# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_04slh029
_database_code_depnum_ccdc_archive 'CCDC 1474143'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H28 N4 Ni O4 P2 S5'
_chemical_formula_weight         669.41

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   11.6939(8)
_cell_length_b                   15.2594(14)
_cell_length_c                   15.9310(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2842.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3652
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7153
_exptl_absorpt_correction_T_max  0.8897
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'Φ & ω scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21763
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3263
_reflns_number_gt                2733
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0576P)²+4.1336P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    difmap
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3263
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0903
_refine_ls_wR_factor_gt          0.0817
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_restrained_S_all      0.860
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.003

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
C1 C -0.1281(2) -0.20887(17) 0.70098(16) 0.0298(5) Uani 1 1 d . . .
C2 C -0.1648(3) -0.2993(2) 0.7249(3) 0.0484(8) Uani 1 1 d . . .
C3 C -0.3763(2) -0.14711(18) 0.5097(2) 0.0367(6) Uani 1 1 d . . .
C4 C -0.4696(3) -0.1091(2) 0.4575(2) 0.0435(7) Uani 1 1 d . . .
C5 C -0.19276(17) 0.11889(14) 0.45002(13) 0.0190(4) Uani 1 1 d . . .
C6 C -0.28608(18) 0.15175(14) 0.40744(14) 0.0206(4) Uani 1 1 d . . .
C7 C -0.32794(16) 0.10532(13) 0.33875(13) 0.0176(4) Uani 1 1 d . . .
C8 C -0.27327(17) 0.02882(14) 0.31555(13) 0.0178(4) Uani 1 1 d . . .
C9 C -0.17814(18) 0.00214(13) 0.36048(13) 0.0177(4) Uani 1 1 d . . .
C10 C -0.42541(17) 0.13973(14) 0.29042(13) 0.0191(4) Uani 1 1 d . . .
N1 N -0.13802(14) 0.04577(11) 0.42748(10) 0.0164(4) Uani 1 1 d . . .
N2 N -0.5000 0.08843(17) 0.2500 0.0190(5) Uani 1 2 d S . .
O1 O -0.21806(13) -0.16754(10) 0.65251(10) 0.0256(4) Uani 1 1 d . . .
O2 O -0.30974(12) -0.07657(10) 0.54748(11) 0.0243(3) Uani 1 1 d . . .
P1 P -0.18616(4) -0.09683(4) 0.58302(3) 0.01874(15) Uani 1 1 d . . .
S1 S -0.11976(5) 0.01194(3) 0.62832(3) 0.01983(14) Uani 1 1 d . . .
S2 S 0.08302(4) 0.14869(3) 0.50288(3) 0.01871(14) Uani 1 1 d . . .
S3 S -0.4577(3) 0.2467(2) 0.2778(3) 0.0240(5) Uani 0.50 1 d P . .
N3 N -0.4314(8) 0.2287(7) 0.2831(8) 0.0220(19) Uani 0.50 1 d P . .
Ni1 Ni 0.0000 0.0000 0.5000 0.01356(12) Uani 1 2 d S . .
H1A H -0.055(2) -0.2102(18) 0.6645(17) 0.031(7) Uiso 1 1 d . . .
H1B H -0.114(3) -0.174(2) 0.749(2) 0.045(8) Uiso 1 1 d . . .
H2A H -0.234(3) -0.294(2) 0.762(2) 0.067(11) Uiso 1 1 d . . .
H2B H -0.177(2) -0.3263(16) 0.6733(18) 0.020(7) Uiso 1 1 d . . .
H2C H -0.098(3) -0.328(3) 0.759(2) 0.071(11) Uiso 1 1 d . . .
H3A H -0.397(3) -0.189(2) 0.552(2) 0.054(10) Uiso 1 1 d . . .
H3B H -0.333(4) -0.169(3) 0.456(3) 0.085(13) Uiso 1 1 d . . .
H4A H -0.435(3) -0.074(3) 0.410(3) 0.073(12) Uiso 1 1 d . . .
H4B H -0.518(3) -0.161(3) 0.428(3) 0.082(13) Uiso 1 1 d . . .
H4C H -0.524(3) -0.072(2) 0.501(2) 0.057(10) Uiso 1 1 d . . .
H5 H -0.161(2) 0.1482(18) 0.4975(16) 0.027(7) Uiso 1 1 d . . .
H6 H -0.320(2) 0.2024(17) 0.4258(16) 0.022(6) Uiso 1 1 d . . .
H8 H -0.296(2) -0.0041(15) 0.2668(17) 0.023(7) Uiso 1 1 d . . .
H9 H -0.135(2) -0.0484(17) 0.3446(16) 0.027(7) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.449(3) . ?
C1 C2 1.495(4) . ?
C1 H1A 1.04(3) . ?
C1 H1B 0.95(3) . ?
C2 H2A 1.00(4) . ?
C2 H2B 0.93(3) . ?
C2 H2C 1.05(4) . ?
C3 O2 1.458(3) . ?
C3 C4 1.489(4) . ?
C3 H3A 0.95(4) . ?
C3 H3B 1.05(4) . ?
C4 H4A 1.01(4) . ?
C4 H4B 1.08(4) . ?
C4 H4C 1.11(4) . ?
C5 N1 1.336(3) . ?
C5 C6 1.379(3) . ?
C5 H5 0.95(3) . ?
C6 C7 1.393(3) . ?
C6 H6 0.92(3) . ?
C7 C8 1.381(3) . ?
C7 C10 1.472(3) . ?
C8 C9 1.384(3) . ?
C8 H8 0.96(3) . ?
C9 N1 1.343(3) . ?
C9 H9 0.96(3) . ?
C10 N2 1.337(3) . ?
C10 N3 1.365(11) . ?
C10 S3 1.687(4) . ?
N1 Ni1 2.1042(16) . ?
N2 C10 1.337(3) 3_455 ?
O1 P1 1.5902(16) . ?
O2 P1 1.5825(15) . ?
P1 S1 1.9693(8) . ?
P1 S2 1.9884(8) 5_556 ?
S1 Ni1 2.4846(5) . ?
S2 P1 1.9884(8) 5_556 ?
S2 Ni1 2.4683(5) . ?
S3 N3 1.642(6) 3_455 ?
N3 S3 1.642(6) 3_455 ?
Ni1 N1 2.1042(16) 5_556 ?
Ni1 S2 2.4683(6) 5_556 ?
Ni1 S1 2.4846(5) 5_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 109.2(2) . . ?
O1 C1 H1A 108.2(15) . . ?
C2 C1 H1A 111.2(15) . . ?
O1 C1 H1B 108.6(19) . . ?
C2 C1 H1B 111.1(19) . . ?
H1A C1 H1B 108(2) . . ?
C1 C2 H2A 108(2) . . ?
C1 C2 H2B 103.2(16) . . ?
H2A C2 H2B 115(3) . . ?
C1 C2 H2C 108(2) . . ?
H2A C2 H2C 109(3) . . ?
H2B C2 H2C 113(3) . . ?
O2 C3 C4 109.5(2) . . ?
O2 C3 H3A 110(2) . . ?
C4 C3 H3A 118(2) . . ?
O2 C3 H3B 108(2) . . ?
C4 C3 H3B 92(2) . . ?
H3A C3 H3B 119(3) . . ?
C3 C4 H4A 109(2) . . ?
C3 C4 H4B 110(2) . . ?
H4A C4 H4B 106(3) . . ?
C3 C4 H4C 105.8(17) . . ?
H4A C4 H4C 115(3) . . ?
H4B C4 H4C 110(3) . . ?
N1 C5 C6 123.4(2) . . ?
N1 C5 H5 114.8(17) . . ?
C6 C5 H5 121.7(17) . . ?
C5 C6 C7 118.7(2) . . ?
C5 C6 H6 119.5(16) . . ?
C7 C6 H6 121.8(16) . . ?
C8 C7 C6 118.52(19) . . ?
C8 C7 C10 121.32(19) . . ?
C6 C7 C10 120.11(19) . . ?
C7 C8 C9 118.83(19) . . ?
C7 C8 H8 122.1(15) . . ?
C9 C8 H8 118.9(15) . . ?
N1 C9 C8 123.11(19) . . ?
N1 C9 H9 115.2(15) . . ?
C8 C9 H9 121.7(16) . . ?
N2 C10 N3 120.5(4) . . ?
N2 C10 C7 123.2(2) . . ?
N3 C10 C7 116.1(4) . . ?
N2 C10 S3 111.3(2) . . ?
N3 C10 S3 10.2(5) . . ?
C7 C10 S3 125.5(2) . . ?
C5 N1 C9 117.42(18) . . ?
C5 N1 Ni1 119.82(13) . . ?
C9 N1 Ni1 122.68(14) . . ?
C10 N2 C10 108.3(3) . 3_455 ?
C1 O1 P1 119.74(14) . . ?
C3 O2 P1 119.41(15) . . ?
O2 P1 O1 99.63(8) . . ?
O2 P1 S1 109.06(7) . . ?
O1 P1 S1 114.15(7) . . ?
O2 P1 S2 112.67(7) . 5_556 ?
O1 P1 S2 110.57(7) . 5_556 ?
S1 P1 S2 110.39(3) . 5_556 ?
P1 S1 Ni1 81.89(2) . . ?
P1 S2 Ni1 81.95(2) 5_556 . ?
N3 S3 C10 94.9(6) 3_455 . ?
C10 N3 S3 104.9(8) . 3_455 ?
N1 Ni1 N1 180.00(8) . 5_556 ?
N1 Ni1 S2 89.61(5) . 5_556 ?
N1 Ni1 S2 90.39(5) 5_556 5_556 ?
N1 Ni1 S2 90.39(5) . . ?
N1 Ni1 S2 89.61(5) 5_556 . ?
S2 Ni1 S2 180.000(10) 5_556 . ?
N1 Ni1 S1 89.72(5) . . ?
N1 Ni1 S1 90.28(5) 5_556 . ?
S2 Ni1 S1 82.010(17) 5_556 . ?
S2 Ni1 S1 97.990(17) . . ?
N1 Ni1 S1 90.28(5) . 5_556 ?
N1 Ni1 S1 89.72(5) 5_556 5_556 ?
S2 Ni1 S1 97.990(17) 5_556 5_556 ?
S2 Ni1 S1 82.010(17) . 5_556 ?
S1 Ni1 S1 180.0 . 5_556 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.088
####################################################################### 
# 
# 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_2007slh1465
_database_code_depnum_ccdc_archive 'CCDC 1474144'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2007slh1465/ssg1554/208
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H56 N8 Ni2 O8 P4 S10'
_chemical_formula_weight         1338.83

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.728(2)
_cell_length_b                   14.435(3)
_cell_length_c                   18.657(4)
_cell_angle_alpha                104.40(3)
_cell_angle_beta                 103.02(3)
_cell_angle_gamma                101.92(3)
_cell_volume                     2862.9(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6204
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      28.08

_exptl_crystal_description       lath
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_absorpt_coefficient_mu    1.188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8904
_exptl_absorpt_correction_T_max  0.9882
_exptl_absorpt_process_details   'Bruker SADABS'


_exptl_special_details           
;
The above values for Tmin and Tmax were calculated with 
the SIZE command in SHELXL-97. SADABS reports the ratio 
of minimum and maximum transmission as 0.849

;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.6893
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'fine-slice ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        5
_diffrn_reflns_number            25481
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         27.50
_reflns_number_total             12921
_reflns_number_gt                9150
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

The crystal quality was suboptimal and in the end synchrotron data had to be
acquired in order to obtain any usuable data. However, the crystal still 
diffracted poorly at higher angles leading to reduced data completeness. 
The ethoxy chains are all severely disordered, but any attempts to model the
disorder failed and resulted in npd thermal parameters. Hence the ADPs were 
restrained with the ISOR command and bond distances were set to more 
appropriate values with the DFIX command.The residual density is associated 
with the disorder described above.  
;

_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)+(0.1059P)²+17.9696P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12921
_refine_ls_number_parameters     657
_refine_ls_number_restraints     148
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0969
_refine_ls_wR_factor_ref         0.2663
_refine_ls_wR_factor_gt          0.2445
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.008
_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
C1 C 0.0906(10) 0.6176(11) -0.1759(7) 0.095(4) Uani 1 1 d DU . .
H1A H 0.1218 0.5649 -0.2033 0.114 Uiso 1 1 calc R . .
H1B H 0.1316 0.6808 -0.1826 0.114 Uiso 1 1 calc R . .
C2 C -0.0508(10) 0.5922(10) -0.2173(7) 0.083(3) Uani 1 1 d DU . .
H2A H -0.0909 0.5239 -0.2208 0.124 Uiso 1 1 calc R . .
H2B H -0.0631 0.5984 -0.2695 0.124 Uiso 1 1 calc R . .
H2C H -0.0857 0.6386 -0.1873 0.124 Uiso 1 1 calc R . .
C3 C 0.2104(18) 0.5722(13) 0.0519(11) 0.142(7) Uani 1 1 d DU . .
H3A H 0.2882 0.5681 0.0835 0.171 Uiso 1 1 calc R . .
H3B H 0.1704 0.5089 0.0093 0.171 Uiso 1 1 calc R . .
C4 C 0.1271(14) 0.5994(12) 0.1008(9) 0.106(5) Uani 1 1 d DU . .
H4A H 0.0735 0.6336 0.0761 0.159 Uiso 1 1 calc R . .
H4B H 0.1765 0.6435 0.1524 0.159 Uiso 1 1 calc R . .
H4C H 0.0775 0.5387 0.1053 0.159 Uiso 1 1 calc R . .
C5 C 0.9880(10) 0.8095(11) -0.0270(8) 0.103(4) Uani 1 1 d DU . .
H5A H 1.0058 0.8179 -0.0748 0.124 Uiso 1 1 calc R . .
H5B H 0.9742 0.7383 -0.0304 0.124 Uiso 1 1 calc R . .
C6 C 1.0958(10) 0.8743(9) 0.0446(7) 0.080(3) Uani 1 1 d DU . .
H6A H 1.1261 0.9396 0.0386 0.120 Uiso 1 1 calc R . .
H6B H 1.1612 0.8416 0.0496 0.120 Uiso 1 1 calc R . .
H6C H 1.0683 0.8829 0.0911 0.120 Uiso 1 1 calc R . .
C7 C 0.7670(19) 0.8656(11) -0.1900(8) 0.139(7) Uani 1 1 d DU . .
H7A H 0.8308 0.9273 -0.1567 0.167 Uiso 1 1 calc R . .
H7B H 0.6868 0.8794 -0.1962 0.167 Uiso 1 1 calc R . .
C8 C 0.7886(10) 0.8318(8) -0.2691(6) 0.069(3) Uani 1 1 d DU . .
H8A H 0.8564 0.8015 -0.2645 0.103 Uiso 1 1 calc R . .
H8B H 0.8086 0.8893 -0.2875 0.103 Uiso 1 1 calc R . .
H8C H 0.7148 0.7828 -0.3060 0.103 Uiso 1 1 calc R . .
C9 C 0.5701(6) 0.8273(5) 0.1095(4) 0.0306(14) Uani 1 1 d . . .
H9 H 0.5573 0.8819 0.0922 0.037 Uiso 1 1 calc R . .
C10 C 0.5995(6) 0.8396(5) 0.1884(4) 0.0300(14) Uani 1 1 d . . .
C11 C 0.6173(6) 0.7595(5) 0.2138(4) 0.0319(14) Uani 1 1 d . . .
H11 H 0.6380 0.7660 0.2674 0.038 Uiso 1 1 calc R . .
C12 C 0.6042(6) 0.6709(5) 0.1598(4) 0.0339(15) Uani 1 1 d . . .
H12 H 0.6160 0.6151 0.1757 0.041 Uiso 1 1 calc R . .
C13 C 0.5738(6) 0.6633(5) 0.0821(4) 0.0336(15) Uani 1 1 d . . .
H13 H 0.5630 0.6010 0.0452 0.040 Uiso 1 1 calc R . .
C14 C 0.6127(6) 0.9375(5) 0.2414(3) 0.0278(13) Uani 1 1 d . . .
C15 C 0.6083(6) 1.0931(5) 0.2793(4) 0.0271(13) Uani 1 1 d . . .
C16 C 0.5670(6) 1.1949(5) 0.1940(4) 0.0258(13) Uani 1 1 d . . .
H16 H 0.5627 1.1396 0.1523 0.031 Uiso 1 1 calc R . .
C17 C 0.5911(6) 1.1858(5) 0.2685(4) 0.0273(13) Uani 1 1 d . . .
C18 C 0.5957(7) 1.2680(5) 0.3284(4) 0.0336(15) Uani 1 1 d . . .
H18 H 0.6087 1.2646 0.3797 0.040 Uiso 1 1 calc R . .
C19 C 0.5814(7) 1.3534(5) 0.3131(4) 0.0354(15) Uani 1 1 d . . .
H19 H 0.5875 1.4105 0.3540 0.042 Uiso 1 1 calc R . .
C20 C 0.5577(6) 1.3563(5) 0.2372(4) 0.0299(14) Uani 1 1 d . . .
H20 H 0.5470 1.4155 0.2267 0.036 Uiso 1 1 calc R . .
N1 N 0.5590(6) 0.7405(4) 0.0568(3) 0.0334(13) Uani 1 1 d . . .
N2 N 0.5939(5) 1.0132(4) 0.2173(3) 0.0275(11) Uani 1 1 d . . .
N3 N 0.6397(4) 1.0731(4) 0.3552(3) 0.0206(10) Uani 1 1 d U . .
N4 N 0.5499(5) 1.2768(4) 0.1787(3) 0.0298(12) Uani 1 1 d . . .
O1 O 0.1254(12) 0.6270(9) -0.0981(7) 0.133(4) Uani 1 1 d DU . .
O2 O 0.2270(13) 0.6537(9) 0.0246(8) 0.142(4) Uani 1 1 d DU . .
O3 O 0.8851(6) 0.8403(7) -0.0189(4) 0.087(3) Uani 1 1 d DU . .
O4 O 0.7706(10) 0.7899(7) -0.1561(4) 0.098(3) Uani 1 1 d DU . .
P1 P 0.2512(3) 0.6582(2) -0.0604(2) 0.0633(7) Uani 1 1 d . . .
P2 P 0.7535(2) 0.7922(2) -0.07437(12) 0.0515(6) Uani 1 1 d . . .
S1 S 0.33627(19) 0.79909(15) -0.04002(10) 0.0389(4) Uani 1 1 d . . .
S2 S 0.34956(18) 0.56838(14) -0.09077(11) 0.0373(4) Uani 1 1 d . . .
S3 S 0.6629(2) 0.88629(15) -0.03672(11) 0.0486(5) Uani 1 1 d . . .
S4 S 0.6759(2) 0.65461(17) -0.08097(14) 0.0494(5) Uani 1 1 d . . .
S5 S 0.6519(2) 0.96999(17) 0.34056(12) 0.0468(5) Uani 1 1 d . . .
Ni1 Ni 0.50499(8) 0.72745(6) -0.06184(5) 0.0299(2) Uani 1 1 d . . .
C21 C 1.2378(7) 0.3797(6) 0.4754(4) 0.0404(17) Uani 1 1 d DU . .
H21A H 1.1610 0.3979 0.4757 0.048 Uiso 1 1 calc R . .
H21B H 1.2173 0.3076 0.4477 0.048 Uiso 1 1 calc R . .
C22 C 1.3092(10) 0.4399(8) 0.4353(6) 0.071(3) Uani 1 1 d DU . .
H22A H 1.3377 0.5102 0.4666 0.107 Uiso 1 1 calc R . .
H22B H 1.2565 0.4329 0.3843 0.107 Uiso 1 1 calc R . .
H22C H 1.3794 0.4152 0.4292 0.107 Uiso 1 1 calc R . .
C23 C 1.5002(6) 0.3616(6) 0.6613(4) 0.0386(16) Uani 1 1 d DU . .
H23A H 1.5112 0.3780 0.6144 0.046 Uiso 1 1 calc R . .
H23B H 1.4890 0.2893 0.6519 0.046 Uiso 1 1 calc R . .
C24 C 1.6098(8) 0.4208(8) 0.7306(5) 0.062(2) Uani 1 1 d DU . .
H24A H 1.6257 0.4917 0.7354 0.093 Uiso 1 1 calc R . .
H24B H 1.6812 0.3985 0.7236 0.093 Uiso 1 1 calc R . .
H24C H 1.5934 0.4102 0.7776 0.093 Uiso 1 1 calc R . .
C25 C 0.5251(10) 0.1153(9) 0.5128(8) 0.099(4) Uani 1 1 d DU . .
H25A H 0.4931 0.0980 0.5540 0.119 Uiso 1 1 calc R . .
H25B H 0.5475 0.0578 0.4839 0.119 Uiso 1 1 calc R . .
C26 C 0.4344(8) 0.1464(7) 0.4598(5) 0.054(2) Uani 1 1 d DU . .
H26A H 0.4161 0.2047 0.4896 0.081 Uiso 1 1 calc R . .
H26B H 0.3593 0.0915 0.4354 0.081 Uiso 1 1 calc R . .
H26C H 0.4684 0.1631 0.4197 0.081 Uiso 1 1 calc R . .
C27 C 0.7617(11) 0.1252(10) 0.7164(7) 0.084(3) Uani 1 1 d DU . .
H27A H 0.8335 0.1820 0.7481 0.101 Uiso 1 1 calc R . .
H27B H 0.7914 0.0698 0.6914 0.101 Uiso 1 1 calc R . .
C28 C 0.6879(15) 0.0917(13) 0.7692(9) 0.116(5) Uani 1 1 d DU . .
H28A H 0.6337 0.1340 0.7780 0.174 Uiso 1 1 calc R . .
H28B H 0.7441 0.0978 0.8189 0.174 Uiso 1 1 calc R . .
H28C H 0.6393 0.0222 0.7442 0.174 Uiso 1 1 calc R . .
C29 C 0.9464(6) 0.2164(5) 0.4377(4) 0.0292(14) Uani 1 1 d . . .
H29 H 0.9653 0.1565 0.4412 0.035 Uiso 1 1 calc R . .
C30 C 0.9125(6) 0.2290(5) 0.3647(4) 0.0343(15) Uani 1 1 d . . .
C31 C 0.8851(6) 0.3171(6) 0.3598(4) 0.0388(17) Uani 1 1 d . . .
H31 H 0.8629 0.3287 0.3113 0.047 Uiso 1 1 calc R . .
C32 C 0.8910(7) 0.3868(6) 0.4271(5) 0.045(2) Uani 1 1 d . . .
H32 H 0.8721 0.4472 0.4253 0.055 Uiso 1 1 calc R . .
C33 C 0.9241(6) 0.3691(6) 0.4968(5) 0.0392(17) Uani 1 1 d . . .
H33 H 0.9266 0.4178 0.5424 0.047 Uiso 1 1 calc R . .
C34 C 0.9021(6) 0.1484(5) 0.2964(4) 0.0325(15) Uani 1 1 d . . .
C35 C 0.8981(6) -0.0025(6) 0.2350(4) 0.0329(15) Uani 1 1 d . . .
C36 C 0.9301(6) -0.1366(5) 0.2902(4) 0.0315(14) Uani 1 1 d . . .
H36 H 0.9446 -0.0899 0.3395 0.038 Uiso 1 1 calc R . .
C37 C 0.9035(6) -0.1061(6) 0.2245(4) 0.0330(15) Uani 1 1 d . . .
C38 C 0.8802(7) -0.1751(6) 0.1523(4) 0.0424(18) Uani 1 1 d . . .
H38 H 0.8618 -0.1567 0.1064 0.051 Uiso 1 1 calc R . .
C39 C 0.8844(7) -0.2715(6) 0.1489(4) 0.0396(17) Uani 1 1 d . . .
H39 H 0.8682 -0.3205 0.1004 0.048 Uiso 1 1 calc R . .
C40 C 0.9125(6) -0.2953(6) 0.2167(4) 0.0387(17) Uani 1 1 d . . .
H40 H 0.9154 -0.3614 0.2140 0.046 Uiso 1 1 calc R . .
N5 N 0.9531(5) 0.2848(4) 0.5027(3) 0.0330(13) Uani 1 1 d . . .
N6 N 0.9168(5) 0.0593(4) 0.3041(3) 0.0303(12) Uani 1 1 d . . .
N7 N 0.8738(5) 0.1503(4) 0.2146(4) 0.0343(13) Uani 1 1 d U . .
N8 N 0.9361(5) -0.2282(4) 0.2868(3) 0.0315(12) Uani 1 1 d . . .
O5 O 1.3122(5) 0.4015(4) 0.5528(3) 0.0366(11) Uani 1 1 d D . .
O6 O 1.3962(4) 0.3892(4) 0.6798(3) 0.0314(10) Uani 1 1 d D . .
O7 O 0.6240(7) 0.2007(6) 0.5433(6) 0.099(3) Uani 1 1 d D . .
O8 O 0.6906(8) 0.1531(7) 0.6599(5) 0.106(3) Uani 1 1 d D . .
P5 P 1.26771(16) 0.35601(13) 0.61486(10) 0.0289(4) Uani 1 1 d . . .
P6 P 0.7510(2) 0.1883(2) 0.60592(15) 0.0700(9) Uani 1 1 d . . .
S11 S 1.19048(15) 0.21060(12) 0.57210(9) 0.0293(3) Uani 1 1 d . . .
S12 S 1.16163(16) 0.42579(13) 0.66208(10) 0.0331(4) Uani 1 1 d . . .
S13 S 0.85133(19) 0.32668(19) 0.65326(13) 0.0534(6) Uani 1 1 d . . .
S14 S 0.83885(17) 0.10219(15) 0.55453(10) 0.0387(4) Uani 1 1 d . . .
S15 S 0.8613(2) 0.0515(2) 0.16462(12) 0.0569(6) Uani 1 1 d . . .
Ni2 Ni 1.00993(8) 0.26181(6) 0.60979(5) 0.0290(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
C1 O1 1.381(9) . ?
C1 C2 1.585(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 O2 1.389(9) . ?
C3 C4 1.525(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 O3 1.395(9) . ?
C5 C6 1.545(9) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 O4 1.396(9) . ?
C7 C8 1.530(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N1 1.348(9) . ?
C9 C10 1.390(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(9) . ?
C10 C14 1.464(9) . ?
C11 C12 1.372(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(10) . ?
C12 H12 0.9500 . ?
C13 N1 1.341(9) . ?
C13 H13 0.9500 . ?
C14 N2 1.320(9) . ?
C14 S5 1.718(6) . ?
C15 N2 1.366(8) . ?
C15 C17 1.450(9) . ?
C15 N3 1.494(8) . ?
C16 N4 1.326(8) . ?
C16 C17 1.398(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.395(9) . ?
C18 C19 1.367(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.393(10) . ?
C19 H19 0.9500 . ?
C20 N4 1.344(8) . ?
C20 H20 0.9500 . ?
N1 Ni1 2.110(6) . ?
N3 S5 1.488(5) . ?
N4 Ni1 2.111(6) 2_675 ?
O1 P1 1.404(13) . ?
O2 P1 1.686(13) . ?
O3 P2 1.554(8) . ?
O4 P2 1.574(7) . ?
P1 S2 1.970(3) . ?
P1 S1 1.971(4) . ?
P2 S4 1.967(4) . ?
P2 S3 1.981(4) . ?
S1 Ni1 2.480(2) . ?
S2 Ni1 2.469(2) . ?
S3 Ni1 2.496(2) . ?
S4 Ni1 2.501(2) . ?
Ni1 N4 2.111(6) 2_675 ?
C21 O5 1.427(7) . ?
C21 C22 1.524(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 O6 1.445(7) . ?
C23 C24 1.517(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 O7 1.397(9) . ?
C25 C26 1.501(9) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 O8 1.386(9) . ?
C27 C28 1.550(9) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 N5 1.335(9) . ?
C29 C30 1.398(9) . ?
C29 H29 0.9500 . ?
C30 C31 1.393(10) . ?
C30 C34 1.459(10) . ?
C31 C32 1.378(12) . ?
C31 H31 0.9500 . ?
C32 C33 1.372(11) . ?
C32 H32 0.9500 . ?
C33 N5 1.352(9) . ?
C33 H33 0.9500 . ?
C34 N6 1.369(9) . ?
C34 N7 1.497(9) . ?
C35 N6 1.313(9) . ?
C35 C37 1.475(11) . ?
C35 S15 1.706(7) . ?
C36 N8 1.323(9) . ?
C36 C37 1.397(10) . ?
C36 H36 0.9500 . ?
C37 C38 1.392(10) . ?
C38 C39 1.390(12) . ?
C38 H38 0.9500 . ?
C39 C40 1.379(11) . ?
C39 H39 0.9500 . ?
C40 N8 1.349(9) . ?
C40 H40 0.9500 . ?
N5 Ni2 2.090(6) . ?
N7 S15 1.454(7) . ?
N8 Ni2 2.099(6) 2_756 ?
O5 P5 1.598(5) . ?
O6 P5 1.599(5) . ?
O7 P6 1.745(10) . ?
O8 P6 1.485(9) . ?
P5 S12 1.977(3) . ?
P5 S11 1.980(3) . ?
P6 S13 1.959(4) . ?
P6 S14 1.977(4) . ?
S11 Ni2 2.566(2) . ?
S12 Ni2 2.460(2) . ?
S13 Ni2 2.453(2) . ?
S14 Ni2 2.525(2) . ?
Ni2 N8 2.099(6) 2_756 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 117.2(11) . . ?
O1 C1 H1A 108.0 . . ?
C2 C1 H1A 108.0 . . ?
O1 C1 H1B 108.0 . . ?
C2 C1 H1B 108.0 . . ?
H1A C1 H1B 107.2 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O2 C3 C4 99.2(12) . . ?
O2 C3 H3A 111.9 . . ?
C4 C3 H3A 111.9 . . ?
O2 C3 H3B 111.9 . . ?
C4 C3 H3B 111.9 . . ?
H3A C3 H3B 109.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C5 C6 107.6(10) . . ?
O3 C5 H5A 110.2 . . ?
C6 C5 H5A 110.2 . . ?
O3 C5 H5B 110.2 . . ?
C6 C5 H5B 110.2 . . ?
H5A C5 H5B 108.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O4 C7 C8 108.5(10) . . ?
O4 C7 H7A 110.0 . . ?
C8 C7 H7A 110.0 . . ?
O4 C7 H7B 110.0 . . ?
C8 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 122.2(6) . . ?
N1 C9 H9 118.9 . . ?
C10 C9 H9 118.9 . . ?
C11 C10 C9 118.9(6) . . ?
C11 C10 C14 122.9(6) . . ?
C9 C10 C14 118.2(6) . . ?
C12 C11 C10 118.6(6) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C11 C12 C13 119.6(7) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
N1 C13 C12 122.4(7) . . ?
N1 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
N2 C14 C10 122.9(6) . . ?
N2 C14 S5 111.1(5) . . ?
C10 C14 S5 126.0(5) . . ?
N2 C15 C17 120.6(6) . . ?
N2 C15 N3 113.6(5) . . ?
C17 C15 N3 125.7(5) . . ?
N4 C16 C17 123.3(6) . . ?
N4 C16 H16 118.3 . . ?
C17 C16 H16 118.3 . . ?
C18 C17 C16 117.0(6) . . ?
C18 C17 C15 123.8(6) . . ?
C16 C17 C15 119.2(6) . . ?
C19 C18 C17 119.8(7) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C20 119.6(6) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
N4 C20 C19 121.2(7) . . ?
N4 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C13 N1 C9 118.1(6) . . ?
C13 N1 Ni1 122.5(5) . . ?
C9 N1 Ni1 119.1(4) . . ?
C14 N2 C15 109.6(5) . . ?
S5 N3 C15 108.3(4) . . ?
C16 N4 C20 119.1(6) . . ?
C16 N4 Ni1 118.4(4) . 2_675 ?
C20 N4 Ni1 122.2(5) . 2_675 ?
C1 O1 P1 116.7(10) . . ?
C3 O2 P1 128.0(10) . . ?
C5 O3 P2 126.1(8) . . ?
C7 O4 P2 126.2(8) . . ?
O1 P1 O2 91.6(7) . . ?
O1 P1 S2 118.1(6) . . ?
O2 P1 S2 110.2(4) . . ?
O1 P1 S1 117.1(5) . . ?
O2 P1 S1 104.1(5) . . ?
S2 P1 S1 112.41(15) . . ?
O3 P2 O4 103.1(5) . . ?
O3 P2 S4 116.4(4) . . ?
O4 P2 S4 107.1(4) . . ?
O3 P2 S3 103.5(4) . . ?
O4 P2 S3 114.0(4) . . ?
S4 P2 S3 112.53(15) . . ?
P1 S1 Ni1 82.06(10) . . ?
P1 S2 Ni1 82.34(11) . . ?
P2 S3 Ni1 81.64(10) . . ?
P2 S4 Ni1 81.75(11) . . ?
N3 S5 C14 97.2(3) . . ?
N1 Ni1 N4 176.6(2) . 2_675 ?
N1 Ni1 S2 91.48(18) . . ?
N4 Ni1 S2 90.71(17) 2_675 . ?
N1 Ni1 S1 88.65(17) . . ?
N4 Ni1 S1 89.02(16) 2_675 . ?
S2 Ni1 S1 82.86(7) . . ?
N1 Ni1 S3 90.05(18) . . ?
N4 Ni1 S3 87.80(17) 2_675 . ?
S2 Ni1 S3 178.20(8) . . ?
S1 Ni1 S3 98.13(8) . . ?
N1 Ni1 S4 90.12(18) . . ?
N4 Ni1 S4 92.23(17) 2_675 . ?
S2 Ni1 S4 96.88(8) . . ?
S1 Ni1 S4 178.73(8) . . ?
S3 Ni1 S4 82.17(9) . . ?
O5 C21 C22 107.8(7) . . ?
O5 C21 H21A 110.1 . . ?
C22 C21 H21A 110.1 . . ?
O5 C21 H21B 110.1 . . ?
C22 C21 H21B 110.1 . . ?
H21A C21 H21B 108.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O6 C23 C24 106.4(6) . . ?
O6 C23 H23A 110.4 . . ?
C24 C23 H23A 110.4 . . ?
O6 C23 H23B 110.4 . . ?
C24 C23 H23B 110.4 . . ?
H23A C23 H23B 108.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O7 C25 C26 102.3(9) . . ?
O7 C25 H25A 111.3 . . ?
C26 C25 H25A 111.3 . . ?
O7 C25 H25B 111.3 . . ?
C26 C25 H25B 111.3 . . ?
H25A C25 H25B 109.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O8 C27 C28 110.9(11) . . ?
O8 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
O8 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.0 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N5 C29 C30 122.8(6) . . ?
N5 C29 H29 118.6 . . ?
C30 C29 H29 118.6 . . ?
C31 C30 C29 118.5(7) . . ?
C31 C30 C34 122.4(6) . . ?
C29 C30 C34 119.1(6) . . ?
C32 C31 C30 118.2(7) . . ?
C32 C31 H31 120.9 . . ?
C30 C31 H31 120.9 . . ?
C33 C32 C31 120.1(7) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
N5 C33 C32 122.4(7) . . ?
N5 C33 H33 118.8 . . ?
C32 C33 H33 118.8 . . ?
N6 C34 C30 119.8(6) . . ?
N6 C34 N7 113.5(6) . . ?
C30 C34 N7 126.7(6) . . ?
N6 C35 C37 121.2(6) . . ?
N6 C35 S15 111.3(6) . . ?
C37 C35 S15 127.4(5) . . ?
N8 C36 C37 122.7(6) . . ?
N8 C36 H36 118.7 . . ?
C37 C36 H36 118.7 . . ?
C38 C37 C36 118.7(7) . . ?
C38 C37 C35 123.1(7) . . ?
C36 C37 C35 118.2(6) . . ?
C39 C38 C37 118.4(7) . . ?
C39 C38 H38 120.8 . . ?
C37 C38 H38 120.8 . . ?
C40 C39 C38 119.3(7) . . ?
C40 C39 H39 120.4 . . ?
C38 C39 H39 120.4 . . ?
N8 C40 C39 122.3(8) . . ?
N8 C40 H40 118.8 . . ?
C39 C40 H40 118.8 . . ?
C29 N5 C33 117.9(6) . . ?
C29 N5 Ni2 120.3(5) . . ?
C33 N5 Ni2 121.8(5) . . ?
C35 N6 C34 108.7(6) . . ?
S15 N7 C34 108.2(5) . . ?
C36 N8 C40 118.7(6) . . ?
C36 N8 Ni2 119.0(5) . 2_756 ?
C40 N8 Ni2 122.3(5) . 2_756 ?
C21 O5 P5 123.2(4) . . ?
C23 O6 P5 120.7(4) . . ?
C25 O7 P6 114.4(8) . . ?
C27 O8 P6 116.4(8) . . ?
O5 P5 O6 98.3(3) . . ?
O5 P5 S12 112.9(2) . . ?
O6 P5 S12 106.22(19) . . ?
O5 P5 S11 112.2(2) . . ?
O6 P5 S11 115.2(2) . . ?
S12 P5 S11 111.36(11) . . ?
O8 P6 O7 98.5(5) . . ?
O8 P6 S13 111.3(4) . . ?
O7 P6 S13 102.0(3) . . ?
O8 P6 S14 117.1(5) . . ?
O7 P6 S14 114.4(3) . . ?
S13 P6 S14 111.85(14) . . ?
P5 S11 Ni2 82.10(8) . . ?
P5 S12 Ni2 84.97(8) . . ?
P6 S13 Ni2 84.22(11) . . ?
P6 S14 Ni2 81.97(10) . . ?
N7 S15 C35 98.0(4) . . ?
N5 Ni2 N8 176.0(2) . 2_756 ?
N5 Ni2 S13 91.46(18) . . ?
N8 Ni2 S13 90.39(17) 2_756 . ?
N5 Ni2 S12 91.13(17) . . ?
N8 Ni2 S12 92.25(17) 2_756 . ?
S13 Ni2 S12 93.39(8) . . ?
N5 Ni2 S14 86.37(17) . . ?
N8 Ni2 S14 90.44(17) 2_756 . ?
S13 Ni2 S14 81.82(8) . . ?
S12 Ni2 S14 174.53(7) . . ?
N5 Ni2 S11 89.57(18) . . ?
N8 Ni2 S11 88.92(16) 2_756 . ?
S13 Ni2 S11 174.41(8) . . ?
S12 Ni2 S11 81.09(7) . . ?
S14 Ni2 S11 103.73(7) . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         3.191
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.154

####################################################################### 
# 
# 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_RD0728
_database_code_depnum_ccdc_archive 'CCDC 1474145'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H28 N4 Ni P2 S5'
_chemical_formula_sum            'C36 H28 N4 Ni P2 S5'
_chemical_formula_weight         797.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8385(2)
_cell_length_b                   12.0415(3)
_cell_length_c                   22.6405(4)
_cell_angle_alpha                101.922(2)
_cell_angle_beta                 97.350(2)
_cell_angle_gamma                93.086(2)
_cell_volume                     1802.94(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    12883
_cell_measurement_theta_min      3.6594
_cell_measurement_theta_max      32.3861

_exptl_crystal_description       tablets
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93155
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) 
(compiled May  8 2007,13:10:02) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur 3'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 15.9863
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30395
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0664
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.67
_diffrn_reflns_theta_max         32.41
_reflns_number_total             11661
_reflns_number_gt                7622
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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)+(0.0651P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11661
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1140
_refine_ls_wR_factor_gt          0.1033
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_restrained_S_all      0.964
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 1.0000 0.5000 0.01919(8) Uani 1 2 d S . .
Ni2 Ni 0.5000 0.5000 1.0000 0.01990(8) Uani 1 2 d S . .
P1 P -0.05602(8) 0.77328(5) 0.41210(2) 0.02419(12) Uani 1 1 d . . .
P2 P 0.28260(8) 0.27351(5) 0.94590(2) 0.02214(11) Uani 1 1 d . . .
S1 S 0.15509(8) 0.89579(5) 0.41352(2) 0.02570(11) Uani 1 1 d . . .
S2 S -0.22510(8) 0.82348(5) 0.47711(2) 0.02546(11) Uani 1 1 d . . .
S3 S 0.15367(7) 0.42016(4) 0.95689(2) 0.02404(11) Uani 1 1 d . . .
S4 S 0.57586(7) 0.30334(5) 0.95116(2) 0.02505(11) Uani 1 1 d . . .
N1 N 0.1850(2) 0.92861(15) 0.56351(7) 0.0225(3) Uani 1 1 d . . .
C2 C 0.1097(3) 0.88200(19) 0.60544(9) 0.0254(4) Uani 1 1 d . . .
H2A H -0.0286 0.8821 0.6067 0.031 Uiso 1 1 calc R . .
C3 C 0.2231(3) 0.83383(19) 0.64696(9) 0.0261(4) Uani 1 1 d . . .
H3A H 0.1628 0.8017 0.6758 0.031 Uiso 1 1 calc R . .
C4 C 0.4239(3) 0.83277(18) 0.64628(8) 0.0221(4) Uani 1 1 d . . .
C5 C 0.5029(3) 0.8808(2) 0.60306(10) 0.0361(6) Uani 1 1 d . . .
H5A H 0.6407 0.8816 0.6008 0.043 Uiso 1 1 calc R . .
C6 C 0.3793(3) 0.9274(2) 0.56342(10) 0.0338(5) Uani 1 1 d . . .
H6A H 0.4362 0.9606 0.5343 0.041 Uiso 1 1 calc R . .
C7 C 0.5502(3) 0.78011(19) 0.68940(9) 0.0258(4) Uani 1 1 d . . .
N8 N 0.7480(3) 0.7671(2) 0.68585(8) 0.0374(5) Uani 1 1 d . . .
S9 S 0.83296(10) 0.70943(8) 0.73938(3) 0.0562(2) Uani 1 1 d . . .
C10 C 0.6115(3) 0.69559(19) 0.76494(9) 0.0264(4) Uani 1 1 d . . .
N11 N 0.4712(2) 0.73891(15) 0.73353(7) 0.0248(4) Uani 1 1 d . . .
C12 C 0.5812(3) 0.64396(19) 0.81700(9) 0.0250(4) Uani 1 1 d . . .
C13 C 0.7257(3) 0.58423(19) 0.84272(9) 0.0277(4) Uani 1 1 d . . .
H13A H 0.8452 0.5730 0.8259 0.033 Uiso 1 1 calc R . .
C14 C 0.6932(3) 0.54155(19) 0.89305(9) 0.0256(4) Uani 1 1 d . . .
H14A H 0.7928 0.5008 0.9102 0.031 Uiso 1 1 calc R . .
N15 N 0.5277(2) 0.55499(15) 0.91881(7) 0.0231(3) Uani 1 1 d . . .
C16 C 0.3864(3) 0.61086(19) 0.89284(9) 0.0256(4) Uani 1 1 d . . .
H16A H 0.2672 0.6198 0.9101 0.031 Uiso 1 1 calc R . .
C17 C 0.4071(3) 0.65553(19) 0.84248(9) 0.0275(4) Uani 1 1 d . . .
H17A H 0.3035 0.6938 0.8254 0.033 Uiso 1 1 calc R . .
C18 C -0.2085(4) 0.7332(2) 0.33800(10) 0.0375(6) Uani 1 1 d . . .
C19 C -0.4049(4) 0.7577(3) 0.33110(12) 0.0509(8) Uani 1 1 d . . .
H19A H -0.4619 0.7944 0.3653 0.061 Uiso 1 1 calc R . .
C20 C -0.5183(6) 0.7281(4) 0.27359(16) 0.0839(14) Uani 1 1 d . . .
H20A H -0.6537 0.7431 0.2687 0.101 Uiso 1 1 calc R . .
C21 C -0.4335(7) 0.6770(4) 0.22393(15) 0.0948(17) Uani 1 1 d . . .
H21A H -0.5105 0.6582 0.1847 0.114 Uiso 1 1 calc R . .
C22 C -0.2409(8) 0.6531(3) 0.23046(13) 0.0798(14) Uani 1 1 d . . .
H22A H -0.1846 0.6176 0.1958 0.096 Uiso 1 1 calc R . .
C23 C -0.1253(5) 0.6804(3) 0.28776(11) 0.0516(7) Uani 1 1 d . . .
H23A H 0.0090 0.6630 0.2923 0.062 Uiso 1 1 calc R . .
C24 C 0.0536(4) 0.6426(2) 0.42081(11) 0.0349(5) Uani 1 1 d . . .
C25 C -0.0699(5) 0.5447(2) 0.41569(15) 0.0591(8) Uani 1 1 d . . .
H25A H -0.2090 0.5462 0.4064 0.071 Uiso 1 1 calc R . .
C26 C 0.0100(7) 0.4453(3) 0.42416(18) 0.0774(12) Uani 1 1 d . . .
H26A H -0.0749 0.3788 0.4216 0.093 Uiso 1 1 calc R . .
C27 C 0.2088(8) 0.4419(3) 0.43612(19) 0.0853(14) Uani 1 1 d . . .
H27A H 0.2628 0.3724 0.4403 0.102 Uiso 1 1 calc R . .
C28 C 0.3318(6) 0.5383(4) 0.4422(2) 0.0871(14) Uani 1 1 d . . .
H28A H 0.4707 0.5357 0.4517 0.104 Uiso 1 1 calc R . .
C29 C 0.2555(5) 0.6408(3) 0.43456(16) 0.0600(9) Uani 1 1 d . . .
H29A H 0.3411 0.7076 0.4388 0.072 Uiso 1 1 calc R . .
C30 C 0.1775(3) 0.17906(18) 0.87416(9) 0.0266(4) Uani 1 1 d . . .
C31 C -0.0214(3) 0.1789(2) 0.85168(10) 0.0324(5) Uani 1 1 d . . .
H31A H -0.1029 0.2281 0.8741 0.039 Uiso 1 1 calc R . .
C32 C -0.1013(4) 0.1076(2) 0.79692(11) 0.0422(6) Uani 1 1 d . . .
H32A H -0.2375 0.1075 0.7818 0.051 Uiso 1 1 calc R . .
C33 C 0.0176(5) 0.0361(3) 0.76397(12) 0.0516(7) Uani 1 1 d . . .
H33A H -0.0363 -0.0124 0.7260 0.062 Uiso 1 1 calc R . .
C34 C 0.2134(5) 0.0359(3) 0.78656(13) 0.0590(8) Uani 1 1 d . . .
H34A H 0.2945 -0.0136 0.7642 0.071 Uiso 1 1 calc R . .
C35 C 0.2949(4) 0.1065(2) 0.84129(12) 0.0438(6) Uani 1 1 d . . .
H35A H 0.4307 0.1054 0.8564 0.053 Uiso 1 1 calc R . .
C36 C 0.2214(3) 0.19631(18) 1.00326(9) 0.0254(4) Uani 1 1 d . . .
C37 C 0.0370(4) 0.2018(2) 1.02216(11) 0.0398(6) Uani 1 1 d . . .
H37A H -0.0559 0.2472 1.0057 0.048 Uiso 1 1 calc R . .
C38 C -0.0138(4) 0.1421(3) 1.06459(12) 0.0479(7) Uani 1 1 d . . .
H38A H -0.1411 0.1467 1.0771 0.057 Uiso 1 1 calc R . .
C39 C 0.1178(5) 0.0766(2) 1.08865(13) 0.0517(7) Uani 1 1 d . . .
H39A H 0.0832 0.0362 1.1182 0.062 Uiso 1 1 calc R . .
C40 C 0.3013(5) 0.0694(3) 1.06990(15) 0.0591(8) Uani 1 1 d . . .
H40A H 0.3926 0.0229 1.0861 0.071 Uiso 1 1 calc R . .
C41 C 0.3537(4) 0.1296(2) 1.02754(12) 0.0432(6) Uani 1 1 d . . .
H41A H 0.4812 0.1249 1.0152 0.052 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.1377(15) 2_576 ?
Ni1 N1 2.1377(15) . ?
Ni1 S2 2.4788(5) 2_576 ?
Ni1 S2 2.4788(5) . ?
Ni1 S1 2.4884(5) . ?
Ni1 S1 2.4884(5) 2_576 ?
Ni2 N15 2.1053(15) . ?
Ni2 N15 2.1052(15) 2_667 ?
Ni2 S3 2.5023(5) 2_667 ?
Ni2 S3 2.5023(5) . ?
Ni2 S4 2.5094(5) 2_667 ?
Ni2 S4 2.5094(5) . ?
P1 C24 1.815(2) . ?
P1 C18 1.816(2) . ?
P1 S1 2.0001(7) . ?
P1 S2 2.0030(7) . ?
P2 C30 1.816(2) . ?
P2 C36 1.823(2) . ?
P2 S3 2.0000(7) . ?
P2 S4 2.0022(7) . ?
N1 C6 1.329(3) . ?
N1 C2 1.340(2) . ?
C2 C3 1.381(3) . ?
C3 C4 1.376(3) . ?
C4 C5 1.386(3) . ?
C4 C7 1.483(3) . ?
C5 C6 1.378(3) . ?
C7 N11 1.360(2) . ?
C7 N8 1.381(3) . ?
N8 S9 1.5808(18) . ?
S9 C10 1.701(2) . ?
C10 N11 1.315(2) . ?
C10 C12 1.473(3) . ?
C12 C17 1.389(3) . ?
C12 C13 1.391(3) . ?
C13 C14 1.380(3) . ?
C14 N15 1.341(3) . ?
N15 C16 1.349(2) . ?
C16 C17 1.377(3) . ?
C18 C19 1.387(4) . ?
C18 C23 1.389(4) . ?
C19 C20 1.394(4) . ?
C20 C21 1.378(6) . ?
C21 C22 1.359(6) . ?
C22 C23 1.396(4) . ?
C24 C29 1.379(4) . ?
C24 C25 1.388(4) . ?
C25 C26 1.382(5) . ?
C26 C27 1.356(6) . ?
C27 C28 1.369(6) . ?
C28 C29 1.399(4) . ?
C30 C35 1.386(3) . ?
C30 C31 1.390(3) . ?
C31 C32 1.382(3) . ?
C32 C33 1.387(4) . ?
C33 C34 1.372(4) . ?
C34 C35 1.380(4) . ?
C36 C41 1.378(3) . ?
C36 C37 1.383(3) . ?
C37 C38 1.380(3) . ?
C38 C39 1.363(4) . ?
C39 C40 1.376(4) . ?
C40 C41 1.386(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
N1 Ni1 N1 180.00(6) 2_576 . ?
N1 Ni1 S2 88.77(5) 2_576 2_576 ?
N1 Ni1 S2 91.23(5) . 2_576 ?
N1 Ni1 S2 91.23(5) 2_576 . ?
N1 Ni1 S2 88.77(5) . . ?
S2 Ni1 S2 180.0 2_576 . ?
N1 Ni1 S1 88.78(5) 2_576 . ?
N1 Ni1 S1 91.22(5) . . ?
S2 Ni1 S1 97.054(17) 2_576 . ?
S2 Ni1 S1 82.946(17) . . ?
N1 Ni1 S1 91.22(5) 2_576 2_576 ?
N1 Ni1 S1 88.78(5) . 2_576 ?
S2 Ni1 S1 82.946(17) 2_576 2_576 ?
S2 Ni1 S1 97.054(17) . 2_576 ?
S1 Ni1 S1 180.000(1) . 2_576 ?
N15 Ni2 N15 180.000(1) . 2_667 ?
N15 Ni2 S3 90.41(5) . 2_667 ?
N15 Ni2 S3 89.59(5) 2_667 2_667 ?
N15 Ni2 S3 89.59(5) . . ?
N15 Ni2 S3 90.41(5) 2_667 . ?
S3 Ni2 S3 180.0 2_667 . ?
N15 Ni2 S4 89.67(5) . 2_667 ?
N15 Ni2 S4 90.33(5) 2_667 2_667 ?
S3 Ni2 S4 81.900(17) 2_667 2_667 ?
S3 Ni2 S4 98.100(17) . 2_667 ?
N15 Ni2 S4 90.33(5) . . ?
N15 Ni2 S4 89.67(5) 2_667 . ?
S3 Ni2 S4 98.100(17) 2_667 . ?
S3 Ni2 S4 81.900(17) . . ?
S4 Ni2 S4 180.0 2_667 . ?
C24 P1 C18 103.35(12) . . ?
C24 P1 S1 110.29(9) . . ?
C18 P1 S1 111.35(8) . . ?
C24 P1 S2 111.09(8) . . ?
C18 P1 S2 110.04(9) . . ?
S1 P1 S2 110.53(3) . . ?
C30 P2 C36 103.76(10) . . ?
C30 P2 S3 110.53(7) . . ?
C36 P2 S3 109.54(7) . . ?
C30 P2 S4 111.46(7) . . ?
C36 P2 S4 111.05(7) . . ?
S3 P2 S4 110.32(3) . . ?
P1 S1 Ni1 83.17(2) . . ?
P1 S2 Ni1 83.36(2) . . ?
P2 S3 Ni2 81.98(2) . . ?
P2 S4 Ni2 81.76(2) . . ?
C6 N1 C2 116.58(16) . . ?
C6 N1 Ni1 122.15(12) . . ?
C2 N1 Ni1 121.26(13) . . ?
N1 C2 C3 123.32(18) . . ?
C4 C3 C2 119.56(17) . . ?
C3 C4 C5 117.45(17) . . ?
C3 C4 C7 121.20(17) . . ?
C5 C4 C7 121.34(18) . . ?
C6 C5 C4 119.26(19) . . ?
N1 C6 C5 123.82(18) . . ?
N11 C7 N8 117.10(17) . . ?
N11 C7 C4 120.25(18) . . ?
N8 C7 C4 122.61(16) . . ?
C7 N8 S9 108.08(12) . . ?
N8 S9 C10 94.30(9) . . ?
N11 C10 C12 123.95(18) . . ?
N11 C10 S9 111.90(14) . . ?
C12 C10 S9 124.13(15) . . ?
C10 N11 C7 108.54(17) . . ?
C17 C12 C13 118.07(17) . . ?
C17 C12 C10 120.45(17) . . ?
C13 C12 C10 121.47(18) . . ?
C14 C13 C12 119.18(19) . . ?
N15 C14 C13 123.01(18) . . ?
C14 N15 C16 117.48(16) . . ?
C14 N15 Ni2 120.67(12) . . ?
C16 N15 Ni2 121.73(13) . . ?
N15 C16 C17 123.02(19) . . ?
C16 C17 C12 119.19(18) . . ?
C19 C18 C23 120.1(2) . . ?
C19 C18 P1 120.5(2) . . ?
C23 C18 P1 119.4(2) . . ?
C18 C19 C20 119.6(3) . . ?
C21 C20 C19 119.9(4) . . ?
C22 C21 C20 120.7(3) . . ?
C21 C22 C23 120.4(3) . . ?
C18 C23 C22 119.3(3) . . ?
C29 C24 C25 120.1(3) . . ?
C29 C24 P1 120.9(2) . . ?
C25 C24 P1 118.9(2) . . ?
C26 C25 C24 119.9(4) . . ?
C27 C26 C25 120.4(4) . . ?
C26 C27 C28 120.2(3) . . ?
C27 C28 C29 120.8(4) . . ?
C24 C29 C28 118.6(3) . . ?
C35 C30 C31 119.4(2) . . ?
C35 C30 P2 120.34(18) . . ?
C31 C30 P2 120.30(17) . . ?
C32 C31 C30 120.4(2) . . ?
C31 C32 C33 119.9(2) . . ?
C34 C33 C32 119.5(2) . . ?
C33 C34 C35 121.1(3) . . ?
C34 C35 C30 119.7(3) . . ?
C41 C36 C37 118.7(2) . . ?
C41 C36 P2 121.40(18) . . ?
C37 C36 P2 119.92(16) . . ?
C38 C37 C36 120.8(2) . . ?
C39 C38 C37 120.3(3) . . ?
C38 C39 C40 119.6(2) . . ?
C39 C40 C41 120.4(3) . . ?
C36 C41 C40 120.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.901
_diffrn_reflns_theta_full        32.41
_diffrn_measured_fraction_theta_full 0.901
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.087

#===END
####################################################################### 
# 
# 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_2007slh0908
_database_code_depnum_ccdc_archive 'CCDC 1474146'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2007slh0908/189
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H28 N4 Ni O4 P2 S5'
_chemical_formula_weight         765.49

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2/n

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

_cell_length_a                   12.8213(3)
_cell_length_b                   7.2342(2)
_cell_length_c                   19.1246(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.1860(10)
_cell_angle_gamma                90.00
_cell_volume                     1703.53(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    16332
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       shard
_exptl_crystal_colour            'light green'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8885
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19777
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.50
_reflns_number_total             3900
_reflns_number_gt                3388
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0134P)²+2.6910P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3900
_refine_ls_number_parameters     213
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0778
_refine_ls_wR_factor_gt          0.0741
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_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
C1 C 0.19495(17) -0.1686(3) 0.49831(12) 0.0210(4) Uani 1 1 d . . .
C2 C 0.20254(18) -0.3601(3) 0.50438(12) 0.0246(5) Uani 1 1 d . . .
H2 H 0.2445 -0.4262 0.4789 0.030 Uiso 1 1 calc R . .
C3 C 0.14948(18) -0.4558(3) 0.54726(13) 0.0269(5) Uani 1 1 d . . .
H3 H 0.1560 -0.5864 0.5516 0.032 Uiso 1 1 calc R . .
C4 C 0.08672(17) -0.3596(3) 0.58378(12) 0.0233(5) Uani 1 1 d . . .
C5 C 0.07885(17) -0.1674(3) 0.57832(12) 0.0228(5) Uani 1 1 d . . .
H5 H 0.0362 -0.1016 0.6034 0.027 Uiso 1 1 calc R . .
C6 C 0.13312(17) -0.0733(3) 0.53645(12) 0.0214(4) Uani 1 1 d . . .
H6 H 0.1285 0.0577 0.5335 0.026 Uiso 1 1 calc R . .
C7 C 0.0378(2) -0.6345(4) 0.63548(15) 0.0374(6) Uani 1 1 d . . .
H7A H 0.0116 -0.6940 0.5877 0.056 Uiso 1 1 calc R . .
H7B H -0.0067 -0.6746 0.6668 0.056 Uiso 1 1 calc R . .
H7C H 0.1137 -0.6694 0.6578 0.056 Uiso 1 1 calc R . .
C8 C 0.1674(2) 0.1405(6) 0.32131(16) 0.0584(10) Uani 1 1 d . . .
H8A H 0.2313 0.2190 0.3404 0.088 Uiso 1 1 calc R . .
H8B H 0.1024 0.2181 0.3056 0.088 Uiso 1 1 calc R . .
H8C H 0.1762 0.0694 0.2797 0.088 Uiso 1 1 calc R . .
C9 C 0.58237(17) 0.1056(3) 0.36948(11) 0.0206(4) Uani 1 1 d . . .
H9 H 0.5954 -0.0237 0.3695 0.025 Uiso 1 1 calc R . .
C10 C 0.62095(17) 0.2162(3) 0.32289(11) 0.0208(5) Uani 1 1 d . A .
C11 C 0.59845(18) 0.4044(3) 0.32005(13) 0.0255(5) Uani 1 1 d . . .
H11 H 0.6240 0.4839 0.2889 0.031 Uiso 1 1 calc R . .
C12 C 0.53789(19) 0.4728(3) 0.36383(13) 0.0283(5) Uani 1 1 d . . .
H12 H 0.5184 0.5998 0.3618 0.034 Uiso 1 1 calc R . .
C13 C 0.50586(18) 0.3534(3) 0.41083(13) 0.0253(5) Uani 1 1 d . . .
H13 H 0.4665 0.4029 0.4419 0.030 Uiso 1 1 calc R . .
C14 C 0.69101(17) 0.1376(3) 0.28138(11) 0.0203(4) Uani 1 1 d . . .
N1 N 0.52769(14) 0.1718(3) 0.41452(10) 0.0206(4) Uani 1 1 d . . .
S3 S 0.7114(6) -0.0848(11) 0.2741(4) 0.0244(7) Uani 0.508(7) 1 d P A 1
N2 N 0.7005(18) -0.052(3) 0.2749(12) 0.031(6) Uani 0.492(7) 1 d P A 2
N3 N 0.7500 0.2450(4) 0.2500 0.0182(5) Uani 1 2 d S . .
O1 O 0.03027(13) -0.4386(2) 0.62679(9) 0.0288(4) Uani 1 1 d . . .
O2 O 0.15599(13) 0.0153(3) 0.37751(9) 0.0326(4) Uani 1 1 d . . .
P1 P 0.26068(4) -0.03953(9) 0.44239(3) 0.02152(13) Uani 1 1 d . . .
S1 S 0.33393(4) 0.18447(8) 0.49487(3) 0.02267(13) Uani 1 1 d . . .
S2 S 0.36728(5) -0.18974(9) 0.40842(3) 0.02579(14) Uani 1 1 d . . .
Ni1 Ni 0.5000 0.0000 0.5000 0.01855(10) Uani 1 2 d S . .


_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
C1 C2 1.392(3) . ?
C1 C6 1.399(3) . ?
C1 P1 1.797(2) . ?
C2 C3 1.388(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(3) . ?
C3 H3 0.9500 . ?
C4 O1 1.363(3) . ?
C4 C5 1.396(3) . ?
C5 C6 1.378(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O1 1.427(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 O2 1.444(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N1 1.341(3) . ?
C9 C10 1.387(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(3) . ?
C10 C14 1.469(3) . ?
C11 C12 1.382(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(3) . ?
C12 H12 0.9500 . ?
C13 N1 1.342(3) . ?
C13 H13 0.9500 . ?
C14 N3 1.337(3) . ?
C14 N2 1.39(2) . ?
C14 S3 1.643(8) . ?
N1 Ni1 2.1601(18) . ?
N3 C14 1.337(3) 2_655 ?
O2 P1 1.6032(17) . ?
P1 S2 1.9915(8) . ?
P1 S1 1.9974(8) . ?
S1 Ni1 2.4915(5) . ?
S2 Ni1 2.4870(6) . ?
Ni1 N1 2.1601(18) 3_656 ?
Ni1 S2 2.4870(6) 3_656 ?
Ni1 S1 2.4915(5) 3_656 ?

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
C2 C1 C6 118.9(2) . . ?
C2 C1 P1 122.24(17) . . ?
C6 C1 P1 118.83(18) . . ?
C3 C2 C1 120.8(2) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C2 C3 C4 119.7(2) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
O1 C4 C3 124.9(2) . . ?
O1 C4 C5 115.0(2) . . ?
C3 C4 C5 120.1(2) . . ?
C6 C5 C4 119.9(2) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C1 120.7(2) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 123.4(2) . . ?
N1 C9 H9 118.3 . . ?
C10 C9 H9 118.3 . . ?
C9 C10 C11 118.9(2) . . ?
C9 C10 C14 120.3(2) . . ?
C11 C10 C14 120.6(2) . . ?
C12 C11 C10 118.2(2) . . ?
C12 C11 H11 120.9 . . ?
C10 C11 H11 120.9 . . ?
C11 C12 C13 119.1(2) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
N1 C13 C12 123.2(2) . . ?
N1 C13 H13 118.4 . . ?
C12 C13 H13 118.4 . . ?
N3 C14 N2 117.4(10) . . ?
N3 C14 C10 121.7(2) . . ?
N2 C14 C10 120.9(10) . . ?
N3 C14 S3 114.1(3) . . ?
N2 C14 S3 4.1(11) . . ?
C10 C14 S3 124.1(3) . . ?
C9 N1 C13 117.04(19) . . ?
C9 N1 Ni1 120.41(15) . . ?
C13 N1 Ni1 121.84(15) . . ?
C14 N3 C14 109.0(3) 2_655 . ?
C4 O1 C7 117.1(2) . . ?
C8 O2 P1 119.66(17) . . ?
O2 P1 C1 99.14(9) . . ?
O2 P1 S2 112.66(7) . . ?
C1 P1 S2 112.90(8) . . ?
O2 P1 S1 111.28(8) . . ?
C1 P1 S1 110.81(8) . . ?
S2 P1 S1 109.71(3) . . ?
P1 S1 Ni1 82.08(2) . . ?
P1 S2 Ni1 82.31(3) . . ?
N1 Ni1 N1 180.0 . 3_656 ?
N1 Ni1 S2 90.52(5) . . ?
N1 Ni1 S2 89.48(5) 3_656 . ?
N1 Ni1 S2 89.48(5) . 3_656 ?
N1 Ni1 S2 90.52(5) 3_656 3_656 ?
S2 Ni1 S2 180.0 . 3_656 ?
N1 Ni1 S1 91.09(5) . 3_656 ?
N1 Ni1 S1 88.91(5) 3_656 3_656 ?
S2 Ni1 S1 98.138(19) . 3_656 ?
S2 Ni1 S1 81.862(19) 3_656 3_656 ?
N1 Ni1 S1 88.91(5) . . ?
N1 Ni1 S1 91.09(5) 3_656 . ?
S2 Ni1 S1 81.862(19) . . ?
S2 Ni1 S1 98.138(19) 3_656 . ?
S1 Ni1 S1 180.00(3) 3_656 . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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_04slh027
_database_code_depnum_ccdc_archive 'CCDC 1474147'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H20 N4 Ni O4 P2 S5'
_chemical_formula_weight         613.31

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   16.542(3)
_cell_length_b                   7.489(2)
_cell_length_c                   20.642(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.29(2)
_cell_angle_gamma                90.00
_cell_volume                     2550.0(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6098
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       'cut needle'
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8788
_exptl_absorpt_correction_T_max  0.9489
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'Φ & ω scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32091
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5840
_reflns_number_gt                4078
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0431P)²+4.9629P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    difmap
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5840
_refine_ls_number_parameters     400
_refine_ls_number_restraints     154
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1031
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.239
_refine_ls_shift/su_mean         0.007

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
C1 C 0.9971(3) 0.9411(8) 0.2113(2) 0.0418(12) Uani 1 1 d . . .
C2 C 1.1535(3) 0.5285(5) 0.1540(2) 0.0305(9) Uani 1 1 d . . .
C3 C 0.5953(3) 0.6267(9) 0.6508(3) 0.0521(15) Uani 1 1 d . . .
C4 C 0.7674(3) 0.9530(8) 0.4962(2) 0.0381(11) Uani 1 1 d . . .
C5 C 0.8520(2) 1.0419(5) 0.07790(19) 0.0241(8) Uani 1 1 d . . .
C6 C 0.8038(2) 1.1120(5) 0.12292(18) 0.0217(8) Uani 1 1 d . A .
C7 C 0.8230(2) 1.2785(5) 0.14897(17) 0.0194(7) Uani 1 1 d . . .
C8 C 0.8889(2) 1.3693(5) 0.12769(18) 0.0222(8) Uani 1 1 d . A .
C9 C 0.9344(2) 1.2874(5) 0.08300(17) 0.0204(8) Uani 1 1 d . . .
C10 C 0.7772(2) 1.3547(5) 0.20150(17) 0.0223(6) Uani 0.618(5) 1 d PDU A 1
C11 C 0.7017(2) 1.3568(5) 0.28326(18) 0.0241(7) Uani 0.618(5) 1 d PDU A 1
N2 N 0.732(4) 1.253(2) 0.238(3) 0.0227(10) Uani 0.618(5) 1 d PDU A 1
N3 N 0.7199(7) 1.5303(13) 0.2851(5) 0.0249(13) Uani 0.618(5) 1 d PDU A 1
S5 S 0.77885(17) 1.5711(3) 0.22598(12) 0.0242(5) Uani 0.618(5) 1 d PDU A 1
C110 C 0.7017(2) 1.3568(5) 0.28326(18) 0.0241(7) Uani 0.382(5) 1 d PDU A 2
C111 C 0.7772(2) 1.3547(5) 0.20150(17) 0.0223(6) Uani 0.382(5) 1 d PDU A 2
N12 N 0.729(6) 1.254(4) 0.237(4) 0.0228(12) Uani 0.382(5) 1 d PDU A 2
N13 N 0.7836(10) 1.5272(16) 0.2145(7) 0.0233(14) Uani 0.382(5) 1 d PDU A 2
S15 S 0.7301(3) 1.5690(5) 0.2768(2) 0.0252(8) Uani 0.382(5) 1 d PDU A 2
C12 C 0.6533(2) 1.2786(5) 0.33333(17) 0.0218(8) Uani 1 1 d . . .
C13 C 0.6211(2) 1.1090(5) 0.32516(18) 0.0233(8) Uani 1 1 d . A .
C14 C 0.5791(2) 1.0353(5) 0.37404(18) 0.0244(8) Uani 1 1 d . . .
C15 C 0.6000(2) 1.2830(5) 0.43755(18) 0.0220(8) Uani 1 1 d . . .
C16 C 0.6428(2) 1.3674(5) 0.39122(19) 0.0240(8) Uani 1 1 d . A .
N1 N 0.91829(17) 1.1244(4) 0.05833(14) 0.0193(6) Uani 1 1 d . A .
N4 N 0.56767(17) 1.1206(4) 0.42985(14) 0.0192(6) Uani 1 1 d . A .
O1 O 1.06623(16) 0.8403(4) 0.19291(12) 0.0276(6) Uani 1 1 d . . .
O2 O 1.16132(15) 0.7033(3) 0.12483(13) 0.0261(6) Uani 1 1 d . . .
O3 O 0.66430(17) 0.7009(4) 0.62206(14) 0.0350(7) Uani 1 1 d . . .
O4 O 0.74383(15) 0.8425(4) 0.54871(14) 0.0321(7) Uani 1 1 d . . .
P1 P 1.08453(6) 0.83101(13) 0.11791(5) 0.0216(2) Uani 1 1 d . . .
P2 P 0.65075(6) 0.83463(14) 0.56278(5) 0.0248(2) Uani 1 1 d . . .
S1 S 1.11588(6) 1.06334(13) 0.08270(5) 0.0238(2) Uani 1 1 d . A .
S2 S 0.99157(6) 0.72574(12) 0.06498(4) 0.0218(2) Uani 1 1 d . A .
S3 S 0.58108(6) 0.72748(12) 0.49081(5) 0.0242(2) Uani 1 1 d . A .
S4 S 0.60842(5) 1.07063(13) 0.58668(4) 0.0231(2) Uani 1 1 d . A .
Ni1A Ni 1.0000 1.0000 0.0000 0.01760(16) Uani 1 2 d S . .
Ni1B Ni 0.5000 1.0000 0.5000 0.01645(16) Uani 1 2 d S . .
H1A H 0.945(3) 0.884(7) 0.186(2) 0.053(14) Uiso 1 1 d . . .
H1B H 0.998(2) 0.937(5) 0.254(2) 0.021(10) Uiso 1 1 d . . .
H1C H 1.010(3) 1.072(8) 0.200(3) 0.073(18) Uiso 1 1 d . . .
H2A H 1.108(3) 0.460(7) 0.128(2) 0.056(15) Uiso 1 1 d . . .
H2B H 1.142(3) 0.545(6) 0.200(2) 0.037(12) Uiso 1 1 d . . .
H2C H 1.207(3) 0.469(7) 0.154(2) 0.061(16) Uiso 1 1 d . . .
H3A H 0.547(4) 0.586(9) 0.617(3) 0.09(2) Uiso 1 1 d . . .
H3B H 0.621(4) 0.524(9) 0.672(3) 0.08(2) Uiso 1 1 d . . .
H3C H 0.574(4) 0.716(8) 0.677(3) 0.072(19) Uiso 1 1 d . . .
H4A H 0.831(3) 0.927(7) 0.491(3) 0.070(16) Uiso 1 1 d . . .
H4B H 0.742(3) 0.919(6) 0.458(2) 0.037(13) Uiso 1 1 d . . .
H4C H 0.751(3) 1.069(7) 0.500(2) 0.039(13) Uiso 1 1 d . . .
H5 H 0.842(2) 0.928(5) 0.0614(17) 0.016(9) Uiso 1 1 d . . .
H6 H 0.757(2) 1.041(5) 0.1341(17) 0.021(10) Uiso 1 1 d . . .
H8 H 0.902(2) 1.482(5) 0.1419(17) 0.016(9) Uiso 1 1 d . . .
H9 H 0.980(2) 1.341(4) 0.0684(15) 0.006(8) Uiso 1 1 d . . .
H13 H 0.628(2) 1.042(5) 0.2914(19) 0.024(11) Uiso 1 1 d . . .
H14 H 0.552(2) 0.931(6) 0.3685(18) 0.022(10) Uiso 1 1 d . . .
H15 H 0.591(2) 1.342(5) 0.4752(19) 0.024(10) Uiso 1 1 d . . .
H16 H 0.661(2) 1.479(5) 0.3973(16) 0.009(9) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.445(5) . ?
C1 H1A 1.07(5) . ?
C1 H1B 0.88(4) . ?
C1 H1C 1.03(6) . ?
C2 O2 1.450(5) . ?
C2 H2A 1.02(5) . ?
C2 H2B 0.98(4) . ?
C2 H2C 0.99(5) . ?
C3 O3 1.437(6) . ?
C3 H3A 1.05(7) . ?
C3 H3B 0.97(7) . ?
C3 H3C 0.94(6) . ?
C4 O4 1.440(5) . ?
C4 H4A 1.08(6) . ?
C4 H4B 0.91(5) . ?
C4 H4C 0.92(5) . ?
C5 N1 1.347(5) . ?
C5 C6 1.373(5) . ?
C5 H5 0.93(4) . ?
C6 C7 1.386(5) . ?
C6 H6 0.99(4) . ?
C7 C8 1.384(5) . ?
C7 C10 1.483(5) . ?
C8 C9 1.377(5) . ?
C8 H8 0.92(4) . ?
C9 N1 1.342(5) . ?
C9 H9 0.93(3) . ?
C10 N2 1.33(2) . ?
C10 S5 1.698(4) . ?
C11 N3 1.334(10) . ?
C11 N2 1.35(2) . ?
C11 C12 1.475(5) . ?
N3 S5 1.646(8) . ?
N13 S15 1.644(11) . ?
C12 C13 1.383(5) . ?
C12 C16 1.389(5) . ?
C13 C14 1.381(5) . ?
C13 H13 0.87(4) . ?
C14 N4 1.343(5) . ?
C14 H14 0.91(4) . ?
C15 N4 1.333(5) . ?
C15 C16 1.385(5) . ?
C15 H15 0.92(4) . ?
C16 H16 0.89(4) . ?
N1 Ni1A 2.095(3) . ?
N4 Ni1B 2.100(3) . ?
O1 P1 1.601(3) . ?
O2 P1 1.588(3) . ?
O3 P2 1.584(3) . ?
O4 P2 1.589(3) . ?
P1 S1 1.9700(14) . ?
P1 S2 1.9821(14) . ?
P2 S4 1.9772(14) . ?
P2 S3 1.9806(15) . ?
S1 Ni1A 2.5147(11) . ?
S2 Ni1A 2.4628(10) . ?
S3 Ni1B 2.4573(10) . ?
S4 Ni1B 2.4935(11) . ?
Ni1A N1 2.095(3) 3_775 ?
Ni1A S2 2.4628(10) 3_775 ?
Ni1A S1 2.5147(11) 3_775 ?
Ni1B N4 2.100(3) 3_676 ?
Ni1B S3 2.4573(10) 3_676 ?
Ni1B S4 2.4935(11) 3_676 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 H1A 107(3) . . ?
O1 C1 H1B 107(3) . . ?
H1A C1 H1B 116(4) . . ?
O1 C1 H1C 105(3) . . ?
H1A C1 H1C 116(4) . . ?
H1B C1 H1C 106(4) . . ?
O2 C2 H2A 109(3) . . ?
O2 C2 H2B 108(3) . . ?
H2A C2 H2B 112(4) . . ?
O2 C2 H2C 108(3) . . ?
H2A C2 H2C 113(4) . . ?
H2B C2 H2C 107(4) . . ?
O3 C3 H3A 115(3) . . ?
O3 C3 H3B 99(4) . . ?
H3A C3 H3B 110(5) . . ?
O3 C3 H3C 108(4) . . ?
H3A C3 H3C 106(5) . . ?
H3B C3 H3C 119(5) . . ?
O4 C4 H4A 107(3) . . ?
O4 C4 H4B 111(3) . . ?
H4A C4 H4B 105(4) . . ?
O4 C4 H4C 112(3) . . ?
H4A C4 H4C 118(4) . . ?
H4B C4 H4C 103(4) . . ?
N1 C5 C6 123.7(3) . . ?
N1 C5 H5 116(2) . . ?
C6 C5 H5 120(2) . . ?
C5 C6 C7 118.6(3) . . ?
C5 C6 H6 117(2) . . ?
C7 C6 H6 124(2) . . ?
C8 C7 C6 118.8(3) . . ?
C8 C7 C10 120.1(3) . . ?
C6 C7 C10 121.0(3) . . ?
C9 C8 C7 118.5(4) . . ?
C9 C8 H8 120(2) . . ?
C7 C8 H8 122(2) . . ?
N1 C9 C8 123.8(3) . . ?
N1 C9 H9 115(2) . . ?
C8 C9 H9 122(2) . . ?
N2 C10 C7 121.9(8) . . ?
N2 C10 S5 112.1(8) . . ?
C7 C10 S5 125.9(3) . . ?
N3 C11 N2 118.8(9) . . ?
N3 C11 C12 120.0(5) . . ?
N2 C11 C12 121.0(8) . . ?
C10 N2 C11 108.7(6) . . ?
C11 N3 S5 107.8(7) . . ?
N3 S5 C10 92.6(4) . . ?
C13 C12 C16 118.2(3) . . ?
C13 C12 C11 120.2(3) . . ?
C16 C12 C11 121.5(3) . . ?
C14 C13 C12 119.2(3) . . ?
C14 C13 H13 117(3) . . ?
C12 C13 H13 124(3) . . ?
N4 C14 C13 123.2(3) . . ?
N4 C14 H14 115(2) . . ?
C13 C14 H14 122(2) . . ?
N4 C15 C16 123.7(3) . . ?
N4 C15 H15 117(2) . . ?
C16 C15 H15 119(2) . . ?
C15 C16 C12 118.6(4) . . ?
C15 C16 H16 121(2) . . ?
C12 C16 H16 120(2) . . ?
C9 N1 C5 116.5(3) . . ?
C9 N1 Ni1A 120.3(2) . . ?
C5 N1 Ni1A 122.9(2) . . ?
C15 N4 C14 117.1(3) . . ?
C15 N4 Ni1B 122.7(2) . . ?
C14 N4 Ni1B 120.3(2) . . ?
C1 O1 P1 119.2(3) . . ?
C2 O2 P1 119.0(2) . . ?
C3 O3 P2 119.5(3) . . ?
C4 O4 P2 118.7(3) . . ?
O2 P1 O1 98.46(14) . . ?
O2 P1 S1 109.53(11) . . ?
O1 P1 S1 113.11(11) . . ?
O2 P1 S2 113.10(11) . . ?
O1 P1 S2 110.81(11) . . ?
S1 P1 S2 111.27(6) . . ?
O3 P2 O4 94.68(15) . . ?
O3 P2 S4 113.86(12) . . ?
O4 P2 S4 112.24(12) . . ?
O3 P2 S3 111.35(13) . . ?
O4 P2 S3 113.28(12) . . ?
S4 P2 S3 110.63(6) . . ?
P1 S1 Ni1A 82.85(4) . . ?
P1 S2 Ni1A 83.99(4) . . ?
P2 S3 Ni1B 84.03(4) . . ?
P2 S4 Ni1B 83.13(4) . . ?
N1 Ni1A N1 180.00(12) . 3_775 ?
N1 Ni1A S2 89.57(8) . . ?
N1 Ni1A S2 90.43(8) 3_775 . ?
N1 Ni1A S2 90.43(8) . 3_775 ?
N1 Ni1A S2 89.57(8) 3_775 3_775 ?
S2 Ni1A S2 180.00(4) . 3_775 ?
N1 Ni1A S1 88.98(9) . 3_775 ?
N1 Ni1A S1 91.02(9) 3_775 3_775 ?
S2 Ni1A S1 98.11(3) . 3_775 ?
S2 Ni1A S1 81.89(3) 3_775 3_775 ?
N1 Ni1A S1 91.02(9) . . ?
N1 Ni1A S1 88.98(9) 3_775 . ?
S2 Ni1A S1 81.89(3) . . ?
S2 Ni1A S1 98.11(3) 3_775 . ?
S1 Ni1A S1 180.00(3) 3_775 . ?
N4 Ni1B N4 180.000(1) 3_676 . ?
N4 Ni1B S3 91.04(8) 3_676 . ?
N4 Ni1B S3 88.96(8) . . ?
N4 Ni1B S3 88.96(8) 3_676 3_676 ?
N4 Ni1B S3 91.04(8) . 3_676 ?
S3 Ni1B S3 180.00(4) . 3_676 ?
N4 Ni1B S4 89.33(9) 3_676 . ?
N4 Ni1B S4 90.67(9) . . ?
S3 Ni1B S4 82.19(3) . . ?
S3 Ni1B S4 97.81(3) 3_676 . ?
N4 Ni1B S4 90.67(9) 3_676 3_676 ?
N4 Ni1B S4 89.33(9) . 3_676 ?
S3 Ni1B S4 97.81(3) . 3_676 ?
S3 Ni1B S4 82.19(3) 3_676 3_676 ?
S4 Ni1B S4 180.0 . 3_676 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.104
####################################################################### 
# 
# 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_2007slh0906
_database_code_depnum_ccdc_archive 'CCDC 1474148'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 2007slh0906/187
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H28 N4 Ni O4 P2 S5'
_chemical_formula_weight         765.49

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7075(2)
_cell_length_b                   10.6736(2)
_cell_length_c                   17.4582(3)
_cell_angle_alpha                73.2300(10)
_cell_angle_beta                 87.0860(10)
_cell_angle_gamma                72.1310(10)
_cell_volume                     1647.02(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    23735
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       fragment
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_absorpt_coefficient_mu    1.044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7587
_exptl_absorpt_correction_T_max  0.9211
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'

_exptl_special_details           
;
The values for minimum and maximum transmission are based
on the cell dimensions only and were generated using the 
size command in SHELX. SADABS reports the maximum and minimum
transmission factors as 0.6717 and 0.7456, respectively.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36271
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7555
_reflns_number_gt                6352
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0273P)²+1.7248P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0045(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7555
_refine_ls_number_parameters     424
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0850
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.002
_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
C1 C -0.7435(2) -0.2816(2) 0.50136(14) 0.0230(5) Uani 1 1 d . . .
C2 C -0.8408(3) -0.2147(3) 0.54936(15) 0.0278(5) Uani 1 1 d . . .
H2 H -0.8394 -0.1271 0.5514 0.033 Uiso 1 1 calc R . .
C3 C -0.9390(3) -0.2728(3) 0.59393(15) 0.0319(6) Uani 1 1 d . . .
H3 H -1.0029 -0.2268 0.6271 0.038 Uiso 1 1 calc R . .
C4 C -0.9427(3) -0.3991(3) 0.58951(17) 0.0347(6) Uani 1 1 d . . .
C5 C -0.8511(3) -0.4648(3) 0.53962(19) 0.0383(7) Uani 1 1 d . . .
H5 H -0.8575 -0.5495 0.5352 0.046 Uiso 1 1 calc R . .
C6 C -0.7505(3) -0.4078(3) 0.49623(17) 0.0314(6) Uani 1 1 d . . .
H6 H -0.6867 -0.4543 0.4632 0.038 Uiso 1 1 calc R . .
C7 C -1.1261(3) -0.4061(4) 0.6861(2) 0.0550(9) Uani 1 1 d . . .
H7A H -1.1937 -0.3180 0.6561 0.082 Uiso 1 1 calc R . .
H7B H -1.0672 -0.3908 0.7244 0.082 Uiso 1 1 calc R . .
H7C H -1.1808 -0.4674 0.7150 0.082 Uiso 1 1 calc R . .
C8 C -0.4292(3) -0.2613(3) 0.34296(16) 0.0357(6) Uani 1 1 d . . .
H8A H -0.3472 -0.2721 0.3774 0.054 Uiso 1 1 calc R . .
H8B H -0.4630 -0.1665 0.3084 0.054 Uiso 1 1 calc R . .
H8C H -0.3985 -0.3243 0.3098 0.054 Uiso 1 1 calc R . .
C9 C 0.6956(3) 0.7069(2) 0.11849(14) 0.0263(5) Uani 1 1 d . . .
C10 C 0.8261(4) 0.6640(3) 0.1612(3) 0.0775(14) Uani 1 1 d . . .
H10 H 0.8599 0.5728 0.1956 0.093 Uiso 1 1 calc R . .
C11 C 0.9078(5) 0.7519(4) 0.1547(3) 0.0852(16) Uani 1 1 d . . .
H11 H 0.9968 0.7210 0.1848 0.102 Uiso 1 1 calc R . .
C12 C 0.8608(3) 0.8846(3) 0.10444(16) 0.0312(6) Uani 1 1 d . . .
C13 C 0.7327(3) 0.9285(2) 0.06142(15) 0.0267(5) Uani 1 1 d . . .
H13 H 0.6997 1.0193 0.0265 0.032 Uiso 1 1 calc R . .
C14 C 0.6502(3) 0.8387(2) 0.06905(15) 0.0263(5) Uani 1 1 d . . .
H14 H 0.5608 0.8700 0.0393 0.032 Uiso 1 1 calc R . .
C15 C 0.9017(3) 1.1031(3) 0.05750(16) 0.0304(5) Uani 1 1 d . . .
H15A H 0.8789 1.1102 0.0021 0.046 Uiso 1 1 calc R . .
H15B H 0.9778 1.1454 0.0584 0.046 Uiso 1 1 calc R . .
H15C H 0.8146 1.1508 0.0809 0.046 Uiso 1 1 calc R . .
C16 C 0.5105(5) 0.4597(3) 0.2712(2) 0.0606(10) Uani 1 1 d . . .
H16A H 0.4054 0.5038 0.2666 0.091 Uiso 1 1 calc R . .
H16B H 0.5432 0.4286 0.3277 0.091 Uiso 1 1 calc R . .
H16C H 0.5345 0.3806 0.2498 0.091 Uiso 1 1 calc R . .
C17 C -0.2079(2) -0.1169(2) 0.43567(13) 0.0189(4) Uani 1 1 d . . .
H17 H -0.1997 -0.1850 0.4857 0.023 Uiso 1 1 calc R . .
C18 C -0.0880(2) -0.1254(2) 0.38903(13) 0.0204(5) Uani 1 1 d . . .
H18 H -0.0012 -0.1993 0.4057 0.025 Uiso 1 1 calc R . .
C19 C -0.0973(2) -0.0230(2) 0.31709(13) 0.0186(4) Uani 1 1 d . A .
C20 C -0.2299(2) 0.0784(2) 0.29318(13) 0.0210(5) Uani 1 1 d . . .
H20 H -0.2406 0.1483 0.2437 0.025 Uiso 1 1 calc R . .
C21 C -0.3460(2) 0.0758(2) 0.34257(13) 0.0187(4) Uani 1 1 d . . .
H21 H -0.4370 0.1432 0.3250 0.022 Uiso 1 1 calc R . .
C22 C 0.0334(2) -0.0204(2) 0.27074(13) 0.0199(4) Uani 1 1 d . . .
C23 C 0.1927(2) 0.0634(2) 0.20009(13) 0.0212(5) Uani 1 1 d U . .
C24 C 0.2602(2) 0.1685(2) 0.15711(13) 0.0214(5) Uani 1 1 d . A .
C25 C 0.4101(3) 0.1321(2) 0.14940(14) 0.0245(5) Uani 1 1 d . . .
H25 H 0.4692 0.0402 0.1721 0.029 Uiso 1 1 calc R A .
C26 C 0.4712(3) 0.2325(2) 0.10809(14) 0.0255(5) Uani 1 1 d . A .
H26 H 0.5733 0.2070 0.1033 0.031 Uiso 1 1 calc R . .
C27 C 0.2503(3) 0.3984(2) 0.08359(14) 0.0250(5) Uani 1 1 d . A .
H27 H 0.1941 0.4916 0.0613 0.030 Uiso 1 1 calc R . .
C28 C 0.1799(3) 0.3050(2) 0.12406(14) 0.0245(5) Uani 1 1 d . . .
H28 H 0.0779 0.3341 0.1291 0.029 Uiso 1 1 calc R A .
N1 N -0.33548(19) -0.01810(18) 0.41441(10) 0.0169(4) Uani 1 1 d . . .
N3 N 0.0602(2) 0.0965(2) 0.23108(11) 0.0203(4) Uani 1 1 d . A .
N4 N 0.3935(2) 0.36380(19) 0.07449(11) 0.0209(4) Uani 1 1 d . . .
O1 O -0.54656(18) -0.29273(17) 0.39250(10) 0.0271(4) Uani 1 1 d . . .
O2 O -1.0342(2) -0.4673(2) 0.63195(14) 0.0499(6) Uani 1 1 d . . .
O3 O 0.5812(2) 0.55603(18) 0.22688(10) 0.0374(5) Uani 1 1 d . . .
O4 O 0.9503(2) 0.96267(19) 0.10264(12) 0.0389(5) Uani 1 1 d . . .
P1 P -0.60416(6) -0.20929(6) 0.45658(3) 0.01942(13) Uani 1 1 d . . .
P2 P 0.59272(7) 0.58807(6) 0.13221(3) 0.02280(14) Uani 1 1 d . A .
S1 S -0.67809(6) -0.00680(6) 0.40520(3) 0.02015(13) Uani 1 1 d . . .
S2 S -0.44867(6) -0.24991(5) 0.53924(3) 0.01822(12) Uani 1 1 d . . .
S3 S 0.70253(6) 0.41822(6) 0.10203(3) 0.02403(13) Uani 1 1 d . . .
S4 S 0.39884(6) 0.67068(6) 0.07535(4) 0.02580(14) Uani 1 1 d . . .
N2A N 0.2706(14) -0.0689(9) 0.2110(8) 0.027(2) Uani 0.601(4) 1 d P A 1
S5A S 0.1724(3) -0.1609(4) 0.2676(2) 0.0228(5) Uani 0.601(4) 1 d P A 1
N2B N 0.1293(10) -0.1436(17) 0.2684(11) 0.017(3) Uani 0.399(4) 1 d PU A 2
S5B S 0.2651(6) -0.1068(5) 0.2175(4) 0.0229(7) Uani 0.399(4) 1 d PU A 2
Ni1 Ni -0.5000 0.0000 0.5000 0.01471(10) Uani 1 2 d S . .
Ni2 Ni 0.5000 0.5000 0.0000 0.01912(10) Uani 1 2 d S . .


_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
C1 C6 1.398(3) . ?
C1 C2 1.398(3) . ?
C1 P1 1.795(2) . ?
C2 C3 1.381(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 O2 1.373(3) . ?
C4 C5 1.390(4) . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 O2 1.424(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 O1 1.458(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C14 1.370(3) . ?
C9 C10 1.384(4) . ?
C9 P2 1.800(2) . ?
C10 C11 1.382(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.366(3) . ?
C12 O4 1.370(3) . ?
C13 C14 1.401(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 O4 1.419(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 O3 1.431(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N1 1.343(3) . ?
C17 C18 1.381(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.392(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.394(3) . ?
C19 C22 1.473(3) . ?
C20 C21 1.386(3) . ?
C20 H20 0.9500 . ?
C21 N1 1.346(3) . ?
C21 H21 0.9500 . ?
C22 N3 1.337(3) . ?
C22 N2B 1.369(14) . ?
C22 S5A 1.695(4) . ?
C23 N2A 1.344(11) . ?
C23 N3 1.354(3) . ?
C23 C24 1.471(3) . ?
C23 S5B 1.675(5) . ?
C24 C28 1.389(3) . ?
C24 C25 1.396(3) . ?
C25 C26 1.385(3) . ?
C25 H25 0.9500 . ?
C26 N4 1.341(3) . ?
C26 H26 0.9500 . ?
C27 N4 1.338(3) . ?
C27 C28 1.387(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
N1 Ni1 2.1344(17) . ?
N4 Ni2 2.1370(18) . ?
O1 P1 1.6008(16) . ?
O3 P2 1.5937(17) . ?
P1 S1 1.9964(8) . ?
P1 S2 2.0020(8) . ?
P2 S4 1.9929(9) . ?
P2 S3 2.0021(8) . ?
S1 Ni1 2.4840(5) . ?
S2 Ni1 2.4489(5) . ?
S3 Ni2 2.4912(6) . ?
S4 Ni2 2.4833(6) . ?
N2A S5A 1.664(10) . ?
N2B S5B 1.637(14) . ?
Ni1 N1 2.1344(17) 2_456 ?
Ni1 S2 2.4489(5) 2_456 ?
Ni1 S1 2.4840(5) 2_456 ?
Ni2 N4 2.1370(18) 2_665 ?
Ni2 S4 2.4833(6) 2_665 ?
Ni2 S3 2.4912(6) 2_665 ?

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
C6 C1 C2 118.7(2) . . ?
C6 C1 P1 122.75(19) . . ?
C2 C1 P1 118.26(17) . . ?
C3 C2 C1 121.6(2) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 118.9(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
O2 C4 C3 123.9(3) . . ?
O2 C4 C5 115.7(2) . . ?
C3 C4 C5 120.4(2) . . ?
C6 C5 C4 120.6(2) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C1 119.6(2) . . ?
C5 C6 H6 120.2 . . ?
C1 C6 H6 120.2 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 C8 H8A 109.5 . . ?
O1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C14 C9 C10 118.1(2) . . ?
C14 C9 P2 123.45(19) . . ?
C10 C9 P2 118.4(2) . . ?
C11 C10 C9 121.0(3) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 O4 125.1(2) . . ?
C13 C12 C11 119.6(2) . . ?
O4 C12 C11 115.3(2) . . ?
C12 C13 C14 119.6(2) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C9 C14 C13 121.4(2) . . ?
C9 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
O4 C15 H15A 109.5 . . ?
O4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C17 C18 123.8(2) . . ?
N1 C17 H17 118.1 . . ?
C18 C17 H17 118.1 . . ?
C17 C18 C19 118.5(2) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C18 C19 C20 118.35(19) . . ?
C18 C19 C22 119.7(2) . . ?
C20 C19 C22 121.9(2) . . ?
C21 C20 C19 119.0(2) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
N1 C21 C20 122.9(2) . . ?
N1 C21 H21 118.6 . . ?
C20 C21 H21 118.6 . . ?
N3 C22 N2B 119.6(7) . . ?
N3 C22 C19 122.6(2) . . ?
N2B C22 C19 117.8(7) . . ?
N3 C22 S5A 112.14(19) . . ?
N2B C22 S5A 9.0(7) . . ?
C19 C22 S5A 125.0(2) . . ?
N2A C23 N3 120.5(5) . . ?
N2A C23 C24 117.4(5) . . ?
N3 C23 C24 122.1(2) . . ?
N2A C23 S5B 9.0(6) . . ?
N3 C23 S5B 111.8(2) . . ?
C24 C23 S5B 126.1(2) . . ?
C28 C24 C25 117.9(2) . . ?
C28 C24 C23 122.2(2) . . ?
C25 C24 C23 119.8(2) . . ?
C26 C25 C24 118.9(2) . . ?
C26 C25 H25 120.6 . . ?
C24 C25 H25 120.6 . . ?
N4 C26 C25 123.4(2) . . ?
N4 C26 H26 118.3 . . ?
C25 C26 H26 118.3 . . ?
N4 C27 C28 123.2(2) . . ?
N4 C27 H27 118.4 . . ?
C28 C27 H27 118.4 . . ?
C27 C28 C24 119.2(2) . . ?
C27 C28 H28 120.4 . . ?
C24 C28 H28 120.4 . . ?
C17 N1 C21 117.23(18) . . ?
C17 N1 Ni1 119.39(14) . . ?
C21 N1 Ni1 122.84(14) . . ?
C22 N3 C23 107.88(19) . . ?
C27 N4 C26 117.41(19) . . ?
C27 N4 Ni2 123.56(16) . . ?
C26 N4 Ni2 118.71(15) . . ?
C8 O1 P1 117.47(15) . . ?
C4 O2 C7 117.5(2) . . ?
C16 O3 P2 121.36(19) . . ?
C12 O4 C15 117.8(2) . . ?
O1 P1 C1 101.21(10) . . ?
O1 P1 S1 112.20(7) . . ?
C1 P1 S1 113.10(8) . . ?
O1 P1 S2 110.97(7) . . ?
C1 P1 S2 109.76(8) . . ?
S1 P1 S2 109.39(3) . . ?
O3 P2 C9 97.54(10) . . ?
O3 P2 S4 112.16(9) . . ?
C9 P2 S4 113.62(9) . . ?
O3 P2 S3 110.93(8) . . ?
C9 P2 S3 112.11(9) . . ?
S4 P2 S3 110.00(4) . . ?
P1 S1 Ni1 83.48(2) . . ?
P1 S2 Ni1 84.29(2) . . ?
P2 S3 Ni2 83.03(3) . . ?
P2 S4 Ni2 83.42(3) . . ?
C23 N2A S5A 105.9(8) . . ?
N2A S5A C22 93.6(5) . . ?
C22 N2B S5B 106.0(11) . . ?
N2B S5B C23 94.5(6) . . ?
N1 Ni1 N1 180.00(7) 2_456 . ?
N1 Ni1 S2 89.12(5) 2_456 2_456 ?
N1 Ni1 S2 90.88(5) . 2_456 ?
N1 Ni1 S2 90.88(5) 2_456 . ?
N1 Ni1 S2 89.12(5) . . ?
S2 Ni1 S2 180.0 2_456 . ?
N1 Ni1 S1 89.07(5) 2_456 . ?
N1 Ni1 S1 90.93(5) . . ?
S2 Ni1 S1 97.171(18) 2_456 . ?
S2 Ni1 S1 82.829(18) . . ?
N1 Ni1 S1 90.93(5) 2_456 2_456 ?
N1 Ni1 S1 89.07(5) . 2_456 ?
S2 Ni1 S1 82.829(18) 2_456 2_456 ?
S2 Ni1 S1 97.171(18) . 2_456 ?
S1 Ni1 S1 180.000(18) . 2_456 ?
N4 Ni2 N4 180.00(9) 2_665 . ?
N4 Ni2 S4 90.70(5) 2_665 2_665 ?
N4 Ni2 S4 89.30(5) . 2_665 ?
N4 Ni2 S4 89.30(5) 2_665 . ?
N4 Ni2 S4 90.70(5) . . ?
S4 Ni2 S4 180.00(2) 2_665 . ?
N4 Ni2 S3 89.08(5) 2_665 . ?
N4 Ni2 S3 90.92(5) . . ?
S4 Ni2 S3 97.73(2) 2_665 . ?
S4 Ni2 S3 82.27(2) . . ?
N4 Ni2 S3 90.92(5) 2_665 2_665 ?
N4 Ni2 S3 89.08(5) . 2_665 ?
S4 Ni2 S3 82.27(2) 2_665 2_665 ?
S4 Ni2 S3 97.73(2) . 2_665 ?
S3 Ni2 S3 180.0 . 2_665 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.073
####################################################################### 
# 
# 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_RD0729
_database_code_depnum_ccdc_archive 'CCDC 1474149'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H28 N4 Ni P2 S5, 2(C7 H8)'
_chemical_formula_sum            'C50 H44 N4 Ni P2 S5'
_chemical_formula_weight         981.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   26.52841(17)
_cell_length_b                   25.85346(16)
_cell_length_c                   7.00906(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4807.17(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    35895
_cell_measurement_theta_min      1.6660
_cell_measurement_theta_max      71.2169

_exptl_crystal_description       'blocky needles'
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2040
_exptl_absorpt_coefficient_mu    3.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.59066
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) 
(compiled May  8 2007,13:10:02) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 8.2556
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            65823
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0130
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.33
_diffrn_reflns_theta_max         71.38
_reflns_number_total             4757
_reflns_number_gt                4485
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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)+(0.0661P)²+25.4336P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4757
_refine_ls_number_parameters     302
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0861
_refine_ls_wR_factor_ref         0.2246
_refine_ls_wR_factor_gt          0.2236
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_restrained_S_all      1.207
_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
Ni Ni 0.66250(4) 0.2500 0.76419(17) 0.0291(3) Uani 1 2 d S . .
P P 0.66809(5) 0.36537(5) 0.7784(2) 0.0385(4) Uani 1 1 d . . .
S1 S 0.62930(5) 0.32160(5) 0.96355(19) 0.0367(3) Uani 1 1 d . . .
S2 S 0.69540(5) 0.32268(6) 0.5647(2) 0.0403(3) Uani 1 1 d . . .
N1 N 0.7313(2) 0.2500 0.9206(8) 0.0325(13) Uani 1 2 d S . .
C2 C 0.7769(3) 0.2500 0.8376(11) 0.0354(16) Uani 1 2 d S . .
H2A H 0.7786 0.2500 0.7022 0.042 Uiso 1 2 calc SR . .
C3 C 0.8218(3) 0.2500 0.9402(10) 0.0357(16) Uani 1 2 d SD A .
C4 C 0.8186(3) 0.2500 1.1375(11) 0.047(2) Uani 1 2 d S . .
H4A H 0.8484 0.2500 1.2125 0.057 Uiso 1 2 calc SR . .
C5 C 0.7725(3) 0.2500 1.2239(12) 0.054(2) Uani 1 2 d S . .
H5A H 0.7698 0.2500 1.3591 0.065 Uiso 1 2 calc SR . .
C6 C 0.7301(3) 0.2500 1.1119(11) 0.0425(19) Uani 1 2 d S . .
H6A H 0.6982 0.2500 1.1732 0.051 Uiso 1 2 calc SR . .
C7 C 0.8712(2) 0.2500 0.8463(9) 0.0355(16) Uani 1 2 d SD . .
N8 N 0.8775(7) 0.2500 0.657(3) 0.055(6) Uiso 0.615(10) 2 d SPDU A 1
S9 S 0.93728(15) 0.2500 0.6069(7) 0.0436(13) Uani 0.615(10) 2 d SPDU A 1
N8' N 0.9455(8) 0.2500 0.653(3) 0.046(9) Uiso 0.385(10) 2 d SPDU A 2
S9' S 0.8850(3) 0.2500 0.6143(10) 0.048(2) Uani 0.385(10) 2 d SPDU A 2
C10 C 0.9533(2) 0.2500 0.8418(9) 0.0311(15) Uani 1 2 d SD . .
N11 N 0.9130(2) 0.2500 0.9524(8) 0.0340(14) Uani 1 2 d SD A .
C12 C 1.0044(2) 0.2500 0.9249(10) 0.0320(15) Uani 1 2 d SD A .
C13 C 1.0482(2) 0.2500 0.8189(11) 0.0324(15) Uani 1 2 d S . .
H13A H 1.0455 0.2500 0.6837 0.039 Uiso 1 2 calc SR A .
N14 N 1.0943(2) 0.2500 0.8967(9) 0.0332(13) Uani 1 2 d S . .
C15 C 1.0976(3) 0.2500 1.0885(11) 0.043(2) Uani 1 2 d S . .
H15A H 1.1299 0.2500 1.1468 0.052 Uiso 1 2 calc SR A .
C16 C 1.0550(3) 0.2500 1.2029(12) 0.049(2) Uani 1 2 d S A .
H16A H 1.0583 0.2500 1.3378 0.058 Uiso 1 2 calc SR . .
C17 C 1.0081(3) 0.2500 1.1212(11) 0.0411(18) Uani 1 2 d S . .
H17A H 0.9786 0.2500 1.1984 0.049 Uiso 1 2 calc SR A .
C18 C 0.6277(2) 0.4173(2) 0.6912(12) 0.0552(17) Uani 1 1 d . . .
C19 C 0.6129(3) 0.4195(4) 0.4995(14) 0.079(3) Uani 1 1 d . . .
H19A H 0.6237 0.3942 0.4098 0.095 Uiso 1 1 calc R . .
C20 C 0.5815(4) 0.4606(5) 0.446(2) 0.113(4) Uani 1 1 d . . .
H20A H 0.5711 0.4636 0.3170 0.136 Uiso 1 1 calc R . .
C21 C 0.5652(4) 0.4968(5) 0.577(2) 0.118(5) Uani 1 1 d . . .
H21A H 0.5440 0.5244 0.5374 0.142 Uiso 1 1 calc R . .
C22 C 0.5791(4) 0.4934(3) 0.758(2) 0.108(4) Uani 1 1 d . . .
H22A H 0.5669 0.5180 0.8468 0.130 Uiso 1 1 calc R . .
C23 C 0.6115(3) 0.4543(3) 0.8205(15) 0.076(2) Uani 1 1 d . . .
H23A H 0.6222 0.4530 0.9498 0.091 Uiso 1 1 calc R . .
C24 C 0.7186(2) 0.3995(2) 0.8993(10) 0.0517(15) Uani 1 1 d . . .
C25 C 0.7471(4) 0.4339(4) 0.7974(15) 0.094(3) Uani 1 1 d . . .
H25A H 0.7399 0.4405 0.6669 0.112 Uiso 1 1 calc R . .
C26 C 0.7873(4) 0.4592(5) 0.889(2) 0.120(4) Uani 1 1 d . . .
H26A H 0.8080 0.4822 0.8180 0.143 Uiso 1 1 calc R . .
C27 C 0.7968(4) 0.4514(5) 1.0734(19) 0.111(4) Uani 1 1 d . . .
H27A H 0.8237 0.4697 1.1327 0.133 Uiso 1 1 calc R . .
C28 C 0.7684(4) 0.4174(5) 1.1794(16) 0.109(4) Uani 1 1 d . . .
H28A H 0.7756 0.4116 1.3105 0.131 Uiso 1 1 calc R . .
C29 C 0.7284(3) 0.3913(3) 1.0893(12) 0.072(2) Uani 1 1 d . . .
H29A H 0.7080 0.3679 1.1601 0.087 Uiso 1 1 calc R . .
C30 C 0.4660(15) 0.610(2) 1.258(7) 0.22(2) Uiso 0.227(4) 1 d PDU B 1
H30A H 0.4394 0.5915 1.1904 0.331 Uiso 0.227(4) 1 d PR B 1
H30B H 0.4537 0.6448 1.2935 0.331 Uiso 0.227(4) 1 d PR B 1
H30C H 0.4753 0.5912 1.3737 0.331 Uiso 0.227(4) 1 d PR B 1
C31 C 0.5102(9) 0.6157(13) 1.130(5) 0.074(10) Uiso 0.227(4) 1 d PGD B 1
C32 C 0.5585(12) 0.6117(12) 1.205(3) 0.14(2) Uiso 0.227(4) 1 d PGD B 1
H32A H 0.5632 0.6045 1.3370 0.162 Uiso 0.227(4) 1 calc PR B 1
C33 C 0.6002(8) 0.6184(11) 1.087(4) 0.046(7) Uiso 0.227(4) 1 d PG B 1
H33A H 0.6332 0.6157 1.1385 0.056 Uiso 0.227(4) 1 calc PR B 1
C34 C 0.5934(8) 0.6289(11) 0.895(4) 0.063(9) Uiso 0.227(4) 1 d PG B 1
H34A H 0.6219 0.6335 0.8140 0.075 Uiso 0.227(4) 1 calc PR B 1
C35 C 0.5451(11) 0.6329(12) 0.820(3) 0.064(8) Uiso 0.227(4) 1 d PG B 1
H35A H 0.5405 0.6401 0.6880 0.077 Uiso 0.227(4) 1 calc PR B 1
C36 C 0.5034(7) 0.6262(13) 0.938(5) 0.086(16) Uiso 0.227(4) 1 d PGD B 1
H36A H 0.4704 0.6289 0.8864 0.103 Uiso 0.227(4) 1 calc PR B 1
C30' C 0.6626(7) 0.6263(17) 1.004(5) 0.213(18) Uiso 0.392(15) 1 d PDU C 2
H30D H 0.6727 0.6250 0.8692 0.319 Uiso 0.392(15) 1 d PR C 2
H30E H 0.6777 0.5972 1.0722 0.319 Uiso 0.392(15) 1 d PR C 2
H30F H 0.6741 0.6589 1.0603 0.319 Uiso 0.392(15) 1 d PR C 2
C31' C 0.6072(5) 0.6229(8) 1.021(3) 0.105(13) Uiso 0.392(15) 1 d PGD C 2
C32' C 0.5769(8) 0.6306(8) 0.861(2) 0.081(7) Uiso 0.392(15) 1 d PGD C 2
H32B H 0.5919 0.6373 0.7408 0.097 Uiso 0.392(15) 1 calc PR C 2
C33' C 0.5248(8) 0.6285(9) 0.879(3) 0.097(8) Uiso 0.392(15) 1 d PG C 2
H33B H 0.5041 0.6337 0.7697 0.116 Uiso 0.392(15) 1 calc PR C 2
C34' C 0.5029(5) 0.6186(9) 1.055(4) 0.082(8) Uiso 0.392(15) 1 d PG C 2
H34B H 0.4672 0.6172 1.0668 0.099 Uiso 0.392(15) 1 calc PR C 2
C35' C 0.5332(8) 0.6109(9) 1.214(3) 0.128(12) Uiso 0.392(15) 1 d PG C 2
H35B H 0.5182 0.6042 1.3351 0.154 Uiso 0.392(15) 1 calc PR C 2
C36' C 0.5853(7) 0.6130(8) 1.197(2) 0.079(7) Uiso 0.392(15) 1 d PGD C 2
H36B H 0.6060 0.6078 1.3062 0.095 Uiso 0.392(15) 1 calc PR C 2
C30" C 0.6403(11) 0.6173(18) 1.158(5) 0.206(17) Uiso 0.382(15) 1 d PDU D 3
H30G H 0.6287 0.6269 1.2858 0.310 Uiso 0.382(15) 1 d PR D 3
H30H H 0.6682 0.6400 1.1199 0.310 Uiso 0.382(15) 1 d PR D 3
H30I H 0.6518 0.5813 1.1584 0.310 Uiso 0.382(15) 1 d PR D 3
C31" C 0.5972(7) 0.6229(9) 1.025(3) 0.26(4) Uiso 0.382(15) 1 d PGD D 3
C32" C 0.6051(8) 0.6343(9) 0.833(3) 0.095(8) Uiso 0.382(15) 1 d PGD D 3
H32C H 0.6384 0.6397 0.7871 0.114 Uiso 0.382(15) 1 calc PR D 3
C33" C 0.5644(10) 0.6376(10) 0.709(3) 0.139(14) Uiso 0.382(15) 1 d PG D 3
H33C H 0.5698 0.6454 0.5780 0.166 Uiso 0.382(15) 1 calc PR D 3
C34" C 0.5157(9) 0.6296(12) 0.776(4) 0.177(18) Uiso 0.382(15) 1 d PG D 3
H34C H 0.4879 0.6319 0.6913 0.213 Uiso 0.382(15) 1 calc PR D 3
C35" C 0.5078(7) 0.6183(11) 0.968(5) 0.15(2) Uiso 0.382(15) 1 d PG D 3
H35C H 0.4745 0.6128 1.0137 0.182 Uiso 0.382(15) 1 calc PR D 3
C36" C 0.5485(8) 0.6149(9) 1.092(3) 0.095(8) Uiso 0.382(15) 1 d PGD D 3
H36C H 0.5431 0.6072 1.2228 0.114 Uiso 0.382(15) 1 calc PR D 3


_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
Ni N1 2.128(6) . ?
Ni N14 2.133(6) 6_557 ?
Ni S1 2.4809(15) 7_565 ?
Ni S1 2.4809(15) . ?
Ni S2 2.4994(15) . ?
Ni S2 2.4994(15) 7_565 ?
P C24 1.816(6) . ?
P C18 1.823(6) . ?
P S2 1.996(2) . ?
P S1 2.0061(19) . ?
N1 C6 1.342(10) . ?
N1 C2 1.342(9) . ?
C2 C3 1.392(10) . ?
C3 C4 1.386(11) . ?
C3 C7 1.467(9) . ?
C4 C5 1.365(11) . ?
C5 C6 1.370(11) . ?
C7 N11 1.334(9) . ?
C7 N8 1.338(19) . ?
C7 S9' 1.667(9) . ?
N8 S9 1.624(17) . ?
S9 C10 1.701(8) . ?
N8' C10 1.34(2) . ?
N8' S9' 1.628(18) . ?
C10 N11 1.320(8) . ?
C10 C12 1.475(8) . ?
C12 C17 1.380(10) . ?
C12 C13 1.380(10) . ?
C13 N14 1.338(8) . ?
N14 C15 1.347(10) . ?
N14 Ni 2.133(6) 6_657 ?
C15 C16 1.385(10) . ?
C16 C17 1.370(10) . ?
C18 C23 1.385(11) . ?
C18 C19 1.401(12) . ?
C19 C20 1.402(12) . ?
C20 C21 1.381(18) . ?
C21 C22 1.320(18) . ?
C22 C23 1.399(12) . ?
C24 C25 1.368(10) . ?
C24 C29 1.373(10) . ?
C25 C26 1.404(12) . ?
C26 C27 1.333(15) . ?
C27 C28 1.377(15) . ?
C28 C29 1.408(10) . ?
C30 C31 1.482(14) . ?
C31 C32 1.3900 . ?
C31 C36 1.3900 . ?
C32 C33 1.3900 . ?
C33 C34 1.3900 . ?
C34 C35 1.3900 . ?
C35 C36 1.3900 . ?
C30' C31' 1.476(14) . ?
C31' C32' 1.3900 . ?
C31' C36' 1.3900 . ?
C32' C33' 1.3900 . ?
C33' C34' 1.3900 . ?
C34' C35' 1.3900 . ?
C35' C36' 1.3900 . ?
C30" C31" 1.484(14) . ?
C31" C32" 1.3900 . ?
C31" C36" 1.3900 . ?
C32" C33" 1.3900 . ?
C33" C34" 1.3900 . ?
C34" C35" 1.3900 . ?
C35" C36" 1.3900 . ?

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
N1 Ni N14 179.1(2) . 6_557 ?
N1 Ni S1 90.82(11) . 7_565 ?
N14 Ni S1 89.80(11) 6_557 7_565 ?
N1 Ni S1 90.82(11) . . ?
N14 Ni S1 89.80(11) 6_557 . ?
S1 Ni S1 96.51(7) 7_565 . ?
N1 Ni S2 89.36(11) . . ?
N14 Ni S2 90.03(11) 6_557 . ?
S1 Ni S2 179.48(6) 7_565 . ?
S1 Ni S2 83.00(4) . . ?
N1 Ni S2 89.36(11) . 7_565 ?
N14 Ni S2 90.03(11) 6_557 7_565 ?
S1 Ni S2 83.00(4) 7_565 7_565 ?
S1 Ni S2 179.48(6) . 7_565 ?
S2 Ni S2 97.49(8) . 7_565 ?
C24 P C18 103.4(3) . . ?
C24 P S2 110.5(2) . . ?
C18 P S2 111.7(3) . . ?
C24 P S1 110.5(2) . . ?
C18 P S1 109.4(2) . . ?
S2 P S1 111.07(9) . . ?
P S1 Ni 82.78(6) . . ?
P S2 Ni 82.49(6) . . ?
C6 N1 C2 117.0(6) . . ?
C6 N1 Ni 119.7(5) . . ?
C2 N1 Ni 123.3(5) . . ?
N1 C2 C3 123.2(7) . . ?
C4 C3 C2 117.6(7) . . ?
C4 C3 C7 120.2(6) . . ?
C2 C3 C7 122.2(6) . . ?
C5 C4 C3 119.9(7) . . ?
C4 C5 C6 118.7(8) . . ?
N1 C6 C5 123.6(7) . . ?
N11 C7 N8 116.7(10) . . ?
N11 C7 C3 119.5(6) . . ?
N8 C7 C3 123.8(10) . . ?
N11 C7 S9' 111.2(5) . . ?
N8 C7 S9' 5.5(9) . . ?
C3 C7 S9' 129.3(6) . . ?
C7 N8 S9 109.6(13) . . ?
N8 S9 C10 92.0(7) . . ?
C10 N8' S9' 108.5(14) . . ?
N8' S9' C7 93.0(9) . . ?
N11 C10 N8' 117.0(10) . . ?
N11 C10 C12 120.8(6) . . ?
N8' C10 C12 122.1(10) . . ?
N11 C10 S9 111.5(5) . . ?
N8' C10 S9 5.6(9) . . ?
C12 C10 S9 127.7(5) . . ?
C10 N11 C7 110.2(6) . . ?
C17 C12 C13 118.5(6) . . ?
C17 C12 C10 117.3(6) . . ?
C13 C12 C10 124.2(6) . . ?
N14 C13 C12 123.4(7) . . ?
C13 N14 C15 117.8(6) . . ?
C13 N14 Ni 124.0(5) . 6_657 ?
C15 N14 Ni 118.2(4) . 6_657 ?
N14 C15 C16 121.6(7) . . ?
C17 C16 C15 120.0(7) . . ?
C16 C17 C12 118.8(7) . . ?
C23 C18 C19 120.9(7) . . ?
C23 C18 P 118.1(6) . . ?
C19 C18 P 121.0(6) . . ?
C18 C19 C20 116.9(10) . . ?
C21 C20 C19 121.6(12) . . ?
C22 C21 C20 120.3(10) . . ?
C21 C22 C23 121.5(12) . . ?
C18 C23 C22 118.9(10) . . ?
C25 C24 C29 120.2(7) . . ?
C25 C24 P 118.7(6) . . ?
C29 C24 P 121.1(5) . . ?
C24 C25 C26 118.9(10) . . ?
C27 C26 C25 121.2(10) . . ?
C26 C27 C28 121.0(9) . . ?
C27 C28 C29 118.5(10) . . ?
C24 C29 C28 120.2(8) . . ?
C32 C31 C36 120.0 . . ?
C32 C31 C30 119.7(8) . . ?
C36 C31 C30 120.3(8) . . ?
C31 C32 C33 120.0 . . ?
C32 C33 C34 120.0 . . ?
C35 C34 C33 120.0 . . ?
C34 C35 C36 120.0 . . ?
C35 C36 C31 120.0 . . ?
C32' C31' C36' 120.0 . . ?
C32' C31' C30' 120.1(8) . . ?
C36' C31' C30' 119.9(8) . . ?
C33' C32' C31' 120.0 . . ?
C32' C33' C34' 120.0 . . ?
C35' C34' C33' 120.0 . . ?
C34' C35' C36' 120.0 . . ?
C35' C36' C31' 120.0 . . ?
C32" C31" C36" 120.0 . . ?
C32" C31" C30" 120.7(8) . . ?
C36" C31" C30" 119.2(8) . . ?
C33" C32" C31" 120.0 . . ?
C32" C33" C34" 120.0 . . ?
C33" C34" C35" 120.0 . . ?
C36" C35" C34" 120.0 . . ?
C35" C36" C31" 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        71.38
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.306
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.101

#===END
####################################################################### 
# 
# 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_04slh021
_database_code_depnum_ccdc_archive 'CCDC 1474150'
_audit_update_record             
;
2016-04-14 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H20 N4 Ni O4 P2 S5'
_chemical_formula_weight         613.31

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   14.0311(13)
_cell_length_b                   14.9236(13)
_cell_length_c                   12.8460(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.786(5)
_cell_angle_gamma                90.00
_cell_volume                     2461.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5097
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6676
_exptl_absorpt_correction_T_max  0.9471
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'Φ & ω scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19049
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5601
_reflns_number_gt                4837
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0617P)²+25.6697P] 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     SHELXL
_refine_ls_extinction_coef       0.0051(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5601
_refine_ls_number_parameters     330
_refine_ls_number_restraints     154
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1964
_refine_ls_wR_factor_gt          0.1917
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          2.303
_refine_ls_shift/su_mean         0.025

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
C1 C 0.1701(7) 0.2456(5) 0.1773(6) 0.0381(18) Uani 1 1 d . . .
H1A H 0.1118 0.2210 0.1114 0.057 Uiso 1 1 calc R . .
H1B H 0.2135 0.1964 0.2223 0.057 Uiso 1 1 calc R . .
H1C H 0.2119 0.2847 0.1510 0.057 Uiso 1 1 calc R . .
C2 C 0.3564(6) 0.2719(5) 0.5357(7) 0.0412(19) Uani 1 1 d . . .
H2A H 0.3829 0.2136 0.5704 0.062 Uiso 1 1 calc R . .
H2B H 0.3380 0.3082 0.5885 0.062 Uiso 1 1 calc R . .
H2C H 0.4103 0.3028 0.5190 0.062 Uiso 1 1 calc R . .
C3 C 0.1436(6) 0.8154(5) 0.2857(6) 0.0311(15) Uani 1 1 d . . .
H3A H 0.1238 0.8750 0.2517 0.047 Uiso 1 1 calc R . .
H3B H 0.0822 0.7853 0.2876 0.047 Uiso 1 1 calc R . .
H3C H 0.1714 0.7799 0.2401 0.047 Uiso 1 1 calc R . .
C4 C 0.4073(5) 0.7346(5) 0.6801(5) 0.0316(15) Uani 1 1 d . . .
H4A H 0.4462 0.7748 0.7434 0.047 Uiso 1 1 calc R . .
H4B H 0.4561 0.7016 0.6572 0.047 Uiso 1 1 calc R . .
H4C H 0.3669 0.6921 0.7042 0.047 Uiso 1 1 calc R . .
C5 C 0.0236(5) 0.5633(4) 0.2287(5) 0.0191(11) Uani 1 1 d . A .
H5 H 0.0033 0.5501 0.2892 0.023 Uiso 1 1 calc R . .
C6 C -0.0537(4) 0.5742(4) 0.1208(5) 0.0177(11) Uani 1 1 d . . .
C7 C -0.0240(5) 0.5981(4) 0.0337(5) 0.0213(12) Uani 1 1 d . A .
H7 H -0.0749 0.6063 -0.0415 0.026 Uiso 1 1 calc R . .
C8 C 0.0804(5) 0.6098(4) 0.0580(5) 0.0213(12) Uani 1 1 d . . .
H8 H 0.1024 0.6284 0.0004 0.026 Uiso 1 1 calc R A .
C9 C 0.1525(5) 0.5940(4) 0.1677(5) 0.0197(12) Uani 1 1 d . A .
H9 H 0.2244 0.6001 0.1835 0.024 Uiso 1 1 calc R . .
C10A C -0.1625(4) 0.5594(4) 0.1020(4) 0.0180(8) Uani 0.688(7) 1 d PDU A 1
C11A C -0.2937(4) 0.5384(4) 0.1485(5) 0.0186(9) Uani 0.688(7) 1 d PDU . 1
N2A N -0.1891(12) 0.5483(13) 0.1889(8) 0.0176(13) Uani 0.688(7) 1 d PDU A 1
N3A N -0.3483(8) 0.5345(8) 0.0378(8) 0.0197(15) Uani 0.688(7) 1 d PDU A 1
S5A S -0.2660(2) 0.54901(17) -0.02445(19) 0.0197(6) Uani 0.688(7) 1 d PDU A 1
C10B C -0.2937(4) 0.5384(4) 0.1485(5) 0.0186(9) Uani 0.312(7) 1 d PDU . 2
C11B C -0.1625(4) 0.5594(4) 0.1020(4) 0.0180(8) Uani 0.312(7) 1 d PDU A 2
N2B N -0.191(2) 0.550(3) 0.1907(14) 0.0178(16) Uani 0.312(7) 1 d PDU A 2
N3B N -0.2356(12) 0.5639(16) -0.0016(13) 0.0188(17) Uani 0.312(7) 1 d PDU A 2
S5B S -0.3484(5) 0.5456(5) 0.0073(5) 0.0216(12) Uani 0.312(7) 1 d PDU A 2
C12 C 0.2894(4) 0.4971(4) 0.6627(5) 0.0171(11) Uani 1 1 d . A .
H12 H 0.2167 0.5068 0.6388 0.020 Uiso 1 1 calc R . .
C13 C 0.3467(4) 0.4722(4) 0.7750(5) 0.0189(11) Uani 1 1 d . . .
C14 C 0.4532(5) 0.4567(5) 0.8099(6) 0.0271(14) Uani 1 1 d . . .
C15 C 0.4965(5) 0.4685(5) 0.7311(6) 0.0266(14) Uani 1 1 d . . .
C16 C 0.4340(5) 0.4948(4) 0.6217(5) 0.0219(12) Uani 1 1 d . A .
N1 N 0.1252(4) 0.5705(3) 0.2526(4) 0.0179(10) Uani 1 1 d . . .
N4 N 0.3310(4) 0.5082(3) 0.5857(4) 0.0179(10) Uani 1 1 d . . .
O1 O 0.1304(4) 0.2963(3) 0.2464(4) 0.0287(10) Uani 1 1 d . . .
O2 O 0.2654(4) 0.2590(3) 0.4316(4) 0.0295(10) Uani 1 1 d . . .
O3 O 0.2221(4) 0.8242(3) 0.4003(4) 0.0235(9) Uani 1 1 d . . .
O4 O 0.3377(4) 0.7865(3) 0.5853(4) 0.0255(9) Uani 1 1 d . . .
P1 P 0.20794(13) 0.34404(10) 0.35952(14) 0.0219(3) Uani 1 1 d . A .
P2 P 0.26650(12) 0.73593(10) 0.47290(13) 0.0190(3) Uani 1 1 d . A .
S1 S 0.12323(12) 0.40826(10) 0.42612(12) 0.0211(3) Uani 1 1 d . . .
S2 S 0.30967(12) 0.42463(10) 0.33551(13) 0.0221(3) Uani 1 1 d . . .
S3 S 0.15626(12) 0.66268(10) 0.49039(12) 0.0202(3) Uani 1 1 d . . .
S4 S 0.35002(11) 0.66105(10) 0.41285(12) 0.0189(3) Uani 1 1 d . . .
Ni1 Ni 0.23266(5) 0.54002(5) 0.41724(6) 0.0153(2) Uani 1 1 d . A .
H14 H 0.494(7) 0.438(6) 0.886(7) 0.04(2) Uiso 1 1 d . . .
H15 H 0.563(7) 0.459(5) 0.741(7) 0.04(2) Uiso 1 1 d . . .
H16 H 0.459(6) 0.500(5) 0.561(6) 0.027(19) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.439(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O2 1.442(8) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 O3 1.445(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 O4 1.441(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N1 1.337(8) . ?
C5 C6 1.382(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(8) . ?
C6 C10A 1.463(8) . ?
C7 C8 1.381(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.384(8) . ?
C8 H8 0.9500 . ?
C9 N1 1.340(7) . ?
C9 H9 0.9500 . ?
C10A N2A 1.323(17) . ?
C10A S5A 1.693(6) . ?
C11A N3A 1.317(11) . ?
C11A N2A 1.352(18) . ?
C11A C13 1.461(8) 3_566 ?
N3A S5A 1.663(10) . ?
N3B S5B 1.655(15) . ?
C12 N4 1.346(7) . ?
C12 C13 1.390(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(9) . ?
C13 C10B 1.461(8) 3_566 ?
C13 C11A 1.461(8) 3_566 ?
C14 C15 1.386(9) . ?
C14 H14 0.95(9) . ?
C15 C16 1.380(9) . ?
C15 H15 0.90(9) . ?
C16 N4 1.342(8) . ?
C16 H16 0.97(7) . ?
N1 Ni1 2.093(5) . ?
N4 Ni1 2.099(5) . ?
O1 P1 1.590(5) . ?
O2 P1 1.587(5) . ?
O3 P2 1.589(4) . ?
O4 P2 1.578(4) . ?
P1 S1 1.971(2) . ?
P1 S2 1.983(2) . ?
P2 S3 1.980(2) . ?
P2 S4 1.987(2) . ?
S1 Ni1 2.5255(16) . ?
S2 Ni1 2.4800(16) . ?
S3 Ni1 2.4891(16) . ?
S4 Ni1 2.4602(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N1 C5 C6 123.6(5) . . ?
N1 C5 H5 118.2 . . ?
C6 C5 H5 118.2 . . ?
C5 C6 C7 118.0(5) . . ?
C5 C6 C10A 119.5(5) . . ?
C7 C6 C10A 122.5(5) . . ?
C8 C7 C6 119.1(6) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C7 C8 C9 118.8(5) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
N1 C9 C8 122.8(5) . . ?
N1 C9 H9 118.6 . . ?
C8 C9 H9 118.6 . . ?
N2A C10A C6 120.7(7) . . ?
N2A C10A S5A 111.9(7) . . ?
C6 C10A S5A 127.4(4) . . ?
N3A C11A N2A 119.2(8) . . ?
N3A C11A C13 119.3(7) . 3_566 ?
N2A C11A C13 121.4(7) . 3_566 ?
C10A N2A C11A 108.7(6) . . ?
C11A N3A S5A 107.4(7) . . ?
N3A S5A C10A 92.5(4) . . ?
N4 C12 C13 123.7(5) . . ?
N4 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C12 C13 C14 118.3(5) . . ?
C12 C13 C10B 119.3(5) . 3_566 ?
C14 C13 C10B 122.4(5) . 3_566 ?
C12 C13 C11A 119.3(5) . 3_566 ?
C14 C13 C11A 122.4(5) . 3_566 ?
C10B C13 C11A 0.0(5) 3_566 3_566 ?
C15 C14 C13 118.2(6) . . ?
C15 C14 H14 122(5) . . ?
C13 C14 H14 120(5) . . ?
C16 C15 C14 119.6(6) . . ?
C16 C15 H15 113(5) . . ?
C14 C15 H15 127(5) . . ?
N4 C16 C15 123.1(5) . . ?
N4 C16 H16 113(4) . . ?
C15 C16 H16 123(4) . . ?
C5 N1 C9 117.6(5) . . ?
C5 N1 Ni1 118.8(4) . . ?
C9 N1 Ni1 123.6(4) . . ?
C16 N4 C12 117.0(5) . . ?
C16 N4 Ni1 123.9(4) . . ?
C12 N4 Ni1 119.0(4) . . ?
C1 O1 P1 120.5(5) . . ?
C2 O2 P1 119.0(4) . . ?
C3 O3 P2 118.7(4) . . ?
C4 O4 P2 118.7(4) . . ?
O2 P1 O1 100.0(3) . . ?
O2 P1 S1 112.9(2) . . ?
O1 P1 S1 107.7(2) . . ?
O2 P1 S2 110.4(2) . . ?
O1 P1 S2 113.57(19) . . ?
S1 P1 S2 111.74(10) . . ?
O4 P2 O3 95.4(2) . . ?
O4 P2 S3 113.30(19) . . ?
O3 P2 S3 112.65(19) . . ?
O4 P2 S4 111.69(19) . . ?
O3 P2 S4 113.04(18) . . ?
S3 P2 S4 110.11(9) . . ?
P1 S1 Ni1 82.81(7) . . ?
P1 S2 Ni1 83.77(7) . . ?
P2 S3 Ni1 83.57(7) . . ?
P2 S4 Ni1 84.20(7) . . ?
N1 Ni1 N4 175.76(18) . . ?
N1 Ni1 S4 91.92(14) . . ?
N4 Ni1 S4 91.25(14) . . ?
N1 Ni1 S2 88.98(14) . . ?
N4 Ni1 S2 93.54(14) . . ?
S4 Ni1 S2 95.17(5) . . ?
N1 Ni1 S3 88.71(14) . . ?
N4 Ni1 S3 88.93(14) . . ?
S4 Ni1 S3 82.12(5) . . ?
S2 Ni1 S3 176.38(6) . . ?
N1 Ni1 S1 90.65(14) . . ?
N4 Ni1 S1 86.35(14) . . ?
S4 Ni1 S1 175.89(6) . . ?
S2 Ni1 S1 81.67(5) . . ?
S3 Ni1 S1 101.15(5) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.849
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.146
