.7838 0.0964 0.3003 0.093 Uiso 1 1 calc R U . . .
C33 C 0.93031(19) 0.08128(18) 0.42731(18) 0.0733(7) Uani 1 1 d . . . . .
H33A H 0.9300 0.1329 0.3873 0.088 Uiso 1 1 calc R U . . .
H33B H 0.9955 0.0622 0.4462 0.088 Uiso 1 1 calc R U . . .
C34 C 0.88922(18) 0.10412(19) 0.51342(17) 0.0760(8) Uani 1 1 d . . . . .
H34A H 0.8928 0.0533 0.5551 0.091 Uiso 1 1 calc R U . . .
H34B H 0.9256 0.1515 0.5478 0.091 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 S1 2.2303(6) . ?
Ni1 S2 2.2086(6) . ?
Ni1 C1 1.914(2) . ?
Ni1 C2 1.803(2) . ?
S1 P1 2.0274(7) . ?
S2 P1 2.0335(8) . ?
P1 O1 1.4767(15) . ?
P1 O2 1.5941(16) . ?
O2 C8 1.447(3) . ?
N1 H1 0.78(2) . ?
N1 C1 1.331(2) . ?
N1 C11 1.438(3) . ?
N2 C2 1.155(3) . ?
N2 C21 1.396(3) . ?
N3 C1 1.318(2) . ?
N3 C31 1.471(3) . ?
N3 C34 1.469(3) . ?
N4 H4 0.89(3) . ?
N4 C32 1.457(3) . ?
N4 C33 1.442(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.420(4) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C11 C12 1.387(3) . ?
C11 C16 1.396(3) . ?
C12 C13 1.386(3) . ?
C12 C17 1.501(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.370(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.372(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.385(3) . ?
C16 C18 1.503(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.387(3) . ?
C21 C26 1.389(4) . ?
C22 C23 1.376(4) . ?
C22 C27 1.493(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.356(5) . ?
C24 H24 0.9300 . ?
C24 C25 1.383(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.396(4) . ?
C26 C28 1.492(4) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.489(3) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.496(3) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?

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
S2 Ni1 S1 88.03(2) . . ?
C1 Ni1 S1 176.52(6) . . ?
C1 Ni1 S2 90.77(6) . . ?
C2 Ni1 S1 89.86(7) . . ?
C2 Ni1 S2 169.43(7) . . ?
C2 Ni1 C1 91.91(9) . . ?
P1 S1 Ni1 86.35(3) . . ?
P1 S2 Ni1 86.78(3) . . ?
S1 P1 S2 98.85(3) . . ?
O1 P1 S1 116.87(7) . . ?
O1 P1 S2 116.62(8) . . ?
O1 P1 O2 106.06(9) . . ?
O2 P1 S1 109.46(6) . . ?
O2 P1 S2 108.70(7) . . ?
C8 O2 P1 120.93(14) . . ?
C1 N1 H1 120.7(17) . . ?
C1 N1 C11 121.90(17) . . ?
C11 N1 H1 116.4(17) . . ?
C2 N2 C21 174.2(2) . . ?
C1 N3 C31 121.49(18) . . ?
C1 N3 C34 125.07(18) . . ?
C34 N3 C31 112.92(18) . . ?
C32 N4 H4 109.6(19) . . ?
C33 N4 H4 112(2) . . ?
C33 N4 C32 108.7(2) . . ?
N1 C1 Ni1 119.01(15) . . ?
N3 C1 Ni1 122.13(15) . . ?
N3 C1 N1 118.84(18) . . ?
N2 C2 Ni1 174.37(19) . . ?
O2 C8 H8A 109.3 . . ?
O2 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C9 C8 O2 111.7(2) . . ?
C9 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C12 C11 N1 119.0(2) . . ?
C12 C11 C16 122.4(2) . . ?
C16 C11 N1 118.6(2) . . ?
C11 C12 C17 122.3(2) . . ?
C13 C12 C11 117.5(3) . . ?
C13 C12 C17 120.1(3) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.1(3) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.3(3) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 121.0(3) . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C18 121.7(2) . . ?
C15 C16 C11 117.4(3) . . ?
C15 C16 C18 120.8(2) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C21 N2 116.7(2) . . ?
C22 C21 C26 124.8(2) . . ?
C26 C21 N2 118.5(2) . . ?
C21 C22 C27 121.9(2) . . ?
C23 C22 C21 116.5(3) . . ?
C23 C22 C27 121.6(3) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 C22 121.3(3) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 H24 119.3 . . ?
C23 C24 C25 121.3(3) . . ?
C25 C24 H24 119.3 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.4(4) . . ?
C26 C25 H25 119.8 . . ?
C21 C26 C25 115.7(3) . . ?
C21 C26 C28 121.5(2) . . ?
C25 C26 C28 122.9(3) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C31 H31A 109.3 . . ?
N3 C31 H31B 109.3 . . ?
N3 C31 C32 111.7(2) . . ?
H31A C31 H31B 107.9 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
N4 C32 C31 109.6(2) . . ?
N4 C32 H32A 109.7 . . ?
N4 C32 H32B 109.7 . . ?
C31 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
N4 C33 H33A 109.7 . . ?
N4 C33 H33B 109.7 . . ?
N4 C33 C34 109.9(2) . . ?
H33A C33 H33B 108.2 . . ?
C34 C33 H33A 109.7 . . ?
C34 C33 H33B 109.7 . . ?
N3 C34 C33 110.05(19) . . ?
N3 C34 H34A 109.7 . . ?
N3 C34 H34B 109.7 . . ?
C33 C34 H34A 109.7 . . ?
C33 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?

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
S1 P1 O2 C8 43.1(2) . . . . ?
S2 P1 O2 C8 -63.8(2) . . . . ?
P1 O2 C8 C9 160.0(3) . . . . ?
O1 P1 O2 C8 170.0(2) . . . . ?
N1 C11 C12 C13 177.1(2) . . . . ?
N1 C11 C12 C17 -5.6(3) . . . . ?
N1 C11 C16 C15 -177.5(2) . . . . ?
N1 C11 C16 C18 6.1(3) . . . . ?
N2 C21 C22 C23 179.3(2) . . . . ?
N2 C21 C22 C27 0.1(3) . . . . ?
N2 C21 C26 C25 -178.9(2) . . . . ?
N2 C21 C26 C28 1.1(4) . . . . ?
N3 C31 C32 N4 55.2(3) . . . . ?
N4 C33 C34 N3 -58.3(3) . . . . ?
C1 N1 C11 C12 -88.2(3) . . . . ?
C1 N1 C11 C16 94.6(2) . . . . ?
C1 N3 C31 C32 137.9(2) . . . . ?
C1 N3 C34 C33 -137.4(2) . . . . ?
C11 N1 C1 Ni1 3.0(3) . . . . ?
C11 N1 C1 N3 -178.3(2) . . . . ?
C11 C12 C13 C14 1.8(4) . . . . ?
C12 C11 C16 C15 5.4(3) . . . . ?
C12 C11 C16 C18 -171.0(2) . . . . ?
C12 C13 C14 C15 2.5(4) . . . . ?
C13 C14 C15 C16 -3.0(4) . . . . ?
C14 C15 C16 C11 -0.8(4) . . . . ?
C14 C15 C16 C18 175.5(3) . . . . ?
C16 C11 C12 C13 -5.8(3) . . . . ?
C16 C11 C12 C17 171.5(2) . . . . ?
C17 C12 C13 C14 -175.6(2) . . . . ?
C21 C22 C23 C24 -0.3(4) . . . . ?
C22 C21 C26 C25 -0.1(4) . . . . ?
C22 C21 C26 C28 179.9(3) . . . . ?
C22 C23 C24 C25 -0.1(5) . . . . ?
C23 C24 C25 C26 0.4(6) . . . . ?
C24 C25 C26 C21 -0.4(5) . . . . ?
C24 C25 C26 C28 179.7(3) . . . . ?
C26 C21 C22 C23 0.4(4) . . . . ?
C26 C21 C22 C27 -178.7(2) . . . . ?
C27 C22 C23 C24 178.8(3) . . . . ?
C31 N3 C1 Ni1 -14.7(3) . . . . ?
C31 N3 C1 N1 166.6(2) . . . . ?
C31 N3 C34 C33 50.8(3) . . . . ?
C32 N4 C33 C34 64.6(3) . . . . ?
C33 N4 C32 C31 -62.7(3) . . . . ?
C34 N3 C1 Ni1 174.16(19) . . . . ?
C34 N3 C1 N1 -4.5(3) . . . . ?
C34 N3 C31 C32 -50.0(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.169 0.256 0.528 144.3 25.8 ?
2 -0.169 0.744 0.472 144.3 26.1 ?
3 0.331 0.756 0.972 144.3 25.9 ?
4 0.669 0.244 0.028 144.3 26.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.537
_oxdiff_exptl_absorpt_empirical_full_min 0.690
####################################################################### 
# 
# 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_lam992a
_database_code_depnum_ccdc_archive 'CCDC 2299286'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2023-10-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C43 H67 N3 Ni O2 P S2, B F4'
_chemical_formula_sum            'C43 H67 B F4 N3 Ni O2 P S2'
_chemical_formula_weight         898.60
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C86  H134  B2  F8  N6  Ni2  O4  P2  S4  '
_chemical_oxdiff_usercomment     'yellow needle'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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                   9.1019(4)
_cell_length_b                   14.9066(6)
_cell_length_c                   17.7025(10)
_cell_angle_alpha                82.659(4)
_cell_angle_beta                 89.705(4)
_cell_angle_gamma                86.302(4)
_cell_volume                     2377.2(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5612
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6350
_cell_measurement_theta_min      2.7410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             956
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -17 -17 0.0892
0 17 17 0.1102
-1 -11 19 0.0669
-12 -6 -3 0.1268
12 6 3 0.0848
-1 -14 16 0.0802
-1 12 -18 0.1789

_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.199
loop_
_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
0.2944 -16.7365 -17.4024 0.4720 -0.8699 0.1435
-0.2944 16.7365 17.4024 -0.4720 0.8699 -0.1435
-1.1504 -11.0265 19.3580 0.6392 0.5466 0.5410
-12.4273 -6.1194 -3.2786 -0.3289 -0.2825 0.9011
12.4273 6.1194 3.2786 0.3289 0.2825 -0.9011
-1.0000 -14.0000 16.0000 0.7239 0.3829 0.5570
-1.0000 12.0000 -18.0000 -0.7542 -0.4965 -0.4070

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.828
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18610
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.828
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.606
_diffrn_reflns_theta_min         2.242
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00  59.00   1.00    3.76    --  -10.80  57.00  60.00   98
  2  ω    -79.00  11.00   1.00    3.76    --  -10.80 -57.00 -90.00   90
  3  ω    -17.00  79.00   1.00    3.76    --   12.36  77.00-180.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0430892000
_diffrn_orient_matrix_UB_12      -0.0404691000
_diffrn_orient_matrix_UB_13      0.0125276000
_diffrn_orient_matrix_UB_21      0.0061719000
_diffrn_orient_matrix_UB_22      0.0140303000
_diffrn_orient_matrix_UB_23      0.0365958000
_diffrn_orient_matrix_UB_31      -0.0648348000
_diffrn_orient_matrix_UB_32      -0.0218333000
_diffrn_orient_matrix_UB_33      0.0116574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7164
_reflns_number_total             11088
_reflns_odcompleteness_completeness 99.83
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.025
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0678
_refine_ls_restrained_S_all      1.044
_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)+(0.0904P)²+1.4775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1702
_refine_ls_wR_factor_ref         0.2042
_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. Restrained distances
 C31-C32 = C34-C35
 1.457 with sigma of 0.004
3.a Ternary CH refined with riding coordinates:
 C41(H41), C44(H44), C47(H47), C50(H50), C61(H61), C71(H71)
3.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B),
 C66(H66A,H66B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B),
  C76(H76A,H76B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
3.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.76677(5) 0.67810(3) 0.25713(3) 0.03948(15) Uani 1 1 d . . . . .
S1 S 0.85324(12) 0.55572(6) 0.33602(6) 0.0512(3) Uani 1 1 d . . . . .
S2 S 0.75054(11) 0.59116(7) 0.16549(6) 0.0512(3) Uani 1 1 d . . . . .
P1 P 0.81280(10) 0.49173(6) 0.24777(6) 0.0420(2) Uani 1 1 d . . . . .
O1 O 0.9519(3) 0.43229(17) 0.22846(16) 0.0509(6) Uani 1 1 d . . . . .
O2 O 0.6957(3) 0.41929(16) 0.26310(17) 0.0540(7) Uani 1 1 d . . . . .
N1 N 0.5482(3) 0.80205(19) 0.18526(18) 0.0422(7) Uani 1 1 d . . . . .
H1 H 0.5190 0.8581 0.1734 0.051 Uiso 1 1 calc R U . . .
N2 N 0.8135(3) 0.7930(2) 0.3786(2) 0.0524(8) Uani 1 1 d . . . . .
N3 N 0.7851(3) 0.8357(2) 0.1550(2) 0.0707(12) Uani 1 1 d . . . . .
C1 C 0.6916(3) 0.7815(2) 0.1904(2) 0.0406(8) Uani 1 1 d . . . . .
C2 C 0.7931(4) 0.7494(2) 0.3311(2) 0.0447(9) Uani 1 1 d . . . . .
C11 C 0.4372(3) 0.7369(2) 0.1982(2) 0.0412(8) Uani 1 1 d . . . . .
C12 C 0.3943(4) 0.6958(3) 0.1361(2) 0.0489(9) Uani 1 1 d . . . . .
C13 C 0.2837(4) 0.6356(3) 0.1478(3) 0.0619(12) Uani 1 1 d . . . . .
H13 H 0.2535 0.6067 0.1075 0.074 Uiso 1 1 calc R U . . .
C14 C 0.2181(4) 0.6179(3) 0.2176(3) 0.0672(13) Uani 1 1 d . . . . .
H14 H 0.1443 0.5773 0.2242 0.081 Uiso 1 1 calc R U . . .
C15 C 0.2602(4) 0.6591(3) 0.2765(3) 0.0633(12) Uani 1 1 d . . . . .
H15 H 0.2150 0.6458 0.3235 0.076 Uiso 1 1 calc R U . . .
C16 C 0.3703(4) 0.7214(3) 0.2695(2) 0.0493(9) Uani 1 1 d . . . . .
C21 C 0.8327(4) 0.8393(3) 0.4408(3) 0.0589(11) Uani 1 1 d . . . . .
C22 C 0.7760(5) 0.9288(3) 0.4376(3) 0.0752(15) Uani 1 1 d . . . . .
C23 C 0.7899(7) 0.9694(4) 0.5026(4) 0.109(2) Uani 1 1 d . . . . .
H23 H 0.7543 1.0293 0.5026 0.131 Uiso 1 1 calc R U . . .
C24 C 0.8539(8) 0.9245(5) 0.5668(4) 0.118(3) Uani 1 1 d . . . . .
H24 H 0.8584 0.9532 0.6103 0.141 Uiso 1 1 calc R U . . .
C25 C 0.9124(6) 0.8368(4) 0.5681(3) 0.0917(18) Uani 1 1 d . . . . .
H25 H 0.9576 0.8075 0.6122 0.110 Uiso 1 1 calc R U . . .
C26 C 0.9051(5) 0.7918(3) 0.5048(3) 0.0600(11) Uani 1 1 d . . . . .
C31 C 0.7451(5) 0.9148(3) 0.0980(4) 0.099(2) Uani 1 1 d D . . . .
H31A H 0.7647 0.8989 0.0473 0.119 Uiso 1 1 calc R U . . .
H31B H 0.6407 0.9313 0.1015 0.119 Uiso 1 1 calc R U . . .
C32 C 0.8275(7) 0.9902(4) 0.1102(6) 0.171(5) Uani 1 1 d D . . . .
H32A H 0.8019 1.0094 0.1592 0.205 Uiso 1 1 calc R U . . .
H32B H 0.8033 1.0405 0.0710 0.205 Uiso 1 1 calc R U . . .
C33 C 0.9948(7) 0.9629(5) 0.1081(6) 0.186(5) Uani 1 1 d . . . . .
H33A H 1.0213 0.9440 0.0591 0.223 Uiso 1 1 calc R U . . .
H33B H 1.0512 1.0140 0.1159 0.223 Uiso 1 1 calc R U . . .
C34 C 1.0276(7) 0.8845(4) 0.1719(5) 0.152(4) Uani 1 1 d D . . . .
H34A H 1.1320 0.8664 0.1730 0.182 Uiso 1 1 calc R U . . .
H34B H 1.0008 0.9036 0.2208 0.182 Uiso 1 1 calc R U . . .
C35 C 0.9448(5) 0.8102(3) 0.1582(4) 0.101(2) Uani 1 1 d D . . . .
H35A H 0.9645 0.7604 0.1985 0.121 Uiso 1 1 calc R U . . .
H35B H 0.9757 0.7898 0.1104 0.121 Uiso 1 1 calc R U . . .
C41 C 0.4588(5) 0.7185(3) 0.0583(3) 0.0630(11) Uani 1 1 d . . . . .
H41 H 0.5602 0.7342 0.0656 0.076 Uiso 1 1 calc R U . . .
C42 C 0.3763(7) 0.8025(4) 0.0157(3) 0.0948(18) Uani 1 1 d . . . . .
H42A H 0.2742 0.7913 0.0111 0.142 Uiso 1 1 calc R U . . .
H42B H 0.4178 0.8157 -0.0342 0.142 Uiso 1 1 calc R U . . .
H42C H 0.3851 0.8532 0.0434 0.142 Uiso 1 1 calc R U . . .
C43 C 0.4664(7) 0.6403(4) 0.0096(3) 0.0956(18) Uani 1 1 d . . . . .
H43A H 0.5080 0.5862 0.0391 0.143 Uiso 1 1 calc R U . . .
H43B H 0.5268 0.6554 -0.0342 0.143 Uiso 1 1 calc R U . . .
H43C H 0.3690 0.6303 -0.0067 0.143 Uiso 1 1 calc R U . . .
C44 C 0.4078(5) 0.7689(3) 0.3361(3) 0.0646(12) Uani 1 1 d . . . . .
H44 H 0.4904 0.8063 0.3211 0.078 Uiso 1 1 calc R U . . .
C45 C 0.2759(6) 0.8329(4) 0.3546(4) 0.0975(19) Uani 1 1 d . . . . .
H45A H 0.2600 0.8807 0.3131 0.146 Uiso 1 1 calc R U . . .
H45B H 0.2964 0.8584 0.4002 0.146 Uiso 1 1 calc R U . . .
H45C H 0.1893 0.7994 0.3619 0.146 Uiso 1 1 calc R U . . .
C46 C 0.4561(6) 0.7026(5) 0.4056(3) 0.0968(18) Uani 1 1 d . . . . .
H46A H 0.3748 0.6681 0.4239 0.145 Uiso 1 1 calc R U . . .
H46B H 0.4884 0.7356 0.4450 0.145 Uiso 1 1 calc R U . . .
H46C H 0.5356 0.6624 0.3919 0.145 Uiso 1 1 calc R U . . .
C47 C 0.9707(5) 0.6961(3) 0.5045(3) 0.0623(11) Uani 1 1 d . . . . .
H47 H 0.9908 0.6878 0.4513 0.075 Uiso 1 1 calc R U . . .
C48 C 1.1161(5) 0.6786(4) 0.5476(3) 0.0867(16) Uani 1 1 d . . . . .
H48A H 1.1786 0.7271 0.5321 0.130 Uiso 1 1 calc R U . . .
H48B H 1.1636 0.6224 0.5365 0.130 Uiso 1 1 calc R U . . .
H48C H 1.0980 0.6753 0.6013 0.130 Uiso 1 1 calc R U . . .
C49 C 0.8626(6) 0.6276(4) 0.5346(4) 0.0943(18) Uani 1 1 d . . . . .
H49A H 0.8456 0.6311 0.5877 0.141 Uiso 1 1 calc R U . . .
H49B H 0.9021 0.5678 0.5280 0.141 Uiso 1 1 calc R U . . .
H49C H 0.7714 0.6404 0.5071 0.141 Uiso 1 1 calc R U . . .
C50 C 0.7000(7) 0.9791(3) 0.3665(4) 0.093(2) Uani 1 1 d . . . . .
H50 H 0.6903 0.9351 0.3304 0.112 Uiso 1 1 calc R U . . .
C51 C 0.7865(9) 1.0542(5) 0.3277(4) 0.136(3) Uani 1 1 d . . . . .
H51A H 0.8037 1.0965 0.3628 0.204 Uiso 1 1 calc R U . . .
H51B H 0.7320 1.0848 0.2846 0.204 Uiso 1 1 calc R U . . .
H51C H 0.8791 1.0293 0.3108 0.204 Uiso 1 1 calc R U . . .
C52 C 0.5459(8) 1.0139(5) 0.3856(5) 0.145(3) Uani 1 1 d . . . . .
H52A H 0.4960 0.9660 0.4143 0.217 Uiso 1 1 calc R U . . .
H52B H 0.4925 1.0347 0.3394 0.217 Uiso 1 1 calc R U . . .
H52C H 0.5515 1.0632 0.4153 0.217 Uiso 1 1 calc R U . . .
C61 C 0.9464(4) 0.3783(3) 0.1652(2) 0.0540(10) Uani 1 1 d . . . . .
H61 H 0.8474 0.3862 0.1429 0.065 Uiso 1 1 calc R U . . .
C62 C 1.0555(6) 0.4119(5) 0.1057(3) 0.0935(18) Uani 1 1 d . . . . .
H62A H 1.1533 0.4084 0.1279 0.112 Uiso 1 1 calc R U . . .
H62B H 1.0291 0.4746 0.0861 0.112 Uiso 1 1 calc R U . . .
C63 C 1.0537(9) 0.3532(7) 0.0419(4) 0.156(4) Uani 1 1 d . . . . .
H63A H 0.9575 0.3608 0.0177 0.187 Uiso 1 1 calc R U . . .
H63B H 1.1258 0.3730 0.0038 0.187 Uiso 1 1 calc R U . . .
C64 C 1.0867(13) 0.2564(8) 0.0697(6) 0.191(6) Uani 1 1 d . . . . .
H64A H 1.1865 0.2478 0.0895 0.230 Uiso 1 1 calc R U . . .
H64B H 1.0805 0.2210 0.0277 0.230 Uiso 1 1 calc R U . . .
C65 C 0.9807(13) 0.2228(5) 0.1317(6) 0.176(5) Uani 1 1 d . . . . .
H65A H 1.0100 0.1606 0.1514 0.211 Uiso 1 1 calc R U . . .
H65B H 0.8826 0.2240 0.1102 0.211 Uiso 1 1 calc R U . . .
C66 C 0.9773(7) 0.2806(3) 0.1963(3) 0.0904(18) Uani 1 1 d . . . . .
H66A H 0.9016 0.2616 0.2325 0.108 Uiso 1 1 calc R U . . .
H66B H 1.0713 0.2729 0.2226 0.108 Uiso 1 1 calc R U . . .
C71 C 0.5377(4) 0.4439(3) 0.2722(3) 0.0573(11) Uani 1 1 d . . . . .
H71 H 0.5211 0.5100 0.2674 0.069 Uiso 1 1 calc R U . . .
C72 C 0.4946(5) 0.4032(4) 0.3504(3) 0.0753(14) Uani 1 1 d . . . . .
H72A H 0.3960 0.4266 0.3614 0.090 Uiso 1 1 calc R U . . .
H72B H 0.5610 0.4215 0.3875 0.090 Uiso 1 1 calc R U . . .
C73 C 0.4986(6) 0.2997(4) 0.3587(3) 0.0849(15) Uani 1 1 d . . . . .
H73A H 0.6000 0.2756 0.3573 0.102 Uiso 1 1 calc R U . . .
H73B H 0.4578 0.2772 0.4077 0.102 Uiso 1 1 calc R U . . .
C74 C 0.4130(6) 0.2670(4) 0.2968(4) 0.0866(16) Uani 1 1 d . . . . .
H74A H 0.4245 0.2014 0.3015 0.104 Uiso 1 1 calc R U . . .
H74B H 0.3093 0.2843 0.3022 0.104 Uiso 1 1 calc R U . . .
C75 C 0.4642(6) 0.3058(3) 0.2198(3) 0.0764(14) Uani 1 1 d . . . . .
H75A H 0.4033 0.2860 0.1811 0.092 Uiso 1 1 calc R U . . .
H75B H 0.5648 0.2831 0.2122 0.092 Uiso 1 1 calc R U . . .
C76 C 0.4569(5) 0.4080(3) 0.2105(3) 0.0727(13) Uani 1 1 d . . . . .
H76A H 0.4987 0.4301 0.1617 0.087 Uiso 1 1 calc R U . . .
H76B H 0.3547 0.4307 0.2106 0.087 Uiso 1 1 calc R U . . .
F1 F 0.3656(5) 0.9662(3) 0.1466(4) 0.194(3) Uani 1 1 d . . . . .
F2 F 0.5034(6) 1.0510(7) 0.1945(5) 0.287(5) Uani 1 1 d . . . . .
F3 F 0.3509(9) 1.1038(5) 0.1120(5) 0.271(4) Uani 1 1 d . . . . .
F4 F 0.2656(6) 1.0625(4) 0.2188(3) 0.178(2) Uani 1 1 d . . . . .
B1 B 0.3714(8) 1.0451(5) 0.1708(5) 0.094(2) 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 2.2523(10) . ?
Ni1 S2 2.2130(11) . ?
Ni1 P1 2.8086(10) . ?
Ni1 C1 1.910(3) . ?
Ni1 C2 1.815(4) . ?
S1 P1 1.9795(13) . ?
S2 P1 1.9969(13) . ?
P1 O1 1.560(2) . ?
P1 O2 1.564(3) . ?
O1 C61 1.463(5) . ?
O2 C71 1.474(4) . ?
N1 H1 0.8600 . ?
N1 C1 1.323(4) . ?
N1 C11 1.443(4) . ?
N2 C2 1.149(5) . ?
N2 C21 1.391(5) . ?
N3 C1 1.312(5) . ?
N3 C31 1.478(5) . ?
N3 C35 1.478(5) . ?
C11 C12 1.394(5) . ?
C11 C16 1.397(5) . ?
C12 C13 1.389(5) . ?
C12 C41 1.501(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.372(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.346(6) . ?
C15 H15 0.9300 . ?
C15 C16 1.404(5) . ?
C16 C44 1.503(6) . ?
C21 C22 1.392(6) . ?
C21 C26 1.401(6) . ?
C22 C23 1.377(7) . ?
C22 C50 1.526(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.356(9) . ?
C24 H24 0.9300 . ?
C24 C25 1.377(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.381(7) . ?
C26 C47 1.511(6) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.430(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.552(9) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.534(9) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.426(4) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C41 H41 0.9800 . ?
C41 C42 1.532(7) . ?
C41 C43 1.534(6) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44 0.9800 . ?
C44 C45 1.545(6) . ?
C44 C46 1.524(7) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47 0.9800 . ?
C47 C48 1.522(6) . ?
C47 C49 1.510(7) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50 0.9800 . ?
C50 C51 1.503(9) . ?
C50 C52 1.516(9) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C61 H61 0.9800 . ?
C61 C62 1.504(7) . ?
C61 C66 1.498(6) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C62 C63 1.516(8) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 C64 1.476(13) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C64 C65 1.515(15) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C65 C66 1.516(9) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C71 H71 0.9800 . ?
C71 C72 1.500(7) . ?
C71 C76 1.493(6) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C72 C73 1.529(7) . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C73 C74 1.497(7) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C74 C75 1.495(8) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C75 C76 1.508(7) . ?
C76 H76A 0.9700 . ?
C76 H76B 0.9700 . ?
F1 B1 1.306(8) . ?
F2 B1 1.286(8) . ?
F3 B1 1.278(9) . ?
F4 B1 1.316(9) . ?

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 44.38(3) . . ?
S2 Ni1 S1 89.16(4) . . ?
S2 Ni1 P1 44.95(3) . . ?
C1 Ni1 S1 179.47(11) . . ?
C1 Ni1 S2 90.76(11) . . ?
C1 Ni1 P1 135.50(11) . . ?
C2 Ni1 S1 90.08(11) . . ?
C2 Ni1 S2 176.20(12) . . ?
C2 Ni1 P1 134.45(11) . . ?
C2 Ni1 C1 90.04(15) . . ?
P1 S1 Ni1 82.89(4) . . ?
P1 S2 Ni1 83.52(5) . . ?
S1 P1 Ni1 52.73(3) . . ?
S1 P1 S2 104.03(6) . . ?
S2 P1 Ni1 51.53(4) . . ?
O1 P1 Ni1 132.09(11) . . ?
O1 P1 S1 110.19(11) . . ?
O1 P1 S2 114.42(12) . . ?
O1 P1 O2 101.64(14) . . ?
O2 P1 Ni1 126.27(10) . . ?
O2 P1 S1 114.43(12) . . ?
O2 P1 S2 112.49(11) . . ?
C61 O1 P1 119.6(2) . . ?
C71 O2 P1 122.6(2) . . ?
C1 N1 H1 117.7 . . ?
C1 N1 C11 124.5(3) . . ?
C11 N1 H1 117.7 . . ?
C2 N2 C21 174.6(4) . . ?
C1 N3 C31 125.2(3) . . ?
C1 N3 C35 120.4(3) . . ?
C31 N3 C35 113.3(4) . . ?
N1 C1 Ni1 120.3(3) . . ?
N3 C1 Ni1 118.7(2) . . ?
N3 C1 N1 120.8(3) . . ?
N2 C2 Ni1 178.0(3) . . ?
C12 C11 N1 117.4(3) . . ?
C12 C11 C16 122.4(3) . . ?
C16 C11 N1 120.1(3) . . ?
C11 C12 C41 121.9(3) . . ?
C13 C12 C11 117.5(4) . . ?
C13 C12 C41 120.6(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.3(4) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.2(4) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 118.9 . . ?
C14 C15 C16 122.2(4) . . ?
C16 C15 H15 118.9 . . ?
C11 C16 C15 116.4(4) . . ?
C11 C16 C44 123.6(3) . . ?
C15 C16 C44 119.9(4) . . ?
N2 C21 C22 119.1(4) . . ?
N2 C21 C26 117.5(4) . . ?
C22 C21 C26 123.4(4) . . ?
C21 C22 C50 122.0(4) . . ?
C23 C22 C21 116.6(5) . . ?
C23 C22 C50 121.4(4) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 C22 121.8(5) . . ?
C24 C23 H23 119.1 . . ?
C23 C24 H24 119.7 . . ?
C23 C24 C25 120.6(5) . . ?
C25 C24 H24 119.7 . . ?
C24 C25 H25 119.5 . . ?
C24 C25 C26 121.1(5) . . ?
C26 C25 H25 119.5 . . ?
C21 C26 C47 121.5(4) . . ?
C25 C26 C21 116.4(4) . . ?
C25 C26 C47 122.0(4) . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
H31A C31 H31B 108.1 . . ?
C32 C31 N3 110.7(5) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C31 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C31 C32 C33 109.8(6) . . ?
H32A C32 H32B 108.2 . . ?
C33 C32 H32A 109.7 . . ?
C33 C32 H32B 109.7 . . ?
C32 C33 H33A 110.2 . . ?
C32 C33 H33B 110.2 . . ?
H33A C33 H33B 108.5 . . ?
C34 C33 C32 107.7(6) . . ?
C34 C33 H33A 110.2 . . ?
C34 C33 H33B 110.2 . . ?
C33 C34 H34A 109.9 . . ?
C33 C34 H34B 109.9 . . ?
H34A C34 H34B 108.3 . . ?
C35 C34 C33 108.7(6) . . ?
C35 C34 H34A 109.9 . . ?
C35 C34 H34B 109.9 . . ?
N3 C35 H35A 109.3 . . ?
N3 C35 H35B 109.3 . . ?
C34 C35 N3 111.5(5) . . ?
C34 C35 H35A 109.3 . . ?
C34 C35 H35B 109.3 . . ?
H35A C35 H35B 108.0 . . ?
C12 C41 H41 107.0 . . ?
C12 C41 C42 110.4(4) . . ?
C12 C41 C43 114.6(4) . . ?
C42 C41 H41 107.0 . . ?
C42 C41 C43 110.5(4) . . ?
C43 C41 H41 107.0 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C16 C44 H44 107.7 . . ?
C16 C44 C45 109.8(4) . . ?
C16 C44 C46 112.2(4) . . ?
C45 C44 H44 107.7 . . ?
C46 C44 H44 107.7 . . ?
C46 C44 C45 111.5(4) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C26 C47 H47 107.3 . . ?
C26 C47 C48 112.8(4) . . ?
C48 C47 H47 107.3 . . ?
C49 C47 C26 111.1(4) . . ?
C49 C47 H47 107.3 . . ?
C49 C47 C48 110.9(4) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C22 C50 H50 107.4 . . ?
C51 C50 C22 113.1(5) . . ?
C51 C50 H50 107.4 . . ?
C51 C50 C52 111.1(5) . . ?
C52 C50 C22 110.2(6) . . ?
C52 C50 H50 107.4 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O1 C61 H61 109.0 . . ?
O1 C61 C62 108.7(4) . . ?
O1 C61 C66 108.2(4) . . ?
C62 C61 H61 109.0 . . ?
C66 C61 H61 109.0 . . ?
C66 C61 C62 113.0(4) . . ?
C61 C62 H62A 110.0 . . ?
C61 C62 H62B 110.0 . . ?
C61 C62 C63 108.4(6) . . ?
H62A C62 H62B 108.4 . . ?
C63 C62 H62A 110.0 . . ?
C63 C62 H62B 110.0 . . ?
C62 C63 H63A 109.2 . . ?
C62 C63 H63B 109.2 . . ?
H63A C63 H63B 107.9 . . ?
C64 C63 C62 111.9(6) . . ?
C64 C63 H63A 109.2 . . ?
C64 C63 H63B 109.2 . . ?
C63 C64 H64A 109.3 . . ?
C63 C64 H64B 109.3 . . ?
C63 C64 C65 111.5(6) . . ?
H64A C64 H64B 108.0 . . ?
C65 C64 H64A 109.3 . . ?
C65 C64 H64B 109.3 . . ?
C64 C65 H65A 109.3 . . ?
C64 C65 H65B 109.3 . . ?
C64 C65 C66 111.5(8) . . ?
H65A C65 H65B 108.0 . . ?
C66 C65 H65A 109.3 . . ?
C66 C65 H65B 109.3 . . ?
C61 C66 C65 109.7(5) . . ?
C61 C66 H66A 109.7 . . ?
C61 C66 H66B 109.7 . . ?
C65 C66 H66A 109.7 . . ?
C65 C66 H66B 109.7 . . ?
H66A C66 H66B 108.2 . . ?
O2 C71 H71 109.7 . . ?
O2 C71 C72 107.2(4) . . ?
O2 C71 C76 107.5(4) . . ?
C72 C71 H71 109.7 . . ?
C76 C71 H71 109.7 . . ?
C76 C71 C72 112.9(4) . . ?
C71 C72 H72A 109.1 . . ?
C71 C72 H72B 109.1 . . ?
C71 C72 C73 112.5(4) . . ?
H72A C72 H72B 107.8 . . ?
C73 C72 H72A 109.1 . . ?
C73 C72 H72B 109.1 . . ?
C72 C73 H73A 109.3 . . ?
C72 C73 H73B 109.3 . . ?
H73A C73 H73B 107.9 . . ?
C74 C73 C72 111.7(5) . . ?
C74 C73 H73A 109.3 . . ?
C74 C73 H73B 109.3 . . ?
C73 C74 H74A 109.4 . . ?
C73 C74 H74B 109.4 . . ?
H74A C74 H74B 108.0 . . ?
C75 C74 C73 111.3(4) . . ?
C75 C74 H74A 109.4 . . ?
C75 C74 H74B 109.4 . . ?
C74 C75 H75A 109.2 . . ?
C74 C75 H75B 109.2 . . ?
C74 C75 C76 111.9(5) . . ?
H75A C75 H75B 107.9 . . ?
C76 C75 H75A 109.2 . . ?
C76 C75 H75B 109.2 . . ?
C71 C76 C75 112.4(4) . . ?
C71 C76 H76A 109.1 . . ?
C71 C76 H76B 109.1 . . ?
C75 C76 H76A 109.1 . . ?
C75 C76 H76B 109.1 . . ?
H76A C76 H76B 107.9 . . ?
F1 B1 F4 113.5(8) . . ?
F2 B1 F1 107.6(6) . . ?
F2 B1 F4 115.8(8) . . ?
F3 B1 F1 105.7(8) . . ?
F3 B1 F2 107.3(9) . . ?
F3 B1 F4 106.2(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 P1 O1 C61 -123.0(2) . . . . ?
Ni1 P1 O2 C71 10.5(4) . . . . ?
S1 P1 O1 C61 179.5(2) . . . . ?
S1 P1 O2 C71 71.1(3) . . . . ?
S2 P1 O1 C61 -63.7(3) . . . . ?
S2 P1 O2 C71 -47.4(3) . . . . ?
P1 O1 C61 C62 116.9(3) . . . . ?
P1 O1 C61 C66 -120.1(4) . . . . ?
P1 O2 C71 C72 -119.3(3) . . . . ?
P1 O2 C71 C76 119.1(3) . . . . ?
O1 P1 O2 C71 -170.2(3) . . . . ?
O1 C61 C62 C63 177.8(4) . . . . ?
O1 C61 C66 C65 -177.0(6) . . . . ?
O2 P1 O1 C61 57.8(3) . . . . ?
O2 C71 C72 C73 -68.4(5) . . . . ?
O2 C71 C76 C75 67.1(5) . . . . ?
N1 C11 C12 C13 -177.7(3) . . . . ?
N1 C11 C12 C41 -0.6(5) . . . . ?
N1 C11 C16 C15 178.1(3) . . . . ?
N1 C11 C16 C44 -0.4(5) . . . . ?
N2 C21 C22 C23 175.9(5) . . . . ?
N2 C21 C22 C50 -3.0(8) . . . . ?
N2 C21 C26 C25 -175.0(4) . . . . ?
N2 C21 C26 C47 4.7(6) . . . . ?
N3 C31 C32 C33 56.7(9) . . . . ?
C1 N1 C11 C12 -88.2(4) . . . . ?
C1 N1 C11 C16 95.9(4) . . . . ?
C1 N3 C31 C32 137.6(6) . . . . ?
C1 N3 C35 C34 -135.6(6) . . . . ?
C11 N1 C1 Ni1 -28.4(5) . . . . ?
C11 N1 C1 N3 157.4(4) . . . . ?
C11 C12 C13 C14 0.7(6) . . . . ?
C11 C12 C41 C42 -84.9(5) . . . . ?
C11 C12 C41 C43 149.6(4) . . . . ?
C11 C16 C44 C45 112.0(5) . . . . ?
C11 C16 C44 C46 -123.4(4) . . . . ?
C12 C11 C16 C15 2.4(5) . . . . ?
C12 C11 C16 C44 -176.1(3) . . . . ?
C12 C13 C14 C15 0.0(7) . . . . ?
C13 C12 C41 C42 92.1(5) . . . . ?
C13 C12 C41 C43 -33.3(5) . . . . ?
C13 C14 C15 C16 0.5(7) . . . . ?
C14 C15 C16 C11 -1.6(6) . . . . ?
C14 C15 C16 C44 176.9(4) . . . . ?
C15 C16 C44 C45 -66.4(6) . . . . ?
C15 C16 C44 C46 58.2(5) . . . . ?
C16 C11 C12 C13 -1.9(5) . . . . ?
C16 C11 C12 C41 175.2(4) . . . . ?
C21 C22 C23 C24 -0.6(10) . . . . ?
C21 C22 C50 C51 -111.5(6) . . . . ?
C21 C22 C50 C52 123.4(6) . . . . ?
C21 C26 C47 C48 142.1(5) . . . . ?
C21 C26 C47 C49 -92.7(6) . . . . ?
C22 C21 C26 C25 3.1(7) . . . . ?
C22 C21 C26 C47 -177.3(5) . . . . ?
C22 C23 C24 C25 2.3(12) . . . . ?
C23 C22 C50 C51 69.6(8) . . . . ?
C23 C22 C50 C52 -55.5(8) . . . . ?
C23 C24 C25 C26 -1.2(11) . . . . ?
C24 C25 C26 C21 -1.4(8) . . . . ?
C24 C25 C26 C47 179.0(6) . . . . ?
C25 C26 C47 C48 -38.3(6) . . . . ?
C25 C26 C47 C49 86.9(6) . . . . ?
C26 C21 C22 C23 -2.1(8) . . . . ?
C26 C21 C22 C50 179.0(5) . . . . ?
C31 N3 C1 Ni1 175.8(4) . . . . ?
C31 N3 C1 N1 -10.0(7) . . . . ?
C31 N3 C35 C34 55.8(7) . . . . ?
C31 C32 C33 C34 -60.4(10) . . . . ?
C32 C33 C34 C35 60.7(10) . . . . ?
C33 C34 C35 N3 -58.7(9) . . . . ?
C35 N3 C1 Ni1 8.6(6) . . . . ?
C35 N3 C1 N1 -177.2(4) . . . . ?
C35 N3 C31 C32 -54.4(8) . . . . ?
C41 C12 C13 C14 -176.5(4) . . . . ?
C50 C22 C23 C24 178.3(7) . . . . ?
C61 C62 C63 C64 -57.1(9) . . . . ?
C62 C61 C66 C65 -56.7(7) . . . . ?
C62 C63 C64 C65 56.7(10) . . . . ?
C63 C64 C65 C66 -54.6(10) . . . . ?
C64 C65 C66 C61 53.6(8) . . . . ?
C66 C61 C62 C63 57.7(6) . . . . ?
C71 C72 C73 C74 -51.6(6) . . . . ?
C72 C71 C76 C75 -51.0(6) . . . . ?
C72 C73 C74 C75 54.5(6) . . . . ?
C73 C74 C75 C76 -55.9(6) . . . . ?
C74 C75 C76 C71 54.0(6) . . . . ?
C76 C71 C72 C73 49.8(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.222 0.511 0.970 7.3 0.3 ?
2 0.500 0.500 0.500 37.4 1.0 ?
3 0.500 0.000 0.000 8.8 0.0 ?
4 0.778 0.489 0.030 7.3 0.3 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.288
_oxdiff_exptl_absorpt_empirical_full_min 0.885
####################################################################### 
# 
# 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_m273bza
_database_code_depnum_ccdc_archive 'CCDC 2308595'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2024-04-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2024-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H25 N2 Ni O2 P S2'
_chemical_formula_sum            'C25 H25 N2 Ni O2 P S2'
_chemical_formula_weight         539.27
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C100  H100  N8  Ni4  O8  P4  S8  '
_chemical_oxdiff_usercomment     'orange plate'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   14.2683(17)
_cell_length_b                   12.6497(7)
_cell_length_c                   14.8317(16)
_cell_angle_alpha                90
_cell_angle_beta                 94.874(10)
_cell_angle_gamma                90
_cell_volume                     2667.3(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1852
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.9410
_cell_measurement_theta_min      3.1670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
20 -1 -2 0.0515
-7 17 -1 0.1110
-1 -18 1 0.1208
-3 1 21 0.1090
1 1 -21 0.0968
-20 0 2 0.0329
-20 3 2 0.0426

_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.088
loop_
_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
20.0587 -1.0990 -1.7313 0.0861 -0.1231 -0.9887
-7.4329 16.5369 -0.5730 -0.6945 0.6587 0.2893
-0.7615 -17.8040 1.1168 0.7197 -0.6833 0.1231
-3.1643 0.6913 20.8525 0.6826 0.7193 0.1292
1.2568 1.0275 -20.8867 -0.7598 -0.6488 -0.0428
-20.0962 0.0386 1.5378 -0.0522 0.0738 0.9959
-19.7919 3.0760 2.0773 -0.1487 0.2143 0.9654

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.1063
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10091
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.727
_diffrn_reflns_theta_max         24.727
_diffrn_reflns_theta_min         2.492
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00  22.00   1.00   47.05    --  -10.64 -77.00 -90.00   97
  2  ω    -51.00  32.00   1.00   47.05    --   12.51 -37.00  30.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0051869000
_diffrn_orient_matrix_UB_12      -0.0384604000
_diffrn_orient_matrix_UB_13      0.0347955000
_diffrn_orient_matrix_UB_21      -0.0010726000
_diffrn_orient_matrix_UB_22      0.0404959000
_diffrn_orient_matrix_UB_23      0.0329900000
_diffrn_orient_matrix_UB_31      -0.0496562000
_diffrn_orient_matrix_UB_32      -0.0048644000
_diffrn_orient_matrix_UB_33      -0.0011794000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1824
_reflns_number_total             4547
_reflns_odcompleteness_completeness 83.53
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4547
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0579
_refine_ls_restrained_S_all      0.938
_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)+(0.0290P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1390
_refine_special_details          ?
_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. Rigid body (RIGU) restrains
 C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.40123(5) 0.67219(5) 0.62785(5) 0.0772(3) Uani 1 1 d . . . . .
S1 S 0.38231(12) 0.84034(11) 0.59619(12) 0.0915(5) Uani 1 1 d . . . . .
S2 S 0.25755(12) 0.67218(12) 0.67011(14) 0.1061(7) Uani 1 1 d . . . . .
P1 P 0.24920(12) 0.82902(12) 0.63791(13) 0.0902(6) Uani 1 1 d . . . . .
O1 O 0.2238(3) 0.9036(3) 0.7077(3) 0.1071(14) Uani 1 1 d . . . . .
O2 O 0.1742(3) 0.8436(3) 0.5527(3) 0.1095(15) Uani 1 1 d . . . . .
N1 N 0.5991(4) 0.6952(4) 0.5824(4) 0.0873(16) Uani 1 1 d . . . . .
N2 N 0.4041(3) 0.4394(4) 0.6606(3) 0.0820(15) Uani 1 1 d . . . . .
C1 C 0.5234(5) 0.6832(5) 0.5980(4) 0.0785(19) Uani 1 1 d . . . . .
C2 C 0.4054(4) 0.5290(4) 0.6492(4) 0.0744(17) Uani 1 1 d . . . . .
C11 C 0.6906(6) 0.7218(8) 0.5638(5) 0.105(2) Uani 1 1 d . . . . .
C12 C 0.7547(6) 0.6436(10) 0.5585(5) 0.122(3) Uani 1 1 d . . . . .
C13 C 0.8451(7) 0.6678(11) 0.5376(6) 0.168(4) Uani 1 1 d . . . . .
H13 H 0.8900 0.6152 0.5334 0.202 Uiso 1 1 calc R U . . .
C14 C 0.8666(10) 0.7739(14) 0.5230(10) 0.211(8) Uani 1 1 d . U . . .
H14 H 0.9269 0.7918 0.5089 0.253 Uiso 1 1 calc R U . . .
C15 C 0.8030(10) 0.8499(14) 0.5288(10) 0.215(8) Uani 1 1 d . U . . .
H15 H 0.8195 0.9195 0.5177 0.258 Uiso 1 1 calc R U . . .
C16 C 0.7132(7) 0.8278(9) 0.5510(5) 0.137(3) Uani 1 1 d . . . . .
C17 C 0.7295(5) 0.5284(7) 0.5742(5) 0.132(3) Uani 1 1 d . . . . .
H17A H 0.7174 0.5186 0.6363 0.198 Uiso 1 1 calc R U . . .
H17B H 0.7809 0.4839 0.5603 0.198 Uiso 1 1 calc R U . . .
H17C H 0.6744 0.5100 0.5357 0.198 Uiso 1 1 calc R U . . .
C18 C 0.6399(7) 0.9126(6) 0.5619(6) 0.172(4) Uani 1 1 d . . . . .
H18A H 0.5868 0.9010 0.5189 0.257 Uiso 1 1 calc R U . . .
H18B H 0.6665 0.9808 0.5516 0.257 Uiso 1 1 calc R U . . .
H18C H 0.6201 0.9098 0.6221 0.257 Uiso 1 1 calc R U . . .
C21 C 0.3983(6) 0.3290(4) 0.6715(4) 0.0806(18) Uani 1 1 d . . . . .
C22 C 0.4777(6) 0.2713(5) 0.6577(4) 0.093(2) Uani 1 1 d . . . . .
C23 C 0.4678(7) 0.1616(6) 0.6676(5) 0.117(3) Uani 1 1 d . . . . .
H23 H 0.5193 0.1176 0.6623 0.140 Uiso 1 1 calc R U . . .
C24 C 0.3846(8) 0.1194(6) 0.6846(6) 0.138(4) Uani 1 1 d . . . . .
H24 H 0.3796 0.0462 0.6874 0.165 Uiso 1 1 calc R U . . .
C25 C 0.3075(7) 0.1788(7) 0.6978(5) 0.125(3) Uani 1 1 d . . . . .
H25 H 0.2522 0.1463 0.7119 0.149 Uiso 1 1 calc R U . . .
C26 C 0.3116(6) 0.2895(6) 0.6901(4) 0.099(2) Uani 1 1 d . . . . .
C27 C 0.5677(5) 0.3192(6) 0.6385(5) 0.116(2) Uani 1 1 d . . . . .
H27A H 0.5575 0.3676 0.5888 0.174 Uiso 1 1 calc R U . . .
H27B H 0.6105 0.2648 0.6232 0.174 Uiso 1 1 calc R U . . .
H27C H 0.5939 0.3566 0.6911 0.174 Uiso 1 1 calc R U . . .
C28 C 0.2292(5) 0.3591(6) 0.7034(5) 0.130(3) Uani 1 1 d . . . . .
H28A H 0.2479 0.4138 0.7461 0.195 Uiso 1 1 calc R U . . .
H28B H 0.1798 0.3178 0.7260 0.195 Uiso 1 1 calc R U . . .
H28C H 0.2069 0.3905 0.6467 0.195 Uiso 1 1 calc R U . . .
C30 C 0.1768(5) 0.7838(6) 0.4708(5) 0.148(3) Uani 1 1 d . . . . .
H30A H 0.1661 0.7096 0.4828 0.178 Uiso 1 1 calc R U . . .
H30B H 0.2382 0.7907 0.4478 0.178 Uiso 1 1 calc R U . . .
C31 C 0.1008(4) 0.8247(6) 0.4005(5) 0.101(2) Uani 1 1 d . . . . .
C32 C 0.0490(5) 0.9151(6) 0.4093(6) 0.123(3) Uani 1 1 d . . . . .
H32 H 0.0595 0.9560 0.4613 0.147 Uiso 1 1 calc R U . . .
C33 C -0.0166(6) 0.9454(7) 0.3441(7) 0.147(3) Uani 1 1 d . . . . .
H33 H -0.0499 1.0076 0.3515 0.176 Uiso 1 1 calc R U . . .
C34 C -0.0349(7) 0.8895(11) 0.2707(8) 0.165(4) Uani 1 1 d . U . . .
H34 H -0.0805 0.9127 0.2266 0.198 Uiso 1 1 calc R U . . .
C35 C 0.0119(7) 0.7977(10) 0.2575(7) 0.172(4) Uani 1 1 d . U . . .
H35 H -0.0021 0.7586 0.2049 0.207 Uiso 1 1 calc R U . . .
C36 C 0.0823(5) 0.7612(6) 0.3245(6) 0.135(3) Uani 1 1 d . . . . .
H36 H 0.1142 0.6981 0.3176 0.162 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 S1 2.1901(15) . ?
Ni1 S2 2.1940(19) . ?
Ni1 C1 1.840(8) . ?
Ni1 C2 1.839(6) . ?
S1 P1 2.052(3) . ?
S2 P1 2.042(2) . ?
P1 O1 1.468(4) . ?
P1 O2 1.595(4) . ?
O2 C30 1.434(7) . ?
N1 C1 1.134(7) . ?
N1 C11 1.398(9) . ?
N2 C2 1.146(6) . ?
N2 C21 1.409(7) . ?
C11 C12 1.354(10) . ?
C11 C16 1.396(10) . ?
C12 C13 1.386(10) . ?
C12 C17 1.524(10) . ?
C13 H13 0.9300 . ?
C13 C14 1.397(15) . ?
C14 H14 0.9300 . ?
C14 C15 1.330(19) . ?
C15 H15 0.9300 . ?
C15 C16 1.378(14) . ?
C16 C18 1.517(11) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.378(8) . ?
C21 C26 1.383(9) . ?
C22 C23 1.405(8) . ?
C22 C27 1.469(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.345(11) . ?
C24 H24 0.9300 . ?
C24 C25 1.360(10) . ?
C25 H25 0.9300 . ?
C25 C26 1.406(9) . ?
C26 C28 1.496(9) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.530(8) . ?
C31 C32 1.374(8) . ?
C31 C36 1.391(9) . ?
C32 H32 0.9300 . ?
C32 C33 1.343(9) . ?
C33 H33 0.9300 . ?
C33 C34 1.307(11) . ?
C34 H34 0.9300 . ?
C34 C35 1.361(12) . ?
C35 H35 0.9300 . ?
C35 C36 1.427(11) . ?
C36 H36 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
S1 Ni1 S2 87.72(7) . . ?
C1 Ni1 S1 88.68(18) . . ?
C1 Ni1 S2 174.9(2) . . ?
C2 Ni1 S1 174.38(16) . . ?
C2 Ni1 S2 88.15(18) . . ?
C2 Ni1 C1 95.7(2) . . ?
P1 S1 Ni1 88.16(8) . . ?
P1 S2 Ni1 88.31(8) . . ?
S2 P1 S1 95.81(9) . . ?
O1 P1 S1 117.3(2) . . ?
O1 P1 S2 118.2(2) . . ?
O1 P1 O2 107.1(2) . . ?
O2 P1 S1 109.2(2) . . ?
O2 P1 S2 108.64(18) . . ?
C30 O2 P1 123.1(4) . . ?
C1 N1 C11 173.8(8) . . ?
C2 N2 C21 177.0(6) . . ?
N1 C1 Ni1 176.0(6) . . ?
N2 C2 Ni1 177.0(5) . . ?
C12 C11 N1 118.9(8) . . ?
C12 C11 C16 121.9(9) . . ?
C16 C11 N1 119.2(9) . . ?
C11 C12 C13 119.9(10) . . ?
C11 C12 C17 121.4(8) . . ?
C13 C12 C17 118.8(11) . . ?
C12 C13 H13 121.1 . . ?
C12 C13 C14 117.9(12) . . ?
C14 C13 H13 121.1 . . ?
C13 C14 H14 119.2 . . ?
C15 C14 C13 121.6(16) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 H15 119.3 . . ?
C14 C15 C16 121.5(18) . . ?
C16 C15 H15 119.3 . . ?
C11 C16 C18 119.7(9) . . ?
C15 C16 C11 117.2(12) . . ?
C15 C16 C18 123.0(12) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C21 N2 116.7(6) . . ?
C22 C21 C26 126.8(6) . . ?
C26 C21 N2 116.4(7) . . ?
C21 C22 C23 114.6(8) . . ?
C21 C22 C27 123.6(6) . . ?
C23 C22 C27 121.7(8) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.7(8) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 118.5 . . ?
C23 C24 C25 123.0(8) . . ?
C25 C24 H24 118.5 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 119.9(9) . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 114.8(7) . . ?
C21 C26 C28 122.6(7) . . ?
C25 C26 C28 122.5(8) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O2 C30 H30A 109.8 . . ?
O2 C30 H30B 109.8 . . ?
O2 C30 C31 109.4(6) . . ?
H30A C30 H30B 108.3 . . ?
C31 C30 H30A 109.8 . . ?
C31 C30 H30B 109.8 . . ?
C32 C31 C30 124.9(7) . . ?
C32 C31 C36 119.4(7) . . ?
C36 C31 C30 115.6(7) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 C31 121.1(8) . . ?
C33 C32 H32 119.4 . . ?
C32 C33 H33 119.2 . . ?
C34 C33 C32 121.5(10) . . ?
C34 C33 H33 119.2 . . ?
C33 C34 H34 119.5 . . ?
C33 C34 C35 121.1(11) . . ?
C35 C34 H34 119.5 . . ?
C34 C35 H35 120.0 . . ?
C34 C35 C36 120.0(10) . . ?
C36 C35 H35 120.0 . . ?
C31 C36 C35 116.8(8) . . ?
C31 C36 H36 121.6 . . ?
C35 C36 H36 121.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 P1 O2 C30 51.8(6) . . . . ?
S2 P1 O2 C30 -51.5(6) . . . . ?
P1 O2 C30 C31 -174.8(4) . . . . ?
O1 P1 O2 C30 179.8(6) . . . . ?
O2 C30 C31 C32 9.7(11) . . . . ?
O2 C30 C31 C36 -167.6(7) . . . . ?
N1 C11 C12 C13 178.2(7) . . . . ?
N1 C11 C12 C17 -1.2(11) . . . . ?
N1 C11 C16 C15 -177.2(9) . . . . ?
N1 C11 C16 C18 2.9(11) . . . . ?
N2 C21 C22 C23 -178.8(5) . . . . ?
N2 C21 C22 C27 4.2(9) . . . . ?
N2 C21 C26 C25 178.1(5) . . . . ?
N2 C21 C26 C28 -3.4(9) . . . . ?
C11 C12 C13 C14 0.3(14) . . . . ?
C12 C11 C16 C15 2.6(13) . . . . ?
C12 C11 C16 C18 -177.2(8) . . . . ?
C12 C13 C14 C15 0(2) . . . . ?
C13 C14 C15 C16 1(3) . . . . ?
C14 C15 C16 C11 -2(2) . . . . ?
C14 C15 C16 C18 177.5(14) . . . . ?
C16 C11 C12 C13 -1.7(12) . . . . ?
C16 C11 C12 C17 179.0(7) . . . . ?
C17 C12 C13 C14 179.7(10) . . . . ?
C21 C22 C23 C24 3.2(10) . . . . ?
C22 C21 C26 C25 1.9(10) . . . . ?
C22 C21 C26 C28 -179.5(6) . . . . ?
C22 C23 C24 C25 -3.5(13) . . . . ?
C23 C24 C25 C26 2.7(14) . . . . ?
C24 C25 C26 C21 -1.8(10) . . . . ?
C24 C25 C26 C28 179.7(7) . . . . ?
C26 C21 C22 C23 -2.6(9) . . . . ?
C26 C21 C22 C27 -179.7(6) . . . . ?
C27 C22 C23 C24 -179.6(7) . . . . ?
C30 C31 C32 C33 -180.0(8) . . . . ?
C30 C31 C36 C35 -179.8(8) . . . . ?
C31 C32 C33 C34 1.2(15) . . . . ?
C32 C31 C36 C35 2.7(12) . . . . ?
C32 C33 C34 C35 0.3(18) . . . . ?
C33 C34 C35 C36 -0.2(18) . . . . ?
C34 C35 C36 C31 -1.3(14) . . . . ?
C36 C31 C32 C33 -2.7(12) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 84.8 9.3 ?
2 0.000 0.500 0.500 84.8 9.3 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.165
_oxdiff_exptl_absorpt_empirical_full_min 0.803
####################################################################### 
# 
# 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_mv41a
_database_code_depnum_ccdc_archive 'CCDC 2299288'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2022-06-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H35 N3 Ni O2 P S2, Cl O4'
_chemical_formula_sum            'C24 H35 Cl N3 Ni O6 P S2'
_chemical_formula_weight         650.80
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C96  H140  Cl4  N12  Ni4  O24  P4  S8  '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.8986(2)
_cell_length_b                   15.6526(3)
_cell_length_c                   18.4304(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.3167(16)
_cell_angle_gamma                90
_cell_volume                     3124.97(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5320
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8150
_cell_measurement_theta_min      2.4450
_shelx_estimated_absorpt_T_max   0.856
_shelx_estimated_absorpt_T_min   0.792
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.603
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 7 -4 0.1322
12 -2 15 0.1947
11 -14 6 0.1697
4 -20 -8 0.0673
-3 -17 -15 0.0321
1 9 -24 0.0858
-14 -2 -8 0.0321
-15 -6 1 0.0609
0 -9 24 0.1321
0 22 2 0.1123

_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.209
loop_
_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
15.0000 7.0000 -4.0000 -0.7331 0.2551 -0.6724
12.0000 -2.0000 15.0000 -0.0216 -0.0284 -1.0303
11.0000 -14.0000 6.0000 -0.1575 -0.6160 -0.7799
4.0000 -20.0000 -8.0000 -0.2454 -0.9510 -0.0643
-3.0000 -17.0000 -15.0000 -0.1956 -0.8421 0.4968
1.0000 9.0000 -24.0000 -0.7763 0.2586 0.5932
-14.0000 -2.0000 -8.0000 0.3225 -0.1046 0.9439
-15.0000 -6.0000 1.0000 0.6417 -0.2281 0.7528
0.0000 -9.0000 24.0000 0.7381 -0.2609 -0.6463
-0.0000 22.0000 2.0000 -0.0903 0.9959 0.0129

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13800
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.758
_diffrn_reflns_theta_min         2.224
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  83.00   1.00    7.24    --   21.70  57.00 150.00   83
  2  ω    -63.00  42.00   1.00    7.24    --   21.70 -77.00  30.00  105
  3  ω     25.00  74.00   1.00    7.24    --   21.70 -99.00 150.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0382240000
_diffrn_orient_matrix_UB_12      -0.0066745000
_diffrn_orient_matrix_UB_13      0.0282505000
_diffrn_orient_matrix_UB_21      -0.0022923000
_diffrn_orient_matrix_UB_22      0.0447294000
_diffrn_orient_matrix_UB_23      0.0059023000
_diffrn_orient_matrix_UB_31      -0.0530827000
_diffrn_orient_matrix_UB_32      0.0029322000
_diffrn_orient_matrix_UB_33      -0.0258283000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5159
_reflns_number_total             7138
_reflns_odcompleteness_completeness 99.94
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         7138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0503
_refine_ls_restrained_S_all      1.032
_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)+(0.0695P)²+1.6608P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1517
_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 Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.64804(4) 0.24272(2) 0.36477(2) 0.04160(14) Uani 1 1 d . . . . .
S1 S 0.54748(9) 0.18798(6) 0.45390(4) 0.0593(3) Uani 1 1 d . . . . .
S2 S 0.60491(9) 0.12418(6) 0.30170(5) 0.0586(2) Uani 1 1 d . . . . .
P2 P 0.51616(8) 0.09111(6) 0.38577(5) 0.0500(2) Uani 1 1 d . . . . .
O1 O 0.3770(2) 0.07112(17) 0.36566(15) 0.0668(7) Uani 1 1 d . . . . .
O2 O 0.5523(3) 0.00161(16) 0.41836(15) 0.0683(7) Uani 1 1 d . . . . .
N1 N 0.6652(3) 0.41015(18) 0.43851(15) 0.0536(7) Uani 1 1 d . . . . .
N2 N 0.8651(2) 0.27654(19) 0.30373(15) 0.0539(7) Uani 1 1 d . . . . .
H2 H 0.9101 0.3016 0.2746 0.065 Uiso 1 1 calc R U . . .
N3 N 0.6941(2) 0.33338(19) 0.23802(14) 0.0541(7) Uani 1 1 d . . . . .
C1 C 0.6616(3) 0.3442(2) 0.41078(17) 0.0480(7) Uani 1 1 d . . . . .
C2 C 0.7440(3) 0.2876(2) 0.29366(16) 0.0439(7) Uani 1 1 d . . . . .
C3 C 0.2933(4) 0.1371(3) 0.3368(3) 0.0890(14) Uani 1 1 d . . . . .
H3A H 0.2248 0.1116 0.3073 0.134 Uiso 1 1 calc R U . . .
H3B H 0.3356 0.1756 0.3076 0.134 Uiso 1 1 calc R U . . .
H3C H 0.2637 0.1679 0.3764 0.134 Uiso 1 1 calc R U . . .
C4 C 0.6786(4) -0.0158(3) 0.4471(3) 0.0929(14) Uani 1 1 d . . . . .
H4A H 0.7311 -0.0098 0.4089 0.139 Uiso 1 1 calc R U . . .
H4B H 0.6846 -0.0730 0.4659 0.139 Uiso 1 1 calc R U . . .
H4C H 0.7038 0.0238 0.4856 0.139 Uiso 1 1 calc R U . . .
C5 C 0.5600(3) 0.3458(3) 0.22523(18) 0.0584(9) Uani 1 1 d . . . . .
H5A H 0.5426 0.4064 0.2199 0.070 Uiso 1 1 calc R U . . .
H5B H 0.5227 0.3256 0.2675 0.070 Uiso 1 1 calc R U . . .
C6 C 0.5030(4) 0.3004(4) 0.1594(2) 0.0855(14) Uani 1 1 d . . . . .
H6A H 0.5345 0.3235 0.1169 0.128 Uiso 1 1 calc R U . . .
H6B H 0.4150 0.3077 0.1552 0.128 Uiso 1 1 calc R U . . .
H6C H 0.5225 0.2407 0.1635 0.128 Uiso 1 1 calc R U . . .
C7 C 0.7689(4) 0.3770(3) 0.1868(2) 0.0764(12) Uani 1 1 d . . . . .
H7A H 0.8412 0.4019 0.2143 0.092 Uiso 1 1 calc R U . . .
H7B H 0.7208 0.4232 0.1629 0.092 Uiso 1 1 calc R U . . .
C8 C 0.8095(5) 0.3188(4) 0.1300(2) 0.0980(16) Uani 1 1 d . . . . .
H8A H 0.7386 0.2984 0.0995 0.147 Uiso 1 1 calc R U . . .
H8B H 0.8535 0.2713 0.1532 0.147 Uiso 1 1 calc R U . . .
H8C H 0.8626 0.3494 0.1008 0.147 Uiso 1 1 calc R U . . .
C11 C 0.6742(3) 0.4891(2) 0.4730(2) 0.0583(9) Uani 1 1 d . . . . .
C12 C 0.6916(5) 0.5607(3) 0.4312(3) 0.0907(15) Uani 1 1 d . . . . .
C13 C 0.7014(6) 0.6368(3) 0.4678(5) 0.134(3) Uani 1 1 d . . . . .
H13 H 0.7134 0.6868 0.4422 0.161 Uiso 1 1 calc R U . . .
C14 C 0.6939(7) 0.6410(5) 0.5417(7) 0.162(5) Uani 1 1 d . . . . .
H14 H 0.6993 0.6936 0.5651 0.195 Uiso 1 1 calc R U . . .
C15 C 0.6788(5) 0.5698(6) 0.5803(4) 0.135(3) Uani 1 1 d . . . . .
H15 H 0.6753 0.5739 0.6304 0.163 Uiso 1 1 calc R U . . .
C16 C 0.6685(4) 0.4907(3) 0.5472(2) 0.0816(13) Uani 1 1 d . . . . .
C17 C 0.7019(8) 0.5534(4) 0.3501(3) 0.152(3) Uani 1 1 d . . . . .
H17A H 0.7551 0.5065 0.3415 0.228 Uiso 1 1 calc R U . . .
H17B H 0.7355 0.6054 0.3330 0.228 Uiso 1 1 calc R U . . .
H17C H 0.6215 0.5437 0.3246 0.228 Uiso 1 1 calc R U . . .
C18 C 0.6526(6) 0.4097(5) 0.5881(3) 0.138(3) Uani 1 1 d . . . . .
H18A H 0.5881 0.3762 0.5624 0.207 Uiso 1 1 calc R U . . .
H18B H 0.6312 0.4230 0.6360 0.207 Uiso 1 1 calc R U . . .
H18C H 0.7284 0.3779 0.5923 0.207 Uiso 1 1 calc R U . . .
C21 C 0.9238(3) 0.2248(3) 0.3608(2) 0.0604(9) Uani 1 1 d . . . . .
C22 C 0.9671(3) 0.2625(4) 0.4272(2) 0.0797(14) Uani 1 1 d . . . . .
C23 C 1.0184(4) 0.2091(6) 0.4823(3) 0.107(2) Uani 1 1 d . . . . .
H23 H 1.0464 0.2319 0.5278 0.129 Uiso 1 1 calc R U . . .
C24 C 1.0281(5) 0.1243(6) 0.4706(4) 0.119(3) Uani 1 1 d . . . . .
H24 H 1.0601 0.0894 0.5090 0.142 Uiso 1 1 calc R U . . .
C25 C 0.9925(4) 0.0883(4) 0.4043(4) 0.1039(19) Uani 1 1 d . . . . .
H25 H 1.0026 0.0300 0.3974 0.125 Uiso 1 1 calc R U . . .
C26 C 0.9410(3) 0.1390(3) 0.3470(3) 0.0722(11) Uani 1 1 d . . . . .
C27 C 0.9666(5) 0.3586(4) 0.4370(3) 0.115(2) Uani 1 1 d . . . . .
H27A H 1.0466 0.3811 0.4304 0.172 Uiso 1 1 calc R U . . .
H27B H 0.9473 0.3721 0.4853 0.172 Uiso 1 1 calc R U . . .
H27C H 0.9058 0.3835 0.4017 0.172 Uiso 1 1 calc R U . . .
C28 C 0.9108(5) 0.1013(3) 0.2725(3) 0.0978(16) Uani 1 1 d . . . . .
H28A H 0.8411 0.1307 0.2476 0.147 Uiso 1 1 calc R U . . .
H28B H 0.8913 0.0419 0.2769 0.147 Uiso 1 1 calc R U . . .
H28C H 0.9805 0.1073 0.2453 0.147 Uiso 1 1 calc R U . . .
Cl1 Cl 1.15974(9) 0.33026(8) 0.21620(6) 0.0740(3) Uani 1 1 d . . . . .
O3 O 1.1229(7) 0.2480(4) 0.2090(6) 0.245(4) Uani 1 1 d . . . . .
O4 O 1.0706(4) 0.3722(3) 0.2512(4) 0.182(2) Uani 1 1 d . . . . .
O5 O 1.1587(6) 0.3587(6) 0.1503(3) 0.247(4) Uani 1 1 d . . . . .
O6 O 1.2704(4) 0.3452(5) 0.2534(3) 0.218(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1 2.2428(9) . ?
Ni1 S2 2.2125(9) . ?
Ni1 C1 1.799(4) . ?
Ni1 C2 1.899(3) . ?
S1 P2 1.9744(12) . ?
S2 P2 1.9834(11) . ?
P2 O1 1.553(3) . ?
P2 O2 1.558(3) . ?
O1 C3 1.440(5) . ?
O2 C4 1.444(5) . ?
N1 C1 1.151(4) . ?
N1 C11 1.388(4) . ?
N2 H2 0.8600 . ?
N2 C2 1.324(4) . ?
N2 C21 1.423(4) . ?
N3 C2 1.318(4) . ?
N3 C5 1.468(4) . ?
N3 C7 1.480(4) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.482(5) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.490(6) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C11 C12 1.385(6) . ?
C11 C16 1.377(6) . ?
C12 C13 1.367(8) . ?
C12 C17 1.514(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.374(12) . ?
C14 H14 0.9300 . ?
C14 C15 1.342(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.380(8) . ?
C16 C18 1.496(8) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.392(6) . ?
C21 C26 1.384(6) . ?
C22 C23 1.385(7) . ?
C22 C27 1.515(7) . ?
C23 H23 0.9300 . ?
C23 C24 1.352(9) . ?
C24 H24 0.9300 . ?
C24 C25 1.363(9) . ?
C25 H25 0.9300 . ?
C25 C26 1.389(6) . ?
C26 C28 1.497(7) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Cl1 O3 1.351(6) . ?
Cl1 O4 1.389(5) . ?
Cl1 O5 1.293(5) . ?
Cl1 O6 1.341(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
S2 Ni1 S1 88.38(3) . . ?
C1 Ni1 S1 90.78(10) . . ?
C1 Ni1 S2 171.83(11) . . ?
C1 Ni1 C2 88.60(14) . . ?
C2 Ni1 S1 175.85(10) . . ?
C2 Ni1 S2 92.82(10) . . ?
P2 S1 Ni1 83.79(4) . . ?
P2 S2 Ni1 84.38(4) . . ?
S1 P2 Ni1 52.17(3) . . ?
S1 P2 S2 103.38(5) . . ?
S2 P2 Ni1 51.26(3) . . ?
O1 P2 Ni1 129.44(11) . . ?
O1 P2 S1 113.74(11) . . ?
O1 P2 S2 114.42(12) . . ?
O1 P2 O2 96.31(15) . . ?
O2 P2 Ni1 134.25(11) . . ?
O2 P2 S1 115.25(11) . . ?
O2 P2 S2 114.30(11) . . ?
C3 O1 P2 120.4(3) . . ?
C4 O2 P2 120.1(3) . . ?
C1 N1 C11 177.8(4) . . ?
C2 N2 H2 118.7 . . ?
C2 N2 C21 122.6(3) . . ?
C21 N2 H2 118.7 . . ?
C2 N3 C5 121.0(3) . . ?
C2 N3 C7 122.5(3) . . ?
C5 N3 C7 116.4(3) . . ?
N1 C1 Ni1 176.9(3) . . ?
N2 C2 Ni1 118.1(2) . . ?
N3 C2 Ni1 121.8(2) . . ?
N3 C2 N2 120.0(3) . . ?
O1 C3 H3A 109.5 . . ?
O1 C3 H3B 109.5 . . ?
O1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O2 C4 H4A 109.5 . . ?
O2 C4 H4B 109.5 . . ?
O2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5A 109.0 . . ?
N3 C5 H5B 109.0 . . ?
N3 C5 C6 112.9(3) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 H7A 109.0 . . ?
N3 C7 H7B 109.0 . . ?
N3 C7 C8 113.1(4) . . ?
H7A C7 H7B 107.8 . . ?
C8 C7 H7A 109.0 . . ?
C8 C7 H7B 109.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C12 C11 N1 118.2(4) . . ?
C16 C11 N1 117.5(4) . . ?
C16 C11 C12 124.2(4) . . ?
C11 C12 C17 121.2(4) . . ?
C13 C12 C11 116.0(6) . . ?
C13 C12 C17 122.9(6) . . ?
C12 C13 H13 119.3 . . ?
C12 C13 C14 121.4(7) . . ?
C14 C13 H13 119.3 . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.7(6) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.2(7) . . ?
C16 C15 H15 119.4 . . ?
C11 C16 C15 116.5(6) . . ?
C11 C16 C18 120.4(4) . . ?
C15 C16 C18 123.1(6) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C21 N2 119.3(4) . . ?
C26 C21 N2 118.4(4) . . ?
C26 C21 C22 122.2(4) . . ?
C21 C22 C27 121.4(4) . . ?
C23 C22 C21 117.3(6) . . ?
C23 C22 C27 121.1(5) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.6(6) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 119.0 . . ?
C23 C24 C25 121.9(6) . . ?
C25 C24 H24 119.0 . . ?
C24 C25 H25 120.1 . . ?
C24 C25 C26 119.8(6) . . ?
C26 C25 H25 120.1 . . ?
C21 C26 C25 117.8(5) . . ?
C21 C26 C28 122.0(4) . . ?
C25 C26 C28 120.2(5) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O3 Cl1 O4 106.3(4) . . ?
O5 Cl1 O3 105.3(6) . . ?
O5 Cl1 O4 109.8(5) . . ?
O5 Cl1 O6 109.6(4) . . ?
O6 Cl1 O3 117.2(5) . . ?
O6 Cl1 O4 108.4(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 P2 O1 C3 -5.4(4) . . . . ?
Ni1 P2 O2 C4 1.0(4) . . . . ?
S1 P2 O1 C3 54.2(3) . . . . ?
S1 P2 O2 C4 -59.8(3) . . . . ?
S2 Ni1 C2 N2 -96.0(3) . . . . ?
S2 Ni1 C2 N3 88.3(3) . . . . ?
S2 P2 O1 C3 -64.3(3) . . . . ?
S2 P2 O2 C4 59.7(3) . . . . ?
O1 P2 O2 C4 -179.8(3) . . . . ?
O2 P2 O1 C3 175.4(3) . . . . ?
N1 C11 C12 C13 -179.2(4) . . . . ?
N1 C11 C12 C17 -0.6(7) . . . . ?
N1 C11 C16 C15 179.4(4) . . . . ?
N1 C11 C16 C18 -0.2(6) . . . . ?
N2 C21 C22 C23 177.0(3) . . . . ?
N2 C21 C22 C27 -7.2(6) . . . . ?
N2 C21 C26 C25 -176.7(3) . . . . ?
N2 C21 C26 C28 5.8(5) . . . . ?
C1 Ni1 C2 N2 92.1(3) . . . . ?
C1 Ni1 C2 N3 -83.6(3) . . . . ?
C2 N2 C21 C22 -93.1(4) . . . . ?
C2 N2 C21 C26 89.9(4) . . . . ?
C2 N3 C5 C6 -110.5(4) . . . . ?
C2 N3 C7 C8 80.7(5) . . . . ?
C5 N3 C2 Ni1 -5.1(4) . . . . ?
C5 N3 C2 N2 179.3(3) . . . . ?
C5 N3 C7 C8 -101.2(4) . . . . ?
C7 N3 C2 Ni1 172.9(3) . . . . ?
C7 N3 C2 N2 -2.7(5) . . . . ?
C7 N3 C5 C6 71.4(5) . . . . ?
C11 C12 C13 C14 -0.1(9) . . . . ?
C12 C11 C16 C15 1.2(6) . . . . ?
C12 C11 C16 C18 -178.4(5) . . . . ?
C12 C13 C14 C15 1.2(11) . . . . ?
C13 C14 C15 C16 -1.0(11) . . . . ?
C14 C15 C16 C11 -0.1(8) . . . . ?
C14 C15 C16 C18 179.5(6) . . . . ?
C16 C11 C12 C13 -1.1(7) . . . . ?
C16 C11 C12 C17 177.6(5) . . . . ?
C17 C12 C13 C14 -178.8(7) . . . . ?
C21 N2 C2 Ni1 7.0(5) . . . . ?
C21 N2 C2 N3 -177.2(3) . . . . ?
C21 C22 C23 C24 1.7(7) . . . . ?
C22 C21 C26 C25 6.5(6) . . . . ?
C22 C21 C26 C28 -171.0(4) . . . . ?
C22 C23 C24 C25 2.3(9) . . . . ?
C23 C24 C25 C26 -2.0(8) . . . . ?
C24 C25 C26 C21 -2.3(6) . . . . ?
C24 C25 C26 C28 175.2(5) . . . . ?
C26 C21 C22 C23 -6.1(6) . . . . ?
C26 C21 C22 C27 169.6(4) . . . . ?
C27 C22 C23 C24 -174.1(5) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.015 0.063 0.119 35.9 0.4 ?
2 0.015 -0.063 0.881 35.9 0.4 ?
3 -0.015 0.437 0.619 35.9 0.4 ?
4 0.015 0.563 0.381 35.9 0.4 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.833
####################################################################### 
# 
# 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_lam511a
_database_code_depnum_ccdc_archive 'CCDC 2299483'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2024-04-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT341_lam511a             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01765 Ang.
RESPONSE: This alert is probably due to low quality of crystal, ans some degree of disorder
;
# Added during the CSD deposition process: Thursday 04 April 2024 11:31 AM
# end Validation Reply Form

_audit_creation_date             2024-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H52 N6 Ni2 O4 P2 S4'
_chemical_formula_sum            'C46 H52 N6 Ni2 O4 P2 S4'
_chemical_formula_weight         1060.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C46 H52 N6 O4 P2 S4 Ni2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   15.8519(11)
_cell_length_b                   12.9097(15)
_cell_length_c                   25.918(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.398(8)
_cell_angle_gamma                90
_cell_volume                     5180.2(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1944
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.0350
_cell_measurement_theta_min      2.4250
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 18 1 0.0392
-12 2 -26 0.0303
21 -6 -8 0.1537
2 -2 -36 0.0433
-1 -18 -1 0.0322
-2 2 36 0.0463

_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.071
loop_
_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
1.0397 18.0976 1.0459 -0.9073 -0.3866 0.1405
-11.9139 2.0975 -26.2382 0.1625 -0.1609 0.9849
21.0893 -6.0888 -7.7917 0.4483 -0.5559 -0.7011
2.1671 -1.9534 -36.1172 0.5144 -0.6091 0.6091
-1.0397 -18.0976 -1.0459 0.9073 0.3866 -0.1405
-2.1671 1.9534 36.1172 -0.5144 0.6091 -0.6091

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11394
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.736
_diffrn_reflns_theta_max         24.736
_diffrn_reflns_theta_min         2.054
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     44.00  92.00   1.00   80.50    --   11.75-179.00  60.00   48
  2  ω    -68.00  36.00   1.00   80.50    --   11.75 -19.00  30.00  104
  3  ω    -18.00  38.00   1.00   80.50    --   11.75  77.00  60.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0027175000
_diffrn_orient_matrix_UB_12      -0.0496297000
_diffrn_orient_matrix_UB_13      -0.0113945000
_diffrn_orient_matrix_UB_21      -0.0263016000
_diffrn_orient_matrix_UB_22      -0.0207995000
_diffrn_orient_matrix_UB_23      0.0164118000
_diffrn_orient_matrix_UB_31      -0.0373317000
_diffrn_orient_matrix_UB_32      0.0110483000
_diffrn_orient_matrix_UB_33      -0.0197010000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2225
_reflns_number_total             4420
_reflns_odcompleteness_completeness 99.75
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4420
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.0717
_refine_ls_restrained_S_all      0.989
_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)+(0.0853P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1612
_refine_ls_wR_factor_ref         0.2072
_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. Rigid bond restraints
 C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.63736(5) 0.33415(6) 0.61271(3) 0.0618(3) Uani 1 1 d . . . . .
S1 S 0.73248(11) 0.46065(14) 0.61784(8) 0.0763(6) Uani 1 1 d . . . . .
S2 S 0.74684(10) 0.22319(15) 0.63205(8) 0.0769(6) Uani 1 1 d . . . . .
P1 P 0.82463(11) 0.34857(15) 0.63914(8) 0.0699(6) Uani 1 1 d . . . . .
O1 O 0.8969(3) 0.3478(4) 0.6117(2) 0.0887(15) Uani 1 1 d . . . . .
O2 O 0.8711(3) 0.3642(5) 0.6999(2) 0.1090(19) Uani 1 1 d . . . . .
N1 N 0.5130(3) 0.4827(5) 0.6301(2) 0.0724(18) Uani 1 1 d . . . . .
H1 H 0.480(4) 0.532(6) 0.624(3) 0.087 Uiso 1 1 d . U . . .
N2 N 0.5200(4) 0.1532(6) 0.5846(3) 0.097(2) Uani 1 1 d . . . . .
N3 N 0.5025(3) 0.4354(5) 0.5434(2) 0.0764(17) Uani 1 1 d . . . . .
C1 C 0.5421(4) 0.4288(5) 0.5940(3) 0.0603(17) Uani 1 1 d . . . . .
C2 C 0.5633(5) 0.2238(6) 0.5985(3) 0.074(2) Uani 1 1 d . . . . .
C11 C 0.5492(5) 0.4787(7) 0.6858(3) 0.085(2) Uani 1 1 d . . . . .
C12 C 0.5297(8) 0.4010(11) 0.7166(4) 0.129(4) Uani 1 1 d . . . . .
C13 C 0.5688(11) 0.4009(14) 0.7708(6) 0.171(7) Uani 1 1 d . . . . .
H13 H 0.5592 0.3459 0.7920 0.206 Uiso 1 1 calc R U . . .
C14 C 0.6194(12) 0.4793(16) 0.7919(6) 0.180(9) Uani 1 1 d . . . . .
H14 H 0.6432 0.4789 0.8280 0.216 Uiso 1 1 calc R U . . .
C15 C 0.6378(7) 0.5627(12) 0.7610(5) 0.151(5) Uani 1 1 d . . . . .
H15 H 0.6738 0.6164 0.7763 0.182 Uiso 1 1 calc R U . . .
C16 C 0.6011(6) 0.5629(9) 0.7072(3) 0.096(3) Uani 1 1 d . . . . .
C17 C 0.4647(8) 0.3208(9) 0.6954(5) 0.167(5) Uani 1 1 d . . . . .
H17A H 0.4663 0.3067 0.6592 0.251 Uiso 1 1 calc R U . . .
H17B H 0.4082 0.3453 0.6973 0.251 Uiso 1 1 calc R U . . .
H17C H 0.4773 0.2586 0.7158 0.251 Uiso 1 1 calc R U . . .
C18 C 0.6188(6) 0.6540(8) 0.6761(4) 0.125(3) Uani 1 1 d . . . . .
H18A H 0.6457 0.6313 0.6483 0.188 Uiso 1 1 calc R U . . .
H18B H 0.6566 0.7009 0.6989 0.188 Uiso 1 1 calc R U . . .
H18C H 0.5655 0.6885 0.6612 0.188 Uiso 1 1 calc R U . . .
C20 C 0.8241(7) 0.3727(10) 0.7411(3) 0.169(5) Uani 1 1 d . . . . .
H20A H 0.7661 0.3947 0.7264 0.254 Uiso 1 1 calc R U . . .
H20B H 0.8517 0.4225 0.7668 0.254 Uiso 1 1 calc R U . . .
H20C H 0.8229 0.3066 0.7579 0.254 Uiso 1 1 calc R U . . .
C21 C 0.4713(6) 0.0650(8) 0.5657(4) 0.105(3) Uani 1 1 d . U . . .
C22 C 0.4019(7) 0.0759(10) 0.5222(5) 0.137(4) Uani 1 1 d . U . . .
C23 C 0.3563(7) -0.0165(12) 0.5039(6) 0.165(5) Uani 1 1 d . U . . .
H23 H 0.3105 -0.0147 0.4747 0.198 Uiso 1 1 calc R U . . .
C24 C 0.3811(10) -0.1109(12) 0.5302(7) 0.174(6) Uani 1 1 d . U . . .
H24 H 0.3506 -0.1712 0.5189 0.208 Uiso 1 1 calc R U . . .
C25 C 0.4485(10) -0.1139(10) 0.5716(6) 0.158(4) Uani 1 1 d . U . . .
H25 H 0.4631 -0.1770 0.5885 0.190 Uiso 1 1 calc R U . . .
C26 C 0.4976(7) -0.0274(8) 0.5903(5) 0.117(3) Uani 1 1 d . . . . .
C27 C 0.3764(7) 0.1802(11) 0.4959(6) 0.186(6) Uani 1 1 d . . . . .
H27A H 0.3634 0.2279 0.5215 0.279 Uiso 1 1 calc R U . . .
H27B H 0.3264 0.1716 0.4679 0.279 Uiso 1 1 calc R U . . .
H27C H 0.4233 0.2068 0.4818 0.279 Uiso 1 1 calc R U . . .
C28 C 0.5739(9) -0.0340(9) 0.6322(5) 0.175(5) Uani 1 1 d . . . . .
H28A H 0.6225 -0.0066 0.6201 0.263 Uiso 1 1 calc R U . . .
H28B H 0.5847 -0.1051 0.6423 0.263 Uiso 1 1 calc R U . . .
H28C H 0.5653 0.0053 0.6621 0.263 Uiso 1 1 calc R U . . .
C31 C 0.4253(4) 0.5018(6) 0.5236(3) 0.078(2) Uani 1 1 d . . . . .
H31A H 0.3828 0.4641 0.4979 0.094 Uiso 1 1 calc R U . . .
H31B H 0.3990 0.5221 0.5526 0.094 Uiso 1 1 calc R U . . .
C32 C 0.4544(4) 0.5939(6) 0.4990(2) 0.076(2) Uani 1 1 d . . . . .
H32A H 0.4051 0.6376 0.4848 0.091 Uiso 1 1 calc R U . . .
H32B H 0.4939 0.6334 0.5256 0.091 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 S1 2.207(2) . ?
Ni1 S2 2.2231(18) . ?
Ni1 C1 1.921(6) . ?
Ni1 C2 1.832(8) . ?
S1 P1 2.046(3) . ?
S2 P1 2.019(3) . ?
P1 O1 1.472(5) . ?
P1 O2 1.601(5) . ?
O2 C20 1.434(10) . ?
N1 H1 0.81(7) . ?
N1 C1 1.325(8) . ?
N1 C11 1.436(9) . ?
N2 C2 1.151(9) . ?
N2 C21 1.405(10) . ?
N3 C1 1.331(7) . ?
N3 C31 1.492(8) . ?
N3 C32 1.463(8) 5_666 ?
C11 C12 1.358(13) . ?
C11 C16 1.404(12) . ?
C12 C13 1.407(16) . ?
C12 C17 1.482(15) . ?
C13 H13 0.9300 . ?
C13 C14 1.33(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.41(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.392(13) . ?
C16 C18 1.484(12) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.402(14) . ?
C21 C26 1.374(12) . ?
C22 C23 1.423(15) . ?
C22 C27 1.524(15) . ?
C23 H23 0.9300 . ?
C23 C24 1.410(18) . ?
C24 H24 0.9300 . ?
C24 C25 1.343(17) . ?
C25 H25 0.9300 . ?
C25 C26 1.388(14) . ?
C26 C28 1.445(14) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.468(10) . ?
C32 N3 1.463(8) 5_666 ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?

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 S2 88.45(7) . . ?
C1 Ni1 S1 92.0(2) . . ?
C1 Ni1 S2 178.4(2) . . ?
C2 Ni1 S1 170.8(2) . . ?
C2 Ni1 S2 88.8(2) . . ?
C2 Ni1 C1 90.5(3) . . ?
P1 S1 Ni1 86.10(9) . . ?
P1 S2 Ni1 86.33(9) . . ?
S2 P1 S1 98.96(10) . . ?
O1 P1 S1 117.3(2) . . ?
O1 P1 S2 118.3(2) . . ?
O1 P1 O2 103.5(3) . . ?
O2 P1 S1 109.1(2) . . ?
O2 P1 S2 109.5(2) . . ?
C20 O2 P1 122.7(6) . . ?
C1 N1 H1 125(5) . . ?
C1 N1 C11 124.5(6) . . ?
C11 N1 H1 109(5) . . ?
C2 N2 C21 176.1(8) . . ?
C1 N3 C31 123.7(5) . . ?
C1 N3 C32 121.7(5) . 5_666 ?
C32 N3 C31 111.8(5) 5_666 . ?
N1 C1 Ni1 122.0(5) . . ?
N1 C1 N3 120.0(5) . . ?
N3 C1 Ni1 118.0(5) . . ?
N2 C2 Ni1 172.6(7) . . ?
C12 C11 N1 121.7(10) . . ?
C12 C11 C16 121.9(10) . . ?
C16 C11 N1 116.3(8) . . ?
C11 C12 C13 118.7(14) . . ?
C11 C12 C17 121.7(10) . . ?
C13 C12 C17 119.5(13) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.4(18) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.1 . . ?
C13 C14 C15 121.7(17) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 120.7 . . ?
C16 C15 C14 118.6(14) . . ?
C16 C15 H15 120.7 . . ?
C11 C16 C18 124.2(8) . . ?
C15 C16 C11 118.5(11) . . ?
C15 C16 C18 117.3(12) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N2 118.5(10) . . ?
C26 C21 N2 116.9(10) . . ?
C26 C21 C22 124.6(11) . . ?
C21 C22 C23 116.0(13) . . ?
C21 C22 C27 122.4(10) . . ?
C23 C22 C27 121.6(12) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 C22 119.6(14) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.2(15) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 118.5 . . ?
C24 C25 C26 123.1(15) . . ?
C26 C25 H25 118.5 . . ?
C21 C26 C25 116.4(12) . . ?
C21 C26 C28 121.5(10) . . ?
C25 C26 C28 122.1(13) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C31 H31A 110.2 . . ?
N3 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
C32 C31 N3 107.7(6) . . ?
C32 C31 H31A 110.2 . . ?
C32 C31 H31B 110.2 . . ?
N3 C32 C31 110.9(6) 5_666 . ?
N3 C32 H32A 109.5 5_666 . ?
N3 C32 H32B 109.5 5_666 . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.0 . . ?

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
S1 P1 O2 C20 52.4(8) . . . . ?
S2 P1 O2 C20 -54.9(8) . . . . ?
O1 P1 O2 C20 178.1(8) . . . . ?
N1 C11 C12 C13 178.8(8) . . . . ?
N1 C11 C12 C17 -5.1(13) . . . . ?
N1 C11 C16 C15 -179.9(7) . . . . ?
N1 C11 C16 C18 1.0(11) . . . . ?
N2 C21 C22 C23 178.3(9) . . . . ?
N2 C21 C22 C27 -1.6(15) . . . . ?
N2 C21 C26 C25 179.4(8) . . . . ?
N2 C21 C26 C28 -2.5(15) . . . . ?
N3 C31 C32 N3 57.4(7) . . . 5_666 ?
C1 N1 C11 C12 -80.7(10) . . . . ?
C1 N1 C11 C16 103.4(9) . . . . ?
C1 N3 C31 C32 103.5(7) . . . . ?
C11 N1 C1 Ni1 1.4(10) . . . . ?
C11 N1 C1 N3 177.9(7) . . . . ?
C11 C12 C13 C14 4.3(19) . . . . ?
C12 C11 C16 C15 4.2(12) . . . . ?
C12 C11 C16 C18 -174.9(8) . . . . ?
C12 C13 C14 C15 -2(2) . . . . ?
C13 C14 C15 C16 1(2) . . . . ?
C14 C15 C16 C11 -1.7(14) . . . . ?
C14 C15 C16 C18 177.5(11) . . . . ?
C16 C11 C12 C13 -5.5(13) . . . . ?
C16 C11 C12 C17 170.6(8) . . . . ?
C17 C12 C13 C14 -171.8(14) . . . . ?
C21 C22 C23 C24 1.5(17) . . . . ?
C22 C21 C26 C25 -3.1(15) . . . . ?
C22 C21 C26 C28 175.0(11) . . . . ?
C22 C23 C24 C25 -2(2) . . . . ?
C23 C24 C25 C26 -1(2) . . . . ?
C24 C25 C26 C21 3.0(18) . . . . ?
C24 C25 C26 C28 -175.0(13) . . . . ?
C26 C21 C22 C23 0.9(15) . . . . ?
C26 C21 C22 C27 -179.0(11) . . . . ?
C27 C22 C23 C24 -178.6(12) . . . . ?
C31 N3 C1 Ni1 177.1(5) . . . . ?
C31 N3 C1 N1 0.4(10) . . . . ?
C32 N3 C1 Ni1 -23.3(9) 5_666 . . . ?
C32 N3 C1 N1 160.0(7) 5_666 . . . ?
C32 N3 C31 C32 -57.9(8) 5_666 . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.250 0.238 0.500 130.7 3.7 ?
2 0.250 0.262 0.000 130.7 3.7 ?
3 0.179 0.122 0.741 11.1 0.1 ?
4 0.179 0.378 0.241 11.1 0.1 ?
5 0.250 0.653 0.500 22.2 2.6 ?
6 0.250 0.847 0.000 22.2 2.6 ?
7 0.321 0.122 0.259 11.1 0.1 ?
8 0.321 0.378 0.759 11.1 0.1 ?
9 0.750 0.738 1.000 130.7 3.7 ?
10 0.750 0.762 0.500 130.7 3.7 ?
11 0.679 0.622 0.241 11.1 0.1 ?
12 0.679 0.878 0.741 11.1 0.1 ?
13 0.750 0.153 0.000 22.2 2.6 ?
14 0.750 0.347 0.500 22.2 2.6 ?
15 0.821 0.622 0.759 11.1 0.1 ?
16 0.821 0.878 0.259 11.1 0.1 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.717
_oxdiff_exptl_absorpt_empirical_full_min 0.662
####################################################################### 
# 
# 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_m086b
_database_code_depnum_ccdc_archive 'CCDC 2299303'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2024-04-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT242_m086b               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        C51 Check
RESPONSE: This alert is generated because there is some degree of disorder in the structure
;
# Added during the CSD deposition process: Thursday 04 April 2024 11:25 AM
# end Validation Reply Form

_audit_creation_date             2024-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H43 N3 Ni O2 P S2, Cl O4'
_chemical_formula_sum            'C28 H43 Cl N3 Ni O6 P S2'
_chemical_formula_weight         706.90
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C112  H172  Cl4  N12  Ni4  O24  P4  S8  '
_chemical_oxdiff_usercomment     'yellow block'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   9.2715(2)
_cell_length_b                   21.9434(4)
_cell_length_c                   18.2332(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.038(3)
_cell_angle_gamma                90
_cell_volume                     3598.71(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12980
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5840
_cell_measurement_theta_min      2.4530
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.814
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -15 -22 0.1371
0 -31 -2 0.1096
-6 25 -6 0.1613
5 21 -18 0.1929
-13 -2 7 0.0560
13 8 -4 0.1377
-2 -8 25 0.0866
1 -28 -10 0.1213
-1 29 10 0.0941
0 3 -25 0.1257

_exptl_crystal_size_max          0.295
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.216
loop_
_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
1.0217 -15.2979 -22.0753 -0.8853 0.1160 -0.4504
0.0547 -30.9996 -2.0700 -0.1178 0.3342 -0.9408
-6.1267 24.8379 -6.2625 -0.2693 -0.7628 0.5878
4.7799 20.8560 -18.2854 -0.6623 0.0164 0.7491
-13.0461 -1.6837 6.9545 0.1679 -0.9041 -0.3930
12.6053 7.9579 -4.4507 -0.0649 0.8168 0.5732
-2.1325 -7.9979 24.7618 0.9557 0.0747 -0.2847
1.1157 -28.2798 -10.4178 -0.4372 0.3340 -0.8351
-0.8809 28.5065 9.9633 0.4213 -0.3218 0.8479
-0.1226 2.6079 -24.7898 -0.9814 -0.1818 0.0613

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41217
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.732
_diffrn_reflns_theta_min         2.184
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00  14.00   1.00   10.71    --  -10.48 -37.00 150.00   99
  2  ω    -20.00  30.00   1.00   10.71    --  -10.48 -99.00  30.00   50
  3  ω    -84.00  18.00   1.00   10.71    --  -10.48 -57.00  60.00  102
  4  ω    -20.00  53.00   1.00   10.71    --   12.36 -99.00  90.00   73
  5  ω    -20.00  11.00   1.00   10.71    --   12.36 -99.00 -30.00   31
  6  ω     35.00 101.00   1.00   10.71    --   12.36 178.00 -60.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0081270000
_diffrn_orient_matrix_UB_12      0.0011644000
_diffrn_orient_matrix_UB_13      0.0396718000
_diffrn_orient_matrix_UB_21      0.0738213000
_diffrn_orient_matrix_UB_22      -0.0110384000
_diffrn_orient_matrix_UB_23      0.0058090000
_diffrn_orient_matrix_UB_31      0.0265174000
_diffrn_orient_matrix_UB_32      0.0303571000
_diffrn_orient_matrix_UB_33      0.0005910000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6194
_reflns_number_total             9086
_reflns_odcompleteness_completeness 99.92
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         9086
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0495
_refine_ls_restrained_S_all      1.034
_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)+(0.0570P)²+2.0926P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1391
_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. Rigid bond restraints
 O51, C51, C53, C52
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C52 \\sim C51 \\sim C53: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.02 within 2A
C51 \\sim C53 \\sim C52: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C51, C52, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Ternary CH refined with riding coordinates:
 C41(H41), C51(H51)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C)
;
_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 -0.39103(4) -0.50711(2) -0.25330(2) 0.04409(11) Uani 1 1 d . . . . .
S1 S -0.44336(11) -0.44122(4) -0.16919(5) 0.0695(2) Uani 1 1 d . . . . .
S2 S -0.31416(9) -0.42894(3) -0.31076(5) 0.0609(2) Uani 1 1 d . . . . .
P1 P -0.35774(9) -0.37935(3) -0.22676(5) 0.05514(19) Uani 1 1 d . . . . .
O41 O -0.2215(2) -0.34468(9) -0.17775(13) 0.0681(6) Uani 1 1 d . . . . .
O51 O -0.4587(2) -0.32282(9) -0.25310(12) 0.0661(5) Uani 1 1 d . U . . .
N1 N -0.5274(2) -0.60287(10) -0.17677(13) 0.0520(5) Uani 1 1 d . . . . .
N2 N -0.2106(3) -0.58044(11) -0.32242(14) 0.0531(6) Uani 1 1 d . . . . .
H2 H -0.195(4) -0.6012(15) -0.3490(18) 0.064 Uiso 1 1 d . U . . .
N3 N -0.4584(2) -0.58158(11) -0.38249(12) 0.0538(5) Uani 1 1 d . . . . .
C1 C -0.4696(3) -0.56780(12) -0.20666(15) 0.0467(6) Uani 1 1 d . . . . .
C2 C -0.3493(3) -0.56150(11) -0.32712(14) 0.0434(5) Uani 1 1 d . . . . .
C11 C -0.5961(3) -0.64229(12) -0.13540(18) 0.0564(7) Uani 1 1 d . . . . .
C12 C -0.5489(4) -0.63913(16) -0.0565(2) 0.0722(9) Uani 1 1 d . . . . .
C13 C -0.6203(5) -0.6777(2) -0.0168(3) 0.0981(14) Uani 1 1 d . . . . .
H13 H -0.5940 -0.6771 0.0358 0.118 Uiso 1 1 calc R U . . .
C14 C -0.7279(6) -0.7164(2) -0.0533(4) 0.1118(18) Uani 1 1 d . . . . .
H14 H -0.7733 -0.7422 -0.0251 0.134 Uiso 1 1 calc R U . . .
C15 C -0.7714(4) -0.71851(18) -0.1306(4) 0.1050(16) Uani 1 1 d . . . . .
H15 H -0.8458 -0.7455 -0.1540 0.126 Uiso 1 1 calc R U . . .
C16 C -0.7054(3) -0.68065(14) -0.1749(2) 0.0726(9) Uani 1 1 d . . . . .
C17 C -0.4284(5) -0.5963(2) -0.0175(2) 0.1028(14) Uani 1 1 d . . . . .
H17A H -0.4532 -0.5555 -0.0354 0.154 Uiso 1 1 calc R U . . .
H17B H -0.3360 -0.6080 -0.0284 0.154 Uiso 1 1 calc R U . . .
H17C H -0.4189 -0.5979 0.0360 0.154 Uiso 1 1 calc R U . . .
C18 C -0.7503(5) -0.68114(18) -0.2598(3) 0.1024(14) Uani 1 1 d . . . . .
H18A H -0.6636 -0.6861 -0.2792 0.154 Uiso 1 1 calc R U . . .
H18B H -0.7983 -0.6434 -0.2776 0.154 Uiso 1 1 calc R U . . .
H18C H -0.8177 -0.7143 -0.2767 0.154 Uiso 1 1 calc R U . . .
C21 C -0.0828(3) -0.55884(12) -0.26758(16) 0.0502(6) Uani 1 1 d . . . . .
C22 C -0.0508(3) -0.58278(14) -0.19438(17) 0.0608(7) Uani 1 1 d . . . . .
C23 C 0.0746(4) -0.55903(19) -0.1432(2) 0.0816(11) Uani 1 1 d . . . . .
H23 H 0.0980 -0.5726 -0.0934 0.098 Uiso 1 1 calc R U . . .
C24 C 0.1636(4) -0.51611(19) -0.1652(3) 0.0877(12) Uani 1 1 d . . . . .
H24 H 0.2448 -0.5004 -0.1299 0.105 Uiso 1 1 calc R U . . .
C25 C 0.1337(4) -0.49656(16) -0.2378(3) 0.0797(11) Uani 1 1 d . . . . .
H25 H 0.1973 -0.4687 -0.2523 0.096 Uiso 1 1 calc R U . . .
C26 C 0.0099(3) -0.51733(14) -0.29097(19) 0.0617(7) Uani 1 1 d . . . . .
C27 C -0.1365(4) -0.63395(19) -0.1722(2) 0.0925(12) Uani 1 1 d . . . . .
H27A H -0.0719 -0.6683 -0.1572 0.139 Uiso 1 1 calc R U . . .
H27B H -0.2161 -0.6451 -0.2144 0.139 Uiso 1 1 calc R U . . .
H27C H -0.1766 -0.6215 -0.1308 0.139 Uiso 1 1 calc R U . . .
C28 C -0.0194(4) -0.49589(19) -0.3716(2) 0.0871(11) Uani 1 1 d . . . . .
H28A H -0.1221 -0.4847 -0.3891 0.131 Uiso 1 1 calc R U . . .
H28B H 0.0031 -0.5281 -0.4027 0.131 Uiso 1 1 calc R U . . .
H28C H 0.0421 -0.4612 -0.3746 0.131 Uiso 1 1 calc R U . . .
C31 C -0.4361(4) -0.62730(16) -0.43800(18) 0.0731(9) Uani 1 1 d . . . . .
H31A H -0.3444 -0.6185 -0.4526 0.088 Uiso 1 1 calc R U . . .
H31B H -0.5172 -0.6247 -0.4829 0.088 Uiso 1 1 calc R U . . .
C32 C -0.4290(6) -0.69077(18) -0.4064(3) 0.1096(15) Uani 1 1 d . . . . .
H32A H -0.5218 -0.7004 -0.3945 0.164 Uiso 1 1 calc R U . . .
H32B H -0.3501 -0.6932 -0.3613 0.164 Uiso 1 1 calc R U . . .
H32C H -0.4107 -0.7192 -0.4431 0.164 Uiso 1 1 calc R U . . .
C33 C -0.6117(3) -0.55987(16) -0.39153(17) 0.0664(8) Uani 1 1 d . . . . .
H33A H -0.6215 -0.5421 -0.3442 0.080 Uiso 1 1 calc R U . . .
H33B H -0.6791 -0.5943 -0.4028 0.080 Uiso 1 1 calc R U . . .
C34 C -0.6556(4) -0.5132(2) -0.4534(2) 0.1029(15) Uani 1 1 d . . . . .
H34A H -0.5888 -0.4791 -0.4427 0.154 Uiso 1 1 calc R U . . .
H34B H -0.7552 -0.4996 -0.4563 0.154 Uiso 1 1 calc R U . . .
H34C H -0.6507 -0.5311 -0.5008 0.154 Uiso 1 1 calc R U . . .
C41 C -0.0791(4) -0.37593(17) -0.1446(2) 0.0795(10) Uani 1 1 d . . . . .
H41 H -0.0796 -0.4163 -0.1676 0.095 Uiso 1 1 calc R U . . .
C42 C -0.0635(6) -0.3826(3) -0.0624(3) 0.1322(19) Uani 1 1 d . . . . .
H42A H -0.1485 -0.4038 -0.0537 0.198 Uiso 1 1 calc R U . . .
H42B H -0.0568 -0.3430 -0.0394 0.198 Uiso 1 1 calc R U . . .
H42C H 0.0249 -0.4054 -0.0407 0.198 Uiso 1 1 calc R U . . .
C43 C 0.0378(5) -0.3385(3) -0.1637(4) 0.144(2) Uani 1 1 d . . . . .
H43A H 0.0360 -0.2984 -0.1427 0.216 Uiso 1 1 calc R U . . .
H43B H 0.0210 -0.3356 -0.2176 0.216 Uiso 1 1 calc R U . . .
H43C H 0.1330 -0.3569 -0.1431 0.216 Uiso 1 1 calc R U . . .
C51 C -0.6007(3) -0.32718(15) -0.3115(2) 0.0722(9) Uani 1 1 d . U . . .
H51 H -0.6185 -0.3698 -0.3273 0.087 Uiso 1 1 calc R U . . .
C52 C -0.5872(6) -0.2902(3) -0.3764(3) 0.162(3) Uani 1 1 d . U . . .
H52A H -0.4968 -0.3005 -0.3903 0.243 Uiso 1 1 calc R U . . .
H52B H -0.5855 -0.2478 -0.3632 0.243 Uiso 1 1 calc R U . . .
H52C H -0.6705 -0.2980 -0.4183 0.243 Uiso 1 1 calc R U . . .
C53 C -0.7189(6) -0.3066(4) -0.2774(4) 0.177(3) Uani 1 1 d . U . . .
H53A H -0.7105 -0.2635 -0.2690 0.265 Uiso 1 1 calc R U . . .
H53B H -0.7105 -0.3272 -0.2300 0.265 Uiso 1 1 calc R U . . .
H53C H -0.8136 -0.3158 -0.3107 0.265 Uiso 1 1 calc R U . . .
Cl1 Cl -0.02124(11) -0.66742(5) -0.47684(7) 0.0928(3) Uani 1 1 d . . . . .
O1 O -0.0653(5) -0.6652(2) -0.4080(2) 0.1749(19) Uani 1 1 d . . . . .
O2 O 0.1268(4) -0.6625(3) -0.4625(4) 0.252(3) Uani 1 1 d . . . . .
O3 O -0.0602(5) -0.72347(18) -0.5102(3) 0.1618(17) Uani 1 1 d . . . . .
O4 O -0.1144(6) -0.6235(2) -0.5232(3) 0.1835(19) 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 2.2447(8) . ?
Ni1 S2 2.2159(8) . ?
Ni1 P1 2.8490(8) . ?
Ni1 C1 1.824(3) . ?
Ni1 C2 1.907(2) . ?
S1 P1 1.9949(11) . ?
S2 P1 1.9984(10) . ?
P1 O41 1.557(2) . ?
P1 O51 1.558(2) . ?
O41 C41 1.481(4) . ?
O51 C51 1.482(4) . ?
N1 C1 1.148(3) . ?
N1 C11 1.398(4) . ?
N2 H2 0.71(3) . ?
N2 C2 1.335(3) . ?
N2 C21 1.433(3) . ?
N3 C2 1.319(3) . ?
N3 C31 1.475(4) . ?
N3 C33 1.470(4) . ?
C11 C12 1.400(5) . ?
C11 C16 1.379(4) . ?
C12 C13 1.383(5) . ?
C12 C17 1.501(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.355(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.370(7) . ?
C15 H15 0.9300 . ?
C15 C16 1.399(5) . ?
C16 C18 1.502(6) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.398(4) . ?
C21 C26 1.389(4) . ?
C22 C23 1.402(5) . ?
C22 C27 1.487(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.374(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.356(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.388(5) . ?
C26 C28 1.505(5) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.503(5) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.505(5) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C41 H41 0.9800 . ?
C41 C42 1.478(6) . ?
C41 C43 1.467(6) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C51 H51 0.9800 . ?
C51 C52 1.466(6) . ?
C51 C53 1.456(6) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
Cl1 O1 1.412(4) . ?
Cl1 O2 1.337(4) . ?
Cl1 O3 1.381(4) . ?
Cl1 O4 1.427(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 44.16(3) . . ?
S2 Ni1 S1 88.40(3) . . ?
S2 Ni1 P1 44.32(2) . . ?
C1 Ni1 S1 88.55(8) . . ?
C1 Ni1 S2 174.95(8) . . ?
C1 Ni1 P1 132.70(8) . . ?
C1 Ni1 C2 92.55(11) . . ?
C2 Ni1 S1 178.30(8) . . ?
C2 Ni1 S2 90.42(8) . . ?
C2 Ni1 P1 134.71(8) . . ?
P1 S1 Ni1 84.22(3) . . ?
P1 S2 Ni1 84.90(3) . . ?
S1 P1 Ni1 51.62(3) . . ?
S1 P1 S2 102.29(4) . . ?
S2 P1 Ni1 50.78(3) . . ?
O41 P1 Ni1 128.14(9) . . ?
O41 P1 S1 113.66(10) . . ?
O41 P1 S2 114.78(9) . . ?
O41 P1 O51 97.53(11) . . ?
O51 P1 Ni1 134.34(9) . . ?
O51 P1 S1 114.72(10) . . ?
O51 P1 S2 114.54(10) . . ?
C41 O41 P1 121.8(2) . . ?
C51 O51 P1 122.19(18) . . ?
C1 N1 C11 175.3(3) . . ?
C2 N2 H2 121(3) . . ?
C2 N2 C21 124.2(2) . . ?
C21 N2 H2 115(3) . . ?
C2 N3 C31 122.9(2) . . ?
C2 N3 C33 121.2(2) . . ?
C33 N3 C31 115.9(2) . . ?
N1 C1 Ni1 174.7(2) . . ?
N2 C2 Ni1 120.44(19) . . ?
N3 C2 Ni1 120.02(19) . . ?
N3 C2 N2 119.5(2) . . ?
N1 C11 C12 117.0(3) . . ?
C16 C11 N1 118.0(3) . . ?
C16 C11 C12 125.0(3) . . ?
C11 C12 C17 121.9(3) . . ?
C13 C12 C11 116.0(4) . . ?
C13 C12 C17 122.1(4) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 121.0(4) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.2 . . ?
C13 C14 C15 121.6(4) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 120.9(4) . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 115.5(4) . . ?
C11 C16 C18 121.8(3) . . ?
C15 C16 C18 122.7(4) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C21 N2 119.4(3) . . ?
C26 C21 N2 118.1(3) . . ?
C26 C21 C22 122.4(3) . . ?
C21 C22 C23 116.4(3) . . ?
C21 C22 C27 122.7(3) . . ?
C23 C22 C27 120.7(3) . . ?
C22 C23 H23 119.3 . . ?
C24 C23 C22 121.4(3) . . ?
C24 C23 H23 119.3 . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.4(3) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.4 . . ?
C24 C25 C26 121.1(3) . . ?
C26 C25 H25 119.4 . . ?
C21 C26 C28 121.8(3) . . ?
C25 C26 C21 118.0(3) . . ?
C25 C26 C28 120.2(3) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C31 H31A 109.3 . . ?
N3 C31 H31B 109.3 . . ?
N3 C31 C32 111.5(3) . . ?
H31A C31 H31B 108.0 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.1 . . ?
N3 C33 H33B 109.1 . . ?
N3 C33 C34 112.5(3) . . ?
H33A C33 H33B 107.8 . . ?
C34 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O41 C41 H41 109.4 . . ?
C42 C41 O41 108.6(3) . . ?
C42 C41 H41 109.4 . . ?
C43 C41 O41 106.3(3) . . ?
C43 C41 H41 109.4 . . ?
C43 C41 C42 113.6(4) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O51 C51 H51 109.3 . . ?
C52 C51 O51 108.0(3) . . ?
C52 C51 H51 109.3 . . ?
C53 C51 O51 107.7(4) . . ?
C53 C51 H51 109.3 . . ?
C53 C51 C52 113.2(5) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O1 Cl1 O4 103.8(3) . . ?
O2 Cl1 O1 109.1(3) . . ?
O2 Cl1 O3 107.7(3) . . ?
O2 Cl1 O4 120.4(4) . . ?
O3 Cl1 O1 108.7(3) . . ?
O3 Cl1 O4 106.6(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 P1 O41 C41 7.5(3) . . . . ?
Ni1 P1 O51 C51 -8.5(3) . . . . ?
S1 P1 O41 C41 66.4(3) . . . . ?
S1 P1 O51 C51 -68.1(2) . . . . ?
S2 P1 O41 C41 -50.9(3) . . . . ?
S2 P1 O51 C51 49.8(3) . . . . ?
P1 O41 C41 C42 -106.7(4) . . . . ?
P1 O41 C41 C43 130.8(4) . . . . ?
P1 O51 C51 C52 -116.8(4) . . . . ?
P1 O51 C51 C53 120.7(4) . . . . ?
O41 P1 O51 C51 171.5(2) . . . . ?
O51 P1 O41 C41 -172.4(2) . . . . ?
N1 C11 C12 C13 178.9(3) . . . . ?
N1 C11 C12 C17 -1.0(5) . . . . ?
N1 C11 C16 C15 -179.3(3) . . . . ?
N1 C11 C16 C18 0.4(4) . . . . ?
N2 C21 C22 C23 -179.1(3) . . . . ?
N2 C21 C22 C27 5.5(4) . . . . ?
N2 C21 C26 C25 -179.9(3) . . . . ?
N2 C21 C26 C28 -1.1(4) . . . . ?
C2 N2 C21 C22 80.5(4) . . . . ?
C2 N2 C21 C26 -103.5(3) . . . . ?
C2 N3 C31 C32 79.9(4) . . . . ?
C2 N3 C33 C34 102.1(3) . . . . ?
C11 C12 C13 C14 0.7(5) . . . . ?
C12 C11 C16 C15 0.0(5) . . . . ?
C12 C11 C16 C18 179.7(3) . . . . ?
C12 C13 C14 C15 -0.6(7) . . . . ?
C13 C14 C15 C16 0.2(7) . . . . ?
C14 C15 C16 C11 0.1(5) . . . . ?
C14 C15 C16 C18 -179.6(4) . . . . ?
C16 C11 C12 C13 -0.4(5) . . . . ?
C16 C11 C12 C17 179.7(3) . . . . ?
C17 C12 C13 C14 -179.4(4) . . . . ?
C21 N2 C2 Ni1 -5.3(4) . . . . ?
C21 N2 C2 N3 176.0(3) . . . . ?
C21 C22 C23 C24 -2.3(5) . . . . ?
C22 C21 C26 C25 -3.9(4) . . . . ?
C22 C21 C26 C28 174.9(3) . . . . ?
C22 C23 C24 C25 -1.5(6) . . . . ?
C23 C24 C25 C26 2.6(6) . . . . ?
C24 C25 C26 C21 0.0(5) . . . . ?
C24 C25 C26 C28 -178.9(3) . . . . ?
C26 C21 C22 C23 5.0(4) . . . . ?
C26 C21 C22 C27 -170.5(3) . . . . ?
C27 C22 C23 C24 173.3(3) . . . . ?
C31 N3 C2 Ni1 -175.1(2) . . . . ?
C31 N3 C2 N2 3.6(4) . . . . ?
C31 N3 C33 C34 -78.8(4) . . . . ?
C33 N3 C2 Ni1 3.9(4) . . . . ?
C33 N3 C2 N2 -177.4(3) . . . . ?
C33 N3 C31 C32 -99.2(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 49.7 0.2 ?
2 0.086 0.147 0.873 14.4 0.1 ?
3 0.086 0.353 0.373 14.4 0.1 ?
4 0.000 0.500 1.000 49.7 0.2 ?
5 -0.086 0.647 0.627 14.4 0.1 ?
6 -0.086 0.853 0.127 14.4 0.1 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.291
_oxdiff_exptl_absorpt_empirical_full_min 0.734
####################################################################### 
# 
# 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_m089pa
_database_code_depnum_ccdc_archive 'CCDC 2299289'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2023-10-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2023-10-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H39 N3 Ni O2 P S2, Cl O4'
_chemical_formula_sum            'C27 H39 Cl N3 Ni O6 P S2'
_chemical_formula_weight         690.86
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C108  H156  Cl4  N12  Ni4  O24  P4  S8  '
_chemical_oxdiff_usercomment     orange
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   12.5858(5)
_cell_length_b                   19.6057(7)
_cell_length_c                   14.6622(5)
_cell_angle_alpha                90
_cell_angle_beta                 112.736(4)
_cell_angle_gamma                90
_cell_volume                     3336.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5066
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.3050
_cell_measurement_theta_min      2.5660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1448
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0633
7 21 -12 0.0574
9 -17 -15 0.0953
2 -27 -5 0.0955
2 27 -1 0.1007
-11 0 20 0.1635
2 1 -2 0.0057
1 0 0 0.0856

_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.149
loop_
_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
-1.0005 0.0014 0.0008 -0.0167 0.0559 -0.0181
7.1652 21.4419 -12.4661 -0.5673 -0.1062 0.8166
9.2023 -17.3753 -15.1931 0.8017 0.1477 0.5792
1.5302 -26.7744 -5.1261 0.9582 0.2837 -0.0371
2.2191 27.4146 -1.4078 -0.8938 -0.2652 0.3616
-11.2722 -0.2269 19.7985 -0.2520 -0.0732 -0.9649
2.0001 0.9990 -2.0014 0.0065 -0.0476 0.1226
1.0005 -0.0014 -0.0008 0.0167 -0.0559 0.0181

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17397
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.677
_diffrn_reflns_theta_min         2.077
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  13.00   1.00   13.26    --  -10.64 -99.00  60.00   33
  2  ω     -6.00  67.00   1.00   13.26    --   12.51  37.00 -30.00   73
  3  ω    -41.00  45.00   1.00   13.26    --   12.51 -19.00 -30.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0166316000
_diffrn_orient_matrix_UB_12      -0.0341377000
_diffrn_orient_matrix_UB_13      -0.0036511000
_diffrn_orient_matrix_UB_21      -0.0559523000
_diffrn_orient_matrix_UB_22      -0.0069729000
_diffrn_orient_matrix_UB_23      -0.0356338000
_diffrn_orient_matrix_UB_31      0.0181017000
_diffrn_orient_matrix_UB_32      0.0097579000
_diffrn_orient_matrix_UB_33      -0.0383207000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4455
_reflns_number_total             7911
_reflns_odcompleteness_completeness 99.86
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7911
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0793
_refine_ls_restrained_S_all      1.040
_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)+(0.1104P)²+4.1394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2087
_refine_ls_wR_factor_ref         0.2560
_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. Restrained distances
 C6-C7
 1.476 with sigma of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.33704(6) 0.53981(3) 0.21243(4) 0.0612(2) Uani 1 1 d . . . . .
S1 S 0.17509(15) 0.50315(10) 0.09604(12) 0.0898(5) Uani 1 1 d . . . . .
S2 S 0.43158(17) 0.45101(9) 0.17939(14) 0.0941(5) Uani 1 1 d . . . . .
P1 P 0.27853(18) 0.43060(9) 0.07846(12) 0.0885(5) Uani 1 1 d . . . . .
O1 O 0.2476(5) 0.3554(2) 0.0947(3) 0.1053(15) Uani 1 1 d . . . . .
O2 O 0.2714(5) 0.4277(2) -0.0313(3) 0.1183(19) Uani 1 1 d . . . . .
N1 N 0.5346(4) 0.5716(2) 0.3983(3) 0.0678(11) Uani 1 1 d . . . . .
N2 N 0.2772(5) 0.6772(2) 0.1825(4) 0.0696(12) Uani 1 1 d . . . . .
H2 H 0.245(6) 0.706(3) 0.177(5) 0.083 Uiso 1 1 d . U . . .
N3 N 0.2105(4) 0.6259(2) 0.2905(3) 0.0693(11) Uani 1 1 d . . . . .
C1 C 0.4610(5) 0.5603(3) 0.3242(4) 0.0649(13) Uani 1 1 d . . . . .
C2 C 0.2657(4) 0.6222(3) 0.2294(3) 0.0591(11) Uani 1 1 d . . . . .
C4 C 0.1533(8) 0.3228(6) 0.0337(6) 0.154(4) Uani 1 1 d . . . . .
H4A H 0.1554 0.3208 -0.0317 0.185 Uiso 1 1 calc R U . . .
H4B H 0.0858 0.3489 0.0288 0.185 Uiso 1 1 calc R U . . .
C5 C 0.1423(8) 0.2552(5) 0.0649(8) 0.150(4) Uani 1 1 d . . . . .
H5A H 0.0652 0.2391 0.0294 0.225 Uiso 1 1 calc R U . . .
H5B H 0.1586 0.2552 0.1345 0.225 Uiso 1 1 calc R U . . .
H5C H 0.1958 0.2257 0.0519 0.225 Uiso 1 1 calc R U . . .
C6 C 0.2946(14) 0.4897(5) -0.0725(7) 0.193(6) Uani 1 1 d D . . . .
H6A H 0.3633 0.5111 -0.0252 0.231 Uiso 1 1 calc R U . . .
H6B H 0.2308 0.5211 -0.0859 0.231 Uiso 1 1 calc R U . . .
C7 C 0.3111(12) 0.4759(6) -0.1638(8) 0.189(5) Uani 1 1 d D . . . .
H7A H 0.3683 0.4410 -0.1522 0.283 Uiso 1 1 calc R U . . .
H7B H 0.3363 0.5168 -0.1856 0.283 Uiso 1 1 calc R U . . .
H7C H 0.2397 0.4610 -0.2137 0.283 Uiso 1 1 calc R U . . .
C11 C 0.6206(4) 0.5913(3) 0.4877(3) 0.0633(12) Uani 1 1 d . . . . .
C12 C 0.7357(5) 0.5851(3) 0.4976(5) 0.0815(16) Uani 1 1 d . . . . .
C13 C 0.8184(6) 0.6068(4) 0.5871(5) 0.0915(19) Uani 1 1 d . . . . .
H13 H 0.8959 0.6045 0.5972 0.110 Uiso 1 1 calc R U . . .
C14 C 0.7876(7) 0.6313(4) 0.6598(5) 0.100(2) Uani 1 1 d . . . . .
H14 H 0.8448 0.6454 0.7190 0.121 Uiso 1 1 calc R U . . .
C15 C 0.6757(6) 0.6359(4) 0.6485(4) 0.0894(19) Uani 1 1 d . . . . .
H15 H 0.6575 0.6527 0.6999 0.107 Uiso 1 1 calc R U . . .
C16 C 0.5886(5) 0.6159(3) 0.5614(4) 0.0722(14) Uani 1 1 d . . . . .
C17 C 0.7651(7) 0.5579(4) 0.4141(6) 0.116(3) Uani 1 1 d . . . . .
H17A H 0.8465 0.5499 0.4373 0.174 Uiso 1 1 calc R U . . .
H17B H 0.7429 0.5906 0.3613 0.174 Uiso 1 1 calc R U . . .
H17C H 0.7245 0.5159 0.3904 0.174 Uiso 1 1 calc R U . . .
C18 C 0.4644(5) 0.6212(4) 0.5480(5) 0.0930(19) Uani 1 1 d . . . . .
H18A H 0.4264 0.6544 0.4979 0.139 Uiso 1 1 calc R U . . .
H18B H 0.4597 0.6348 0.6092 0.139 Uiso 1 1 calc R U . . .
H18C H 0.4277 0.5777 0.5282 0.139 Uiso 1 1 calc R U . . .
C21 C 0.3484(5) 0.6798(3) 0.1251(4) 0.0679(13) Uani 1 1 d . . . . .
C22 C 0.2949(6) 0.6698(3) 0.0228(4) 0.0810(16) Uani 1 1 d . . . . .
C23 C 0.3656(8) 0.6703(3) -0.0305(5) 0.100(2) Uani 1 1 d . . . . .
H23 H 0.3336 0.6632 -0.0985 0.119 Uiso 1 1 calc R U . . .
C24 C 0.4811(9) 0.6812(4) 0.0156(7) 0.112(3) Uani 1 1 d . . . . .
H24 H 0.5278 0.6789 -0.0204 0.135 Uiso 1 1 calc R U . . .
C25 C 0.5288(6) 0.6953(4) 0.1143(7) 0.107(2) Uani 1 1 d . . . . .
H25 H 0.6073 0.7043 0.1441 0.128 Uiso 1 1 calc R U . . .
C26 C 0.4628(5) 0.6968(3) 0.1713(5) 0.0832(17) Uani 1 1 d . . . . .
C27 C 0.1678(6) 0.6620(4) -0.0283(5) 0.106(2) Uani 1 1 d . . . . .
H27A H 0.1418 0.6262 0.0027 0.160 Uiso 1 1 calc R U . . .
H27B H 0.1488 0.6508 -0.0966 0.160 Uiso 1 1 calc R U . . .
H27C H 0.1307 0.7040 -0.0240 0.160 Uiso 1 1 calc R U . . .
C28 C 0.5135(7) 0.7207(4) 0.2778(5) 0.110(2) Uani 1 1 d . . . . .
H28A H 0.5305 0.7686 0.2797 0.165 Uiso 1 1 calc R U . . .
H28B H 0.5831 0.6960 0.3132 0.165 Uiso 1 1 calc R U . . .
H28C H 0.4591 0.7129 0.3080 0.165 Uiso 1 1 calc R U . . .
C31 C 0.1621(5) 0.6892(3) 0.3131(5) 0.0816(16) Uani 1 1 d . . . . .
H31A H 0.1899 0.7282 0.2880 0.098 Uiso 1 1 calc R U . . .
H31B H 0.1871 0.6943 0.3842 0.098 Uiso 1 1 calc R U . . .
C32 C 0.0321(6) 0.6870(4) 0.2663(5) 0.103(2) Uani 1 1 d . . . . .
H32A H 0.0068 0.6856 0.1949 0.124 Uiso 1 1 calc R U . . .
H32B H 0.0006 0.7277 0.2838 0.124 Uiso 1 1 calc R U . . .
C33 C -0.0112(6) 0.6240(4) 0.3021(6) 0.109(2) Uani 1 1 d . . . . .
H33A H -0.0940 0.6204 0.2670 0.131 Uiso 1 1 calc R U . . .
H33B H 0.0047 0.6288 0.3720 0.131 Uiso 1 1 calc R U . . .
C34 C 0.0465(6) 0.5582(4) 0.2855(6) 0.100(2) Uani 1 1 d . . . . .
H34A H 0.0241 0.5199 0.3159 0.120 Uiso 1 1 calc R U . . .
H34B H 0.0209 0.5492 0.2152 0.120 Uiso 1 1 calc R U . . .
C35 C 0.1762(5) 0.5657(3) 0.3299(4) 0.0774(15) Uani 1 1 d . . . . .
H35A H 0.2027 0.5695 0.4012 0.093 Uiso 1 1 calc R U . . .
H35B H 0.2114 0.5256 0.3148 0.093 Uiso 1 1 calc R U . . .
Cl1 Cl 0.16802(15) 0.85835(9) 0.13806(12) 0.0844(4) Uani 1 1 d . . . . .
O3 O 0.1191(8) 0.8991(7) 0.1787(11) 0.286(7) Uani 1 1 d . . . . .
O4 O 0.1567(19) 0.8870(8) 0.0613(7) 0.407(13) Uani 1 1 d . . . . .
O5 O 0.2782(6) 0.8467(6) 0.2027(7) 0.217(4) Uani 1 1 d . . . . .
O6 O 0.1109(7) 0.7981(4) 0.1150(8) 0.225(5) 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 2.2124(17) . ?
Ni1 S2 2.2643(18) . ?
Ni1 P1 2.8048(17) . ?
Ni1 C1 1.818(6) . ?
Ni1 C2 1.910(5) . ?
S1 P1 2.011(3) . ?
S2 P1 1.964(3) . ?
P1 O1 1.567(5) . ?
P1 O2 1.577(4) . ?
O1 C4 1.340(9) . ?
O2 C6 1.438(10) . ?
N1 C1 1.145(7) . ?
N1 C11 1.393(7) . ?
N2 H2 0.68(6) . ?
N2 C2 1.317(6) . ?
N2 C21 1.446(7) . ?
N3 C2 1.331(6) . ?
N3 C31 1.475(7) . ?
N3 C35 1.451(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.427(12) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.457(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C11 C12 1.405(8) . ?
C11 C16 1.378(7) . ?
C12 C13 1.389(9) . ?
C12 C17 1.507(9) . ?
C13 H13 0.9300 . ?
C13 C14 1.355(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.356(10) . ?
C15 H15 0.9300 . ?
C15 C16 1.380(8) . ?
C16 C18 1.501(8) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C21 C22 1.401(8) . ?
C21 C26 1.375(8) . ?
C22 C23 1.394(9) . ?
C22 C27 1.489(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.362(11) . ?
C24 H24 0.9300 . ?
C24 C25 1.363(12) . ?
C25 H25 0.9300 . ?
C25 C26 1.388(9) . ?
C26 C28 1.516(10) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.510(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.523(10) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.545(10) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 C35 1.512(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
Cl1 O3 1.287(9) . ?
Cl1 O4 1.216(8) . ?
Cl1 O5 1.363(7) . ?
Cl1 O6 1.356(8) . ?

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 S2 89.36(7) . . ?
S1 Ni1 P1 45.38(7) . . ?
S2 Ni1 P1 44.00(7) . . ?
C1 Ni1 S1 168.82(17) . . ?
C1 Ni1 S2 91.39(17) . . ?
C1 Ni1 P1 134.58(17) . . ?
C1 Ni1 C2 88.7(2) . . ?
C2 Ni1 S1 92.06(15) . . ?
C2 Ni1 S2 171.98(15) . . ?
C2 Ni1 P1 136.66(15) . . ?
P1 S1 Ni1 83.08(8) . . ?
P1 S2 Ni1 82.78(9) . . ?
S1 P1 Ni1 51.54(6) . . ?
S2 P1 Ni1 53.22(6) . . ?
S2 P1 S1 104.73(10) . . ?
O1 P1 Ni1 128.75(18) . . ?
O1 P1 S1 115.8(2) . . ?
O1 P1 S2 107.8(2) . . ?
O1 P1 O2 101.6(2) . . ?
O2 P1 Ni1 129.61(19) . . ?
O2 P1 S1 111.8(3) . . ?
O2 P1 S2 115.4(2) . . ?
C4 O1 P1 123.7(6) . . ?
C6 O2 P1 117.3(5) . . ?
C1 N1 C11 174.9(5) . . ?
C2 N2 H2 123(6) . . ?
C2 N2 C21 123.4(4) . . ?
C21 N2 H2 113(6) . . ?
C2 N3 C31 124.5(5) . . ?
C2 N3 C35 122.4(5) . . ?
C35 N3 C31 112.5(4) . . ?
N1 C1 Ni1 175.1(5) . . ?
N2 C2 Ni1 118.2(4) . . ?
N2 C2 N3 119.9(5) . . ?
N3 C2 Ni1 121.9(4) . . ?
O1 C4 H4A 108.9 . . ?
O1 C4 H4B 108.9 . . ?
O1 C4 C5 113.5(8) . . ?
H4A C4 H4B 107.7 . . ?
C5 C4 H4A 108.9 . . ?
C5 C4 H4B 108.9 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 C6 H6A 109.5 . . ?
O2 C6 H6B 109.5 . . ?
O2 C6 C7 110.7(7) . . ?
H6A C6 H6B 108.1 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C11 C12 117.9(5) . . ?
C16 C11 N1 118.6(5) . . ?
C16 C11 C12 123.5(5) . . ?
C11 C12 C17 120.9(6) . . ?
C13 C12 C11 115.9(6) . . ?
C13 C12 C17 123.1(6) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 120.9(6) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 119.1 . . ?
C13 C14 C15 121.8(6) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.7(6) . . ?
C16 C15 H15 119.6 . . ?
C11 C16 C15 117.2(5) . . ?
C11 C16 C18 121.7(5) . . ?
C15 C16 C18 121.1(6) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C22 C21 N2 117.9(5) . . ?
C26 C21 N2 119.2(5) . . ?
C26 C21 C22 122.7(5) . . ?
C21 C22 C27 122.1(6) . . ?
C23 C22 C21 116.9(7) . . ?
C23 C22 C27 120.9(6) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.8(7) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.4(7) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 119.2 . . ?
C24 C25 C26 121.5(7) . . ?
C26 C25 H25 119.2 . . ?
C21 C26 C25 117.1(7) . . ?
C21 C26 C28 121.8(6) . . ?
C25 C26 C28 121.0(7) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C31 H31A 109.7 . . ?
N3 C31 H31B 109.7 . . ?
N3 C31 C32 110.0(5) . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
C31 C32 H32A 109.7 . . ?
C31 C32 H32B 109.7 . . ?
C31 C32 C33 109.7(6) . . ?
H32A C32 H32B 108.2 . . ?
C33 C32 H32A 109.7 . . ?
C33 C32 H32B 109.7 . . ?
C32 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
C32 C33 C34 111.6(6) . . ?
H33A C33 H33B 108.0 . . ?
C34 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C33 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
C35 C34 C33 110.3(6) . . ?
C35 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
N3 C35 C34 110.2(5) . . ?
N3 C35 H35A 109.6 . . ?
N3 C35 H35B 109.6 . . ?
C34 C35 H35A 109.6 . . ?
C34 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
O3 Cl1 O5 108.8(6) . . ?
O3 Cl1 O6 110.7(7) . . ?
O4 Cl1 O3 103.7(12) . . ?
O4 Cl1 O5 116.4(12) . . ?
O4 Cl1 O6 108.1(8) . . ?
O6 Cl1 O5 109.1(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 P1 O1 C4 129.0(7) . . . . ?
Ni1 P1 O2 C6 -1.9(10) . . . . ?
S1 P1 O1 C4 68.9(8) . . . . ?
S1 P1 O2 C6 55.5(9) . . . . ?
S2 P1 O1 C4 -174.2(7) . . . . ?
S2 P1 O2 C6 -64.0(9) . . . . ?
P1 O1 C4 C5 -178.7(8) . . . . ?
P1 O2 C6 C7 166.8(9) . . . . ?
O1 P1 O2 C6 179.6(8) . . . . ?
O2 P1 O1 C4 -52.5(8) . . . . ?
N1 C11 C12 C13 178.5(5) . . . . ?
N1 C11 C12 C17 0.0(9) . . . . ?
N1 C11 C16 C15 -179.1(5) . . . . ?
N1 C11 C16 C18 0.6(8) . . . . ?
N2 C21 C22 C23 -178.0(5) . . . . ?
N2 C21 C22 C27 4.7(8) . . . . ?
N2 C21 C26 C25 177.0(5) . . . . ?
N2 C21 C26 C28 -7.2(8) . . . . ?
N3 C31 C32 C33 56.8(7) . . . . ?
C2 N2 C21 C22 96.5(7) . . . . ?
C2 N2 C21 C26 -88.3(7) . . . . ?
C2 N3 C31 C32 109.2(6) . . . . ?
C2 N3 C35 C34 -110.5(6) . . . . ?
C11 C12 C13 C14 1.1(10) . . . . ?
C12 C11 C16 C15 0.8(9) . . . . ?
C12 C11 C16 C18 -179.4(6) . . . . ?
C12 C13 C14 C15 -0.2(11) . . . . ?
C13 C14 C15 C16 -0.4(11) . . . . ?
C14 C15 C16 C11 0.1(10) . . . . ?
C14 C15 C16 C18 -179.7(7) . . . . ?
C16 C11 C12 C13 -1.4(9) . . . . ?
C16 C11 C12 C17 -179.9(6) . . . . ?
C17 C12 C13 C14 179.5(7) . . . . ?
C21 N2 C2 Ni1 -5.0(7) . . . . ?
C21 N2 C2 N3 171.7(5) . . . . ?
C21 C22 C23 C24 -1.0(10) . . . . ?
C22 C21 C26 C25 -8.1(9) . . . . ?
C22 C21 C26 C28 167.8(6) . . . . ?
C22 C23 C24 C25 -3.5(11) . . . . ?
C23 C24 C25 C26 2.4(12) . . . . ?
C24 C25 C26 C21 3.3(10) . . . . ?
C24 C25 C26 C28 -172.6(7) . . . . ?
C26 C21 C22 C23 6.9(9) . . . . ?
C26 C21 C22 C27 -170.4(6) . . . . ?
C27 C22 C23 C24 176.4(7) . . . . ?
C31 N3 C2 Ni1 174.7(4) . . . . ?
C31 N3 C2 N2 -1.9(8) . . . . ?
C31 N3 C35 C34 60.7(7) . . . . ?
C31 C32 C33 C34 -53.5(8) . . . . ?
C32 C33 C34 C35 52.6(8) . . . . ?
C33 C34 C35 N3 -55.0(7) . . . . ?
C35 N3 C2 Ni1 -15.2(7) . . . . ?
C35 N3 C2 N2 168.3(5) . . . . ?
C35 N3 C31 C32 -61.8(7) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.005 0.073 0.676 9.9 0.0 ?
2 0.005 0.427 0.176 9.9 0.0 ?
3 -0.005 0.573 0.824 9.9 0.0 ?
4 -0.005 0.927 0.324 9.9 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.795
####################################################################### 
# 
# 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_dm857c
_database_code_depnum_ccdc_archive 'CCDC 2300163'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2024-04-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2024-04-03
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C80 H122 N6 Ni2 O4 P2 S4, 2(B F4)'
_chemical_formula_sum            'C80 H122 B2 F8 N6 Ni2 O4 P2 S4'
_chemical_formula_weight         1713.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C106  H132  B2  O4  F8  P2  S4  Ni2  N1  '
_chemical_oxdiff_usercomment     'yellow chunk'
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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                   13.0354(7)
_cell_length_b                   13.3201(7)
_cell_length_c                   14.2399(5)
_cell_angle_alpha                90.782(4)
_cell_angle_beta                 106.703(4)
_cell_angle_gamma                96.437(5)
_cell_volume                     2350.5(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5736
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1400
_cell_measurement_theta_min      2.4910
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.585
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             908
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-18 7 7 0.0739
2 1 18 0.0947
-2 -2 -18 0.0555
7 16 0 0.0984
-8 -13 14 0.0589
18 -3 -1 0.1014

_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.155
loop_
_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
-17.7549 6.6153 6.8794 0.7909 -0.6069 0.0777
1.8176 1.1992 18.4169 -0.3984 -0.4183 0.8163
-2.2050 -2.1717 -18.0912 0.4308 0.4525 -0.7808
6.8699 16.3128 -0.2514 -0.6428 -0.6778 -0.3568
-7.5437 -12.6963 13.6220 0.4221 0.2304 0.8768
17.7003 -3.4553 -0.5328 -0.9336 0.3310 0.1370

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22453
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.565
_diffrn_reflns_theta_min         2.094
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00 -12.00   1.00   12.18    --  -10.48 -37.00   0.00   73
  2  ω    -19.00  35.00   1.00   12.18    --  -10.48  39.00 129.00   54
  3  ω    -13.00  29.00   1.00   12.18    --  -10.48 -99.00  30.00   42
  4  ω    -65.00   4.00   1.00   12.18    --  -10.48 -37.00 -90.00   69
  5  ω    -38.00  23.00   1.00   12.18    --  -10.48  57.00-180.00   61
  6  ω     44.00  96.00   1.00   12.18    --   12.36 178.00 -30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0563085000
_diffrn_orient_matrix_UB_12      -0.0159239000
_diffrn_orient_matrix_UB_13      -0.0150406000
_diffrn_orient_matrix_UB_21      0.0091513000
_diffrn_orient_matrix_UB_22      -0.0457246000
_diffrn_orient_matrix_UB_23      -0.0206384000
_diffrn_orient_matrix_UB_31      0.0045951000
_diffrn_orient_matrix_UB_32      -0.0231099000
_diffrn_orient_matrix_UB_33      0.0453723000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6016
_reflns_number_total             11134
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         11134
_refine_ls_number_restraints     243
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0939
_refine_ls_restrained_S_all      1.063
_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)+(0.1724P)²+1.0602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2553
_refine_ls_wR_factor_ref         0.3134
_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. Rigid bond restraints
 C51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61, C62, C63, C64, C65, C66
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 2A
C51 \\sim O1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C27) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C51) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C28, C48, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C55, C54, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C61, C66, C62
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C46, C27, C45
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C51, O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Ternary CH refined with riding coordinates:
 C17(H17), C18(H18), C27(H27), C28(H28), C51(H51), C61(H61)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C56(H56A,H56B), C62(H62A,H62B), C63(H63A,H63B),
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25)
5.d Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.29707(5) 0.32929(4) 0.28461(4) 0.0523(2) Uani 1 1 d . . . . .
S1 S 0.18151(11) 0.33394(13) 0.13498(9) 0.0704(4) Uani 1 1 d . . . . .
S2 S 0.16463(14) 0.34717(14) 0.34783(11) 0.0808(5) Uani 1 1 d . . . . .
P1 P 0.07440(11) 0.34583(11) 0.20797(11) 0.0672(4) Uani 1 1 d . . . . .
O1 O -0.0235(4) 0.2603(4) 0.1807(4) 0.1032(14) Uani 1 1 d . U . . .
O2 O 0.0091(3) 0.4370(3) 0.1838(3) 0.0861(12) Uani 1 1 d . . . . .
N1 N 0.4027(4) 0.2457(3) 0.4637(3) 0.0613(10) Uani 1 1 d . . . . .
H1 H 0.4495 0.2486 0.5205 0.074 Uiso 1 1 calc R U . . .
N2 N 0.4796(4) 0.3386(4) 0.1981(3) 0.0688(11) Uani 1 1 d . . . . .
N3 N 0.4654(5) 0.4095(3) 0.4455(3) 0.0907(18) Uani 1 1 d . . . . .
C1 C 0.3965(4) 0.3277(3) 0.4123(3) 0.0608(12) Uani 1 1 d . . . . .
C2 C 0.4084(4) 0.3306(4) 0.2304(4) 0.0595(12) Uani 1 1 d . . . . .
C11 C 0.3345(4) 0.1509(3) 0.4290(3) 0.0583(12) Uani 1 1 d . . . . .
C12 C 0.3615(5) 0.0884(4) 0.3630(4) 0.0726(15) Uani 1 1 d . . . . .
C13 C 0.2934(9) -0.0033(5) 0.3326(6) 0.109(3) Uani 1 1 d . . . . .
H13 H 0.3063 -0.0472 0.2871 0.131 Uiso 1 1 calc R U . . .
C14 C 0.2100(9) -0.0276(6) 0.3690(8) 0.135(4) Uani 1 1 d . . . . .
H14 H 0.1645 -0.0873 0.3465 0.162 Uiso 1 1 calc R U . . .
C15 C 0.1908(7) 0.0321(6) 0.4370(7) 0.114(3) Uani 1 1 d . . . . .
H15 H 0.1351 0.0104 0.4633 0.137 Uiso 1 1 calc R U . . .
C16 C 0.2504(5) 0.1238(4) 0.4690(5) 0.0773(16) Uani 1 1 d . . . . .
C17 C 0.4621(7) 0.1123(5) 0.3311(5) 0.097(2) Uani 1 1 d . . . . .
H17 H 0.4825 0.1857 0.3387 0.116 Uiso 1 1 calc R U . . .
C18 C 0.2299(7) 0.1877(6) 0.5480(5) 0.102(2) Uani 1 1 d . . . . .
H18 H 0.2630 0.2568 0.5448 0.122 Uiso 1 1 calc R U . . .
C21 C 0.5630(5) 0.3466(4) 0.1534(4) 0.0710(14) Uani 1 1 d . . . . .
C22 C 0.6666(5) 0.3734(5) 0.2135(4) 0.0756(15) Uani 1 1 d . U . . .
C23 C 0.7462(6) 0.3810(6) 0.1681(6) 0.102(2) Uani 1 1 d . . . . .
H23 H 0.8174 0.3998 0.2051 0.122 Uiso 1 1 calc R U . . .
C24 C 0.7233(7) 0.3614(7) 0.0698(7) 0.112(3) Uani 1 1 d . . . . .
H24 H 0.7790 0.3662 0.0408 0.134 Uiso 1 1 calc R U . . .
C25 C 0.6202(7) 0.3352(7) 0.0136(6) 0.112(3) Uani 1 1 d . . . . .
H25 H 0.6065 0.3241 -0.0537 0.135 Uiso 1 1 calc R U . . .
C26 C 0.5351(6) 0.3243(6) 0.0535(5) 0.094(2) Uani 1 1 d . . . . .
C27 C 0.6935(6) 0.3978(6) 0.3221(5) 0.0942(19) Uani 1 1 d . U . . .
H27 H 0.6255 0.3883 0.3392 0.113 Uiso 1 1 calc R U . . .
C28 C 0.4214(8) 0.2913(9) -0.0068(6) 0.133(3) Uani 1 1 d . U . . .
H28 H 0.3768 0.2830 0.0381 0.159 Uiso 1 1 calc R U . . .
C31 C 0.4505(6) 0.5084(4) 0.3990(4) 0.096(2) Uani 1 1 d . . . . .
H31A H 0.5123 0.5312 0.3765 0.115 Uiso 1 1 calc R U . . .
H31B H 0.3867 0.5006 0.3426 0.115 Uiso 1 1 calc R U . . .
C32 C 0.4393(6) 0.5790(5) 0.4662(5) 0.0900(19) Uani 1 1 d . . . . .
H32A H 0.3748 0.5579 0.4853 0.108 Uiso 1 1 calc R U . . .
H32B H 0.4312 0.6436 0.4361 0.108 Uiso 1 1 calc R U . . .
C41 C 0.4446(12) 0.0794(7) 0.2226(7) 0.168(5) Uani 1 1 d . . . . .
H41A H 0.4188 0.0086 0.2123 0.252 Uiso 1 1 calc R U . . .
H41B H 0.5116 0.0919 0.2070 0.252 Uiso 1 1 calc R U . . .
H41C H 0.3924 0.1174 0.1810 0.252 Uiso 1 1 calc R U . . .
C42 C 0.5534(8) 0.0621(8) 0.3992(8) 0.149(4) Uani 1 1 d . . . . .
H42A H 0.5698 0.0912 0.4647 0.224 Uiso 1 1 calc R U . . .
H42B H 0.6163 0.0729 0.3767 0.224 Uiso 1 1 calc R U . . .
H42C H 0.5314 -0.0091 0.3990 0.224 Uiso 1 1 calc R U . . .
C43 C 0.1093(8) 0.1917(9) 0.5353(8) 0.156(4) Uani 1 1 d . . . . .
H43A H 0.0771 0.1270 0.5484 0.235 Uiso 1 1 calc R U . . .
H43B H 0.0744 0.2082 0.4693 0.235 Uiso 1 1 calc R U . . .
H43C H 0.1012 0.2424 0.5804 0.235 Uiso 1 1 calc R U . . .
C44 C 0.2836(8) 0.1507(8) 0.6481(6) 0.129(3) Uani 1 1 d . . . . .
H44A H 0.2780 0.1972 0.6980 0.194 Uiso 1 1 calc R U . . .
H44B H 0.3583 0.1464 0.6546 0.194 Uiso 1 1 calc R U . . .
H44C H 0.2486 0.0851 0.6553 0.194 Uiso 1 1 calc R U . . .
C45 C 0.7650(11) 0.3265(11) 0.3807(8) 0.183(5) Uani 1 1 d . U . . .
H45A H 0.7356 0.2581 0.3583 0.274 Uiso 1 1 calc R U . . .
H45B H 0.7694 0.3356 0.4488 0.274 Uiso 1 1 calc R U . . .
H45C H 0.8358 0.3400 0.3727 0.274 Uiso 1 1 calc R U . . .
C46 C 0.7413(10) 0.5059(9) 0.3496(8) 0.158(4) Uani 1 1 d . U . . .
H46A H 0.8170 0.5125 0.3556 0.237 Uiso 1 1 calc R U . . .
H46B H 0.7310 0.5256 0.4111 0.237 Uiso 1 1 calc R U . . .
H46C H 0.7063 0.5486 0.2996 0.237 Uiso 1 1 calc R U . . .
C47 C 0.3791(9) 0.3680(11) -0.0762(12) 0.212(6) Uani 1 1 d . U . . .
H47A H 0.3506 0.4171 -0.0439 0.318 Uiso 1 1 calc R U . . .
H47B H 0.3228 0.3360 -0.1311 0.318 Uiso 1 1 calc R U . . .
H47C H 0.4362 0.4010 -0.0990 0.318 Uiso 1 1 calc R U . . .
C48 C 0.4104(12) 0.1944(11) -0.0601(10) 0.213(6) Uani 1 1 d . U . . .
H48A H 0.4549 0.1999 -0.1035 0.319 Uiso 1 1 calc R U . . .
H48B H 0.3365 0.1763 -0.0975 0.319 Uiso 1 1 calc R U . . .
H48C H 0.4327 0.1433 -0.0141 0.319 Uiso 1 1 calc R U . . .
C51 C -0.0062(10) 0.1507(8) 0.1973(9) 0.148(3) Uani 1 1 d . U . . .
H51 H 0.0684 0.1472 0.2369 0.178 Uiso 1 1 calc R U . . .
C52 C -0.0242(12) 0.1004(10) 0.1010(10) 0.181(3) Uani 1 1 d . U . . .
H52A H -0.0062 0.0319 0.1107 0.217 Uiso 1 1 calc R U . . .
H52B H 0.0254 0.1351 0.0693 0.217 Uiso 1 1 calc R U . . .
C53 C -0.1391(12) 0.0956(12) 0.0309(11) 0.201(4) Uani 1 1 d . U . . .
H53A H -0.1593 0.1628 0.0159 0.241 Uiso 1 1 calc R U . . .
H53B H -0.1465 0.0575 -0.0297 0.241 Uiso 1 1 calc R U . . .
C54 C -0.2054(14) 0.0411(13) 0.0912(12) 0.215(4) Uani 1 1 d . U . . .
H54A H -0.2802 0.0298 0.0514 0.258 Uiso 1 1 calc R U . . .
H54B H -0.1810 -0.0246 0.1060 0.258 Uiso 1 1 calc R U . . .
C55 C -0.2005(12) 0.0942(12) 0.1837(11) 0.196(3) Uani 1 1 d . U . . .
H55A H -0.2473 0.0560 0.2160 0.235 Uiso 1 1 calc R U . . .
H55B H -0.2245 0.1603 0.1707 0.235 Uiso 1 1 calc R U . . .
C56 C -0.0811(11) 0.1057(10) 0.2510(10) 0.179(3) Uani 1 1 d . U . . .
H56A H -0.0745 0.1486 0.3085 0.215 Uiso 1 1 calc R U . . .
H56B H -0.0618 0.0399 0.2728 0.215 Uiso 1 1 calc R U . . .
C61 C 0.0564(7) 0.5415(6) 0.2009(5) 0.0971(18) Uani 1 1 d . U . . .
H61 H 0.1351 0.5448 0.2173 0.116 Uiso 1 1 calc R U . . .
C62 C 0.0148(10) 0.5973(7) 0.1086(7) 0.146(3) Uani 1 1 d . U . . .
H62A H -0.0619 0.5764 0.0809 0.175 Uiso 1 1 calc R U . . .
H62B H 0.0504 0.5788 0.0608 0.175 Uiso 1 1 calc R U . . .
C63 C 0.0337(11) 0.7120(8) 0.1269(8) 0.167(3) Uani 1 1 d . U . . .
H63A H -0.0103 0.7439 0.0712 0.200 Uiso 1 1 calc R U . . .
H63B H 0.1088 0.7362 0.1348 0.200 Uiso 1 1 calc R U . . .
C64 C 0.0037(11) 0.7398(9) 0.2205(10) 0.172(3) Uani 1 1 d . U . . .
H64A H 0.0188 0.8125 0.2335 0.206 Uiso 1 1 calc R U . . .
H64B H -0.0731 0.7211 0.2094 0.206 Uiso 1 1 calc R U . . .
C65 C 0.0604(10) 0.6917(8) 0.3028(9) 0.158(3) Uani 1 1 d . U . . .
H65A H 0.0442 0.7154 0.3611 0.189 Uiso 1 1 calc R U . . .
H65B H 0.1374 0.7061 0.3127 0.189 Uiso 1 1 calc R U . . .
C66 C 0.0269(9) 0.5857(8) 0.2846(8) 0.141(2) Uani 1 1 d . U . . .
H66A H -0.0509 0.5737 0.2715 0.169 Uiso 1 1 calc R U . . .
H66B H 0.0591 0.5511 0.3433 0.169 Uiso 1 1 calc R U . . .
F1 F 0.5647(6) 0.2177(4) 0.6529(3) 0.182(3) Uani 1 1 d . . . . .
F2 F 0.6448(6) 0.2018(4) 0.8072(3) 0.168(3) Uani 1 1 d . . . . .
F3 F 0.6871(6) 0.3291(9) 0.7246(9) 0.306(7) Uani 1 1 d . . . . .
F4 F 0.5604(12) 0.3301(6) 0.7558(6) 0.268(6) Uani 1 1 d . . . . .
B1 B 0.6123(9) 0.2630(6) 0.7357(6) 0.090(2) 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 2.2343(14) . ?
Ni1 S2 2.1971(16) . ?
Ni1 P1 2.8273(15) . ?
Ni1 C1 1.908(5) . ?
Ni1 C2 1.828(5) . ?
S1 P1 1.9834(19) . ?
S2 P1 2.000(2) . ?
P1 O1 1.567(5) . ?
P1 O2 1.546(4) . ?
O1 C51 1.513(11) . ?
O2 C61 1.445(9) . ?
N1 H1 0.8600 . ?
N1 C1 1.319(6) . ?
N1 C11 1.452(6) . ?
N2 C2 1.144(6) . ?
N2 C21 1.404(7) . ?
N3 C1 1.319(7) . ?
N3 C31 1.489(7) . ?
N3 C32 1.485(8) 2_666 ?
C11 C12 1.391(7) . ?
C11 C16 1.390(8) . ?
C12 C13 1.409(10) . ?
C12 C17 1.509(10) . ?
C13 H13 0.9300 . ?
C13 C14 1.344(13) . ?
C14 H14 0.9300 . ?
C14 C15 1.339(13) . ?
C15 H15 0.9300 . ?
C15 C16 1.368(10) . ?
C16 C18 1.503(9) . ?
C17 H17 0.9800 . ?
C17 C41 1.546(10) . ?
C17 C42 1.528(11) . ?
C18 H18 0.9800 . ?
C18 C43 1.537(12) . ?
C18 C44 1.513(10) . ?
C21 C22 1.380(8) . ?
C21 C26 1.383(9) . ?
C22 C23 1.368(8) . ?
C22 C27 1.505(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.359(10) . ?
C24 H24 0.9300 . ?
C24 C25 1.356(11) . ?
C25 H25 0.9300 . ?
C25 C26 1.379(10) . ?
C26 C28 1.497(11) . ?
C27 H27 0.9800 . ?
C27 C45 1.497(13) . ?
C27 C46 1.503(12) . ?
C28 H28 0.9800 . ?
C28 C47 1.471(15) . ?
C28 C48 1.460(16) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 C32 1.380(9) . ?
C32 N3 1.485(8) 2_666 ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C51 H51 0.9800 . ?
C51 C52 1.463(15) . ?
C51 C56 1.486(14) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C52 C53 1.536(17) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C53 C54 1.522(19) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C54 C55 1.467(17) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C55 C56 1.565(18) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C61 H61 0.9800 . ?
C61 C62 1.511(11) . ?
C61 C66 1.488(10) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C62 C63 1.526(13) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 C64 1.544(15) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C64 C65 1.400(14) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C65 C66 1.427(13) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
F1 B1 1.271(9) . ?
F2 B1 1.316(8) . ?
F3 B1 1.284(11) . ?
F4 B1 1.256(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Ni1 P1 44.24(5) . . ?
S2 Ni1 S1 88.97(6) . . ?
S2 Ni1 P1 44.75(5) . . ?
C1 Ni1 S1 179.05(15) . . ?
C1 Ni1 S2 91.13(18) . . ?
C1 Ni1 P1 135.89(17) . . ?
C2 Ni1 S1 89.89(15) . . ?
C2 Ni1 S2 173.21(16) . . ?
C2 Ni1 P1 133.89(15) . . ?
C2 Ni1 C1 89.9(2) . . ?
P1 S1 Ni1 83.96(6) . . ?
P1 S2 Ni1 84.57(6) . . ?
S1 P1 Ni1 51.80(5) . . ?
S1 P1 S2 102.46(8) . . ?
S2 P1 Ni1 50.68(5) . . ?
O1 P1 Ni1 129.16(19) . . ?
O1 P1 S1 114.4(2) . . ?
O1 P1 S2 113.5(2) . . ?
O2 P1 Ni1 133.22(18) . . ?
O2 P1 S1 115.63(19) . . ?
O2 P1 S2 113.9(2) . . ?
O2 P1 O1 97.6(2) . . ?
C51 O1 P1 120.7(5) . . ?
C61 O2 P1 124.1(4) . . ?
C1 N1 H1 118.3 . . ?
C1 N1 C11 123.3(4) . . ?
C11 N1 H1 118.3 . . ?
C2 N2 C21 176.8(6) . . ?
C1 N3 C31 121.9(4) . . ?
C1 N3 C32 127.7(5) . 2_666 ?
C32 N3 C31 110.3(4) 2_666 . ?
N1 C1 Ni1 121.9(3) . . ?
N1 C1 N3 120.2(4) . . ?
N3 C1 Ni1 117.7(4) . . ?
N2 C2 Ni1 175.2(5) . . ?
C12 C11 N1 118.3(5) . . ?
C16 C11 N1 118.3(5) . . ?
C16 C11 C12 123.3(5) . . ?
C11 C12 C13 116.0(7) . . ?
C11 C12 C17 122.6(5) . . ?
C13 C12 C17 121.2(7) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.4(8) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.2 . . ?
C15 C14 C13 121.6(8) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 H15 118.9 . . ?
C14 C15 C16 122.3(8) . . ?
C16 C15 H15 118.9 . . ?
C11 C16 C18 122.3(6) . . ?
C15 C16 C11 116.3(7) . . ?
C15 C16 C18 121.3(7) . . ?
C12 C17 H17 108.1 . . ?
C12 C17 C41 112.5(8) . . ?
C12 C17 C42 108.9(5) . . ?
C41 C17 H17 108.1 . . ?
C42 C17 H17 108.1 . . ?
C42 C17 C41 111.2(8) . . ?
C16 C18 H18 107.7 . . ?
C16 C18 C43 113.2(8) . . ?
C16 C18 C44 110.3(6) . . ?
C43 C18 H18 107.7 . . ?
C44 C18 H18 107.7 . . ?
C44 C18 C43 110.1(6) . . ?
C22 C21 N2 117.1(5) . . ?
C22 C21 C26 125.4(6) . . ?
C26 C21 N2 117.5(6) . . ?
C21 C22 C27 123.7(5) . . ?
C23 C22 C21 115.9(6) . . ?
C23 C22 C27 120.4(6) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 C22 121.2(7) . . ?
C24 C23 H23 119.4 . . ?
C23 C24 H24 119.6 . . ?
C25 C24 C23 120.8(7) . . ?
C25 C24 H24 119.6 . . ?
C24 C25 H25 119.1 . . ?
C24 C25 C26 121.8(7) . . ?
C26 C25 H25 119.1 . . ?
C21 C26 C28 122.6(7) . . ?
C25 C26 C21 114.8(7) . . ?
C25 C26 C28 122.6(7) . . ?
C22 C27 H27 107.1 . . ?
C45 C27 C22 111.7(7) . . ?
C45 C27 H27 107.1 . . ?
C45 C27 C46 111.1(9) . . ?
C46 C27 C22 112.4(7) . . ?
C46 C27 H27 107.1 . . ?
C26 C28 H28 107.7 . . ?
C47 C28 C26 111.5(9) . . ?
C47 C28 H28 107.7 . . ?
C48 C28 C26 112.3(11) . . ?
C48 C28 H28 107.7 . . ?
C48 C28 C47 109.7(10) . . ?
N3 C31 H31A 109.7 . . ?
N3 C31 H31B 109.7 . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 N3 109.7(5) . . ?
C32 C31 H31A 109.7 . . ?
C32 C31 H31B 109.7 . . ?
N3 C32 H32A 109.5 2_666 . ?
N3 C32 H32B 109.5 2_666 . ?
C31 C32 N3 110.9(6) . 2_666 ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 108.0 . . ?
C17 C41 H41A 109.5 . . ?
C17 C41 H41B 109.5 . . ?
C17 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C17 C42 H42A 109.5 . . ?
C17 C42 H42B 109.5 . . ?
C17 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C18 C43 H43A 109.5 . . ?
C18 C43 H43B 109.5 . . ?
C18 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C18 C44 H44A 109.5 . . ?
C18 C44 H44B 109.5 . . ?
C18 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C27 C45 H45A 109.5 . . ?
C27 C45 H45B 109.5 . . ?
C27 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C27 C46 H46A 109.5 . . ?
C27 C46 H46B 109.5 . . ?
C27 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C28 C47 H47A 109.5 . . ?
C28 C47 H47B 109.5 . . ?
C28 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C28 C48 H48A 109.5 . . ?
C28 C48 H48B 109.5 . . ?
C28 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O1 C51 H51 109.3 . . ?
C52 C51 O1 107.4(10) . . ?
C52 C51 H51 109.3 . . ?
C52 C51 C56 112.8(11) . . ?
C56 C51 O1 108.7(10) . . ?
C56 C51 H51 109.3 . . ?
C51 C52 H52A 108.3 . . ?
C51 C52 H52B 108.3 . . ?
C51 C52 C53 115.9(13) . . ?
H52A C52 H52B 107.4 . . ?
C53 C52 H52A 108.3 . . ?
C53 C52 H52B 108.3 . . ?
C52 C53 H53A 111.5 . . ?
C52 C53 H53B 111.5 . . ?
H53A C53 H53B 109.3 . . ?
C54 C53 C52 101.6(13) . . ?
C54 C53 H53A 111.5 . . ?
C54 C53 H53B 111.5 . . ?
C53 C54 H54A 108.5 . . ?
C53 C54 H54B 108.5 . . ?
H54A C54 H54B 107.5 . . ?
C55 C54 C53 115.2(14) . . ?
C55 C54 H54A 108.5 . . ?
C55 C54 H54B 108.5 . . ?
C54 C55 H55A 110.0 . . ?
C54 C55 H55B 110.0 . . ?
C54 C55 C56 108.5(14) . . ?
H55A C55 H55B 108.4 . . ?
C56 C55 H55A 110.0 . . ?
C56 C55 H55B 110.0 . . ?
C51 C56 C55 110.8(11) . . ?
C51 C56 H56A 109.5 . . ?
C51 C56 H56B 109.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 108.1 . . ?
O2 C61 H61 109.4 . . ?
O2 C61 C62 108.9(7) . . ?
O2 C61 C66 108.6(7) . . ?
C62 C61 H61 109.4 . . ?
C66 C61 H61 109.4 . . ?
C66 C61 C62 111.2(8) . . ?
C61 C62 H62A 109.1 . . ?
C61 C62 H62B 109.1 . . ?
C61 C62 C63 112.7(8) . . ?
H62A C62 H62B 107.8 . . ?
C63 C62 H62A 109.1 . . ?
C63 C62 H62B 109.1 . . ?
C62 C63 H63A 109.8 . . ?
C62 C63 H63B 109.8 . . ?
C62 C63 C64 109.4(9) . . ?
H63A C63 H63B 108.3 . . ?
C64 C63 H63A 109.8 . . ?
C64 C63 H63B 109.8 . . ?
C63 C64 H64A 109.1 . . ?
C63 C64 H64B 109.1 . . ?
H64A C64 H64B 107.8 . . ?
C65 C64 C63 112.6(11) . . ?
C65 C64 H64A 109.1 . . ?
C65 C64 H64B 109.1 . . ?
C64 C65 H65A 110.3 . . ?
C64 C65 H65B 110.3 . . ?
C64 C65 C66 107.0(11) . . ?
H65A C65 H65B 108.6 . . ?
C66 C65 H65A 110.3 . . ?
C66 C65 H65B 110.3 . . ?
C61 C66 H66A 108.8 . . ?
C61 C66 H66B 108.8 . . ?
C65 C66 C61 113.9(9) . . ?
C65 C66 H66A 108.8 . . ?
C65 C66 H66B 108.8 . . ?
H66A C66 H66B 107.7 . . ?
F1 B1 F2 113.9(7) . . ?
F1 B1 F3 108.1(10) . . ?
F3 B1 F2 114.5(9) . . ?
F4 B1 F1 112.1(10) . . ?
F4 B1 F2 114.1(7) . . ?
F4 B1 F3 92.2(9) . . ?

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 P1 O1 C51 1.9(8) . . . . ?
Ni1 P1 O2 C61 -2.0(6) . . . . ?
S1 P1 O1 C51 61.5(7) . . . . ?
S1 P1 O2 C61 -62.7(5) . . . . ?
S2 P1 O1 C51 -55.6(7) . . . . ?
S2 P1 O2 C61 55.7(5) . . . . ?
P1 O1 C51 C52 -107.5(10) . . . . ?
P1 O1 C51 C56 130.1(8) . . . . ?
P1 O2 C61 C62 130.5(7) . . . . ?
P1 O2 C61 C66 -108.3(7) . . . . ?
O1 P1 O2 C61 175.6(5) . . . . ?
O1 C51 C52 C53 -63.8(14) . . . . ?
O1 C51 C56 C55 69.8(13) . . . . ?
O2 P1 O1 C51 -175.8(7) . . . . ?
O2 C61 C62 C63 163.7(9) . . . . ?
O2 C61 C66 C65 -174.4(9) . . . . ?
N1 C11 C12 C13 179.2(5) . . . . ?
N1 C11 C12 C17 3.8(7) . . . . ?
N1 C11 C16 C15 -177.5(5) . . . . ?
N1 C11 C16 C18 -1.5(8) . . . . ?
N2 C21 C22 C23 -179.8(6) . . . . ?
N2 C21 C22 C27 -2.3(9) . . . . ?
N2 C21 C26 C25 179.0(6) . . . . ?
N2 C21 C26 C28 -0.8(11) . . . . ?
N3 C31 C32 N3 57.9(8) . . . 2_666 ?
C1 N1 C11 C12 80.0(7) . . . . ?
C1 N1 C11 C16 -104.8(6) . . . . ?
C1 N3 C31 C32 118.6(7) . . . . ?
C11 N1 C1 Ni1 -0.9(7) . . . . ?
C11 N1 C1 N3 -175.8(5) . . . . ?
C11 C12 C13 C14 -1.8(11) . . . . ?
C11 C12 C17 C41 -144.4(6) . . . . ?
C11 C12 C17 C42 91.9(8) . . . . ?
C11 C16 C18 C43 141.2(7) . . . . ?
C11 C16 C18 C44 -95.0(8) . . . . ?
C12 C11 C16 C15 -2.6(9) . . . . ?
C12 C11 C16 C18 173.4(5) . . . . ?
C12 C13 C14 C15 -2.2(14) . . . . ?
C13 C12 C17 C41 40.4(8) . . . . ?
C13 C12 C17 C42 -83.2(9) . . . . ?
C13 C14 C15 C16 4.1(15) . . . . ?
C14 C15 C16 C11 -1.7(11) . . . . ?
C14 C15 C16 C18 -177.8(8) . . . . ?
C15 C16 C18 C43 -43.0(9) . . . . ?
C15 C16 C18 C44 80.8(9) . . . . ?
C16 C11 C12 C13 4.2(8) . . . . ?
C16 C11 C12 C17 -171.2(5) . . . . ?
C17 C12 C13 C14 173.6(8) . . . . ?
C21 C22 C23 C24 -0.9(11) . . . . ?
C21 C22 C27 C45 118.9(9) . . . . ?
C21 C22 C27 C46 -115.5(8) . . . . ?
C21 C26 C28 C47 112.6(11) . . . . ?
C21 C26 C28 C48 -123.9(10) . . . . ?
C22 C21 C26 C25 -2.9(11) . . . . ?
C22 C21 C26 C28 177.3(8) . . . . ?
C22 C23 C24 C25 0.9(14) . . . . ?
C23 C22 C27 C45 -63.7(11) . . . . ?
C23 C22 C27 C46 62.0(9) . . . . ?
C23 C24 C25 C26 -1.9(14) . . . . ?
C24 C25 C26 C21 2.7(12) . . . . ?
C24 C25 C26 C28 -177.5(10) . . . . ?
C25 C26 C28 C47 -67.2(14) . . . . ?
C25 C26 C28 C48 56.3(12) . . . . ?
C26 C21 C22 C23 2.0(10) . . . . ?
C26 C21 C22 C27 179.6(7) . . . . ?
C27 C22 C23 C24 -178.6(8) . . . . ?
C31 N3 C1 Ni1 15.3(9) . . . . ?
C31 N3 C1 N1 -169.6(6) . . . . ?
C32 N3 C1 Ni1 -169.2(5) 2_666 . . . ?
C32 N3 C1 N1 5.9(10) 2_666 . . . ?
C32 N3 C31 C32 -57.5(9) 2_666 . . . ?
C51 C52 C53 C54 -57.4(16) . . . . ?
C52 C51 C56 C55 -49.2(16) . . . . ?
C52 C53 C54 C55 62.2(19) . . . . ?
C53 C54 C55 C56 -62.2(19) . . . . ?
C54 C55 C56 C51 51.4(16) . . . . ?
C56 C51 C52 C53 56.0(17) . . . . ?
C61 C62 C63 C64 -44.2(14) . . . . ?
C62 C61 C66 C65 -54.6(13) . . . . ?
C62 C63 C64 C65 56.3(15) . . . . ?
C63 C64 C65 C66 -64.9(14) . . . . ?
C64 C65 C66 C61 64.5(14) . . . . ?
C66 C61 C62 C63 44.1(12) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.500 43.7 0.0 ?
2 0.140 0.860 0.550 9.0 0.0 ?
3 0.198 0.157 0.019 24.2 0.5 ?
4 0.293 0.787 0.450 7.3 0.0 ?
5 0.500 0.000 0.000 14.2 0.0 ?
6 0.707 0.213 0.550 7.3 0.0 ?
7 0.802 0.843 0.981 24.2 0.5 ?
8 0.860 0.140 0.450 9.0 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.456
_oxdiff_exptl_absorpt_empirical_full_min 0.796
####################################################################### 
# 
# 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_m273eb
_database_code_depnum_ccdc_archive 'CCDC 2308594'
loop_
_audit_author_name
_audit_author_address
'Daniel Miguel'
;Universidad de Valladolid
Spain
;
_audit_update_record             
;
2024-04-04 deposited with the CCDC.	2024-08-26 downloaded from the CCDC.
;
_audit_creation_date             2024-04-04
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H46 N2 Ni O4 P2 S4'
_chemical_formula_sum            'C46 H46 N2 Ni O4 P2 S4'
_chemical_formula_weight         939.74
_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   11.1533(6)
_cell_length_b                   8.8012(8)
_cell_length_c                   24.1739(18)
_cell_angle_alpha                90
_cell_angle_beta                 94.913(6)
_cell_angle_gamma                90
_cell_volume                     2364.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1909
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.7310
_cell_measurement_theta_min      4.3060
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.697
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             980
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 0 -33 0.0752
4 -3 31 0.0610
-14 -2 16 0.0759
13 -4 -17 0.1189
1 -12 -12 0.1325
1 12 11 0.0954

_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.159
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.1019
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12866
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.655
_diffrn_reflns_theta_min         2.867
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -13.00  59.00   1.00    6.00    --  -10.56  57.00  30.00   72
  2  ω    -84.00  11.00   1.00    6.00    --  -10.56 -77.00 -90.00   95
  3  ω    -17.00  23.00   1.00    6.00    --   12.51 -99.00 150.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_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                2385
_reflns_number_total             5650
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1764
_refine_ls_R_factor_gt           0.0670
_refine_ls_restrained_S_all      1.027
_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)+(0.0685P)²+0.5857P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1975
_refine_special_details          ?
_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. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01 within 2A
Uanis(C1) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
3.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C40(H40A,H40B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.5000 0.0000 0.5000 0.0592(3) Uani 1 2 d S . P . .
S1 S 0.40228(11) 0.25271(16) 0.51234(6) 0.0740(4) Uani 1 1 d . . . . .
S2 S 0.53981(13) 0.02412(17) 0.60317(6) 0.0783(4) Uani 1 1 d . . . . .
P1 P 0.45052(11) 0.21783(16) 0.59115(6) 0.0645(4) Uani 1 1 d . . . . .
O30 O 0.5251(3) 0.3551(4) 0.62005(14) 0.0736(10) Uani 1 1 d . . . . .
O40 O 0.3324(3) 0.2288(4) 0.62305(15) 0.0825(11) Uani 1 1 d . . . . .
N1 N 0.7423(3) 0.1694(5) 0.48204(16) 0.0631(11) Uani 1 1 d . . . . .
C1 C 0.6544(4) 0.1067(6) 0.4893(2) 0.0664(14) Uani 1 1 d . U . . .
C11 C 0.8481(4) 0.2437(6) 0.4710(3) 0.0746(16) Uani 1 1 d . U . . .
C12 C 0.8475(9) 0.3329(9) 0.4256(4) 0.134(3) Uani 1 1 d . U . . .
C13 C 0.9728(11) 0.3969(11) 0.4153(4) 0.160(3) Uani 1 1 d . U . . .
H13 H 0.9891 0.4561 0.3849 0.192 Uiso 1 1 calc R U . . .
C14 C 1.0530(10) 0.3557(12) 0.4556(5) 0.159(3) Uani 1 1 d . U . . .
H14 H 1.1287 0.3944 0.4500 0.191 Uiso 1 1 calc R U . . .
C15 C 1.0562(8) 0.2755(12) 0.5012(5) 0.163(3) Uani 1 1 d . U . . .
H15 H 1.1249 0.2605 0.5252 0.196 Uiso 1 1 calc R U . . .
C16 C 0.9477(6) 0.2175(10) 0.5091(4) 0.126(3) Uani 1 1 d . U . . .
C17 C 0.7403(14) 0.3599(11) 0.3904(3) 0.224(6) Uani 1 1 d . . . . .
H17A H 0.7102 0.2653 0.3750 0.336 Uiso 1 1 calc R U . . .
H17B H 0.7577 0.4272 0.3608 0.336 Uiso 1 1 calc R U . . .
H17C H 0.6808 0.4053 0.4116 0.336 Uiso 1 1 calc R U . . .
C18 C 0.9367(9) 0.1212(13) 0.5604(4) 0.193(5) Uani 1 1 d . . . . .
H18A H 0.9201 0.1854 0.5909 0.289 Uiso 1 1 calc R U . . .
H18B H 1.0107 0.0675 0.5694 0.289 Uiso 1 1 calc R U . . .
H18C H 0.8723 0.0496 0.5533 0.289 Uiso 1 1 calc R U . . .
C30 C 0.6385(5) 0.3980(7) 0.5998(2) 0.0867(18) Uani 1 1 d . . . . .
H30A H 0.6242 0.4528 0.5650 0.104 Uiso 1 1 calc R U . . .
H30B H 0.6850 0.3077 0.5931 0.104 Uiso 1 1 calc R U . . .
C31 C 0.7065(4) 0.4956(6) 0.6415(2) 0.0629(13) Uani 1 1 d . . . . .
C32 C 0.7883(5) 0.4308(7) 0.6805(3) 0.0864(17) Uani 1 1 d . . . . .
H32 H 0.8006 0.3263 0.6808 0.104 Uiso 1 1 calc R U . . .
C33 C 0.8522(5) 0.5218(9) 0.7193(3) 0.098(2) Uani 1 1 d . . . . .
H33 H 0.9079 0.4785 0.7455 0.117 Uiso 1 1 calc R U . . .
C34 C 0.8337(5) 0.6738(9) 0.7191(3) 0.0896(18) Uani 1 1 d . . . . .
H34 H 0.8751 0.7342 0.7460 0.108 Uiso 1 1 calc R U . . .
C35 C 0.7552(5) 0.7384(7) 0.6802(3) 0.0839(16) Uani 1 1 d . . . . .
H35 H 0.7444 0.8432 0.6795 0.101 Uiso 1 1 calc R U . . .
C36 C 0.6923(4) 0.6485(7) 0.6420(2) 0.0680(14) Uani 1 1 d . . . . .
H36 H 0.6380 0.6934 0.6156 0.082 Uiso 1 1 calc R U . . .
C40 C 0.3371(5) 0.2157(9) 0.6805(2) 0.105(2) Uani 1 1 d . . . . .
H40A H 0.3574 0.3131 0.6976 0.126 Uiso 1 1 calc R U . . .
H40B H 0.3988 0.1431 0.6933 0.126 Uiso 1 1 calc R U . . .
C41 C 0.2163(4) 0.1632(7) 0.6969(2) 0.0724(15) Uani 1 1 d . . . . .
C42 C 0.1613(6) 0.0385(8) 0.6739(3) 0.0931(19) Uani 1 1 d . . . . .
H42 H 0.1964 -0.0133 0.6459 0.112 Uiso 1 1 calc R U . . .
C43 C 0.0548(7) -0.0122(8) 0.6912(3) 0.117(2) Uani 1 1 d . . . . .
H43 H 0.0176 -0.0970 0.6745 0.140 Uiso 1 1 calc R U . . .
C44 C 0.0035(6) 0.0595(10) 0.7322(3) 0.107(2) Uani 1 1 d . . . . .
H44 H -0.0672 0.0216 0.7446 0.129 Uiso 1 1 calc R U . . .
C45 C 0.0528(6) 0.1835(10) 0.7551(3) 0.105(2) Uani 1 1 d . . . . .
H45 H 0.0155 0.2350 0.7825 0.126 Uiso 1 1 calc R U . . .
C46 C 0.1619(5) 0.2366(8) 0.7376(3) 0.103(2) Uani 1 1 d . . . . .
H46 H 0.1976 0.3230 0.7539 0.124 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 S1 2.5059(14) . ?
Ni1 S1 2.5058(14) 3_656 ?
Ni1 S2 2.5046(14) 3_656 ?
Ni1 S2 2.5045(14) . ?
Ni1 C1 1.998(5) . ?
Ni1 C1 1.998(5) 3_656 ?
S1 P1 1.9591(19) . ?
S2 P1 1.983(2) . ?
P1 O30 1.594(3) . ?
P1 O40 1.585(3) . ?
O30 C30 1.446(5) . ?
O40 C40 1.390(6) . ?
N1 C1 1.151(5) . ?
N1 C11 1.394(6) . ?
C11 C12 1.350(10) . ?
C11 C16 1.399(10) . ?
C12 C13 1.547(12) . ?
C12 C17 1.427(13) . ?
C13 H13 0.9300 . ?
C13 C14 1.316(14) . ?
C14 H14 0.9300 . ?
C14 C15 1.308(13) . ?
C15 H15 0.9300 . ?
C15 C16 1.342(11) . ?
C16 C18 1.516(12) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.483(7) . ?
C31 C32 1.378(7) . ?
C31 C36 1.355(7) . ?
C32 H32 0.9300 . ?
C32 C33 1.382(8) . ?
C33 H33 0.9300 . ?
C33 C34 1.353(9) . ?
C34 H34 0.9300 . ?
C34 C35 1.354(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.364(7) . ?
C36 H36 0.9300 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40 C41 1.509(7) . ?
C41 C42 1.354(8) . ?
C41 C46 1.361(8) . ?
C42 H42 0.9300 . ?
C42 C43 1.367(8) . ?
C43 H43 0.9300 . ?
C43 C44 1.344(10) . ?
C44 H44 0.9300 . ?
C44 C45 1.322(9) . ?
C45 H45 0.9300 . ?
C45 C46 1.403(8) . ?
C46 H46 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
S1 Ni1 S1 180.00(5) 3_656 . ?
S2 Ni1 S1 81.26(5) 3_656 3_656 ?
S2 Ni1 S1 98.74(5) 3_656 . ?
S2 Ni1 S1 98.74(5) . 3_656 ?
S2 Ni1 S1 81.26(5) . . ?
S2 Ni1 S2 180.0 . 3_656 ?
C1 Ni1 S1 90.75(14) 3_656 . ?
C1 Ni1 S1 89.25(14) 3_656 3_656 ?
C1 Ni1 S1 89.25(14) . . ?
C1 Ni1 S1 90.75(14) . 3_656 ?
C1 Ni1 S2 90.48(14) 3_656 3_656 ?
C1 Ni1 S2 90.47(14) . . ?
C1 Ni1 S2 89.53(14) . 3_656 ?
C1 Ni1 S2 89.52(14) 3_656 . ?
C1 Ni1 C1 180.0 . 3_656 ?
P1 S1 Ni1 83.72(6) . . ?
P1 S2 Ni1 83.29(6) . . ?
S1 P1 S2 111.70(8) . . ?
O30 P1 S1 113.39(16) . . ?
O30 P1 S2 110.54(15) . . ?
O40 P1 S1 107.04(15) . . ?
O40 P1 S2 114.14(17) . . ?
O40 P1 O30 99.48(18) . . ?
C30 O30 P1 119.2(3) . . ?
C40 O40 P1 121.3(3) . . ?
C1 N1 C11 177.7(5) . . ?
N1 C1 Ni1 178.6(5) . . ?
N1 C11 C16 115.7(6) . . ?
C12 C11 N1 118.9(6) . . ?
C12 C11 C16 125.4(7) . . ?
C11 C12 C13 113.7(9) . . ?
C11 C12 C17 121.8(8) . . ?
C17 C12 C13 124.5(10) . . ?
C12 C13 H13 124.9 . . ?
C14 C13 C12 110.3(9) . . ?
C14 C13 H13 124.9 . . ?
C13 C14 H14 111.1 . . ?
C15 C14 C13 137.8(11) . . ?
C15 C14 H14 111.1 . . ?
C14 C15 H15 124.3 . . ?
C14 C15 C16 111.4(11) . . ?
C16 C15 H15 124.3 . . ?
C11 C16 C18 121.0(6) . . ?
C15 C16 C11 121.3(10) . . ?
C15 C16 C18 117.8(10) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O30 C30 H30A 109.8 . . ?
O30 C30 H30B 109.8 . . ?
O30 C30 C31 109.4(4) . . ?
H30A C30 H30B 108.2 . . ?
C31 C30 H30A 109.8 . . ?
C31 C30 H30B 109.8 . . ?
C32 C31 C30 119.7(6) . . ?
C36 C31 C30 121.8(5) . . ?
C36 C31 C32 118.4(5) . . ?
C31 C32 H32 120.1 . . ?
C31 C32 C33 119.8(6) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 120.1(6) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 119.8 . . ?
C33 C34 C35 120.4(6) . . ?
C35 C34 H34 119.8 . . ?
C34 C35 H35 120.3 . . ?
C34 C35 C36 119.4(6) . . ?
C36 C35 H35 120.3 . . ?
C31 C36 C35 121.9(5) . . ?
C31 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
O40 C40 H40A 109.8 . . ?
O40 C40 H40B 109.8 . . ?
O40 C40 C41 109.3(4) . . ?
H40A C40 H40B 108.3 . . ?
C41 C40 H40A 109.8 . . ?
C41 C40 H40B 109.8 . . ?
C42 C41 C40 121.5(5) . . ?
C42 C41 C46 117.9(5) . . ?
C46 C41 C40 120.5(6) . . ?
C41 C42 H42 119.6 . . ?
C41 C42 C43 120.9(6) . . ?
C43 C42 H42 119.6 . . ?
C42 C43 H43 119.7 . . ?
C44 C43 C42 120.5(7) . . ?
C44 C43 H43 119.7 . . ?
C43 C44 H44 119.7 . . ?
C45 C44 C43 120.6(7) . . ?
C45 C44 H44 119.7 . . ?
C44 C45 H45 120.4 . . ?
C44 C45 C46 119.2(7) . . ?
C46 C45 H45 120.4 . . ?
C41 C46 C45 120.8(7) . . ?
C41 C46 H46 119.6 . . ?
C45 C46 H46 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 P1 O30 C30 -60.9(4) . . . . ?
S1 P1 O40 C40 -177.2(4) . . . . ?
S2 P1 O30 C30 65.4(4) . . . . ?
S2 P1 O40 C40 58.6(5) . . . . ?
P1 O30 C30 C31 -164.3(4) . . . . ?
P1 O40 C40 C41 -155.8(4) . . . . ?
O30 P1 O40 C40 -59.0(5) . . . . ?
O30 C30 C31 C32 93.0(6) . . . . ?
O30 C30 C31 C36 -88.2(6) . . . . ?
O40 P1 O30 C30 -174.3(4) . . . . ?
O40 C40 C41 C42 52.1(8) . . . . ?
O40 C40 C41 C46 -130.9(6) . . . . ?
N1 C11 C12 C13 -174.8(5) . . . . ?
N1 C11 C12 C17 3.6(10) . . . . ?
N1 C11 C16 C15 176.0(6) . . . . ?
N1 C11 C16 C18 -3.3(10) . . . . ?
C11 C12 C13 C14 -3.3(11) . . . . ?
C12 C11 C16 C15 -3.7(11) . . . . ?
C12 C11 C16 C18 176.9(7) . . . . ?
C12 C13 C14 C15 0.6(19) . . . . ?
C13 C14 C15 C16 1(2) . . . . ?
C14 C15 C16 C11 0.5(12) . . . . ?
C14 C15 C16 C18 179.9(9) . . . . ?
C16 C11 C12 C13 4.9(10) . . . . ?
C16 C11 C12 C17 -176.7(7) . . . . ?
C17 C12 C13 C14 178.4(9) . . . . ?
C30 C31 C32 C33 179.6(5) . . . . ?
C30 C31 C36 C35 -179.6(5) . . . . ?
C31 C32 C33 C34 0.5(9) . . . . ?
C32 C31 C36 C35 -0.8(7) . . . . ?
C32 C33 C34 C35 -1.9(10) . . . . ?
C33 C34 C35 C36 1.9(9) . . . . ?
C34 C35 C36 C31 -0.5(8) . . . . ?
C36 C31 C32 C33 0.9(8) . . . . ?
C40 C41 C42 C43 176.6(6) . . . . ?
C40 C41 C46 C45 -176.6(6) . . . . ?
C41 C42 C43 C44 -1.1(11) . . . . ?
C42 C41 C46 C45 0.5(9) . . . . ?
C42 C43 C44 C45 2.5(12) . . . . ?
C43 C44 C45 C46 -2.4(12) . . . . ?
C44 C45 C46 C41 0.9(11) . . . . ?
C46 C41 C42 C43 -0.4(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.109 0.570 0.708 8.1 0.0 ?
2 0.391 0.070 0.792 8.1 0.0 ?
3 0.609 -0.070 0.208 8.1 0.0 ?
4 0.891 0.430 0.292 8.1 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
